Tetrakis(2,2'-bipyridine)di-μ~3~-hydroxido-bis(μ-2-oxidobenzoato)tetracopper(II) dinitrate tetrahydrate
Feng, Miao; Gu, Chao; Mi, Huai-Feng; Hu, Tong-Liang; Acta Crystallographica Section E 67 (2011) m520–; doi:10.1107/S1600536811011433

data_2229983
_publ_section_title
;
 Tetrakis(2,2'-bipyridine)di-\m~3~-hydroxido-bis(\m-2-oxidobenzoato)tetracopper(II)
 dinitrate tetrahydrate
;
_journal_coeditor_code           GK2359
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m520
_journal_paper_doi               10.1107/S1600536811011433
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac
'[Cu4 (C7 H4 O3)2 (O H)2 (C10 H8 N2)4] (N O3)2, 4H2 O'
_chemical_formula_moiety         'C54 H42 Cu4 N8 O8 2+, 2(N O3 -), 4(H2 O)'
_chemical_formula_sum            'C54 H50 Cu4 N10 O18'
_chemical_formula_weight         1381.20
_chemical_name_systematic
;
Tetrakis(2,2'-bipyridine)di-\m~3~-hydroxido-bis(\m-2-
oxidobezoato)tetracopper(II) dinitrate tetrahydrate
;
_space_group_IT_number           2
_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                113.66(3)
_cell_angle_beta                 95.19(3)
_cell_angle_gamma                96.58(3)
_cell_formula_units_Z            1
_cell_length_a                   10.280(2)
_cell_length_b                   11.777(2)
_cell_length_c                   12.276(3)
_cell_measurement_reflns_used    3709
_cell_measurement_temperature    113.2
_cell_measurement_theta_max      27.88
_cell_measurement_theta_min      2.02
_cell_volume                     1337.0(6)
_computing_cell_refinement       'CrystalClear  (Rigaku, 2005)'
_computing_data_collection       'CrystalClear (Rigaku, 2005)'
_computing_data_reduction        'CrystalClear (Rigaku, 2005)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      113.2
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type
;
Rigaku Saturn70
;
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0487
_diffrn_reflns_av_sigmaI/netI    0.0647
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            17013
_diffrn_reflns_theta_full        27.87
_diffrn_reflns_theta_max         27.87
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    1.657
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.870
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrystalClear; Rigaku, 2005)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.715
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             704
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.809
_refine_diff_density_min         -0.547
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         6339
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0596
_refine_ls_R_factor_gt           0.0402
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0365P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0776
_refine_ls_wR_factor_ref         0.0863
_reflns_number_gt                4704
_reflns_number_total             6339
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            gk2359.cif
_cod_data_source_block           I
_cod_original_cell_volume        1337.0(5)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               2229983
_cod_database_fobs_code          2229983