Synthesis, Structural Characterization, and Multifrequency Electron Paramagnetic Resonance Studies of Mononuclear Thiomolybdenyl Complexes
Simon C. Drew; Jason P. Hill; Ian Lane; Graeme R. Hanson; Robert W. Gable; Charles G. Young; Inorganic Chemistry 46 (2007) 2373–2387; doi:10.1021/ic060585j

data_4306840
_publ_section_title
;
Synthesis, Structural Characterization, and Multifrequency Electron
Paramagnetic Resonance Studies of Mononuclear Thiomolybdenyl Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2373
_journal_page_last               2387
_journal_paper_doi               10.1021/ic060585j
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         'C21 H26 B Mo N6 O2 S'
_chemical_formula_sum            'C21 H26 B Mo N6 O2 S'
_chemical_formula_weight         533.29
_chemical_name_common            Tp*MoS(catecholate)
_chemical_name_systematic
;
(catecholato}{hydrotris(3,5-dimethylpyrazol-1-yl)borato}sulfidomolybdenum(V)
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   none
_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                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.167(3)
_cell_length_b                   18.890(5)
_cell_length_c                   17.547(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      13.7
_cell_measurement_theta_min      9.8
_cell_volume                     4695.8(19)
_computing_cell_refinement       'CAD-4 Software'
_computing_data_collection       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_reduction        'PROCESS_DATA (Gable et al., 1993)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL-97
_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  'Enraf-Nonius CAD-4MachS diffractometer'
_diffrn_measurement_method       \w:2\q
_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  0.0394
_diffrn_reflns_av_sigmaI/netI    0.0311
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            5081
_diffrn_reflns_theta_full        24.96
_diffrn_reflns_theta_max         24.96
_diffrn_reflns_theta_min         2.14
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  160
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.678
_exptl_absorpt_correction_T_max  0.9342
_exptl_absorpt_correction_T_min  0.8365
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   ' (Sheldrick, 1976)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.509
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       plate
_exptl_crystal_F_000             2184
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.186
_refine_diff_density_min         -1.767
_refine_diff_density_rms         0.176
_refine_ls_extinction_coef       0.0106(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     754
_refine_ls_number_reflns         4116
_refine_ls_number_restraints     1095
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.1152
_refine_ls_R_factor_gt           0.0903
_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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2435
_refine_ls_wR_factor_ref         0.2769
_reflns_number_gt                2729
_reflns_number_total             4116
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060585jsi20060406_102313_3.cif
_cod_data_source_block           cy_16
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'Gaussian' changed to 'gaussian'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
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_cod_database_code               4306840