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_4105567
_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         'C26 H41 F6 Fe2 N0 P S2'
_chemical_formula_sum            'C26 H41 F6 Fe2 N0 P S2'
_chemical_formula_weight         674.38
_chemical_name_systematic
; 
 ? 
;
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_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
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_atom_sites_solution_secondary   difmap
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_cell_angle_alpha                90.00
_cell_angle_beta                 110.934(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.9480(9)
_cell_length_b                   14.6111(11)
_cell_length_c                   15.6505(13)
_cell_measurement_reflns_used    412
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      25.25
_cell_measurement_theta_min      1.97
_cell_volume                     2979.0(4)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0422
_diffrn_reflns_av_sigmaI/netI    0.0704
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10825
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         1.97
_exptl_absorpt_coefficient_mu    1.220
_exptl_absorpt_correction_T_max  0.9528
_exptl_absorpt_correction_T_min  0.9087
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            dark-green
_exptl_crystal_density_diffrn    1.504
_exptl_crystal_description       block
_exptl_crystal_F_000             1400
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.784
_refine_diff_density_min         -0.422
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         5381
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.1110
_refine_ls_R_factor_gt           0.0609
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0900P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1551
_refine_ls_wR_factor_ref         0.1749
_reflns_number_gt                3185
_reflns_number_total             5381
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja105948r_si_006.cif
_cod_data_source_block           ds1
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