Crystal structure of dichlorido bis[1-((2,4-dimethyl-1H-imidazol-1-yl)methyl)-1H-benzo[d][1,2,3]triazole-κN]cadmium(II), Cd(C12H13N5)2Cl2
Wang, Xia; Ling, Ning; Yang, Jing; Song, Ning; Zeitschrift für Kristallographie - New Crystal Structures 234 (2019) 321–323; doi:10.1515/ncrs-2018-0370

data_8105630
_publ_section_title
;
 Crystal structure of dichlorido
 bis[1-((2,4-dimethyl-1H-imidazol-1-yl)methyl)-1H-benzo[d][1,2,3]triazole-\kN]cadmium(II),
 Cd(C12H13N5)2Cl2
;
_journal_issue                   2
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              321
_journal_page_last               323
_journal_paper_doi               10.1515/ncrs-2018-0370
_journal_volume                  234
_journal_year                    2019
_chemical_formula_moiety         'C24 H26 Cd Cl2 N10'
_chemical_formula_sum            'C24 H26 Cd Cl2 N10'
_chemical_formula_weight         637.85
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 94.184(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.3081(2)
_cell_length_b                   11.7526(3)
_cell_length_c                   24.9876(6)
_cell_measurement_reflns_used    4200
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.0150
_cell_measurement_theta_min      3.8320
_cell_volume                     2726.22(11)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41k (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41k (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41k (Rigaku OD, 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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2312
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.871
_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     18.00  44.00   1.00    1.25    --   18.07  57.00-150.00   26
  2  \w    -46.00  35.00   1.00    1.25    --   18.07 -57.00-150.00   81
  3  \w     50.00  82.00   1.00    1.25    --   18.07  37.00  30.00   32
  4  \w      7.00  51.00   1.00    1.25    --   18.07  57.00-180.00   44
  5  \w     34.00  84.00   1.00    1.25    --   18.07-178.00-180.00   50
  6  \w    -18.00   8.00   1.00    1.25    --  -15.18 -99.00  60.00   26
  7  \w      9.00  70.00   1.00    1.25    --   18.07  57.00-120.00   61
  8  \w     16.00  80.00   1.00    1.25    --   18.07  57.00  90.00   64
  9  \w    -21.00  20.00   1.00    1.25    --   18.07 -99.00 -30.00   41
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0572482000
_diffrn_orient_matrix_UB_12      -0.0085126000
_diffrn_orient_matrix_UB_13      -0.0199163000
_diffrn_orient_matrix_UB_21      -0.0419869000
_diffrn_orient_matrix_UB_22      -0.0249326000
_diffrn_orient_matrix_UB_23      0.0194765000
_diffrn_orient_matrix_UB_31      -0.0282205000
_diffrn_orient_matrix_UB_32      0.0543144000
_diffrn_orient_matrix_UB_33      0.0058193000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_av_unetI/netI     0.0666
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.871
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            12268
_diffrn_reflns_point_group_measured_fraction_full 0.942
_diffrn_reflns_point_group_measured_fraction_max 0.772
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.426
_diffrn_reflns_theta_min         3.319
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.031
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98454
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41k (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.554
_exptl_crystal_description       prism
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.493
_refine_diff_density_min         -0.382
_refine_diff_density_rms         0.073
_refine_ls_abs_structure_details
;
 Flack x determined using 1766 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.073(19)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     338
_refine_ls_number_reflns         5833
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0412
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0101P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0524
_refine_ls_wR_factor_ref         0.0581
_reflns_Friedel_coverage         0.771
_reflns_Friedel_fraction_full    0.887
_reflns_Friedel_fraction_max     0.673
_reflns_number_gt                4973
_reflns_number_total             5833
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2018-0370_suppl.cif
_cod_data_source_block           2018x3
_cod_original_cell_volume        2726.23(11)
_cod_database_code               8105630
_chemical_oxdiff_formula         C22H20N2O8Cd1
_chemical_oxdiff_usercomment     1
_shelx_estimated_absorpt_t_max   0.878
_shelx_estimated_absorpt_t_min   0.852
_reflns_odcompleteness_completeness 99.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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:
 C7(H7A,H7B), C19(H19A,H19B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C9(H9), C13(H13), C14(H14), C15(H15),
 C16(H16), C21(H21)
2.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C)
;