(μ-Butane-1,2,3,4-tetracarboxylato)bis[triaqua(1,10-phenanthroline)nickel(II)] hexahydrate
Zhu, Hong-lin; Acta Crystallographica Section E 66 (2010) m1537–; doi:10.1107/S1600536810045137

data_2228267
_publ_section_title
;
 (\m-Butane-1,2,3,4-tetracarboxylato)bis[triaqua(1,10-phenanthroline)nickel(II)]
 hexahydrate
;
_journal_coeditor_code           CV2791
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1537
_journal_paper_doi               10.1107/S1600536810045137
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[Ni2 (C8 H6 O8) (C12 H8 N2)2 (H2 O)6], 6H2 O'
_chemical_formula_moiety         'C32 H34 N2 Ni2 O14, 6(H2 O)'
_chemical_formula_sum            'C32 H46 N4 Ni2 O20'
_chemical_formula_weight         924.15
_chemical_name_systematic
;
(\m-Butane-1,2,3,4-tetracarboxylato)bis[triaqua(1,10-phenanthroline)nickel(II)]
hexahydrate
;
_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                91.90(3)
_cell_angle_beta                 97.14(3)
_cell_angle_gamma                111.54(3)
_cell_formula_units_Z            1
_cell_length_a                   9.0382(18)
_cell_length_b                   9.5342(19)
_cell_length_c                   12.253(3)
_cell_measurement_reflns_used    6619
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.43
_cell_measurement_theta_min      3.06
_cell_volume                     971.0(4)
_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  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 0.945
_diffrn_measured_fraction_theta_max 0.945
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_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  0.0222
_diffrn_reflns_av_sigmaI/netI    0.0330
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7940
_diffrn_reflns_theta_full        27.43
_diffrn_reflns_theta_max         27.43
_diffrn_reflns_theta_min         3.06
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.057
_exptl_absorpt_correction_T_max  0.713
_exptl_absorpt_correction_T_min  0.641
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.580
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             482
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.743
_refine_diff_density_min         -0.481
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.165
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         4195
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.165
_refine_ls_R_factor_all          0.0477
_refine_ls_R_factor_gt           0.0343
_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^)+(0.0364P)^2^+1.1101P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0903
_refine_ls_wR_factor_ref         0.1082
_reflns_number_gt                3499
_reflns_number_total             4195
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            cv2791.cif
_cod_data_source_block           I
_cod_original_cell_volume        971.0(3)
_cod_database_code               2228267
_cod_database_fobs_code          2228267