Proposed Ligand-Centered Electrocatalytic Hydrogen Evolution and Hydrogen Oxidation at a Noninnocent Mononuclear Metal-Thiolate.
Haddad, Andrew Z.; Kumar, Davinder; Ouch Sampson, Kagna; Matzner, Anna M.; Mashuta, Mark S.; Grapperhaus, Craig A.; Journal of the American Chemical Society 137 (2015) 9238–9241; doi:10.1021/jacs.5b05561

data_4124233
_publ_section_title
;
 Proposed Ligand-Centered Electrocatalytic Hydrogen Evolution and Hydrogen
 Oxidation at a Noninnocent Mononuclear Metal-Thiolate.
;
_journal_issue                   29
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9238
_journal_page_last               9241
_journal_paper_doi               10.1021/jacs.5b05561
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety         'C54 H43 P3 Re S3, P F6'
_chemical_formula_sum            'C54 H43 F6 P4 Re S3'
_chemical_formula_weight         1212.14
_chemical_name_common            Re(DPPBT)~3~H
_chemical_name_systematic
; 
(diphenylphosphinobenzenethiol)
(bis-diphenylphosphinobenzenethiolate)rhenium(II)
 hexafluorophosphate 
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method
;
 <i>CrysAlis PRO</i> (Agilent, 2010) 
;
_audit_update_record
;
May_22_2013 text and data added by Mark S. Mashuta
Jun_27_2013 text and data added by Mark S. Mashuta
Oct_16_2013 text and data added by Mark S. Mashuta
May_21_2015 text and data added by Mark S. Mashuta
;
_cell_angle_alpha                90.00
_cell_angle_beta                 97.5416(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.59553(9)
_cell_length_b                   33.0018(3)
_cell_length_c                   15.41951(15)
_cell_measurement_reflns_used    41852
_cell_measurement_temperature    100.05(10)
_cell_measurement_theta_max      30.6470
_cell_measurement_theta_min      3.4260
_cell_volume                     4840.65(8)
_computing_cell_refinement       '<i>CrysAlis PRO</i> (Agilent, 2010)'
_computing_data_collection       '<i>CrysAlis PRO</i> (Agilent, 2010)'
_computing_data_reduction        '<i>CrysAlis PRO</i> (Agilent, 2010)'
_computing_molecular_graphics
'ORTEP-3 (Farrugia, 1997) and Mercury (Macrae<i>et al.</i>, 2006)'
_computing_publication_material  'PLATON (Spek, 2009)'
_computing_structure_refinement  '<i>SHELXL-97</i> (Sheldrick, 2008)'
_computing_structure_solution    '<i>SHELXS-97</i> (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.05(10)
_diffrn_detector_area_resol_mean 10.2836
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.929
_diffrn_measurement_details
;
  1 omega  -55.00   36.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       15.0832  -57.0000 -150.0000 91

  2 omega  -12.00   83.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       15.0832   57.0000    0.0000 95

  3 omega    5.00   31.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       15.0832  -57.0000   30.0000 26

  4 omega  -44.00   59.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.7707   57.0000   90.0000 103

  5 omega  -15.00   89.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       15.0832   57.0000  120.0000 104

  6 omega  -15.00   15.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       15.0832   57.0000 -120.0000 30

  7 omega  -64.00   49.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       15.0832  -77.0000    0.0000 113

;
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0281
_diffrn_reflns_av_sigmaI/netI    0.0226
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            76686
_diffrn_reflns_theta_full        28.10
_diffrn_reflns_theta_max         30.72
_diffrn_reflns_theta_min         3.25
_exptl_absorpt_coefficient_mu    2.834
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7431
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.663
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'hexagonal prism'
_exptl_crystal_F_000             2416
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.744
_refine_diff_density_min         -1.097
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     598
_refine_ls_number_reflns         13986
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0328
_refine_ls_R_factor_gt           0.0292
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0426P)^2^+5.8473P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0767
_refine_ls_wR_factor_ref         0.0787
_reflns_number_gt                13091
_reflns_number_total             13986
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ja5b05561_si_001.cif
_cod_data_source_block           Re(DPPBT)~3~H
_cod_original_cell_volume        4840.66(8)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4124233