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发表于 2025-4-7 12:09:41
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#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_pfc-72-co
_audit_block_doi 10.5517/ccdc.csd.cc28r9x8
_database_code_depnum_ccdc_archive 'CCDC 2107780'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1002/anie.202115854 2022
2 10.1038/s41467-022-30523-0 2022
loop_
_audit_author_name
_audit_author_address
'Qi Yin'
;Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences
China
;
_audit_update_record
;
2021-09-06 deposited with the CCDC. 2025-04-07 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT420_pfc-72-co
;
PROBLEM: D-H Bond Without Acceptor O3 --H3 . Please Check
RESPONSE: Because of the disorder, we can not find the acceptor.
;
_vrf_PLAT973_pfc-72-co
;
PROBLEM: Check Calcd Positive Resid. Density on Co1 1.77 eA-3
RESPONSE: We have used two different refienement programs (Shelxl and olex2.refine) to check this alert. All programs show much smaller residual density on the Co atom. Therefore, we assume that there s in the checkcif calculation.
;
# Added during the CSD deposition process: ??? 06 ?? 2021 03:47 ??
# end Validation Reply Form
_audit_creation_date 2021-09-06
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_shelx_SHELXL_version_number 2018/3
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C48 H28 Co N4 O8'
_chemical_formula_sum 'C48 H28 Co N4 O8'
_chemical_formula_weight 847.67
_chemical_melting_point ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system monoclinic
_space_group_IT_number 13
_space_group_name_H-M_alt 'P 1 2/c 1'
_space_group_name_Hall '-P 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
_cell_length_a 18.033(2)
_cell_length_b 22.096(2)
_cell_length_c 9.1973(10)
_cell_angle_alpha 90
_cell_angle_beta 104.289(7)
_cell_angle_gamma 90
_cell_volume 3551.3(7)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 25484
_cell_measurement_temperature 180.04
_cell_measurement_theta_max 26.367
_cell_measurement_theta_min 2.181
_shelx_estimated_absorpt_T_max 0.973
_shelx_estimated_absorpt_T_min 0.947
_exptl_absorpt_coefficient_mu 0.277
_exptl_absorpt_correction_T_max 0.973
_exptl_absorpt_correction_T_min 0.967
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details ?
_exptl_absorpt_special_details ?
_exptl_crystal_colour 'dull dark brown'
_exptl_crystal_colour_lustre dull
_exptl_crystal_colour_modifier dark
_exptl_crystal_colour_primary brown
_exptl_crystal_density_diffrn 0.793
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description prism
_exptl_crystal_F_000 870
_exptl_crystal_size_max 0.2
_exptl_crystal_size_mid 0.1
_exptl_crystal_size_min 0.1
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0962
_diffrn_reflns_av_unetI/netI 0.0940
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max 22
_diffrn_reflns_limit_h_min -22
_diffrn_reflns_limit_k_max 27
_diffrn_reflns_limit_k_min -27
_diffrn_reflns_limit_l_max 11
_diffrn_reflns_limit_l_min -11
_diffrn_reflns_number 25484
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 26.367
_diffrn_reflns_theta_min 2.181
_diffrn_ambient_temperature 180.04
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type 'Bruker APEX-II CCD'
_diffrn_measurement_method ?
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source ?
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 3781
_reflns_number_total 7248
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
Structure factors included contributions from the .fab file.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement ?
_computing_data_collection ?
_computing_data_reduction ?
_computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max 1.281
_refine_diff_density_min -0.680
_refine_diff_density_rms 0.101
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.128
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 260
_refine_ls_number_reflns 7248
_refine_ls_number_restraints 591
_refine_ls_R_factor_all 0.1643
_refine_ls_R_factor_gt 0.1066
_refine_ls_restrained_S_all 1.178
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.2976
_refine_ls_wR_factor_ref 0.3512
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.5 times of:
All O(H) groups, H1 of C28
At 1.2 times of:
H27 of C27, H22 of C22, H19 of C19, H24 of C24, H25 of C25, H10 of C10, H16
of C16, H12 of C12, H17 of C17, H11 of C11, H5 of C5, H8 of C8
2. Restrained distances
C28-C20
1.54 with sigma of 0.02
O3-C28
1.27 with sigma of 0.02
O1-C28
1.27 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17
\\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25
\\sim C26 \\sim C27 \\sim C28: within 3.8A with sigma of 0.02 and sigma for
terminal atoms of 0.04 within 3.8A
Uanis(O1) = Uanis(C28) = Uanis(O3)
Uanis(O4) = Uanis(C26)
Uanis(O2) = Uanis(C23)
4. Others
Fixed Sof: H3(0.5) H1(0.5)
5.a Everything fixed:
H3, H4, H1
5.b Aromatic/amide H refined with riding coordinates:
C5(H5), C8(H8), C10(H10), C11(H11), C12(H12), C16(H16), C17(H17), C19(H19),
C22(H22), C24(H24), C25(H25), C27(H27)
;
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary dual
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.500000 0.56591(4) 0.750000 0.0401(4) Uani 1 2 d S T P . .
N1 N 0.5593(2) 0.50392(16) 0.6797(4) 0.0322(9) Uani 1 1 d . . . . .
C1 C 0.500000 0.4123(3) 0.750000 0.0338(14) Uani 1 2 d S TU P . .
N2 N 0.5685(2) 0.62791(17) 0.7101(5) 0.0411(10) Uani 1 1 d . . . . .
C2 C 0.6607(3) 0.5656(2) 0.6213(6) 0.0399(10) Uani 1 1 d . U . . .
C3 C 0.500000 0.3446(3) 0.750000 0.0428(16) Uani 1 2 d S TU P . .
C4 C 0.7341(3) 0.5658(2) 0.5715(7) 0.0483(12) Uani 1 1 d . U . . .
C5 C 0.6338(3) 0.4574(2) 0.5419(6) 0.0388(11) Uani 1 1 d . U . . .
H5 H 0.670560 0.451994 0.484635 0.047 Uiso 1 1 calc R U . . .
C6 C 0.5432(3) 0.44279(18) 0.6674(5) 0.0338(10) Uani 1 1 d . U . . .
C7 C 0.6173(3) 0.5127(2) 0.6094(6) 0.0386(11) Uani 1 1 d . U . . .
C8 C 0.5872(3) 0.4144(2) 0.5752(6) 0.0386(11) Uani 1 1 d . U . . .
H8 H 0.584127 0.373300 0.543836 0.046 Uiso 1 1 calc R U . . .
C9 C 0.6397(3) 0.6192(2) 0.6796(7) 0.0487(13) Uani 1 1 d . U . . .
C10 C 0.6792(3) 0.6754(2) 0.6828(8) 0.0585(14) Uani 1 1 d . U . . .
H10 H 0.728440 0.681309 0.665458 0.070 Uiso 1 1 calc R U . . .
C11 C 0.7319(4) 0.5619(3) 0.4222(9) 0.0688(16) Uani 1 1 d . U . . .
H11 H 0.684442 0.558905 0.349479 0.083 Uiso 1 1 calc R U . . .
C12 C 0.6332(4) 0.7182(2) 0.7151(9) 0.0722(17) Uani 1 1 d . U . . .
H12 H 0.644363 0.760197 0.726697 0.087 Uiso 1 1 calc R U . . .
C13 C 0.500000 0.7195(3) 0.750000 0.075(2) Uani 1 2 d S TU P . .
C14 C 0.5641(4) 0.6892(2) 0.7290(9) 0.0664(17) Uani 1 1 d . U . . .
C15 C 0.500000 0.2182(4) 0.750000 0.075(2) Uani 1 2 d S TU P . .
C16 C 0.4334(5) 0.3143(3) 0.6900(10) 0.083(2) Uani 1 1 d . U . . .
H16 H 0.386671 0.335342 0.652080 0.100 Uiso 1 1 calc R U . . .
C17 C 0.8053(4) 0.5701(3) 0.6741(10) 0.0738(17) Uani 1 1 d . U . . .
H17 H 0.808292 0.571768 0.778635 0.089 Uiso 1 1 calc R U . . .
C18 C 0.500000 0.7880(4) 0.750000 0.089(3) Uani 1 2 d S TU P . .
C19 C 0.8015(4) 0.5622(3) 0.3782(10) 0.085(2) Uani 1 1 d . U . . .
H19 H 0.800423 0.558517 0.274781 0.102 Uiso 1 1 calc R U . . .
O1 O 0.9329(4) 0.5651(4) 0.2885(12) 0.160(2) Uani 1 1 d D . . . .
C20 C 0.8690(4) 0.5677(3) 0.4782(13) 0.093(2) Uani 1 1 d D U . . .
C21 C 0.500000 0.9132(5) 0.750000 0.119(3) Uani 1 2 d S TU P . .
O2 O 0.4457(4) 0.1259(2) 0.6690(11) 0.150(3) Uani 1 1 d . . . . .
C22 C 0.4366(5) 0.2514(3) 0.6866(11) 0.100(3) Uani 1 1 d . U . . .
H22 H 0.391669 0.230226 0.636797 0.120 Uiso 1 1 calc R U . . .
C23 C 0.500000 0.1527(6) 0.750000 0.150(3) Uani 1 2 d S TU P . .
C24 C 0.8710(4) 0.5717(3) 0.6243(11) 0.087(2) Uani 1 1 d . U . . .
H24 H 0.918995 0.575785 0.695060 0.104 Uiso 1 1 calc R U . . .
C25 C 0.5438(6) 0.8200(4) 0.8642(14) 0.120(3) Uani 1 1 d . U . . .
H25 H 0.576115 0.798914 0.945600 0.144 Uiso 1 1 calc R U . . .
O3 O 1.0020(4) 0.5797(4) 0.5135(11) 0.160(2) Uani 1 1 d D . . . .
H3 H 1.055630 0.577240 0.539090 0.240 Uiso 0.5 1 d . U P . .
O4 O 0.5514(5) 1.0074(3) 0.8525(13) 0.177(3) Uani 1 1 d . . . . .
H4 H 0.551330 1.050240 0.865060 0.265 Uiso 1 1 d . U . . .
C26 C 0.500000 0.9816(6) 0.750000 0.177(3) Uani 1 2 d S TU P . .
C27 C 0.5434(6) 0.8817(4) 0.8666(16) 0.140(3) Uani 1 1 d . U . . .
H27 H 0.573757 0.902658 0.950614 0.168 Uiso 1 1 calc R U . . .
C28 C 0.9413(6) 0.5668(6) 0.4229(16) 0.160(2) Uani 1 1 d D U . . .
H1 H 0.982220 0.565630 0.284110 0.240 Uiso 0.5 1 d . U P . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Co1 0.0447(6) 0.0234(5) 0.0671(7) 0.000 0.0421(5) 0.000
N1 0.035(2) 0.0298(19) 0.039(2) -0.0001(16) 0.0229(18) -0.0041(15)
C1 0.034(3) 0.029(3) 0.046(3) 0.000 0.025(3) 0.000
N2 0.048(3) 0.0271(19) 0.060(3) 0.0028(18) 0.036(2) -0.0006(17)
C2 0.042(2) 0.033(2) 0.056(3) 0.009(2) 0.031(2) 0.0018(19)
C3 0.048(4) 0.026(3) 0.067(4) 0.000 0.039(3) 0.000
C4 0.042(3) 0.040(2) 0.074(3) 0.000(2) 0.037(2) -0.001(2)
C5 0.040(2) 0.033(2) 0.053(3) -0.002(2) 0.030(2) 0.0068(19)
C6 0.040(2) 0.026(2) 0.042(3) 0.0036(18) 0.024(2) 0.0075(17)
C7 0.041(2) 0.030(2) 0.056(3) 0.007(2) 0.034(2) 0.0077(18)
C8 0.043(3) 0.037(2) 0.045(3) -0.007(2) 0.028(2) 0.011(2)
C9 0.055(3) 0.026(2) 0.078(3) 0.005(2) 0.042(3) 0.000(2)
C10 0.061(3) 0.038(3) 0.094(4) 0.005(3) 0.051(3) -0.007(2)
C11 0.057(3) 0.078(4) 0.087(4) -0.011(3) 0.047(3) -0.015(3)
C12 0.082(4) 0.029(2) 0.131(5) -0.001(3) 0.073(4) -0.007(2)
C13 0.084(5) 0.024(3) 0.147(6) 0.000 0.084(5) 0.000
C14 0.067(3) 0.031(2) 0.127(5) 0.003(3) 0.072(3) -0.006(2)
C15 0.084(6) 0.028(4) 0.128(7) 0.000 0.052(5) 0.000
C16 0.084(4) 0.040(3) 0.123(5) 0.009(3) 0.019(4) -0.005(3)
C17 0.057(3) 0.072(4) 0.097(4) 0.005(3) 0.027(3) -0.002(3)
C18 0.093(5) 0.037(4) 0.172(7) 0.000 0.097(5) 0.000
C19 0.074(4) 0.098(5) 0.102(5) -0.029(4) 0.057(4) -0.019(4)
O1 0.098(3) 0.174(4) 0.240(6) -0.032(4) 0.100(4) -0.034(3)
C20 0.060(4) 0.083(4) 0.151(6) -0.026(4) 0.055(4) -0.013(3)
C21 0.108(7) 0.040(5) 0.235(10) 0.000 0.091(7) 0.000
O2 0.144(6) 0.039(3) 0.243(7) 0.002(4) 0.005(5) -0.010(3)
C22 0.107(5) 0.042(3) 0.143(6) -0.004(4) 0.012(5) -0.011(4)
C23 0.144(6) 0.039(3) 0.243(7) 0.002(4) 0.005(5) -0.010(3)
C24 0.049(3) 0.090(4) 0.128(5) -0.007(4) 0.034(4) -0.008(3)
C25 0.125(5) 0.045(4) 0.209(7) -0.010(4) 0.078(5) -0.003(4)
O3 0.098(3) 0.174(4) 0.240(6) -0.032(4) 0.100(4) -0.034(3)
O4 0.168(7) 0.039(3) 0.317(9) 0.004(4) 0.048(6) -0.003(3)
C26 0.168(7) 0.039(3) 0.317(9) 0.004(4) 0.048(6) -0.003(3)
C27 0.132(7) 0.062(5) 0.239(9) -0.014(6) 0.071(6) 0.009(5)
C28 0.098(3) 0.174(4) 0.240(6) -0.032(4) 0.100(4) -0.034(3)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 N1 1.944(4) 2_656 ?
Co1 N1 1.944(4) . ?
Co1 N2 1.939(4) 2_656 ?
Co1 N2 1.939(4) . ?
N1 C6 1.380(5) . ?
N1 C7 1.372(5) . ?
C1 C3 1.496(9) . ?
C1 C6 1.389(5) . ?
C1 C6 1.389(5) 2_656 ?
N2 C9 1.394(6) . ?
N2 C14 1.371(6) . ?
C2 C4 1.503(6) . ?
C2 C7 1.398(6) . ?
C2 C9 1.391(7) . ?
C3 C16 1.368(8) 2_656 ?
C3 C16 1.368(8) . ?
C4 C11 1.367(9) . ?
C4 C17 1.397(9) . ?
C5 H5 0.9500 . ?
C5 C7 1.434(6) . ?
C5 C8 1.353(7) . ?
C6 C8 1.440(6) . ?
C8 H8 0.9500 . ?
C9 C10 1.428(7) . ?
C10 H10 0.9500 . ?
C10 C12 1.337(8) . ?
C11 H11 0.9500 . ?
C11 C19 1.411(9) . ?
C12 H12 0.9500 . ?
C12 C14 1.436(7) . ?
C13 C14 1.388(6) 2_656 ?
C13 C14 1.389(6) . ?
C13 C18 1.515(11) . ?
C15 C22 1.362(9) 2_656 ?
C15 C22 1.362(9) . ?
C15 C23 1.447(15) . ?
C16 H16 0.9500 . ?
C16 C22 1.391(9) . ?
C17 H17 0.9500 . ?
C17 C24 1.372(10) . ?
C18 C25 1.349(11) 2_656 ?
C18 C25 1.349(11) . ?
C19 H19 0.9500 . ?
C19 C20 1.337(12) . ?
O1 C28 1.208(13) . ?
O1 H1 0.9004 . ?
C20 C24 1.338(13) . ?
C20 C28 1.512(11) . ?
C21 C26 1.510(18) . ?
C21 C27 1.355(13) . ?
C21 C27 1.355(13) 2_656 ?
O2 C23 1.227(8) . ?
C22 H22 0.9500 . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
C25 C27 1.362(12) . ?
O3 H3 0.9381 . ?
O3 C28 1.235(12) . ?
O4 H4 0.9529 . ?
O4 C26 1.282(10) . ?
C27 H27 0.9500 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Co1 N1 90.4(2) 2_656 . ?
N2 Co1 N1 171.53(18) 2_656 . ?
N2 Co1 N1 171.53(18) . 2_656 ?
N2 Co1 N1 90.36(16) . . ?
N2 Co1 N1 90.36(16) 2_656 2_656 ?
N2 Co1 N2 90.1(2) 2_656 . ?
C6 N1 Co1 126.5(3) . . ?
C7 N1 Co1 127.1(3) . . ?
C7 N1 C6 105.6(4) . . ?
C6 C1 C3 119.0(3) 2_656 . ?
C6 C1 C3 119.0(3) . . ?
C6 C1 C6 122.1(6) 2_656 . ?
C9 N2 Co1 127.0(3) . . ?
C14 N2 Co1 127.9(3) . . ?
C14 N2 C9 104.3(4) . . ?
C7 C2 C4 119.8(4) . . ?
C9 C2 C4 117.4(4) . . ?
C9 C2 C7 122.8(4) . . ?
C16 C3 C1 119.4(4) 2_656 . ?
C16 C3 C1 119.4(4) . . ?
C16 C3 C16 121.3(8) 2_656 . ?
C11 C4 C2 119.8(5) . . ?
C11 C4 C17 118.5(6) . . ?
C17 C4 C2 121.7(6) . . ?
C7 C5 H5 126.5 . . ?
C8 C5 H5 126.5 . . ?
C8 C5 C7 107.0(4) . . ?
N1 C6 C1 124.3(4) . . ?
N1 C6 C8 109.8(4) . . ?
C1 C6 C8 125.2(4) . . ?
N1 C7 C2 124.0(4) . . ?
N1 C7 C5 110.4(4) . . ?
C2 C7 C5 125.1(4) . . ?
C5 C8 C6 106.9(4) . . ?
C5 C8 H8 126.6 . . ?
C6 C8 H8 126.6 . . ?
N2 C9 C10 110.8(4) . . ?
C2 C9 N2 123.2(5) . . ?
C2 C9 C10 124.5(5) . . ?
C9 C10 H10 126.7 . . ?
C12 C10 C9 106.6(5) . . ?
C12 C10 H10 126.7 . . ?
C4 C11 H11 120.6 . . ?
C4 C11 C19 118.8(7) . . ?
C19 C11 H11 120.6 . . ?
C10 C12 H12 126.1 . . ?
C10 C12 C14 107.7(5) . . ?
C14 C12 H12 126.1 . . ?
C14 C13 C14 122.5(7) 2_656 . ?
C14 C13 C18 118.8(3) 2_656 . ?
C14 C13 C18 118.8(3) . . ?
N2 C14 C12 110.5(5) . . ?
N2 C14 C13 124.7(5) . . ?
C13 C14 C12 124.7(5) . . ?
C22 C15 C22 114.8(9) . 2_656 ?
C22 C15 C23 122.6(4) 2_656 . ?
C22 C15 C23 122.6(4) . . ?
C3 C16 H16 121.3 . . ?
C3 C16 C22 117.5(7) . . ?
C22 C16 H16 121.3 . . ?
C4 C17 H17 119.9 . . ?
C24 C17 C4 120.1(8) . . ?
C24 C17 H17 119.9 . . ?
C25 C18 C13 121.7(5) . . ?
C25 C18 C13 121.7(5) 2_656 . ?
C25 C18 C25 116.7(11) . 2_656 ?
C11 C19 H19 119.1 . . ?
C20 C19 C11 121.7(8) . . ?
C20 C19 H19 119.1 . . ?
C28 O1 H1 99.8 . . ?
C19 C20 C24 119.4(7) . . ?
C19 C20 C28 118.8(10) . . ?
C24 C20 C28 121.7(9) . . ?
C27 C21 C26 121.0(6) . . ?
C27 C21 C26 121.0(6) 2_656 . ?
C27 C21 C27 118.0(13) 2_656 . ?
C15 C22 C16 124.3(8) . . ?
C15 C22 H22 117.8 . . ?
C16 C22 H22 117.8 . . ?
O2 C23 C15 118.9(6) 2_656 . ?
O2 C23 C15 118.9(6) . . ?
O2 C23 O2 122.3(12) . 2_656 ?
C17 C24 H24 119.3 . . ?
C20 C24 C17 121.4(8) . . ?
C20 C24 H24 119.3 . . ?
C18 C25 H25 118.9 . . ?
C18 C25 C27 122.2(11) . . ?
C27 C25 H25 118.9 . . ?
C28 O3 H3 147.6 . . ?
C26 O4 H4 120.6 . . ?
O4 C26 C21 116.5(7) . . ?
O4 C26 C21 116.5(7) 2_656 . ?
O4 C26 O4 127.1(14) . 2_656 ?
C21 C27 C25 120.4(12) . . ?
C21 C27 H27 119.8 . . ?
C25 C27 H27 119.8 . . ?
O1 C28 C20 116.4(11) . . ?
O1 C28 O3 124.3(11) . . ?
O3 C28 C20 117.8(11) . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Co1 N1 C6 C1 -24.3(6) . . . . ?
Co1 N1 C6 C8 164.6(3) . . . . ?
Co1 N1 C7 C2 22.9(7) . . . . ?
Co1 N1 C7 C5 -165.6(3) . . . . ?
Co1 N2 C9 C2 23.8(8) . . . . ?
Co1 N2 C9 C10 -169.6(4) . . . . ?
Co1 N2 C14 C12 168.7(5) . . . . ?
Co1 N2 C14 C13 -14.8(10) . . . . ?
N1 C6 C8 C5 4.6(6) . . . . ?
C1 C3 C16 C22 177.4(6) . . . . ?
C1 C6 C8 C5 -166.5(4) . . . . ?
N2 C9 C10 C12 0.1(8) . . . . ?
C2 C4 C11 C19 179.9(5) . . . . ?
C2 C4 C17 C24 -178.3(6) . . . . ?
C2 C9 C10 C12 166.5(7) . . . . ?
C3 C1 C6 N1 -167.5(3) . . . . ?
C3 C1 C6 C8 2.2(6) . . . . ?
C3 C16 C22 C15 5.7(13) . . . . ?
C4 C2 C7 N1 165.5(5) . . . . ?
C4 C2 C7 C5 -4.8(8) . . . . ?
C4 C2 C9 N2 170.7(5) . . . . ?
C4 C2 C9 C10 5.9(9) . . . . ?
C4 C11 C19 C20 -1.5(11) . . . . ?
C4 C17 C24 C20 -1.9(12) . . . . ?
C6 N1 C7 C2 -167.0(5) . . . . ?
C6 N1 C7 C5 4.6(6) . . . . ?
C6 C1 C3 C16 63.9(5) . . . 2_656 ?
C6 C1 C3 C16 -116.1(5) 2_656 . . 2_656 ?
C6 C1 C3 C16 63.9(5) 2_656 . . . ?
C6 C1 C3 C16 -116.1(5) . . . . ?
C6 C1 C6 N1 12.5(3) 2_656 . . . ?
C6 C1 C6 C8 -177.8(6) 2_656 . . . ?
C7 N1 C6 C1 165.6(4) . . . . ?
C7 N1 C6 C8 -5.5(5) . . . . ?
C7 C2 C4 C11 70.1(7) . . . . ?
C7 C2 C4 C17 -109.9(6) . . . . ?
C7 C2 C9 N2 -10.1(9) . . . . ?
C7 C2 C9 C10 -174.9(6) . . . . ?
C7 C5 C8 C6 -1.6(6) . . . . ?
C8 C5 C7 N1 -1.8(6) . . . . ?
C8 C5 C7 C2 169.6(5) . . . . ?
C9 N2 C14 C12 -1.8(8) . . . . ?
C9 N2 C14 C13 174.7(6) . . . . ?
C9 C2 C4 C11 -110.6(7) . . . . ?
C9 C2 C4 C17 69.4(7) . . . . ?
C9 C2 C7 N1 -13.7(9) . . . . ?
C9 C2 C7 C5 176.0(5) . . . . ?
C9 C10 C12 C14 -1.2(9) . . . . ?
C10 C12 C14 N2 2.0(9) . . . . ?
C10 C12 C14 C13 -174.5(7) . . . . ?
C11 C4 C17 C24 1.7(9) . . . . ?
C11 C19 C20 C24 1.4(12) . . . . ?
C11 C19 C20 C28 179.1(8) . . . . ?
C13 C18 C25 C27 -178.9(8) . . . . ?
C14 N2 C9 C2 -165.5(6) . . . . ?
C14 N2 C9 C10 1.1(7) . . . . ?
C14 C13 C14 N2 7.5(5) 2_656 . . . ?
C14 C13 C14 C12 -176.4(9) 2_656 . . . ?
C14 C13 C18 C25 -71.3(6) 2_656 . . 2_656 ?
C14 C13 C18 C25 -71.3(6) . . . . ?
C14 C13 C18 C25 108.7(6) . . . 2_656 ?
C14 C13 C18 C25 108.7(6) 2_656 . . . ?
C16 C3 C16 C22 -2.6(6) 2_656 . . . ?
C17 C4 C11 C19 -0.1(9) . . . . ?
C18 C13 C14 N2 -172.5(5) . . . . ?
C18 C13 C14 C12 3.6(9) . . . . ?
C18 C25 C27 C21 -2.2(16) . . . . ?
C19 C20 C24 C17 0.3(13) . . . . ?
C19 C20 C28 O1 4.7(17) . . . . ?
C19 C20 C28 O3 170.9(11) . . . . ?
C22 C15 C22 C16 -2.9(7) 2_656 . . . ?
C22 C15 C23 O2 12.7(7) 2_656 . . 2_656 ?
C22 C15 C23 O2 -167.3(7) . . . 2_656 ?
C22 C15 C23 O2 12.7(7) . . . . ?
C22 C15 C23 O2 -167.3(7) 2_656 . . . ?
C23 C15 C22 C16 177.1(7) . . . . ?
C24 C20 C28 O1 -177.6(11) . . . . ?
C24 C20 C28 O3 -11.4(18) . . . . ?
C25 C18 C25 C27 1.1(8) 2_656 . . . ?
C26 C21 C27 C25 -178.9(8) . . . . ?
C27 C21 C26 O4 10.7(7) 2_656 . . 2_656 ?
C27 C21 C26 O4 -169.3(7) 2_656 . . . ?
C27 C21 C26 O4 10.7(7) . . . . ?
C27 C21 C26 O4 -169.3(7) . . . 2_656 ?
C27 C21 C27 C25 1.1(8) 2_656 . . . ?
C28 C20 C24 C17 -177.4(9) . . . . ?
_shelx_res_file
;
TITL 080_a.res in P2/c
pfc-72-co.res
created by SHELXL-2018/3 at 10:07:07 on 06-Sep-2021
REM Old TITL 080 in P2/c
REM SHELXT solution in P2/c: R1 0.373, Rweak 0.009, Alpha 0.068
REM <I/s> 0.849 for 189 systematic absences, Orientation as input
REM Formula found by SHELXT: C42 N10 O6 Co
CELL 0.71073 18.0332 22.0956 9.1973 90 104.289 90
ZERR 2 0.0022 0.0021 0.001 0 0.007 0
LATT 1
SYMM -X,+Y,0.5-Z
SFAC C H Co N O
UNIT 96 56 2 8 16
DFIX 1.54 C28 C20
EADP O1 C28 O3
DFIX 1.27 O3 C28
EADP O4 C26
DFIX 1.27 O1 C28
SIMU 0.02 0.04 3.8 C1 C2 C3 C4 C5 C6 C7 C8 C9 C10 C11 C12 C13 C14 C15 C16 =
C17 C18 C19 C20 C21 C22 C23 C24 C25 C26 C27 C28
EADP O2 C23
L.S. 20
PLAN 20
SIZE 0.1 0.2 0.1
TEMP -93.11
CONF
list 4
MORE -1
BOND $H
ABIN
fmap 2
acta
OMIT -1 1 1
REM <olex2.extras>
REM <HklSrc "%.\\PFC-72-Co.hkl">
REM </olex2.extras>
WGHT 0.200000
FVAR 0.28330
CO1 3 0.500000 0.565908 0.750000 10.50000 0.04470 0.02341 =
0.06706 0.00000 0.04212 0.00000
N1 4 0.559342 0.503915 0.679730 11.00000 0.03478 0.02976 =
0.03942 -0.00006 0.02293 -0.00411
C1 1 0.500000 0.412337 0.750000 10.50000 0.03407 0.02919 =
0.04596 0.00000 0.02472 0.00000
N2 4 0.568465 0.627907 0.710078 11.00000 0.04793 0.02709 =
0.06023 0.00284 0.03614 -0.00058
C2 1 0.660744 0.565639 0.621275 11.00000 0.04165 0.03258 =
0.05561 0.00941 0.03109 0.00184
C3 1 0.500000 0.344647 0.750000 10.50000 0.04833 0.02611 =
0.06695 0.00000 0.03885 0.00000
C4 1 0.734098 0.565844 0.571504 11.00000 0.04245 0.04008 =
0.07414 0.00022 0.03656 -0.00148
C5 1 0.633837 0.457386 0.541914 11.00000 0.03989 0.03341 =
0.05268 -0.00164 0.02957 0.00676
AFIX 43
H5 2 0.670560 0.451994 0.484635 11.00000 -1.20000
AFIX 0
C6 1 0.543231 0.442792 0.667394 11.00000 0.04036 0.02598 =
0.04228 0.00361 0.02407 0.00755
C7 1 0.617317 0.512657 0.609420 11.00000 0.04136 0.02999 =
0.05591 0.00708 0.03363 0.00768
C8 1 0.587234 0.414382 0.575230 11.00000 0.04269 0.03727 =
0.04472 -0.00667 0.02754 0.01064
AFIX 43
H8 2 0.584127 0.373300 0.543836 11.00000 -1.20000
AFIX 0
C9 1 0.639685 0.619216 0.679581 11.00000 0.05520 0.02636 =
0.07806 0.00526 0.04234 0.00038
C10 1 0.679151 0.675437 0.682830 11.00000 0.06073 0.03765 =
0.09401 0.00534 0.05131 -0.00681
AFIX 43
H10 2 0.728440 0.681309 0.665458 11.00000 -1.20000
AFIX 0
C11 1 0.731930 0.561867 0.422231 11.00000 0.05675 0.07824 =
0.08674 -0.01070 0.04659 -0.01534
AFIX 43
H11 2 0.684442 0.558905 0.349479 11.00000 -1.20000
AFIX 0
C12 1 0.633222 0.718194 0.715082 11.00000 0.08154 0.02869 =
0.13078 -0.00097 0.07268 -0.00700
AFIX 43
H12 2 0.644363 0.760197 0.726697 11.00000 -1.20000
AFIX 0
C13 1 0.500000 0.719470 0.750000 10.50000 0.08386 0.02417 =
0.14689 0.00000 0.08354 0.00000
C14 1 0.564050 0.689228 0.729005 11.00000 0.06663 0.03075 =
0.12705 0.00341 0.07212 -0.00648
C15 1 0.500000 0.218202 0.750000 10.50000 0.08437 0.02798 =
0.12759 0.00000 0.05187 0.00000
C16 1 0.433382 0.314291 0.690000 11.00000 0.08356 0.03987 =
0.12317 0.00900 0.01923 -0.00538
AFIX 43
H16 2 0.386671 0.335342 0.652080 11.00000 -1.20000
AFIX 0
C17 1 0.805323 0.570051 0.674144 11.00000 0.05680 0.07152 =
0.09713 0.00488 0.02663 -0.00237
AFIX 43
H17 2 0.808292 0.571768 0.778635 11.00000 -1.20000
AFIX 0
C18 1 0.500000 0.788016 0.750000 10.50000 0.09302 0.03661 =
0.17223 0.00000 0.09666 0.00000
C19 1 0.801515 0.562243 0.378190 11.00000 0.07420 0.09846 =
0.10189 -0.02859 0.05682 -0.01876
AFIX 43
H19 2 0.800423 0.558517 0.274781 11.00000 -1.20000
AFIX 0
O1 5 0.932899 0.565113 0.288548 11.00000 0.09840 0.17365 =
0.23957 -0.03247 0.10048 -0.03418
C20 1 0.868961 0.567704 0.478160 11.00000 0.05986 0.08271 =
0.15144 -0.02637 0.05465 -0.01275
C21 1 0.500000 0.913231 0.750000 10.50000 0.10796 0.04008 =
0.23536 0.00000 0.09105 0.00000
O2 5 0.445673 0.125912 0.669013 11.00000 0.14386 0.03942 =
0.24287 0.00192 0.00487 -0.00982
C22 1 0.436618 0.251401 0.686604 11.00000 0.10650 0.04150 =
0.14265 -0.00397 0.01163 -0.01140
AFIX 43
H22 2 0.391669 0.230226 0.636797 11.00000 -1.20000
AFIX 0
C23 1 0.500000 0.152716 0.750000 10.50000 0.14386 0.03942 =
0.24287 0.00192 0.00487 -0.00982
C24 1 0.871011 0.571707 0.624292 11.00000 0.04871 0.08975 =
0.12772 -0.00674 0.03389 -0.00815
AFIX 43
H24 2 0.918995 0.575785 0.695060 11.00000 -1.20000
AFIX 0
C25 1 0.543847 0.820046 0.864162 11.00000 0.12476 0.04534 =
0.20881 -0.01031 0.07750 -0.00299
AFIX 43
H25 2 0.576115 0.798914 0.945600 11.00000 -1.20000
AFIX 0
O3 5 1.002037 0.579658 0.513453 11.00000 0.09840 0.17365 =
0.23957 -0.03247 0.10048 -0.03418
AFIX 1
H3 2 1.055630 0.577240 0.539090 10.50000 -1.50000
AFIX 0
O4 5 0.551391 1.007429 0.852542 11.00000 0.16807 0.03912 =
0.31748 0.00404 0.04804 -0.00302
AFIX 1
H4 2 0.551330 1.050240 0.865060 11.00000 -1.50000
AFIX 0
C26 1 0.500000 0.981574 0.750000 10.50000 0.16807 0.03912 =
0.31748 0.00404 0.04804 -0.00302
C27 1 0.543420 0.881674 0.866613 11.00000 0.13182 0.06157 =
0.23907 -0.01415 0.07069 0.00917
AFIX 43
H27 2 0.573757 0.902658 0.950614 11.00000 -1.20000
AFIX 0
C28 1 0.941258 0.566827 0.422878 11.00000 0.09840 0.17365 =
0.23957 -0.03247 0.10048 -0.03418
AFIX 1
H1 2 0.982220 0.565630 0.284110 10.50000 -1.50000
AFIX 0
HKLF 4
REM 080_a.res in P2/c
REM wR2 = 0.3512, GooF = S = 1.128, Restrained GooF = 1.178 for all data
REM R1 = 0.1066 for 3781 Fo > 4sig(Fo) and 0.1643 for all 7248 data
REM 260 parameters refined using 591 restraints
END
WGHT 0.2000 0.0000
REM Highest difference peak 1.281, deepest hole -0.680, 1-sigma level 0.101
Q1 1 0.8961 0.5772 0.1865 11.00000 0.05 1.17
Q2 1 0.5231 0.5680 0.8471 11.00000 0.05 1.11
Q3 1 0.4735 0.3098 0.6167 11.00000 0.05 0.97
Q4 1 0.9546 0.5413 0.3485 11.00000 0.05 0.89
Q5 1 0.4782 0.2461 0.6116 11.00000 0.05 0.88
Q6 1 0.4998 0.1209 0.6240 11.00000 0.05 0.83
Q7 1 0.5642 0.4336 0.4694 11.00000 0.05 0.73
Q8 1 0.4993 1.0046 0.8733 11.00000 0.05 0.66
Q9 1 0.4986 0.8172 0.8801 11.00000 0.05 0.51
Q10 1 0.5649 0.4313 0.6619 11.00000 0.05 0.49
Q11 1 0.4898 0.8805 0.8758 11.00000 0.05 0.48
Q12 1 0.8963 0.5670 0.3209 11.00000 0.05 0.47
Q13 1 0.7156 0.6003 0.3910 11.00000 0.05 0.47
Q14 1 0.5000 0.5111 0.7500 10.50000 0.05 0.45
Q15 1 0.8438 0.5684 0.3802 11.00000 0.05 0.45
Q16 1 0.4469 0.1233 0.7622 11.00000 0.05 0.44
Q17 1 0.5618 0.5664 0.6834 11.00000 0.05 0.42
Q18 1 0.5501 1.0104 0.7393 11.00000 0.05 0.41
Q19 1 0.5736 0.8132 0.9477 11.00000 0.05 0.40
Q20 1 0.9492 0.5886 0.3176 11.00000 0.05 0.39
;
_shelx_res_checksum 43034
_shelx_hkl_file
;
-1 0 1 0.50 0.40
2 0 -2 335.77 16.90
-2 0 2 404.96 16.90
-3 0 3 -0.60 1.70
3 0 -3 3.40 1.60
-4 0 4 261.07 12.70
-5 0 5 -0.60 2.50
-6 0 6 8.80 3.20
-7 0 7 0.30 3.30
-8 0 8 154.58 9.90
-10 0 10 7.50 5.10
-11 0 11 7.20 4.90
1 -1 -1 88.89 4.20
-1 -1 1 107.29 4.40
-1 1 1 81.79 4.20
2 -1 -2 118.89 5.80
-2 -1 2 130.09 6.20
-2 1 2 124.89 5.90
2 1 -2 112.69 6.00
-3 -1 3 181.88 8.70
3 -1 -3 159.68 8.20
-4 -1 4 7.80 2.50
-4 1 4 11.00 2.20
-5 -1 5 -4.10 2.70
-5 1 5 -2.60 2.40
-6 1 6 9.20 2.90
-7 -1 7 -2.70 3.40
-7 1 7 -0.30 2.90
-8 -1 8 73.09 6.80
-8 1 8 71.19 6.50
-9 -1 9 1.90 4.10
-9 1 9 -3.10 3.80
-10 -1 10 3.30 4.90
-10 1 10 5.70 4.30
-11 -1 11 -4.60 5.00
-11 1 11 5.80 4.90
-1 -2 1 78.49 3.80
1 -2 -1 69.29 3.60
-1 2 1 78.69 3.60
2 -2 -2 152.08 7.60
-2 -2 2 180.58 8.20
2 -2 -2 169.48 7.60
2 -2 -2 169.58 7.60
2 2 -2 158.98 8.00
-2 2 2 159.78 7.60
-3 -2 3 -5.40 2.10
3 -2 -3 2.90 0.90
3 -2 -3 2.20 1.20
3 -2 -3 1.10 1.10
-3 2 3 0.10 1.40
-4 -2 4 4.00 2.40
-4 2 4 4.00 1.80
-5 -2 5 6.50 3.20
-5 2 5 12.80 2.60
-6 -2 6 -5.50 3.00
-6 2 6 1.70 2.30
-7 -2 7 -3.30 3.40
-7 2 7 1.80 2.90
-8 -2 8 11.90 4.50
-8 2 8 21.50 4.10
-9 -2 9 2.70 4.00
-9 2 9 7.70 4.00
-10 -2 10 -2.40 4.60
-10 2 10 -0.80 4.00
-11 -2 11 2.40 5.40
-11 2 11 3.80 4.60
0 -3 0 108.89 4.90
0 3 0 102.39 5.00
-1 -3 1 65.09 3.40
1 -3 -1 64.09 3.20
-1 3 1 59.29 3.20
-2 -3 2 22.10 2.50
2 3 -2 23.40 2.90
-3 -3 3 269.07 13.10
3 -3 -3 282.47 12.40
-3 3 3 258.27 12.40
4 -3 -4 24.60 2.20
-4 -3 4 21.50 3.30
4 -3 -4 23.60 2.40
-4 3 4 23.10 2.50
-5 -3 5 11.10 3.90
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_computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)'
;
_shelx_hkl_checksum 90126
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;
_shelx_fab_checksum 32894
_olex2_submission_special_instructions 'No special instructions were received'
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