Hydrothermal Synthesis of a Three-Dimensional Organic−Inorganic Hybrid Network Formed by Poly(oxomolybdophosphate) Anions and Nickel Coordination Cations
Chang, Wen-Jung; Jiang, Yau-Chen; Wang, Sue-Lein; Lii, Kwang-Hwa; Inorganic Chemistry 45 (2006) 6586–6588; doi:10.1021/ic060911v

data_4332824
_publ_section_title
;
 Hydrothermal Synthesis of a Three-Dimensional Organic&#x2212;Inorganic
 Hybrid Network Formed by Poly(oxomolybdophosphate) Anions and Nickel
 Coordination Cations
;
_journal_issue                   17
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6586
_journal_page_last               6588
_journal_paper_doi               10.1021/ic060911v
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety
(4,4'-C10H10N2)[Ni(4,4'-C10H8N2)(H2O)2Ni0.5Mo6(OH)3O12(HPO4)4].2H2O
_chemical_formula_sum            'C20 H33 Mo6 N4 Ni1.5 O35 P4'
_chemical_formula_weight         1677.09
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           56
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   27.745(2)
_cell_length_b                   16.1583(12)
_cell_length_c                   22.8192(18)
_cell_measurement_temperature    293(2)
_cell_volume                     10230.1(13)
_computing_molecular_graphics    Diamond
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       'omega scan'
_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  0.0476
_diffrn_reflns_av_sigmaI/netI    0.0302
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            72023
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         1.46
_exptl_absorpt_coefficient_mu    2.187
_exptl_absorpt_correction_T_max  0.962
_exptl_absorpt_correction_T_min  0.724
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS program'
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    2.178
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             6520
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.175
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.997
_refine_diff_density_min         -0.870
_refine_diff_density_rms         0.224
_refine_ls_extinction_coef       0.00050(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     634
_refine_ls_number_reflns         12655
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_gt           0.0414
_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^)+(0.0877P)^2^+48.7145P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1498
_refine_ls_wR_factor_ref         0.1568
_reflns_number_gt                10191
_reflns_number_total             12655
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060911vsup1.cif
_cod_data_source_block           wjc346cm
_cod_original_cell_volume        10230.3(14)
_cod_original_sg_symbol_H-M      Pccn
_cod_original_formula_sum        'C20 H33 Mo6 N4 Ni1.50 O35 P4'
_cod_database_code               4332824