Unusual Thiolate-Bridged Diiron Clusters Bearing the cis-HN=NH Ligand and Their Reactivities with Terminal Alkynes
Yanhui Chen; Litao Liu; Ying Peng; Pingping Chen; Yi Luo; Jingping Qu; Journal of the American Chemical Society 133 (2011) 1147–1149; doi:10.1021/ja105948r

data_4105562
_publ_section_title
;
 Unusual Thiolate-Bridged Diiron Clusters Bearing the cis-HN=NH Ligand and
 Their Reactivities with Terminal Alkynes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1147
_journal_page_last               1149
_journal_paper_doi               10.1021/ja105948r
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         'C22 H38 F6 Fe2 N2 P S2'
_chemical_formula_sum            'C22 H38 F6 Fe2 N2 P S2'
_chemical_formula_weight         651.33
_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                76.5240(10)
_cell_angle_beta                 79.2050(10)
_cell_angle_gamma                85.1150(10)
_cell_formula_units_Z            2
_cell_length_a                   8.6394(2)
_cell_length_b                   11.5514(2)
_cell_length_c                   14.9011(3)
_cell_measurement_reflns_used    235
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      27.0
_cell_measurement_theta_min      2.04
_cell_volume                     1419.21(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0179
_diffrn_reflns_av_sigmaI/netI    0.0262
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11579
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.04
_exptl_absorpt_coefficient_mu    1.279
_exptl_absorpt_correction_T_max  0.5396
_exptl_absorpt_correction_T_min  0.4948
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.524
_exptl_crystal_description       block
_exptl_crystal_F_000             674
_exptl_crystal_size_max          0.64
_exptl_crystal_size_mid          0.61
_exptl_crystal_size_min          0.55
_refine_diff_density_max         0.571
_refine_diff_density_min         -0.404
_refine_diff_density_rms         0.056
_refine_ls_extinction_coef       0.0004(8)
_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   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         6030
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_gt           0.0378
_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^)+(0.0657P)^2^+0.3993P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1073
_refine_ls_wR_factor_ref         0.1123
_reflns_number_gt                5015
_reflns_number_total             6030
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja105948r_si_001.cif
_cod_data_source_block           ds1
_cod_database_code               4105562