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_4324229
_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            'C24 H20 As4 Mo4 N8 O36'
_chemical_formula_weight         1679.92
_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                89.474(13)
_cell_angle_beta                 66.129(10)
_cell_angle_gamma                63.926(7)
_cell_formula_units_Z            1
_cell_length_a                   10.7255(19)
_cell_length_b                   10.937(3)
_cell_length_c                   12.000(3)
_cell_measurement_reflns_used    4861
_cell_measurement_temperature    108(2)
_cell_measurement_theta_max      31.1617
_cell_measurement_theta_min      3.3536
_cell_volume                     1131.6(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      108(2)
_diffrn_detector_area_resol_mean none
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0313
_diffrn_reflns_av_sigmaI/netI    0.0302
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            14710
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         3.35
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    4.109
_exptl_absorpt_correction_T_max  0.457
_exptl_absorpt_correction_T_min  0.440
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   crystalclear
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.465
_exptl_crystal_description       'rectangular plate'
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.2000
_exptl_crystal_size_mid          0.2000
_exptl_crystal_size_min          0.2000
_refine_diff_density_max         1.502
_refine_diff_density_min         -0.739
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         3987
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0303
_refine_ls_R_factor_gt           0.0282
_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^)+(0.0547P)^2^+1.5076P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0817
_refine_ls_wR_factor_ref         0.0831
_reflns_number_gt                3612
_reflns_number_total             3987
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101672t_si_005.cif
_cod_data_source_block           a
_cod_database_code               4324229