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_4324227
_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            'C27 H36 As4 Mo4 N7 O25'
_chemical_formula_weight         1542.07
_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                87.426(13)
_cell_angle_beta                 82.265(10)
_cell_angle_gamma                71.005(11)
_cell_formula_units_Z            2
_cell_length_a                   10.207(4)
_cell_length_b                   13.740(5)
_cell_length_c                   19.700(8)
_cell_measurement_reflns_used    9975
_cell_measurement_temperature    118(2)
_cell_measurement_theta_max      31.1552
_cell_measurement_theta_min      2.0866
_cell_volume                     2588.6(17)
_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 0.996
_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     0.71075
_diffrn_reflns_av_R_equivalents  0.1044
_diffrn_reflns_av_sigmaI/netI    0.0872
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            39817
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.25
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    3.567
_exptl_absorpt_correction_T_max  0.700
_exptl_absorpt_correction_T_min  0.531
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   crystalclear
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.978
_exptl_crystal_description       rod-shaped
_exptl_crystal_F_000             1494
_exptl_crystal_size_max          0.2000
_exptl_crystal_size_mid          0.1500
_exptl_crystal_size_min          0.1000
_refine_diff_density_max         2.238
_refine_diff_density_min         -1.076
_refine_diff_density_rms         0.229
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     604
_refine_ls_number_reflns         9114
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0892
_refine_ls_R_factor_gt           0.0836
_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^)+(0.0708P)^2^+78.3892P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1961
_refine_ls_wR_factor_ref         0.2006
_reflns_number_gt                8565
_reflns_number_total             9114
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101672t_si_003.cif
_cod_data_source_block           a
_cod_database_code               4324227