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_4310820
_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
trans-[Mo2(C15H15N2O2)2(O2CCH3)(NCCH3)2]BF4,1.5(C2H5)2O
_chemical_formula_sum            'C42 H54 B F4 Mo2 N6 O7.5'
_chemical_formula_weight         1041.60
_chemical_name_common            trans-[Mo2(DAniF)2(OAc)(NCCH3)2]BF4
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.7610(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.8594(12)
_cell_length_b                   21.6789(14)
_cell_length_c                   12.3258(8)
_cell_measurement_reflns_used    20653
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      25.573
_cell_measurement_theta_min      2.200
_cell_volume                     4755.7(5)
_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 0.426
_diffrn_measured_fraction_theta_max 0.426
_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  0.0272
_diffrn_reflns_av_sigmaI/netI    0.0256
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            11861
_diffrn_reflns_theta_full        25.55
_diffrn_reflns_theta_max         25.55
_diffrn_reflns_theta_min         1.91
_diffrn_standards_number         'none (area detector data)'
_exptl_absorpt_coefficient_mu    0.596
_exptl_absorpt_correction_T_max  0.8117
_exptl_absorpt_correction_T_min  0.6800
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.455
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2132
_exptl_crystal_size_max          0.440
_exptl_crystal_size_mid          0.420
_exptl_crystal_size_min          0.350
_refine_diff_density_max         0.594
_refine_diff_density_min         -0.555
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     489
_refine_ls_number_reflns         3795
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0476
_refine_ls_R_factor_gt           0.0401
_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^)+(0.0495P)^2^+13.7047P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0981
_refine_ls_wR_factor_ref         0.1059
_reflns_number_gt                3327
_reflns_number_total             3795
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic035433ssi20031213_045454_3.cif
_cod_data_source_block           cmpd3
_cod_original_formula_sum        'C42 H54 B F4 Mo2 N6 O7.50'
_cod_database_code               4310820