Systematic Preparation of Mo24+ Building Blocks for Supramolecular Assemblies
F. Albert Cotton; Chun Y. Liu; Carlos A. Murillo; Inorganic Chemistry 43 (2004) 2267–2276; doi:10.1021/ic035433s

data_4310822
_publ_section_title
;
 Systematic Preparation of Mo24+ Building Blocks for Supramolecular
 Assemblies
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2267
_journal_page_last               2276
_journal_paper_doi               10.1021/ic035433s
_journal_volume                  43
_journal_year                    2004
_chemical_formula_moiety         '[Mo2(O2CCH3)(MeCN)6](BF4)3,1.5(CH3CN)'
_chemical_formula_sum            'C17 H25.5 B3 F12 Mo2 N7.5 O2'
_chemical_formula_weight         819.26
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                101.3770(10)
_cell_angle_beta                 95.9570(10)
_cell_angle_gamma                106.3400(10)
_cell_formula_units_Z            4
_cell_length_a                   11.1461(7)
_cell_length_b                   16.2197(11)
_cell_length_c                   19.1059(13)
_cell_measurement_reflns_used    9289
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      27.412
_cell_measurement_theta_min      2.266
_cell_volume                     3202.5(4)
_computing_cell_refinement       SAINT
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    XP
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'BRUKER SMART 1000'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0211
_diffrn_reflns_av_sigmaI/netI    0.0488
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            20605
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         1.93
_diffrn_standards_number         'none (area detector data)'
_exptl_absorpt_coefficient_mu    0.882
_exptl_absorpt_correction_T_max  0.8535
_exptl_absorpt_correction_T_min  0.7395
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.699
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1612
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.171
_refine_diff_density_min         -0.870
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     801
_refine_ls_number_reflns         14186
_refine_ls_number_restraints     117
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0663
_refine_ls_R_factor_gt           0.0481
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0533P)^2^+5.6918P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1166
_refine_ls_wR_factor_ref         0.1279
_reflns_number_gt                10776
_reflns_number_total             14186
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic035433ssi20031213_045454_5.cif
_cod_data_source_block           cmpd5
_cod_original_formula_sum        'C17 H25.50 B3 F12 Mo2 N7.50 O2'
_cod_database_code               4310822