Planar {Ni6} Cluster-Containing Polyoxometalate-based Inorganic-Organic Hybrid Compound and Its Extended Structure.
Wang, Xingquan; Liu, Shuxia; Liu, Yiwei; He, Danfeng; Li, Ning; Miao, Jun; Ji, Yujuan; Yang, Guoyu; Inorganic chemistry  (2014) 141126095850003–; doi:10.1021/ic502321v

data_4341869
_publ_section_title
;
 Planar {Ni6} Cluster-Containing Polyoxometalate-based Inorganic-Organic
 Hybrid Compound and Its Extended Structure.
;
_journal_name_full               'Inorganic chemistry'
_journal_page_first              141126095850003
_journal_paper_doi               10.1021/ic502321v
_journal_year                    2014
_chemical_formula_moiety
'C33 H94 N18 Ni15 O134 P4 W30, 2(C6 H20 N4 Ni), 8(O)'
_chemical_formula_sum            'C45 H134 N26 Ni17 O142 P4 W30'
_chemical_formula_weight         9948.56
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 120.6100(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   28.5520(17)
_cell_length_b                   27.8454(17)
_cell_length_c                   27.887(2)
_cell_measurement_temperature    296(2)
_cell_volume                     19082(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0822
_diffrn_reflns_av_sigmaI/netI    0.0907
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            47960
_diffrn_reflns_theta_full        24.70
_diffrn_reflns_theta_max         24.70
_diffrn_reflns_theta_min         2.04
_exptl_absorpt_coefficient_mu    19.768
_exptl_absorpt_correction_T_max  0.063
_exptl_absorpt_correction_T_min  0.020
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    3.463
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             17912.0
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_platon_squeeze_details
"'The free water molecules were highly disordered and could not be modeled properly, thus the SQUEEZE routine of PLATON was applied to remove the contributions to the scattering from the solvent molecules. The reported refinements are of the guest-free structures using the *.hkp files produced via the SQUEEZE routine.'"
_refine_diff_density_max         2.730
_refine_diff_density_min         -1.756
_refine_diff_density_rms         0.371
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1218
_refine_ls_number_reflns         16274
_refine_ls_number_restraints     342
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0909
_refine_ls_R_factor_gt           0.0469
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0421P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0981
_refine_ls_wR_factor_ref         0.1117
_reflns_number_gt                10562
_reflns_number_total             16274
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic502321v_si_004.cif
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4341869