Synthesis and Characterization of a Tetranuclear Cyclopentadienyl Molybdenum Compound with a μ4-Sulfido Ligand
L. D. Vasquez; B. C. Noll; M. Rakowski DuBois; Inorganic Chemistry 40 (2001) 1391–1393; doi:10.1021/ic001043j

data_4319394
_publ_section_title
;
 Synthesis and Characterization of a Tetranuclear Cyclopentadienyl
 Molybdenum Compound with a \m4-Sulfido Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1391
_journal_page_last               1393
_journal_paper_doi               10.1021/ic001043j
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C38 H42 F6 Mo6 O6 S13'
_chemical_formula_weight         1701.14
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 102.50(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.001(2)
_cell_length_b                   14.964(3)
_cell_length_c                   15.128(3)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      17.5
_cell_measurement_theta_min      0
_cell_volume                     2652.3(9)
_computing_cell_refinement       'Siemens P3'
_computing_data_collection       'Siemens P3'
_computing_data_reduction        'Siemens XTAPE'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Siemens R3 diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.036
_diffrn_reflns_av_sigmaI/netI    0.0594
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9359
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.38
_exptl_absorpt_coefficient_mu    1.952
_exptl_absorpt_correction_T_max  0.80
_exptl_absorpt_correction_T_min  0.71
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
; 
XABS2 (Sean Parkin Dec. 1992) calculates 24 coefficients from 
a least-squares fit of (1/A vs sin^2^(\q)) to a cubic equation 
in sin^2^(\q) by minimization of Fo^2^ and Fc^2^ differences. 
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.130
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         2.208
_refine_diff_density_min         -0.903
_refine_diff_density_rms         0.193
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.22(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     545
_refine_ls_number_reflns         7524
_refine_ls_number_restraints     51
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_gt           0.0529
_refine_ls_shift/su_max          1.343
_refine_ls_shift/su_mean         0.027
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0702P)^2^+10.2076P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1261
_refine_ls_wR_factor_ref         0.1325
_reflns_number_gt                6552
_reflns_number_total             7524
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic001043j.cif
_cod_data_source_block           bc37
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4319394