Crystal structure of dimethanolato-k2 O:O-bis(1-((2-methyl-1H-benzo[d]imidazol-1-yl)methyl)-1H-benzo[d][1,2,3]triazole-κN)-bis(thiocyanato-κN)dicopper(II), C34H32Cu2N12O2S2
Fang, Xiang; Yang, Jing; Zhang, Ya-Wen; Lv, Xin-Ya; Wang, Xia; Song, Ning; Zeitschrift für Kristallographie - New Crystal Structures 236 (2021) 713–715; doi:10.1515/ncrs-2021-0045

data_8104688
_publ_section_title
;
 Crystal structure of dimethanolato-k2
 O:O-bis(1-((2-methyl-1H-benzo[d]imidazol-1-yl)methyl)-1H-benzo[d][1,2,3]triazole-\kN)-bis(thiocyanato-\kN)dicopper(II),
 C34H32Cu2N12O2S2
;
_journal_issue                   4
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              713
_journal_page_last               715
_journal_paper_doi               10.1515/ncrs-2021-0045
_journal_volume                  236
_journal_year                    2021
_chemical_formula_moiety         'C34 H32 Cu2 N12 O2 S2'
_chemical_formula_sum            'C34 H32 Cu2 N12 O2 S2'
_chemical_formula_weight         831.91
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_cell_angle_alpha                71.544(8)
_cell_angle_beta                 79.322(8)
_cell_angle_gamma                83.734(8)
_cell_formula_units_Z            1
_cell_length_a                   7.7970(7)
_cell_length_b                   9.6110(9)
_cell_length_c                   12.7629(12)
_cell_measurement_reflns_used    3055
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      66.9023
_cell_measurement_theta_min      3.6902
_cell_volume                     890.20(15)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      291.15
_diffrn_detector_area_resol_mean 16.2312
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega -102.00  -13.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -33.5000  -37.0000   30.0000 89

  2 omega  -94.00  -56.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -33.5000  178.0000  150.0000 38

  3 omega  -50.00   28.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -33.5000   25.0000 -150.0000 78

  4 omega  -18.00   87.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -19.0000 -120.0000 105

  5 omega   36.00   92.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   57.0000 -150.0000 56

  6 omega   25.00   80.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000   30.0000 55

  7 omega   86.00  124.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000   30.0000 38

  8 omega   17.00   65.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -57.0000   60.0000 48

  9 omega   41.00   68.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   57.0000 -180.0000 27

 10 omega   20.00  108.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000 -125.0000  -30.0000 88

 11 omega  129.00  154.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   63.0000  -60.0000 25

 12 omega   36.00   94.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000   30.0000 58

 13 omega   60.00   92.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -37.0000  -90.0000 32

 14 omega   36.00  113.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000    0.0000 77

 15 omega   56.00   85.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -37.0000  -30.0000 29

 16 omega  102.00  175.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000  150.0000 73

 17 omega   36.00  116.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000 -180.0000 80

 18 omega   92.00  120.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -63.0000  -30.0000 28

 19 omega   43.00   70.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -63.0000  -30.0000 27

 20 omega   87.00  169.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   50.0000 -150.0000 82

 21 omega   46.00   90.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -37.0000 -150.0000 44

 22 omega   43.00   74.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -37.0000  150.0000 31

 23 omega   46.00   89.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -50.0000  120.0000 43

 24 omega   49.00  138.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000 -150.0000 89

 25 omega   76.00  173.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   25.0000  -30.0000 97

 26 omega   84.00  145.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  178.0000 -150.0000 61

 27 omega   35.00   81.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000 -180.0000 46

 28 omega  -56.00   34.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -33.5000   63.0000   60.0000 90

 29 omega -104.00   -3.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -33.5000  -77.0000  150.0000 101

 30 omega -101.00  -11.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -33.5000  -63.0000  -90.0000 90
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0820403000
_diffrn_orient_matrix_UB_12      0.0274799000
_diffrn_orient_matrix_UB_13      -0.1061851000
_diffrn_orient_matrix_UB_21      -0.1587848000
_diffrn_orient_matrix_UB_22      0.0823001000
_diffrn_orient_matrix_UB_23      0.0496805000
_diffrn_orient_matrix_UB_31      0.0927517000
_diffrn_orient_matrix_UB_32      0.1452960000
_diffrn_orient_matrix_UB_33      -0.0536090000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0284
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6384
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.342
_diffrn_reflns_theta_max         67.342
_diffrn_reflns_theta_min         3.699
_diffrn_source                   'Enhance (Cu) X-ray Source'
_diffrn_source_current           n/a
_diffrn_source_voltage           n/a
_exptl_absorpt_coefficient_mu    2.993
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73367
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.552
_exptl_crystal_description       prism
_exptl_crystal_F_000             426
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.753
_refine_diff_density_min         -0.401
_refine_diff_density_rms         0.101
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     238
_refine_ls_number_reflns         6384
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0743
_refine_ls_R_factor_gt           0.0634
_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^)+(0.1381P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1730
_refine_ls_wR_factor_ref         0.1827
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5176
_reflns_number_total             6384
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2021-0045_suppl.cif
_cod_data_source_block           2
_cod_original_cell_volume        890.21(15)
_cod_database_code               8104688
_chemical_oxdiff_formula         'C11 H10 S O2'
_shelx_estimated_absorpt_t_max   0.646
_shelx_estimated_absorpt_t_min   0.586
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.6002(17)
 0.3998(17)
2. 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
3.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C12(H12), C13(H13), C14(H14), C15(H15)
3.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C17(H17A,H17B,H17C)
;