Cobalt(II) chloride complexes with 1,1'-dimethyl-4,4'-bipyrazole featuring first- and second-sphere coordination of the ligand
Domasevitch, Konstantin V.; Acta Crystallographica Section C 70 (2014) 272–276; doi:10.1107/S2053229614002046

data_2019486
_publ_section_title
;
 Cobalt(II) chloride complexes with 1,1'-dimethyl-4,4'-bipyrazole
 featuring first- and second-sphere coordination of the ligand
;
_journal_coeditor_code           OV3046
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              272
_journal_page_last               276
_journal_paper_doi               10.1107/S2053229614002046
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac
'[Co (C8 H10 N4)2 (H2 O)4] Cl2, 2C8 H10 N4, 2H2 O'
_chemical_formula_moiety
'C16 H28 Co N8 O4 2+, 2(Cl -), 2(C8 H10 N4), 2(H2 O)'
_chemical_formula_sum            'C32 H52 Cl2 Co N16 O6'
_chemical_formula_weight         886.73
_chemical_name_systematic
;
Tetraaquabis(1,1'-dimethyl-4,4'-bipyrazole-\k<i>N</i>^2^)cobalt(II)
dichloride--1,1'-dimethyl-4,4'-bipyrazole--water (1/2/2)
;
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                63.071(2)
_cell_angle_beta                 83.665(3)
_cell_angle_gamma                72.592(2)
_cell_formula_units_Z            1
_cell_length_a                   9.2087(8)
_cell_length_b                   11.1415(10)
_cell_length_c                   12.2523(10)
_cell_measurement_reflns_used    10321
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      27.68
_cell_measurement_theta_min      2.32
_cell_volume                     1068.96(16)
_computing_cell_refinement       'SAINT-NT (Bruker, 1999)'
_computing_data_collection       'SMART-NT (Bruker, 1998)'
_computing_data_reduction        'SAINT-NT (Bruker, 1999)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'WinGX (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Siemens SMART CCD area-detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0361
_diffrn_reflns_av_sigmaI/netI    0.0320
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10321
_diffrn_reflns_theta_full        27.68
_diffrn_reflns_theta_max         27.68
_diffrn_reflns_theta_min         2.32
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.587
_exptl_absorpt_correction_T_max  0.9609
_exptl_absorpt_correction_T_min  0.9340
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.377
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             465
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.566
_refine_diff_density_min         -0.707
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     287
_refine_ls_number_reflns         4907
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0397
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0747P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1020
_refine_ls_wR_factor_ref         0.1043
_reflns_number_gt                4058
_reflns_number_total             4907
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ov3046sup1.cif
_cod_data_source_block           2
_cod_database_code               2019486
_cod_database_fobs_code          2019486