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#$Date: 2022-05-04 10:51:18 +0300 (Wed, 04 May 2022) $
#$Revision: 274871 $
#$URL: file:///home/coder/svn-repositories/cod/cif/8/10/51/8105128.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
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data_8105128
loop_
_publ_author_name
'Deng, Xiao-Wei'
'Wu, Wei-Na'
_publ_section_title
;
 Crystal structure of
 bis(3-methoxy-N-(1-(pyridin-2-yl)ethylidene)benzohydrazonato κ3
 O,N,N′)zinc(II), C30H28N6O4Zn
;
_journal_issue                   2
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              421
_journal_page_last               422
_journal_paper_doi               10.1515/ncrs-2019-0726
_journal_volume                  235
_journal_year                    2020
_chemical_formula_sum            'C30 H28 N6 O4 Zn'
_chemical_formula_weight         601.95
_space_group_crystal_system      orthorhombic
_space_group_IT_number           41
_space_group_name_Hall           'A 2 -2ab'
_space_group_name_H-M_alt        'A e a 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.040(9)
_cell_length_b                   22.596(18)
_cell_length_c                   10.344(10)
_cell_measurement_reflns_used    1329
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      20.87
_cell_measurement_theta_min      2.47
_cell_volume                     2814(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0638
_diffrn_reflns_av_unetI/netI     0.0730
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            6692
_diffrn_reflns_point_group_measured_fraction_full 0.790
_diffrn_reflns_point_group_measured_fraction_max 0.790
_diffrn_reflns_theta_full        24.995
_diffrn_reflns_theta_max         24.995
_diffrn_reflns_theta_min         1.802
_exptl_absorpt_coefficient_mu    0.920
_exptl_absorpt_correction_T_max  0.945
_exptl_absorpt_correction_T_min  0.875
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.421
_exptl_crystal_description       plate
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.313
_refine_diff_density_min         -0.647
_refine_diff_density_rms         0.061
_refine_ls_abs_structure_details
; 
 Flack x determined using 274 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.02(3)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     188
_refine_ls_number_reflns         1968
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0973
_refine_ls_R_factor_gt           0.0463
_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/[σ²(Fo²)+(0.0726P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1144
_refine_ls_wR_factor_ref         0.1435
_reflns_Friedel_coverage         0.489
_reflns_Friedel_fraction_full    0.554
_reflns_Friedel_fraction_max     0.554
_reflns_number_gt                1235
_reflns_number_total             1968
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            suppl_ncrs-2019-0726_suppl.cif
_cod_data_source_block           1
_cod_original_sg_symbol_Hall     'A 2 -2ac'
_cod_original_sg_symbol_H-M      'A b a 2'
_cod_database_code               8105128
_shelx_shelxl_version_number     2014/7
_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. 
;
_shelx_estimated_absorpt_t_min   0.874
_shelx_estimated_absorpt_t_max   0.947
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'x+1/2, -y+1, z+1/2'
'-x+1/2, y+1, z+1/2'
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
Zn1 Zn 0.5000 0.5000 0.23455(19) 0.0561(4) Uani 1 2 d S T P . .
N1 N 0.4286(6) 0.5587(4) 0.0735(7) 0.063(2) Uani 1 1 d . . . . .
N2 N 0.3306(5) 0.4821(3) 0.2291(9) 0.0525(17) Uani 1 1 d . . . . .
N3 N 0.2897(5) 0.4393(3) 0.3100(6) 0.0541(18) Uani 1 1 d . . . . .
O1 O 0.4779(4) 0.4300(3) 0.3677(6) 0.0596(17) Uani 1 1 d . . . . .
O2 O 0.4758(7) 0.2707(3) 0.7010(7) 0.103(3) Uani 1 1 d . . . . .
C1 C 0.4782(9) 0.5941(5) -0.0097(12) 0.082(3) Uani 1 1 d . . . . .
H1 H 0.5552 0.5976 -0.0071 0.099 Uiso 1 1 calc R U . . .
C2 C 0.4189(11) 0.6263(5) -0.1014(10) 0.089(4) Uani 1 1 d . . . . .
H2 H 0.4570 0.6515 -0.1568 0.106 Uiso 1 1 calc R U . . .
C3 C 0.3103(9) 0.6220(4) -0.1117(8) 0.064(3) Uani 1 1 d . . . . .
H3 H 0.2719 0.6431 -0.1745 0.077 Uiso 1 1 calc R U . . .
C4 C 0.2570(11) 0.5867(4) -0.0303(10) 0.072(3) Uani 1 1 d . . . . .
H4 H 0.1801 0.5834 -0.0355 0.086 Uiso 1 1 calc R U . . .
C5 C 0.3151(6) 0.5537(4) 0.0648(8) 0.053(2) Uani 1 1 d . . . . .
C6 C 0.2623(7) 0.5121(4) 0.1541(8) 0.051(2) Uani 1 1 d . . . . .
C7 C 0.1383(7) 0.5031(4) 0.1578(9) 0.070(3) Uani 1 1 d . . . . .
H7A H 0.1222 0.4621 0.1736 0.106 Uiso 1 1 calc R U . . .
H7B H 0.1067 0.5147 0.0765 0.106 Uiso 1 1 calc R U . . .
H7C H 0.1069 0.5268 0.2257 0.106 Uiso 1 1 calc R U . . .
C8 C 0.3757(6) 0.4136(4) 0.3750(7) 0.049(2) Uani 1 1 d . . . . .
C9 C 0.3439(6) 0.3628(4) 0.4576(7) 0.049(2) Uani 1 1 d . . . . .
C10 C 0.4191(7) 0.3407(4) 0.5452(8) 0.061(2) Uani 1 1 d . . . . .
H10 H 0.4874 0.3593 0.5560 0.074 Uiso 1 1 calc R U . . .
C11 C 0.3928(9) 0.2900(4) 0.6187(9) 0.071(3) Uani 1 1 d . . . . .
C12 C 0.2918(10) 0.2623(4) 0.6046(11) 0.078(3) Uani 1 1 d . . . . .
H12 H 0.2738 0.2293 0.6541 0.093 Uiso 1 1 calc R U . . .
C13 C 0.2170(9) 0.2849(5) 0.5142(11) 0.084(3) Uani 1 1 d . . . . .
H13 H 0.1489 0.2661 0.5029 0.101 Uiso 1 1 calc R U . . .
C14 C 0.2415(8) 0.3346(4) 0.4407(8) 0.065(3) Uani 1 1 d . . . . .
H14 H 0.1905 0.3490 0.3810 0.078 Uiso 1 1 calc R U . . .
C15 C 0.4678(11) 0.2122(5) 0.7544(16) 0.127(5) Uani 1 1 d . . . . .
H15A H 0.4447 0.1851 0.6883 0.190 Uiso 1 1 calc R U . . .
H15B H 0.4143 0.2121 0.8233 0.190 Uiso 1 1 calc R U . . .
H15C H 0.5389 0.2004 0.7874 0.190 Uiso 1 1 calc R U . . .
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
N2 Zn1 N2 176.9(6) . 2_665
N2 Zn1 O1 106.7(3) . 2_665
N2 Zn1 O1 75.4(3) 2_665 2_665
N2 Zn1 O1 75.4(3) . .
N2 Zn1 O1 106.7(3) 2_665 .
O1 Zn1 O1 98.7(4) 2_665 .
N2 Zn1 N1 103.6(3) . 2_665
N2 Zn1 N1 74.1(3) 2_665 2_665
O1 Zn1 N1 149.1(2) 2_665 2_665
O1 Zn1 N1 95.0(3) . 2_665
N2 Zn1 N1 74.1(3) . .
N2 Zn1 N1 103.6(3) 2_665 .
O1 Zn1 N1 95.0(3) 2_665 .
O1 Zn1 N1 149.1(2) . .
N1 Zn1 N1 87.0(4) 2_665 .
C1 N1 C5 117.3(8) . .
C1 N1 Zn1 130.9(7) . .
C5 N1 Zn1 111.8(6) . .
C6 N2 N3 119.8(6) . .
C6 N2 Zn1 121.8(6) . .
N3 N2 Zn1 118.3(5) . .
C8 N3 N2 109.1(6) . .
C8 O1 Zn1 111.9(5) . .
C11 O2 C15 118.6(9) . .
N1 C1 C2 121.9(10) . .
N1 C1 H1 119.0 . .
C2 C1 H1 119.0 . .
C3 C2 C1 121.8(10) . .
C3 C2 H2 119.1 . .
C1 C2 H2 119.1 . .
C2 C3 C4 118.3(10) . .
C2 C3 H3 120.9 . .
C4 C3 H3 120.9 . .
C3 C4 C5 121.1(11) . .
C3 C4 H4 119.4 . .
C5 C4 H4 119.4 . .
N1 C5 C4 119.6(9) . .
N1 C5 C6 116.3(7) . .
C4 C5 C6 124.1(8) . .
N2 C6 C5 115.5(7) . .
N2 C6 C7 122.3(8) . .
C5 C6 C7 122.2(7) . .
C6 C7 H7A 109.5 . .
C6 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
C6 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
O1 C8 N3 125.1(8) . .
O1 C8 C9 120.2(7) . .
N3 C8 C9 114.7(7) . .
C10 C9 C14 119.9(8) . .
C10 C9 C8 119.4(8) . .
C14 C9 C8 120.6(7) . .
C9 C10 C11 120.1(9) . .
C9 C10 H10 119.9 . .
C11 C10 H10 119.9 . .
C12 C11 O2 124.1(9) . .
C12 C11 C10 120.7(9) . .
O2 C11 C10 115.2(10) . .
C11 C12 C13 118.4(9) . .
C11 C12 H12 120.8 . .
C13 C12 H12 120.8 . .
C14 C13 C12 121.7(10) . .
C14 C13 H13 119.2 . .
C12 C13 H13 119.2 . .
C13 C14 C9 119.2(9) . .
C13 C14 H14 120.4 . .
C9 C14 H14 120.4 . .
O2 C15 H15A 109.5 . .
O2 C15 H15B 109.5 . .
H15A C15 H15B 109.5 . .
O2 C15 H15C 109.5 . .
H15A C15 H15C 109.5 . .
H15B C15 H15C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 N2 2.080(6) .
Zn1 N2 2.080(6) 2_665
Zn1 O1 2.114(6) 2_665
Zn1 O1 2.114(6) .
Zn1 N1 2.297(8) 2_665
Zn1 N1 2.297(8) .
N1 C1 1.317(12) .
N1 C5 1.374(10) .
N2 C6 1.318(11) .
N2 N3 1.371(10) .
N3 C8 1.364(10) .
O1 C8 1.287(9) .
O2 C11 1.383(11) .
O2 C15 1.435(12) .
C1 C2 1.393(15) .
C1 H1 0.9300 .
C2 C3 1.316(14) .
C2 H2 0.9300 .
C3 C4 1.326(13) .
C3 H3 0.9300 .
C4 C5 1.418(13) .
C4 H4 0.9300 .
C5 C6 1.464(11) .
C6 C7 1.508(12) .
C7 H7A 0.9600 .
C7 H7B 0.9600 .
C7 H7C 0.9600 .
C8 C9 1.482(11) .
C9 C10 1.374(11) .
C9 C14 1.398(12) .
C10 C11 1.412(13) .
C10 H10 0.9300 .
C11 C12 1.376(14) .
C12 C13 1.394(15) .
C12 H12 0.9300 .
C13 C14 1.389(12) .
C13 H13 0.9300 .
C14 H14 0.9300 .
C15 H15A 0.9600 .
C15 H15B 0.9600 .
C15 H15C 0.9600 .
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
C6 N2 N3 C8 178.5(8) . . . .
Zn1 N2 N3 C8 -4.0(9) . . . .
C5 N1 C1 C2 1.4(16) . . . .
Zn1 N1 C1 C2 179.9(8) . . . .
N1 C1 C2 C3 -1.7(19) . . . .
C1 C2 C3 C4 1.3(18) . . . .
C2 C3 C4 C5 -0.8(15) . . . .
C1 N1 C5 C4 -0.8(13) . . . .
Zn1 N1 C5 C4 -179.6(7) . . . .
C1 N1 C5 C6 177.2(9) . . . .
Zn1 N1 C5 C6 -1.6(9) . . . .
C3 C4 C5 N1 0.5(14) . . . .
C3 C4 C5 C6 -177.4(8) . . . .
N3 N2 C6 C5 -175.8(7) . . . .
Zn1 N2 C6 C5 6.9(11) . . . .
N3 N2 C6 C7 2.8(13) . . . .
Zn1 N2 C6 C7 -174.6(7) . . . .
N1 C5 C6 N2 -3.0(12) . . . .
C4 C5 C6 N2 175.0(8) . . . .
N1 C5 C6 C7 178.5(8) . . . .
C4 C5 C6 C7 -3.6(13) . . . .
Zn1 O1 C8 N3 -2.8(10) . . . .
Zn1 O1 C8 C9 176.5(5) . . . .
N2 N3 C8 O1 4.5(12) . . . .
N2 N3 C8 C9 -174.9(6) . . . .
O1 C8 C9 C10 12.7(11) . . . .
N3 C8 C9 C10 -167.9(7) . . . .
O1 C8 C9 C14 -162.7(8) . . . .
N3 C8 C9 C14 16.7(11) . . . .
C14 C9 C10 C11 -0.5(12) . . . .
C8 C9 C10 C11 -175.9(8) . . . .
C15 O2 C11 C12 13.9(15) . . . .
C15 O2 C11 C10 -164.7(10) . . . .
C9 C10 C11 C12 -0.5(14) . . . .
C9 C10 C11 O2 178.2(7) . . . .
O2 C11 C12 C13 -177.4(10) . . . .
C10 C11 C12 C13 1.2(15) . . . .
C11 C12 C13 C14 -1.0(16) . . . .
C12 C13 C14 C9 0.0(15) . . . .
C10 C9 C14 C13 0.7(12) . . . .
C8 C9 C14 C13 176.1(8) . . . .
