Synthesis and Study of Hexanuclear Molybdenum Clusters Containing Thiolate Ligands
Lisa F. Szczepura; Karen A. Ketcham; Betty A. Ooro; Julia A. Edwards; Jeffrey N. Templeton; David L. Cedeño; Alan J. Jircitano; Inorganic Chemistry 47 (2008) 7271–7278; doi:10.1021/ic800613d

data_4305634
_publ_contact_author             'Szczepura, Lisa F.'
_publ_contact_author_email       lfszcze@ilstu.edu
_publ_section_title
;
Synthesis and Study of Hexanuclear Molybdenum Clusters Containing Thiolate
Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7271
_journal_page_last               7278
_journal_paper_doi               10.1021/ic800613d
_journal_volume                  47
_journal_year                    2008
_chemical_compound_source        'synthesis as described'
_chemical_formula_sum            'C82 H84 Cl8 Mo6 N2 O4 P2 S6'
_chemical_formula_weight         2275.05
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_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_date             2008-01-10T17:46:03-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                89.654(2)
_cell_angle_beta                 88.365(2)
_cell_angle_gamma                71.179(2)
_cell_formula_units_Z            1
_cell_length_a                   12.1574(16)
_cell_length_b                   13.4441(17)
_cell_length_c                   14.2132(18)
_cell_measurement_reflns_used    841
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      22.69
_cell_measurement_theta_min      3.07
_cell_measurement_wavelength     0.71073
_cell_volume                     2198.0(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR2004 (Giacovazzo et al, 2004)'
_diffrn_ambient_temperature      466(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0735
_diffrn_reflns_av_unetI/netI     0.1666
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            22968
_diffrn_reflns_theta_full        25.39
_diffrn_reflns_theta_max         25.39
_diffrn_reflns_theta_min         1.6
_exptl_absorpt_coefficient_mu    1.301
_exptl_absorpt_correction_T_max  0.8877
_exptl_absorpt_correction_T_min  0.8030
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.719
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.421
_refine_diff_density_min         -0.393
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.651
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         8042
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      0.651
_refine_ls_R_factor_all          0.0895
_refine_ls_R_factor_gt           0.0303
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0144P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0534
_refine_ls_wR_factor_ref         0.0573
_reflns_number_gt                3493
_reflns_number_total             8042
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800613d-file003_1.cif
_cod_data_source_block           g37l
_cod_database_code               4305634