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_4324226
_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 N2 O25'
_chemical_formula_weight         1419.86
_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                117.09(2)
_cell_angle_beta                 96.03(2)
_cell_angle_gamma                98.454(18)
_cell_formula_units_Z            2
_cell_length_a                   10.009(4)
_cell_length_b                   15.767(5)
_cell_length_c                   17.287(5)
_cell_measurement_reflns_used    8889
_cell_measurement_temperature    118(2)
_cell_measurement_theta_max      31.1502
_cell_measurement_theta_min      1.3490
_cell_volume                     2356.1(15)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      118(2)
_diffrn_detector_area_resol_mean none
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.1174
_diffrn_reflns_av_sigmaI/netI    0.1058
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            36989
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.38
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    3.906
_exptl_absorpt_correction_T_max  0.823
_exptl_absorpt_correction_T_min  0.476
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   crystalclear
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.001
_exptl_crystal_description       'triangular plate'
_exptl_crystal_F_000             1356
_exptl_crystal_size_max          0.2000
_exptl_crystal_size_mid          0.2000
_exptl_crystal_size_min          0.0500
_refine_diff_density_max         2.217
_refine_diff_density_min         -2.503
_refine_diff_density_rms         0.297
_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     577
_refine_ls_number_reflns         8303
_refine_ls_number_restraints     2128
_refine_ls_restrained_S_all      0.949
_refine_ls_R_factor_all          0.1171
_refine_ls_R_factor_gt           0.0985
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1622P)^2^+50.5641P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2684
_refine_ls_wR_factor_ref         0.2869
_reflns_number_gt                7487
_reflns_number_total             8303
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101672t_si_002.cif
_cod_data_source_block           a
_cod_original_cell_volume        2356.1(14)
_cod_database_code               4324226