Crystal structure of diaqua-bis(5′-(pyridin-1-ium-4-yl)-1H-[3,3′-bi(1,2,4-triazol)]-2′-ide-κ2 N,N′)cobalt(II) — bis(5-(pyridin-4-yl-κN)-1H,1′H-3,3′-bi(1,2,4-triazole))octamolybdate – water (2/1/8), C27H33CoMo4N21O19
Huang, Shan-Xiu; Zhang, Lan-He; Ma, Ming-Jie; Dan, Zhao; Zeitschrift für Kristallographie - New Crystal Structures 232 (2017) 769–771; doi:10.1515/ncrs-2017-0026

data_8106672
_publ_section_title
;
 Crystal structure of
 diaqua-bis(5&#x2032;-(pyridin-1-ium-4-yl)-1H-[3,3&#x2032;-bi(1,2,4-triazol)]-2&#x2032;-ide-\k2
 N,N&#x2032;)cobalt(II) ---
 bis(5-(pyridin-4-yl-\kN)-1H,1&#x2032;H-3,3&#x2032;-bi(1,2,4-triazole))octamolybdate
 -- water (2/1/8), C27H33CoMo4N21O19
;
_journal_issue                   5
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              769
_journal_page_last               771
_journal_paper_doi               10.1515/ncrs-2017-0026
_journal_volume                  232
_journal_year                    2017
_chemical_formula_sum            'C27 H33 Co Mo4 N21 O19'
_chemical_formula_weight         1398.43
_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   mixed
_cell_angle_alpha                103.8000(10)
_cell_angle_beta                 98.4270(10)
_cell_angle_gamma                110.2780(10)
_cell_formula_units_Z            2
_cell_length_a                   12.1200(6)
_cell_length_b                   13.0412(6)
_cell_length_c                   15.7235(7)
_cell_measurement_reflns_used    549
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.86
_cell_measurement_theta_min      2.17
_cell_volume                     2191.08(18)
_computing_cell_refinement       'SAINT (Bruker, 2014) [1]'
_computing_data_collection       'SMART Apex2 (Bruker, 2014) [1]'
_computing_data_reduction        'SAINT (Bruker, 2014) [1]'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2014) [1]'
_computing_publication_material  'SHELXTL (Sheldrick, 2014) [1]'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014) [2]'
_computing_structure_solution    'SHELXS (Sheldrick, 2014) [2]'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 83.33
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker Smart Apex2 CCD area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_av_unetI/netI     0.0437
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            27388
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.276
_diffrn_reflns_theta_min         1.851
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.586
_exptl_absorpt_correction_T_max  0.940
_exptl_absorpt_correction_T_min  0.857
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.120
_exptl_crystal_description       prism
_exptl_crystal_F_000             1378
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.525
_refine_diff_density_min         -0.581
_refine_diff_density_rms         0.096
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     649
_refine_ls_number_reflns         10748
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0445
_refine_ls_R_factor_gt           0.0302
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0309P)^2^+0.5355P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0672
_refine_ls_wR_factor_ref         0.0726
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8584
_reflns_number_total             10748
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2017-0026_suppl.cif
_cod_data_source_block           a
_cod_database_code               8106672
_shelx_estimated_absorpt_t_min   0.851
_shelx_estimated_absorpt_t_max   0.946
_shelx_res_checksum              81807
_shelx_hkl_checksum              96053
_publcif_info_exptl_table_max_cols 4
_publcif_info_exptl_table_use_headnotes n