Crystal structure of 4-bromo-N′-[(3-bromo-2-hydroxyphenyl)methylidene]benzohydrazide methanol solvate, C15H14Br2N2O3
Xu, Xindi; Ma, Xun; Huang, Meifen; Li, Tianyu; Wu, Qiong; Zeitschrift für Kristallographie - New Crystal Structures 236 (2021) 323–324; doi:10.1515/ncrs-2020-0540

data_8104819
_publ_section_title
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 Crystal structure of
 4-bromo-N&#x2032;-[(3-bromo-2-hydroxyphenyl)methylidene]benzohydrazide
 methanol solvate, C15H14Br2N2O3
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_journal_issue                   2
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              323
_journal_page_last               324
_journal_paper_doi               10.1515/ncrs-2020-0540
_journal_volume                  236
_journal_year                    2021
_chemical_formula_moiety         'C14 H10 Br2 N2 O2, C H4 O'
_chemical_formula_sum            'C15 H14 Br2 N2 O3'
_chemical_formula_weight         430.10
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_cell_angle_alpha                99.458(2)
_cell_angle_beta                 100.401(2)
_cell_angle_gamma                99.499(2)
_cell_formula_units_Z            2
_cell_length_a                   7.2748(3)
_cell_length_b                   9.0786(4)
_cell_length_c                   12.8613(5)
_cell_measurement_reflns_used    5335
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.15
_cell_measurement_theta_min      2.56
_cell_volume                     807.35(6)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0360
_diffrn_reflns_av_unetI/netI     0.0255
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15976
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.447
_diffrn_reflns_theta_min         2.321
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.033
_exptl_absorpt_correction_T_max  0.0276
_exptl_absorpt_correction_T_min  0.0085
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0988 before and 0.0469 after correction.
The Ratio of minimum to maximum transmission is 0.3080.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.769
_exptl_crystal_F_000             424
_refine_diff_density_max         0.321
_refine_diff_density_min         -0.260
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     202
_refine_ls_number_reflns         3303
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0347
_refine_ls_R_factor_gt           0.0253
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0334P)^2^+0.1877P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0639
_refine_ls_wR_factor_ref         0.0673
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2746
_reflns_number_total             3303
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2020-0540_suppl.cif
_cod_data_source_block           X3
_cod_database_code               8104819
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C13(H13), N2(H2A), C8(H8), C2(H2B), C5(H5), C14(H14), C3(H3), C6(H6), C12(H12)
2.b Idealised Me refined as rotating group:
 C3AA(H3AA,H3AB,H3AC)
2.c Idealised tetrahedral OH refined as rotating group:
 O2(H2), O3(H3A)
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_olex2_submission_special_instructions 'No special instructions were received'