Crystal structure of N,N′-bis(4-bromosalicylidene) ethylene-1,2-diaminopropan, C34H32Br4N4O4
Li, Tianyu; Xu, Xindi; Wang, Man; Wang, Xia; Wu, Qiong; Zeitschrift für Kristallographie - New Crystal Structures 236 (2021) 319–321; doi:10.1515/ncrs-2020-0546

data_8104818
_publ_section_title
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 Crystal structure of N,N&#x2032;-bis(4-bromosalicylidene)
 ethylene-1,2-diaminopropan, C34H32Br4N4O4
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_journal_issue                   2
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              319
_journal_page_last               321
_journal_paper_doi               10.1515/ncrs-2020-0546
_journal_volume                  236
_journal_year                    2021
_chemical_formula_moiety         'C17 H16 Br2 N2 O2'
_chemical_formula_sum            'C17 H16 Br2 N2 O2'
_chemical_formula_weight         440.13
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 92.7260(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.3126(5)
_cell_length_b                   6.9654(2)
_cell_length_c                   29.3000(10)
_cell_measurement_reflns_used    7377
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.93
_cell_measurement_theta_min      3.18
_cell_volume                     3325.41(18)
_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)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0752
_diffrn_reflns_av_unetI/netI     0.0372
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            54956
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.428
_diffrn_reflns_theta_min         2.382
_exptl_absorpt_coefficient_mu    4.886
_exptl_absorpt_correction_T_max  0.0276
_exptl_absorpt_correction_T_min  0.0091
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
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SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0988 before and 0.0655 after correction.
The Ratio of minimum to maximum transmission is 0.3297.
The \l/2 correction factor is Not present.
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_exptl_crystal_density_diffrn    1.758
_exptl_crystal_density_meas      .
_exptl_crystal_description       block
_exptl_crystal_F_000             1744
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.619
_refine_diff_density_min         -0.292
_refine_diff_density_rms         0.070
_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     421
_refine_ls_number_reflns         6827
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0615
_refine_ls_R_factor_gt           0.0349
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0260P)^2^+2.4493P]
 where P=(Fo^2^+2Fc^2^)/3
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_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0701
_refine_ls_wR_factor_ref         0.0799
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4981
_reflns_number_total             6827
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2020-0546_suppl.cif
_cod_data_source_block           sk12
_cod_depositor_comments
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2025-04-22
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
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_cod_original_formula_sum            'C34 H32 Br4 N4 O4'
_cod_original_formula_weight         880.27
_cod_original_formula_moiety         '2(C17 H16 Br2 N2 O2)'
_cod_original_formula_units_Z            4
_cod_database_code               8104818
_shelx_estimated_absorpt_t_max   0.473
_shelx_estimated_absorpt_t_min   0.413
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C9(H9), C26(H26)
2.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C25(H25A,H25B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2A), C3(H3), C5(H5), C7(H7), C11(H11), C14(H14), C16(H16), C17(H17),
 C20(H20), C22(H22), C23(H23), C24(H24), C28(H28), C30(H30), C31(H31), C33(H33)
2.d Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C27(H27A,H27B,H27C)
2.e Idealised tetrahedral OH refined as rotating group:
 O1(H1), O2(H2), O3(H3A), O4(H4)
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