Crystal structure of catena-poly[(μ2-2,5-di(pyridin-3-yl)-1,3,4-thiadiazole-κ2 N:N′)-bis(2,5-di(pyridin-3-yl)-1,3,4-thiadiazole-κ1 N)-bis(thiocyanato-κ1 N)cobalt(II)], C38H24CoN14S5
Sun, Xiao-Juan; Zeitschrift für Kristallographie - New Crystal Structures 234 (2018) 39–40; doi:10.1515/ncrs-2018-0118

data_8105534
_publ_section_title
;
 Crystal structure of
 catena-poly[(\m2-2,5-di(pyridin-3-yl)-1,3,4-thiadiazole-\k2
 N:N&#x2032;)-bis(2,5-di(pyridin-3-yl)-1,3,4-thiadiazole-\k1
 N)-bis(thiocyanato-\k1 N)cobalt(II)], C38H24CoN14S5
;
_journal_issue                   1
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              39
_journal_page_last               40
_journal_paper_doi               10.1515/ncrs-2018-0118
_journal_volume                  234
_journal_year                    2018
_chemical_formula_moiety         'C38 H24 Co N14 S5'
_chemical_formula_sum            'C38 H24 Co N14 S5'
_chemical_formula_weight         895.94
_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     dual
_cell_angle_alpha                81.039(4)
_cell_angle_beta                 82.393(4)
_cell_angle_gamma                66.803(4)
_cell_formula_units_Z            2
_cell_length_a                   10.6306(6)
_cell_length_b                   13.1604(5)
_cell_length_c                   15.1858(7)
_cell_measurement_reflns_used    13322
_cell_measurement_temperature    291.6(7)
_cell_measurement_theta_max      25.0730
_cell_measurement_theta_min      3.5620
_cell_volume                     1923.04(17)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41r (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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      291.6(7)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0584
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.968
_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    -81.00  20.00   1.00    5.00    --   -9.62 -19.00 -30.00  101
  2  \w     -6.00  78.00   1.00    5.00    --   10.64  57.00 -90.00   84
  3  \w     -6.00  78.00   1.00    5.00    --   10.64  57.00   0.00   84
  4  \w    -20.00  50.00   1.00    5.00    --   10.64 -99.00-180.00   70
  5  \w    -20.00  50.00   1.00    5.00    --   10.64 -99.00 -30.00   70
  6  \w    -20.00  50.00   1.00    5.00    --   10.64 -99.00-120.00   70
  7  \w    -20.00  50.00   1.00    5.00    --   10.64 -99.00  90.00   70
  8  \w     -8.00  80.00   1.00    5.00    --   10.64  38.00 150.00   88
  9  \w     -6.00  78.00   1.00    5.00    --   10.64  57.00-150.00   84
 10  \w    -20.00  29.00   1.00    5.00    --   -9.62 -99.00-180.00   49
 11  \w    -20.00  50.00   1.00    5.00    --   10.64 -99.00 120.00   70
 12  \w    -20.00  50.00   1.00    5.00    --   10.64 -99.00  30.00   70
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0374953000
_diffrn_orient_matrix_UB_12      0.0583331000
_diffrn_orient_matrix_UB_13      -0.0057397000
_diffrn_orient_matrix_UB_21      0.0357270000
_diffrn_orient_matrix_UB_22      0.0035357000
_diffrn_orient_matrix_UB_23      -0.0425271000
_diffrn_orient_matrix_UB_31      -0.0511820000
_diffrn_orient_matrix_UB_32      -0.0082547000
_diffrn_orient_matrix_UB_33      -0.0202028000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0387
_diffrn_reflns_av_unetI/netI     0.0350
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            35727
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.496
_diffrn_reflns_theta_min         3.290
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.769
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87910
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41r (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.547
_exptl_crystal_description       block
_exptl_crystal_F_000             914
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.588
_refine_diff_density_min         -0.498
_refine_diff_density_rms         0.050
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     523
_refine_ls_number_reflns         6923
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0529
_refine_ls_R_factor_gt           0.0420
_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^)+(0.0300P)^2^+1.2870P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0838
_refine_ls_wR_factor_ref         0.0882
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5886
_reflns_number_total             6923
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2018-0118_suppl.cif
_cod_data_source_block           1
_cod_database_code               8105534
_chemical_oxdiff_usercomment     'C1 H1 N1 O1 P1 Cu1'
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     23.21
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5), C8(H8), C10(H10), C11(H11), C12(H12),
 C13(H13), C14(H14), C15(H15), C17(H17), C20(H20), C22(H22), C23(H23), C24(H24),
  C25(H25), C26(H26), C27(H27), C29(H29), C32(H32), C34(H34), C35(H35), C36(H36)
;