Thermal Stability of Tris(3,5-dimethylpyrazolyl)hydridoboratorhenium(V)(oxo)- (1,2-dithiolate) and -(1,2-monothiodiolate) Complexes and DFT Studies of C−S Bond Cleavage
Gable, Kevin P.; Chuawong, Pitak; Yokochi, Alexandre F. T.; Organometallics 21 (2002) 929–; doi:10.1021/om0107385

data_4076637
_publ_section_title
;
 Thermal Stability of
 Tris(3,5-dimethylpyrazolyl)hydridoboratorhenium(V)(oxo)- (1,2-dithiolate)
 and -(1,2-monothiodiolate) Complexes and DFT Studies of C&#x2212;S Bond
 Cleavage
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              929
_journal_paper_doi               10.1021/om0107385
_journal_volume                  21
_journal_year                    2002
_chemical_formula_sum            'C17 H26 B N6 O Re S2'
_chemical_formula_weight         591.57
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.5673(5)
_cell_length_b                   11.4116(12)
_cell_length_c                   22.8696(19)
_cell_measurement_reflns_used    65
_cell_measurement_temperature    290(2)
_cell_measurement_theta_max      28.665
_cell_measurement_theta_min      10.995
_cell_volume                     2235.9(3)
_computing_cell_refinement       'XSCANS V2.2'
_computing_data_collection       'XSCANS V2.2'
_computing_data_reduction        'XSCANS V2.2'
_computing_molecular_graphics    'ORTEP-III for windows (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      290(2)
_diffrn_measured_fraction_theta_full 0.929
_diffrn_measured_fraction_theta_max 0.929
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       '\w/2\q 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  0.0332
_diffrn_reflns_av_sigmaI/netI    0.0357
_diffrn_reflns_limit_h_max       1
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       1
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            2817
_diffrn_reflns_theta_full        67.41
_diffrn_reflns_theta_max         67.41
_diffrn_reflns_theta_min         3.87
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    12.535
_exptl_absorpt_correction_T_max  0.3670
_exptl_absorpt_correction_T_min  0.3670
_exptl_absorpt_correction_type   'Analytical (face indexing using Pluton)'
_exptl_crystal_colour            'Deep purple'
_exptl_crystal_density_diffrn    1.757
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.868
_refine_diff_density_min         -0.831
_refine_diff_density_rms         0.113
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.000(19)
_refine_ls_extinction_coef       0.00035(4)
_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   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         2627
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0300
_refine_ls_R_factor_gt           0.0284
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0425P)^2^+2.3975P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0721
_refine_ls_wR_factor_ref         0.0744
_reflns_number_gt                2494
_reflns_number_total             2627
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0107385.cif
_cod_data_source_block           xl
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 2(1) 2(1) 2(1)'
_cod_database_code               4076637