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_4306839
_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         'C33 H44 B Mo N6 O2 S'
_chemical_formula_sum            'C33 H44 B Mo N6 O2 S'
_chemical_formula_weight         695.55
_chemical_name_common            Tp*MoS(2-propylphenolate)2
_chemical_name_systematic
;
{hydrotris(3,5-dimethylpyrazol-1-yl)borato}bis{2-propylphenolato}sulfidomolybdenum(V)
;
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.183(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.0547(12)
_cell_length_b                   10.085(2)
_cell_length_c                   24.747(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      16.0
_cell_measurement_theta_min      10.0
_cell_volume                     3507.7(9)
_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  0.0179
_diffrn_reflns_av_sigmaI/netI    0.0229
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            7824
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         2.18
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  160
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.471
_exptl_absorpt_correction_T_max  0.9120
_exptl_absorpt_correction_T_min  0.7223
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   '(Sheldrick, 1976)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.317
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       plate
_exptl_crystal_F_000             1452
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.735
_refine_diff_density_min         -0.367
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     465
_refine_ls_number_reflns         6160
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0396
_refine_ls_R_factor_gt           0.0314
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0524P)^2^+1.2745P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0819
_refine_ls_wR_factor_ref         0.0870
_reflns_number_gt                5313
_reflns_number_total             6160
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060585jsi20060406_102313_2.cif
_cod_data_source_block           cy_15
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_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 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4306839