{6,6′-((1E,1′E)-((2,2-dimethylpropane-1,3-diyl)bis(azaneylylidene))bis(methaneylylidene))bis(2-bromo-4-chlorophenolate)-κ4N,N′,O,O′}copper(II), C19H16Br2Cl2CuN2O2
Wu, Qiong; Yu, Guojun; Yang, Jiao; Yang, Qiuling; Zeitschrift für Kristallographie - New Crystal Structures 237 (2022) 1101–1103; doi:10.1515/ncrs-2022-0296

data_8107304
_publ_section_title
;
 {6,6&#x2032;-((1E,1&#x2032;E)-((2,2-dimethylpropane-1,3-diyl)bis(azaneylylidene))bis(methaneylylidene))bis(2-bromo-4-chlorophenolate)-\k4N,N&#x2032;,O,O&#x2032;}copper(II),
 C19H16Br2Cl2CuN2O2
;
_journal_issue                   6
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              1101
_journal_page_last               1103
_journal_paper_doi               10.1515/ncrs-2022-0296
_journal_volume                  237
_journal_year                    2022
_chemical_formula_moiety         'C19 H16 Br2 Cl2 Cu N2 O2'
_chemical_formula_sum            'C19 H16 Br2 Cl2 Cu N2 O2'
_chemical_formula_weight         598.60
_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
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 97.1610(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.4679(2)
_cell_length_b                   8.61760(10)
_cell_length_c                   19.7854(3)
_cell_measurement_reflns_used    7535
_cell_measurement_temperature    212.99(10)
_cell_measurement_theta_max      75.7450
_cell_measurement_theta_min      3.9430
_cell_volume                     2109.23(5)
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_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 0.990
_diffrn_measured_fraction_theta_max 0.939
_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     92.00 178.00   1.00    0.80    --  105.98  54.00 153.00   86
  2  \w     93.00 177.00   1.00    0.80    --  105.98  30.00  90.00   84
  3  \w     56.00 121.00   1.00    0.20    --   48.46  54.00 153.00   65
  4  \w     97.00 174.00   1.00    0.80    --  105.98 125.00   0.00   77
  5  \w    -19.00  46.00   1.00    0.20    --   48.46 -54.00   9.00   65
  6  \w     37.00  69.00   1.00    0.80    --  105.98 -61.00  90.00   32
  7  \w     33.00 104.00   1.00    0.80    --  105.98 -77.00  30.00   71
  8  \w     34.00  60.00   1.00    0.80    --  105.98 -54.00   9.00   26
  9  \w     34.00 103.00   1.00    0.80    --  105.98 -77.00 -60.00   69
 10  \w    -23.00  27.00   1.00    0.20    --  -48.46  19.00 -90.00   50
 11  \w    -69.00 -19.00   1.00    0.80    --  -91.75  61.00-150.00   50
 12  \w    -54.00  24.00   1.00    0.20    --  -48.46  54.00 153.00   78
 13  \w    -62.00 -37.00   1.00    0.80    --  -91.75  54.00 153.00   25
 14  \w   -119.00 -74.00   1.00    0.20    --  -48.46 -54.00   9.00   45
 15  \w   -144.00-119.00   1.00    0.80    --  -91.75 -54.00   9.00   25
 16  \w   -156.00 -79.00   1.00    0.80    --  -91.75 -45.00 -90.00   77
;
_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      0.1216274000
_diffrn_orient_matrix_UB_12      0.0172155000
_diffrn_orient_matrix_UB_13      0.0245311000
_diffrn_orient_matrix_UB_21      -0.0258752000
_diffrn_orient_matrix_UB_22      0.1151803000
_diffrn_orient_matrix_UB_23      0.0553204000
_diffrn_orient_matrix_UB_31      -0.0064959000
_diffrn_orient_matrix_UB_32      -0.1356829000
_diffrn_orient_matrix_UB_33      0.0499651000
_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  0.0422
_diffrn_reflns_av_unetI/netI     0.0420
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.939
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            13085
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.939
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.948
_diffrn_reflns_theta_min         3.979
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.386
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65752
_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            'clear greenish green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.885
_exptl_crystal_description       block
_exptl_crystal_F_000             1172
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.518
_refine_diff_density_min         -0.494
_refine_diff_density_rms         0.084
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         4118
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0383
_refine_ls_R_factor_gt           0.0325
_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^)+(0.0328P)^2^+1.5977P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0832
_refine_ls_wR_factor_ref         0.0865
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3541
_reflns_number_total             4118
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2022-0296_suppl.cif
_cod_data_source_block           yj14
_cod_database_code               8107304
_chemical_oxdiff_formula         CHON
_shelx_estimated_absorpt_t_max   0.850
_shelx_estimated_absorpt_t_min   0.591
_reflns_odcompleteness_completeness 99.06
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
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
2.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C10(H10A,H10B)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C7(H7), C11(H11), C15(H15), C17(H17)
2.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C)
;
_shelx_res_checksum              28021
_shelx_hkl_checksum              72916
_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 1.739
_oxdiff_exptl_absorpt_empirical_full_min 0.753