First Three-Dimensional Inorganic-Organic Hybrid Material Constructed From an "Inverted Keggin" Polyoxometalate and a Copper(I)-Organic Complex
Bo Liu; Zhen-Tao Yu; Jin Yang; Wu Hua; Ying-Ying Liu; Jian-Fang Ma; Inorganic Chemistry 50 (2011) 8967–8972; doi:10.1021/ic201135g

data_4326244
_publ_contact_author_address
;
Key Lab of Polyoxometalate Science
Department of Chemistry
Northeast Normal University
Changchun 130024
P.R.China
;
_publ_contact_author_email       jianfangma@yahoo.com.cn
_publ_contact_author_fax         +86-431-85098620
_publ_contact_author_name        'Jian-Fang Ma'
_publ_contact_author_phone       +86-431-85098620
_publ_section_title
;
 First Three-Dimensional Inorganic-Organic Hybrid Material Constructed
 From an "Inverted Keggin" Polyoxometalate and a Copper(I)-Organic Complex
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8967
_journal_page_last               8972
_journal_paper_doi               10.1021/ic201135g
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C48 H64 As4 Cu4 Mo12 N24 O52'
_chemical_formula_sum            'C48 H64 As4 Cu4 Mo12 N24 O52'
_chemical_formula_weight         3514.35
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           114
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P -4 2n'
_symmetry_space_group_name_H-M   'P -4 21 c'
_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            2
_cell_length_a                   18.30830(10)
_cell_length_b                   18.30830(10)
_cell_length_c                   13.5804(2)
_cell_measurement_reflns_used    14596
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.1461
_cell_measurement_theta_min      2.8992
_cell_volume                     4552.07(8)
_computing_cell_refinement       CrysAlis
_computing_data_collection       'CrysAlis (Oxford Diffraction, 2006)'
_computing_data_reduction        CrysAlis
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Oxford Diffraction Gemini R Ultra'
_diffrn_measurement_method       '\w 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  0.0245
_diffrn_reflns_av_sigmaI/netI    0.0248
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            19822
_diffrn_reflns_theta_full        26.36
_diffrn_reflns_theta_max         26.36
_diffrn_reflns_theta_min         2.91
_exptl_absorpt_coefficient_mu    4.058
_exptl_absorpt_correction_T_max  0.6004
_exptl_absorpt_correction_T_min  0.3962
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis (Oxford Diffraction, 2006)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.564
_exptl_crystal_description       block
_exptl_crystal_F_000             3376
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.274
_refine_diff_density_min         -0.361
_refine_diff_density_rms         0.064
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.005(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         4648
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.984
_refine_ls_R_factor_all          0.0195
_refine_ls_R_factor_gt           0.0172
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0207P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0358
_refine_ls_wR_factor_ref         0.0360
_reflns_number_gt                4345
_reflns_number_total             4648
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic201135g_si_002_2.cif
_cod_data_source_block           2
_cod_database_code               4326244