Catalytic Hydrogen Evolution by Fe(II) Carbonyls Featuring a Dithiolate and a Chelating Phosphine.
Roy, Souvik; Mazinani, Shobeir K. S.; Groy, Thomas L.; Gan, Lu; Tarakeshwar, Pilarisetty; Mujica, Vladimiro; Jones, Anne K.; Inorganic chemistry 53 (2014) 8919–8929; doi:10.1021/ic5012988

data_4340726
_publ_section_title
;
 Catalytic Hydrogen Evolution by Fe(II) Carbonyls Featuring a Dithiolate
 and a Chelating Phosphine.
;
_journal_issue                   17
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8919
_journal_page_last               8929
_journal_paper_doi               10.1021/ic5012988
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C36 H33 Fe N O3 P2 S2, C H Cl3'
_chemical_formula_sum            'C37 H34 Cl3 Fe N O3 P2 S2'
_chemical_formula_weight         828.91
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_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
_cell_angle_alpha                90
_cell_angle_beta                 94.357(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.9358(18)
_cell_length_b                   19.445(3)
_cell_length_c                   17.386(3)
_cell_measurement_reflns_used    5070
_cell_measurement_temperature    123.(2)
_cell_measurement_theta_max      24.9947
_cell_measurement_theta_min      2.3496
_cell_volume                     3686.4(10)
_computing_cell_refinement       'SAINT V7.68A (Bruker AXS, 2009)'
_computing_data_collection
'Bruker Instrument Service v2010, 9, 0, 0 (Bruker AXS, 2010)'
_computing_data_reduction        'SAINT V7.68A (Bruker AXS, 2009)'
_computing_molecular_graphics    'XShell ver. 6.3.1 (Bruker AXS, 2004)'
_computing_publication_material  'Bruker APEX2 v2010.9-1 (Bruker AXS, 2010)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123.(2)
_diffrn_detector_area_resol_mean 8.3330
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Smart APEX'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0794
_diffrn_reflns_av_sigmaI/netI    0.0648
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            29548
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         1.87
_diffrn_source_type              'sealed tube'
_exptl_absorpt_coefficient_mu    0.865
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_correction_T_min  0.65
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS Version 2008/1 (Bruker AXS, 2008)'
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_density_diffrn    1.494
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1704
_exptl_crystal_size_max          0.380
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.080
_refine_diff_density_max         1.317
_refine_diff_density_min         -0.511
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     443
_refine_ls_number_reflns         6735
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0843
_refine_ls_R_factor_gt           0.0535
_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^)+(0.0811P)^2^+2.7073P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1326
_refine_ls_wR_factor_ref         0.1552
_reflns_number_gt                4852
_reflns_number_total             6735
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5012988_si_003.cif
_cod_data_source_block           glyP2FeCObdt
_cod_depositor_comments
'Adding full bibliography for 4340725--4340726.cif.'
_cod_database_code               4340726