[2,2′-{Ethane-1,2-diylbis[(azanylylidene)methanylylidene]}bis(3-bromo-2-hydroxyphenyl)]iron(III) nitrate, C20H12Br2CuN2O2
Yang, Jiao; Xu, Jiajun; Liao, Nichan; Wu, Qiong; Zeitschrift für Kristallographie - New Crystal Structures 237 (2022) 1091–1092; doi:10.1515/ncrs-2022-0297

data_8107301
_publ_section_title
;
 [2,2&#x2032;-{Ethane-1,2-diylbis[(azanylylidene)methanylylidene]}bis(3-bromo-2-hydroxyphenyl)]iron(III)
 nitrate, C20H12Br2CuN2O2
;
_journal_issue                   6
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              1091
_journal_page_last               1092
_journal_paper_doi               10.1515/ncrs-2022-0297
_journal_volume                  237
_journal_year                    2022
_chemical_formula_moiety         'C20 H12 Br2 Cu N2 O2'
_chemical_formula_sum            'C20 H12 Br2 Cu N2 O2'
_chemical_formula_weight         535.68
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   7.7117(2)
_cell_length_b                   18.7735(4)
_cell_length_c                   24.8518(4)
_cell_measurement_reflns_used    4574
_cell_measurement_temperature    212.99(10)
_cell_measurement_theta_max      74.7470
_cell_measurement_theta_min      3.5170
_cell_volume                     3597.93(13)
_computing_cell_refinement       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      212.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.920
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w     32.00 119.00   1.00    1.30    --   48.46  62.00  93.00   87
  2  \w     93.00 169.00   1.00    5.00    --  105.98  62.00  93.00   76
  3  \w     35.00  65.00   1.00    5.00    --  105.98 -68.00 178.00   30
  4  \w     35.00 106.00   1.00    5.00    --  105.98 -94.00  80.00   71
  5  \w    -14.00  25.00   1.00    1.30    --  -48.46  19.00 -60.00   39
  6  \w    -51.00 -26.00   1.00    5.00    --  -91.75  45.00  60.00   25
  7  \w    -63.00 -37.00   1.00    5.00    --  -91.75  68.00 -48.00   26
  8  \w    -64.00 -34.00   1.00    5.00    --  -91.75  61.00 -60.00   30
  9  \w    -51.00 -19.00   1.00    5.00    --  -91.75  61.00-120.00   32
 10  \w    -81.00 -28.00   1.00    5.00    --  -91.75 125.00-150.00   53
 11  \w   -119.00 -77.00   1.00    1.30    --  -48.46-125.00 120.00   42
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1340665000
_diffrn_orient_matrix_UB_12      0.0269711000
_diffrn_orient_matrix_UB_13      0.0411926000
_diffrn_orient_matrix_UB_21      0.1284507000
_diffrn_orient_matrix_UB_22      0.0577954000
_diffrn_orient_matrix_UB_23      0.0186160000
_diffrn_orient_matrix_UB_31      -0.0735776000
_diffrn_orient_matrix_UB_32      0.0516097000
_diffrn_orient_matrix_UB_33      -0.0424597000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0449
_diffrn_reflns_av_unetI/netI     0.0474
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.920
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            11830
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.920
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.425
_diffrn_reflns_theta_min         3.557
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.077
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94505
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.119a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.978
_exptl_crystal_description       plate
_exptl_crystal_F_000             2088
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.522
_refine_diff_density_min         -0.564
_refine_diff_density_rms         0.104
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         3438
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0507
_refine_ls_R_factor_gt           0.0399
_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^)+(0.0536P)^2^+4.3308P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1073
_refine_ls_wR_factor_ref         0.1125
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2901
_reflns_number_total             3438
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2022-0297_suppl.cif
_cod_data_source_block           yj16
_cod_database_code               8107301
_chemical_oxdiff_formula         CHNO
_shelx_estimated_absorpt_t_max   0.871
_shelx_estimated_absorpt_t_min   0.719
_reflns_odcompleteness_completeness 99.13
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11), C12(H12),
 C14(H14), C17(H17), C19(H19), C20(H20)
;
_shelx_res_checksum              31419
_shelx_hkl_checksum              15900
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.190
_oxdiff_exptl_absorpt_empirical_full_min 0.784