Synthesis and Characterization of the Face-Sharing Bioctahedral [Mo2O6F3]3- Anion
Janet E. Kirsch; Heather K. Izumi; Charlotte L. Stern; Kenneth R. Poeppelmeier; Inorganic Chemistry 44 (2005) 4586–4593; doi:10.1021/ic0502877

data_4309121
_publ_section_title
;
Synthesis and Characterization of the Face-Sharing Bioctahedral
[Mo2O6F3]3- Anion
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4586
_journal_page_last               4593
_journal_paper_doi               10.1021/ic0502877
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C60 H72 Cu3 F6 Mo4 N24 O12'
_chemical_formula_weight         2009.80
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           148
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   13.8811(9)
_cell_length_b                   13.8811(9)
_cell_length_c                   31.783(3)
_cell_measurement_reflns_used    2965
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      29
_cell_measurement_theta_min      2.5
_cell_volume                     5303.6(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.955
_diffrn_measured_fraction_theta_max 0.955
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0387
_diffrn_reflns_av_sigmaI/netI    0.0252
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            16734
_diffrn_reflns_theta_full        28.92
_diffrn_reflns_theta_max         28.92
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    16.66
_exptl_absorpt_correction_T_max  0.9566
_exptl_absorpt_correction_T_min  0.6796
_exptl_absorpt_correction_type   'face indexed'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.888
_exptl_crystal_density_meas      1.886(5)
_exptl_crystal_density_method    'flotation pycnometry'
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             3015
_exptl_crystal_size_max          0.108
_exptl_crystal_size_mid          0.102
_exptl_crystal_size_min          0.013
_refine_diff_density_max         1.350
_refine_diff_density_min         -2.661
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         2965
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0504
_refine_ls_R_factor_gt           0.0401
_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^)+(0.0518P)^2^+35.1923P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1014
_refine_ls_wR_factor_ref         0.1079
_reflns_number_gt                2461
_reflns_number_total             2965
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0502877si20050223_031724.cif
_cod_data_source_block           s17n
_cod_original_cell_volume        5303.7(7)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4309121