A two-dimensional hydrogen-bonded water layer in the structure of a cobalt(III) cubane complex
Qi, Ji; Zhai, Xiang-Sheng; Zhu, Hong-Lin; Lin, Jian-Li; Acta Crystallographica Section C 70 (2014) 198–201; doi:10.1107/S2053229614001107

data_2019401
_publ_section_title
;
 A two-dimensional hydrogen-bonded water layer in the structure of a
 cobalt(III) cubane complex
;
_journal_coeditor_code           BG3165
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              198
_journal_page_last               201
_journal_paper_doi               10.1107/S2053229614001107
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          '[Co4 (C O3)2 O4 (C10 H8 N2)4] , 15H2 O'
_chemical_formula_moiety         'C42 H32 Co4 N8 O10, 15(H2 O1)'
_chemical_formula_sum            'C42 H62 Co4 N8 O25'
_chemical_formula_weight         1314.71
_chemical_name_systematic
'Tetrakis(2,2'-bipyridine-\k^2^<i>N</i>,<i>N</i>')di-\m~2~-carbonato-\k^4^<i>O</i>:<i>O</i>'-tetra-\m~3~-oxido-tetracobalt(III) pentadecahydrate'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   30.712(6)
_cell_length_b                   16.820(3)
_cell_length_c                   10.588(2)
_cell_measurement_reflns_used    31250
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.02
_cell_volume                     5469.5(18)
_computing_cell_refinement       'RAPID-AUTO (Rigaku, 1998)'
_computing_data_collection       'RAPID-AUTO (Rigaku, 1998)'
_computing_data_reduction        'CrystalStructure (Rigaku/MSC, 2004)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0770
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            49124
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         3.021
_exptl_absorpt_coefficient_mu    1.282
_exptl_absorpt_correction_T_max  0.902
_exptl_absorpt_correction_T_min  0.742
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.597
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2712
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.688
_refine_diff_density_min         -0.406
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     435
_refine_ls_number_reflns         6455
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      0.984
_refine_ls_R_factor_all          0.0677
_refine_ls_R_factor_gt           0.0424
_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^)+(0.0605P)^2^+5.6408P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1061
_refine_ls_wR_factor_ref         0.1188
_reflns_number_gt                4752
_reflns_number_total             6456
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bg3165sup1.cf
_cod_data_source_block           I
_cod_original_cell_volume        5469.5(19)
_cod_database_code               2019401
_cod_database_fobs_code          2019401
_shelx_hkl_checksum              80613
_shelx_res_checksum              53993
_shelxl_version_number           .2013