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发表于 2025-4-11 17:31:52
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这是CIF文件内容：
#######################################################################
#
# 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_1
_audit_block_doi 10.5517/cc13crs0
_database_code_depnum_ccdc_archive 'CCDC 1024202'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1107/S2053229614020634 2014
_audit_update_record
;
2014-09-14 deposited with the CCDC. 2025-04-11 downloaded from the CCDC.
;
_publcif_datablock.id {a6cf52d7-5ed5-497c-a18b-2f430342d64e}
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C12 H9 N'
_chemical_formula_sum 'C12 H9 N'
_chemical_formula_weight 167.20
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting orthorhombic
_symmetry_space_group_name_H-M Pnma
_symmetry_space_group_name_Hall '-P 2ac 2n'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'
_cell_length_a 7.6371(2)
_cell_length_b 19.0042(6)
_cell_length_c 5.67758(14)
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_volume 824.03(4)
_cell_formula_units_Z 4
_cell_measurement_temperature 100.0(1)
_cell_measurement_reflns_used 831
_cell_measurement_theta_min 3.75
_cell_measurement_theta_max 25.99
_exptl_crystal_description plate
_exptl_crystal_colour colourless
_exptl_crystal_size_max 0.38
_exptl_crystal_size_mid 0.25
_exptl_crystal_size_min 0.12
_exptl_crystal_preparation
;
recrytalization from ethanol
;
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.348
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 352
_exptl_absorpt_coefficient_mu 0.079
_exptl_absorpt_correction_type none
_exptl_absorpt_correction_T_min ?
_exptl_absorpt_correction_T_max ?
_exptl_absorpt_process_details ?
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 100.0(1)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type Xcalibur
_diffrn_measurement_method \w--scan
_diffrn_detector_area_resol_mean '1024 x 1024 with blocks 2 x 2'
_diffrn_standards_number 0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time 0
_diffrn_standards_decay_% 0
_diffrn_reflns_number 5112
_diffrn_reflns_av_R_equivalents 0.0167
_diffrn_reflns_av_sigmaI/netI 0.0118
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_h_max 8
_diffrn_reflns_limit_k_min -21
_diffrn_reflns_limit_k_max 23
_diffrn_reflns_limit_l_min -6
_diffrn_reflns_limit_l_max 7
_diffrn_reflns_theta_min 3.75
_diffrn_reflns_theta_max 25.99
_reflns_number_total 831
_reflns_number_gt 717
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'CrysAlisCCD (Oxford Diffraction Ltd., 2008)'
_computing_cell_refinement 'CrysAlisRED (Oxford Diffraction Ltd., 2008)'
_computing_data_reduction 'CrysAlisRED (Oxford Diffraction Ltd., 2008)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)'
_computing_publication_material 'SHELXL-97 (Sheldrick, 2008)'
_refine_special_details
;
Refinement of <i>F</i>^2^ against ALL reflections. The weighted <i>R</i>-factor
<i>wR</i> and goodness of fit <i>S</i> are based on <i>F</i>^2^, conventional
<i>R</i>-factors <i>R</i> are based on <i>F</i>, with <i>F</i> set to zero for
negative <i>F</i>^2^. The threshold expression of <i>F</i>^2^ >
\s(<i>F</i>^2^) is used only for calculating <i>R</i>-factors(gt) <i>etc</i>.
and is not relevant to the choice of reflections for refinement.
<i>R</i>-factors based on <i>F</i>^2^ are statistically about twice as large
as those based on <i>F</i>, and <i>R</i>- factors based on ALL data will be
even larger.
;
_iucr_refine_instructions_details
;
TITL ke150 in Pnma
REM Pnma (#62 in standard setting)
CELL 0.71073 7.637142 19.004191 5.677575 90.0000 90.0000 90.0000
ZERR 4.00 0.000199 0.000574 0.000144 0.0000 0.0000 0.0000
LATT 1
SYMM -x+1/2,-y, z+1/2
SYMM -x, y+1/2,-z
SYMM x+1/2,-y+1/2,-z+1/2
SFAC C H N
UNIT 48.00 36.00 4.00
OMIT -4 52
L.S. 10
CONF
ACTA
BOND $H
MPLA 6 C1 C2 C3 C4 C4A C9A
MPLA 5 N9 C9A C4A C4A_$1 C9A_$1
EQIV $1 X, 3/2-Y, Z
FMAP 2
PLAN 20
WGHT 0.057200 0.142900
FVAR 3.56136
C1 1 0.263854 0.619739 0.303802 11.00000 0.01957 0.03235 =
0.02047 -0.00563 0.00192 -0.00480
AFIX 43
H1 2 0.207549 0.606204 0.165807 11.00000 -1.20000
AFIX 0
C2 1 0.323909 0.570437 0.464174 11.00000 0.02432 0.02337 =
0.03056 -0.00313 0.00726 -0.00395
AFIX 43
H2 2 0.307554 0.522853 0.432890 11.00000 -1.20000
AFIX 0
C3 1 0.408693 0.590493 0.672372 11.00000 0.02237 0.02615 =
0.02527 0.00571 0.00415 0.00129
AFIX 43
H3 2 0.448085 0.556097 0.776142 11.00000 -1.20000
AFIX 0
C4 1 0.434660 0.660723 0.725818 11.00000 0.01703 0.02955 =
0.01792 0.00082 0.00137 -0.00046
AFIX 43
H4 2 0.490973 0.673747 0.864356 11.00000 -1.20000
AFIX 0
C4A 1 0.374825 0.711759 0.568070 11.00000 0.01359 0.02538 =
0.01766 -0.00126 0.00328 -0.00095
N9 3 0.243478 0.750000 0.232256 10.50000 0.02242 0.02910 =
0.01563 0.00000 -0.00410 0.00000
AFIX 43
H9 2 0.192131 0.750000 0.097447 10.50000 -1.20000
AFIX 0
C9A 1 0.291175 0.690501 0.357482 11.00000 0.01514 0.02791 =
0.01746 0.00168 0.00316 -0.00020
HKLF 4
REM ke150 in Pnma
REM R1 = 0.0327 for 717 Fo > 4sig(Fo) and 0.0385 for all 831 data
REM 61 parameters refined using 0 restraints
END
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0572P)^2^+0.1429P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment noref
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 831
_refine_ls_number_parameters 61
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0385
_refine_ls_R_factor_gt 0.0327
_refine_ls_wR_factor_ref 0.0929
_refine_ls_wR_factor_gt 0.0898
_refine_ls_goodness_of_fit_ref 1.077
_refine_ls_restrained_S_all 1.077
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.26385(15) 0.61974(6) 0.3038(2) 0.0241(3) Uani 1 1 d . . .
H1 H 0.2075 0.6062 0.1658 0.029 Uiso 1 1 calc R . .
C2 C 0.32391(14) 0.57044(6) 0.4642(2) 0.0261(3) Uani 1 1 d . . .
H2 H 0.3076 0.5229 0.4329 0.031 Uiso 1 1 calc R . .
C3 C 0.40869(14) 0.59049(6) 0.6724(2) 0.0246(3) Uani 1 1 d . . .
H3 H 0.4481 0.5561 0.7761 0.030 Uiso 1 1 calc R . .
C4 C 0.43466(14) 0.66072(6) 0.72582(19) 0.0215(3) Uani 1 1 d . . .
H4 H 0.4910 0.6737 0.8644 0.026 Uiso 1 1 calc R . .
C4A C 0.37483(12) 0.71176(6) 0.56807(18) 0.0189(3) Uani 1 1 d . . .
N9 N 0.24348(17) 0.7500 0.2323(2) 0.0224(3) Uani 1 2 d S . .
H9 H 0.1921 0.7500 0.0974 0.027 Uiso 1 2 calc SR . .
C9A C 0.29118(13) 0.69050(6) 0.35748(19) 0.0202(3) Uani 1 1 d . . .
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
C1 0.0196(6) 0.0323(7) 0.0205(6) -0.0056(5) 0.0019(4) -0.0048(5)
C2 0.0243(6) 0.0234(6) 0.0306(7) -0.0031(5) 0.0073(5) -0.0040(5)
C3 0.0224(6) 0.0261(6) 0.0253(6) 0.0057(5) 0.0042(4) 0.0013(4)
C4 0.0170(6) 0.0296(7) 0.0179(5) 0.0008(4) 0.0014(4) -0.0005(5)
C4A 0.0136(5) 0.0254(6) 0.0177(6) -0.0013(4) 0.0033(4) -0.0009(4)
N9 0.0224(7) 0.0291(8) 0.0156(7) 0.000 -0.0041(5) 0.000
C9A 0.0151(5) 0.0279(6) 0.0175(5) 0.0017(5) 0.0032(4) -0.0002(4)
_geom_special_details
;
All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell e.s.d.'s are taken
into account individually in the estimation of e.s.d.'s in distances, angles
and torsion angles; correlations between e.s.d.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell e.s.d.'s is used for estimating e.s.d.'s 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
C1 C2 1.3847(17) . ?
C1 C9A 1.3946(16) . ?
C1 H1 0.9300 . ?
C2 C3 1.4006(17) . ?
C2 H2 0.9300 . ?
C3 C4 1.3830(17) . ?
C3 H3 0.9300 . ?
C4 C4A 1.3970(16) . ?
C4 H4 0.9300 . ?
C4A C9A 1.4145(15) . ?
C4A C4A 1.453(2) 7_575 ?
N9 C9A 1.3845(13) 7_575 ?
N9 C9A 1.3845(13) . ?
N9 H9 0.8600 . ?
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
C2 C1 C9A 117.34(11) . . ?
C2 C1 H1 121.3 . . ?
C9A C1 H1 121.3 . . ?
C1 C2 C3 121.60(11) . . ?
C1 C2 H2 119.2 . . ?
C3 C2 H2 119.2 . . ?
C4 C3 C2 120.93(11) . . ?
C4 C3 H3 119.5 . . ?
C2 C3 H3 119.5 . . ?
C3 C4 C4A 118.84(11) . . ?
C3 C4 H4 120.6 . . ?
C4A C4 H4 120.6 . . ?
C4 C4A C9A 119.43(10) . . ?
C4 C4A C4A 133.97(7) . 7_575 ?
C9A C4A C4A 106.60(6) . 7_575 ?
C9A N9 C9A 109.52(13) 7_575 . ?
C9A N9 H9 125.2 7_575 . ?
C9A N9 H9 125.2 . . ?
N9 C9A C1 129.49(10) . . ?
N9 C9A C4A 108.64(10) . . ?
C1 C9A C4A 121.85(10) . . ?
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
C9A C1 C2 C3 0.04(16) . . . . ?
C1 C2 C3 C4 0.35(16) . . . . ?
C2 C3 C4 C4A -0.04(16) . . . . ?
C3 C4 C4A C9A -0.64(15) . . . . ?
C3 C4 C4A C4A 178.17(6) . . . 7_575 ?
C9A N9 C9A C1 177.51(8) 7_575 . . . ?
C9A N9 C9A C4A -1.00(16) 7_575 . . . ?
C2 C1 C9A N9 -179.08(12) . . . . ?
C2 C1 C9A C4A -0.75(16) . . . . ?
C4 C4A C9A N9 179.71(10) . . . . ?
C4A C4A C9A N9 0.60(9) 7_575 . . . ?
C4 C4A C9A C1 1.06(15) . . . . ?
C4A C4A C9A C1 -178.05(8) 7_575 . . . ?
_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full 25.99
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max 0.191
_refine_diff_density_min -0.216
_refine_diff_density_rms 0.037
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发表于 2025-4-11 17:17:07
