Crystal structure of poly[dibromido-bis(μ2-1,6-di(1H-imidazol-1-yl)hexane-κ2 N:N′)cadmium(II)], C24H36Br2N8Cd
Guo, Jin-Bo; Li, Guan-Feng; Zeitschrift für Kristallographie - New Crystal Structures 235 (2020) 1155–1156; doi:10.1515/ncrs-2020-0217

data_8105406
_publ_section_title
;
 Crystal structure of
 poly[dibromido-bis(\m2-1,6-di(1H-imidazol-1-yl)hexane-\k2
 N:N&#x2032;)cadmium(II)], C24H36Br2N8Cd
;
_journal_issue                   5
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              1155
_journal_page_last               1156
_journal_paper_doi               10.1515/ncrs-2020-0217
_journal_volume                  235
_journal_year                    2020
_chemical_formula_moiety         '0.5(C48 H72 Br4 Cd2 N16)'
_chemical_formula_sum            'C24 H36 Br2 Cd N8'
_chemical_formula_weight         708.83
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 100.529(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.6915(4)
_cell_length_b                   7.6614(2)
_cell_length_c                   19.0851(8)
_cell_measurement_reflns_used    9186
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.0900
_cell_measurement_theta_min      3.7810
_cell_volume                     1393.22(9)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0584
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -68.00  -3.00   1.00    1.00    --  -13.96 126.00 -95.00   65
  2  \w    -20.00  25.00   1.00    1.00    --  -13.96 -99.00 -30.00   45
  3  \w    -83.00   5.00   1.00    1.00    --  -13.96 -38.00-120.00   88
  4  \w    -66.00   1.00   1.00    1.00    --  -13.96 122.00  51.77   67
  5  \w    -41.00  54.00   1.00    1.00    --  -13.96  77.00 -60.00   95
  6  \w    -82.00  13.00   1.00    1.00    --  -13.96 -77.00-180.00   95
  7  \w    -52.00  32.00   1.00    1.00    --   14.89 -57.00  30.00   84
  8  \w     -4.00  84.00   1.00    1.00    --   14.89  38.00 150.00   88
  9  \w    -20.00  54.00   1.00    1.00    --   14.89 -99.00-120.00   74
 10  \w    -54.00  84.00   1.00    1.00    --   14.89   0.00 120.00  138
 11  \w    -20.00  25.00   1.00    1.00    --  -13.96 -99.00  30.00   45
 12  \w    -20.00  25.00   1.00    1.00    --  -13.96 -99.00 120.00   45
 13  \w    -65.00   2.00   1.00    1.00    --  -13.96 120.00 -17.31   67
 14  \w     35.00  66.00   1.00    1.00    --   14.89 178.00   0.00   31
 15  \w      3.00  35.00   1.00    1.00    --   14.89-126.00-171.00   32
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0406772000
_diffrn_orient_matrix_UB_12      -0.0168156000
_diffrn_orient_matrix_UB_13      -0.0265954000
_diffrn_orient_matrix_UB_21      -0.0604750000
_diffrn_orient_matrix_UB_22      0.0113340000
_diffrn_orient_matrix_UB_23      -0.0268031000
_diffrn_orient_matrix_UB_31      0.0151568000
_diffrn_orient_matrix_UB_32      0.0903254000
_diffrn_orient_matrix_UB_33      -0.0016027000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0844
_diffrn_reflns_av_unetI/netI     0.0385
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            29900
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         3.41
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.680
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.33229
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.690
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             708
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.26
_refine_diff_density_max         1.214
_refine_diff_density_min         -1.448
_refine_diff_density_rms         0.163
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.191
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     160
_refine_ls_number_reflns         2585
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.191
_refine_ls_R_factor_all          0.0801
_refine_ls_R_factor_gt           0.0744
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0599P)^2^+15.7231P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1789
_refine_ls_wR_factor_ref         0.1823
_reflns_number_gt                2356
_reflns_number_total             2585
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            suppl_ncrs-2020-0217_suppl.cif
_cod_data_source_block           194
_cod_original_cell_volume        1393.21(9)
_cod_database_code               8105406
_chemical_oxdiff_formula         'c h n o zn'
_reflns_odcompleteness_completeness 99.64
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C10(H10), C11(H11), C12(H12)
;
_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 1.934
_oxdiff_exptl_absorpt_empirical_full_min 0.630