Crystal structure of catena-poly[(μ2-methanolato-κ2 O:O)-(μ2-1-((2-methyl-1H-benzo[d]imidazol-1-yl)methyl)-1H-benzo[d][1,2,3]triazole-κ2N:N′)-(thiocyanato-κ1 N)copper(II)] 0.25 hydrate, C17H16CuN6OS ⋅ 0.5H2O
Zhang, Ya-Wen; Wang, Xin-Ling; Yang, Jing; Wang, Xia; Yuan, Xian-Xian; Lv, Xin-Ya; Zeitschrift für Kristallographie - New Crystal Structures 236 (2021) 721–723; doi:10.1515/ncrs-2021-0051

data_8104691
_publ_section_title
;
 Crystal structure of catena-poly[(\m2-methanolato-\k2
 O:O)-(\m2-1-((2-methyl-1H-benzo[d]imidazol-1-yl)methyl)-1H-benzo[d][1,2,3]triazole-\k2N:N&#x2032;)-(thiocyanato-\k1
 N)copper(II)] 0.25 hydrate, C17H16CuN6OS &#x22C5; 0.5H2O
;
_journal_issue                   4
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              721
_journal_page_last               723
_journal_paper_doi               10.1515/ncrs-2021-0051
_journal_volume                  236
_journal_year                    2021
_chemical_formula_moiety         '2(C34 H32 Cu2 N12 O2 S2), H2 O'
_chemical_formula_sum            'C68 H66 Cu4 N24 O5 S4'
_chemical_formula_weight         1681.84
_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   mixed
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 103.918(4)
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   10.3523(4)
_cell_length_b                   18.2609(9)
_cell_length_c                   9.9688(4)
_cell_measurement_reflns_used    2731
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      66.9500
_cell_measurement_theta_min      4.3948
_cell_volume                     1829.20(14)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      291.15
_diffrn_detector_area_resol_mean 16.2312
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -37.00   -3.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      -33.5000   37.0000  150.0000 34

  2 omega  -28.00   15.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      -33.5000  111.0000 -150.0000 43

  3 omega    2.00   38.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      -33.5000   37.0000  150.0000 36

  4 omega  -52.00  -24.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      -33.5000   57.0000  -60.0000 28

  5 omega  -59.00  -31.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      -33.5000  111.0000    0.0000 28

  6 omega  -11.00   80.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -37.0000  -60.0000 91

  7 omega   -7.00   80.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -77.0000 -120.0000 87

  8 omega   21.00   46.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   82.0000   91.0000 25

  9 omega   22.00   47.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   81.0000 -159.0000 25

 10 omega   32.00   75.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000 -125.0000 -180.0000 43

 11 omega   65.00  100.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -109.0000  173.0000 35

 12 omega   37.00   78.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -37.0000 -180.0000 41

 13 omega   41.00   92.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000  -30.0000 51

 14 omega   78.00  153.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000    0.0000 75

 15 omega   89.00  122.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   37.0000    0.0000 33

 16 omega   78.00  106.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -63.0000  -30.0000 28

 17 omega   62.00   93.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000 -180.0000 31

 18 omega   56.00  116.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000    0.0000 60

 19 omega   48.00   86.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -37.0000   30.0000 38

 20 omega   99.00  124.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   63.0000 -150.0000 25

 21 omega  148.00  175.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   63.0000 -150.0000 27

 22 omega   50.00   86.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -37.0000 -120.0000 36

 23 omega   45.00  136.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000 -180.0000 91
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.1061068000
_diffrn_orient_matrix_UB_12      -0.0608035000
_diffrn_orient_matrix_UB_13      -0.0307948000
_diffrn_orient_matrix_UB_21      -0.1026477000
_diffrn_orient_matrix_UB_22      0.0553523000
_diffrn_orient_matrix_UB_23      -0.0795846000
_diffrn_orient_matrix_UB_31      0.0413819000
_diffrn_orient_matrix_UB_32      -0.0187893000
_diffrn_orient_matrix_UB_33      -0.1343910000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0305
_diffrn_reflns_av_unetI/netI     0.0371
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            7722
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.107
_diffrn_reflns_theta_max         67.107
_diffrn_reflns_theta_min         4.400
_diffrn_source                   'Enhance (Cu) X-ray Source'
_diffrn_source_current           n/a
_diffrn_source_voltage           n/a
_exptl_absorpt_coefficient_mu    2.930
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50761
_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    1.527
_exptl_crystal_description       prism
_exptl_crystal_F_000             862
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.434
_refine_diff_density_min         -0.310
_refine_diff_density_rms         0.055
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     251
_refine_ls_number_reflns         3249
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0549
_refine_ls_R_factor_gt           0.0409
_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^)+(0.0539P)^2^+0.4157P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1020
_refine_ls_wR_factor_ref         0.1099
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2577
_reflns_number_total             3249
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2021-0051_suppl.cif
_cod_data_source_block           2
_cod_original_cell_volume        1829.21(14)
_cod_database_code               8104691
_chemical_oxdiff_formula         'C11 H10 S O2'
_shelx_estimated_absorpt_t_max   0.758
_shelx_estimated_absorpt_t_min   0.621
_reflns_odcompleteness_completeness 99.91
_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, All O(H,H) groups
2. Others
 Sof(S1A)=1-FVAR(1)
 Sof(S1)=FVAR(1)
 Fixed Sof: O2(0.25) H2A(0.25) H2B(0.25)
3.a Riding coordinates:
 O2(H2A,H2B)
3.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B)
3.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C12(H12), C13(H13), C14(H14), C15(H15)
3.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C17(H17A,H17B,H17C)
;