Synthesis of a FeIISH Complex Stabilized by an Intramolecular N-H...S Hydrogen Bond, Which Acts as a H2S Donor
Erwan Galardon; Thomas Roger; Patrick Deschamps; Pascal Roussel; Alain Tomas; Isabelle Artaud; Inorganic Chemistry 51 (2012) 10068–10070; doi:10.1021/ic300952d

data_4330453
_publ_section_title
;
 Synthesis of a FeIISH Complex Stabilized by an Intramolecular N-H...S
 Hydrogen Bond, Which Acts as a H2S Donor
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10068
_journal_page_last               10070
_journal_paper_doi               10.1021/ic300952d
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C55.5 H57 B Cl2 Fe N6 O S'
_chemical_formula_weight         993.69
_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-97
_cell_angle_alpha                91.5890(10)
_cell_angle_beta                 104.0310(10)
_cell_angle_gamma                109.7940(10)
_cell_formula_units_Z            2
_cell_length_a                   11.5670(3)
_cell_length_b                   13.1673(3)
_cell_length_c                   17.9318(4)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.
_cell_measurement_theta_min      1.2
_cell_volume                     2474.98(10)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_molecular_graphics    ORTEP(III)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.879
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_method       '\f & \w scans'
_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  0.0288
_diffrn_reflns_av_sigmaI/netI    0.0298
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            55702
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         30.49
_diffrn_reflns_theta_min         1.18
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.502
_exptl_absorpt_correction_T_max  0.951
_exptl_absorpt_correction_T_min  0.914
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1042
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.138
_refine_diff_density_min         -1.046
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     598
_refine_ls_number_reflns         13260
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0624
_refine_ls_R_factor_gt           0.0504
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0590P)^2^+3.4538P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1272
_refine_ls_wR_factor_ref         0.1360
_reflns_number_gt                11109
_reflns_number_total             13260
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300952d_si_001.cif
_cod_data_source_block           erw
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C55.50 H57 B Cl2 Fe N6 O S'
_cod_database_code               4330453