Bis(guanidinium) hexahydroxooctadecaoxodisodiohexamolybdonickelate decahydrate
Bo Liu; Shi Zhou; Chuan-Bi Li; Hong-Gang Zhang; Acta Crystallographica Section E 62 (2006) m3185–m3187; doi:10.1107/S160053680604503X

data_2211415
_publ_section_title
;
 Bis(guanidinium) hexahydroxooctadecaoxodisodiohexamolybdonickelate
 decahydrate
;
_journal_coeditor_code           HB2182
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m3185
_journal_page_last               m3187
_journal_paper_doi               10.1107/S160053680604503X
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '(C H6 N3)2 [Na2 Ni (O H)6 Mo6 O18] , 10H2 O'
_chemical_formula_moiety         '2C H6 N3 + , H14 Mo6 Na2 Ni O28 2- , 6H2 O'
_chemical_formula_sum            'C2 H38 Mo6 N6 Na2 Ni O34'
_chemical_formula_weight         1370.69
_chemical_name_systematic
;Bis(guanidinium) hexahydroxooctadecaoxodisodiohexamolybdonickelate
 decahydrate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 114.918(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.2247(9)
_cell_length_b                   11.6583(4)
_cell_length_c                   13.7668(5)
_cell_measurement_reflns_used    5347
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.05
_cell_measurement_theta_min      1.80
_cell_volume                     3671.6(3)
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_collection       'SMART (Bruker, 2002)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Bruker, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker SMART APEXII CCD area-detector'
_diffrn_measurement_method       '\w and \f'
_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  0.0174
_diffrn_reflns_av_sigmaI/netI    0.0206
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9516
_diffrn_reflns_theta_full        26.01
_diffrn_reflns_theta_max         26.01
_diffrn_reflns_theta_min         2.78
_exptl_absorpt_coefficient_mu    2.622
_exptl_absorpt_correction_T_max  0.630
_exptl_absorpt_correction_T_min  0.475
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2002)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.480
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2664
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.645
_refine_diff_density_min         -0.633
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     233
_refine_ls_number_reflns         3557
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0266
_refine_ls_R_factor_gt           0.0235
_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^)+(0.0316P)^2^+13.3478P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0584
_refine_ls_wR_factor_ref         0.0597
_reflns_number_gt                3275
_reflns_number_total             3557
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb2182.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2211415
_cod_database_fobs_code          2211415