A Thioketene Complex of Molybdenum(IV): Crystal Structure of [Mo{η2-κ(C,S),σ-κ(S')- SCCRC(O)S}(O){HB(pz)3}] (R = C6H4Me-4, pz = Pyrazol-1-yl)
Anthony F. Hill; John M. Malget; Andrew J. P. White; David J. Williams; Inorganic Chemistry 37 (1998) 598–600; doi:10.1021/ic970712z

data_4322631
_publ_section_title
;
 A Thioketene Complex of Molybdenum(IV): Crystal Structure of
 [Mo{\h2-\k(C,S),\s-\k(S')- SCCRC(O)S}(O){HB(pz)3}] (R = C6H4Me-4, pz =
 Pyrazol-1-yl)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              598
_journal_page_last               600
_journal_paper_doi               10.1021/ic970712z
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C19 H17 B Mo N6 O2 S2'
_chemical_formula_weight         532.26
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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_method           SHELXL
_cell_angle_alpha                83.38(3)
_cell_angle_beta                 83.21(3)
_cell_angle_gamma                77.10(3)
_cell_formula_units_Z            2
_cell_length_a                   9.417(3)
_cell_length_b                   10.337(4)
_cell_length_c                   11.554(4)
_cell_measurement_temperature    293(2)
_cell_volume                     1084.0(7)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0453
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            3405
_diffrn_reflns_theta_max         61.93
_diffrn_reflns_theta_min         3.87
_diffrn_standards_interval_count 50
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    7.001
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.631
_exptl_crystal_description       'Thin plates'
_exptl_crystal_F_000             536
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.644
_refine_diff_density_min         -0.970
_refine_diff_density_rms         0.097
_refine_ls_extinction_coef       0.0009(3)
_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_all   1.044
_refine_ls_goodness_of_fit_obs   1.080
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         3399
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.261
_refine_ls_restrained_S_obs      1.080
_refine_ls_R_factor_all          0.0672
_refine_ls_R_factor_obs          0.0500
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0833P)^2^+0.8082P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1649
_refine_ls_wR_factor_obs         0.1268
_reflns_number_observed          2764
_reflns_number_total             3405
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic970712z.cif
_cod_data_source_block           AFH9532
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0833P)^2^+0.8082P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0833P)^2^+0.8082P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1084.1(7)
_cod_original_formula_sum        'C19 H17 N6 O2 B S2 Mo'
_cod_database_code               4322631