Self-Assembly of Hybrid Organic-Inorganic Polyoxomolybdates: Solid-State Structures and Investigation of Formation and Core Rearrangements in Solution
Camelia I. Onet; Lei Zhang; Rodolphe Clérac; J. Bernard Jean-Denis; Martin Feeney; Thomas McCabe; Wolfgang Schmitt; Inorganic Chemistry 50 (2011) 604–613; doi:10.1021/ic101672t

data_4324228
_publ_section_title
;
 Self-Assembly of Hybrid Organic-Inorganic Polyoxomolybdates: Solid-State
 Structures and Investigation of Formation and Core Rearrangements in
 Solution
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              604
_journal_page_last               613
_journal_paper_doi               10.1021/ic101672t
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C60 H46 As10 Mo10 N10 O80'
_chemical_formula_weight         3895.67
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_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                113.09(3)
_cell_angle_beta                 112.90(3)
_cell_angle_gamma                99.16(3)
_cell_formula_units_Z            2
_cell_length_a                   19.417(4)
_cell_length_b                   21.040(4)
_cell_length_c                   21.562(4)
_cell_measurement_reflns_used    23284
_cell_measurement_temperature    108.1500
_cell_measurement_theta_max      31.3788
_cell_measurement_theta_min      2.2536
_cell_volume                     6941(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      108.1500
_diffrn_detector_area_resol_mean none
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0648
_diffrn_reflns_av_sigmaI/netI    0.0591
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            103006
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.26
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    3.334
_exptl_absorpt_correction_T_max  0.264
_exptl_absorpt_correction_T_min  0.220
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   crystalclear
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.864
_exptl_crystal_description       'rectangular plate'
_exptl_crystal_F_000             3732
_exptl_crystal_size_max          0.5000
_exptl_crystal_size_mid          0.4000
_exptl_crystal_size_min          0.4000
_refine_diff_density_max         2.729
_refine_diff_density_min         -2.598
_refine_diff_density_rms         0.227
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1587
_refine_ls_number_reflns         24429
_refine_ls_number_restraints     15280
_refine_ls_restrained_S_all      0.872
_refine_ls_R_factor_all          0.0789
_refine_ls_R_factor_gt           0.0704
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0866P)^2^+90.2909P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1844
_refine_ls_wR_factor_ref         0.1930
_reflns_number_gt                20611
_reflns_number_total             24429
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101672t_si_004.cif
_cod_data_source_block           a
_cod_original_cell_volume        6941(2)
_cod_database_code               4324228