Dinitrogen Complexes of Sulfur-Ligated Iron
Ayumi Takaoka; Neal P. Mankad; Jonas C. Peters; Journal of the American Chemical Society 133 (2011) 8440–8443; doi:10.1021/ja2020907

data_4106199
_publ_contact_author             'Jonas C. Peters'
_publ_contact_author_email       jpeters@caltech.edu
_publ_section_title
;
 Dinitrogen Complexes of Sulfur-Ligated Iron
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8440
_journal_page_last               8443
_journal_paper_doi               10.1021/ja2020907
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C58 H80 Fe N2 P S2 Si'
_chemical_formula_weight         984.27
_chemical_name_common            '[SiPiprSAd2]Fe(H)(N2)'
_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                93.7520(10)
_cell_angle_beta                 105.5900(10)
_cell_angle_gamma                91.5850(10)
_cell_formula_units_Z            2
_cell_length_a                   11.0806(5)
_cell_length_b                   13.0186(6)
_cell_length_c                   19.1039(8)
_cell_measurement_reflns_used    9104
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.45
_cell_measurement_theta_min      2.22
_cell_volume                     2645.8(2)
_computing_cell_refinement       'SAINT-Plus v7.66A (Bruker-AXS, 2009)'
_computing_data_collection       'APEX2 v2009.7-0 (Bruker-AXS, 2009)'
_computing_data_reduction        'SAINT-Plus v7.66A (Bruker-AXS, 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker KAPPA APEX II'
_diffrn_measurement_method       '\w and \f 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  0.0660
_diffrn_reflns_av_sigmaI/netI    0.0731
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            58590
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         2.22
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.456
_exptl_absorpt_correction_T_max  0.9516
_exptl_absorpt_correction_T_min  0.9104
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2008/1 (Bruker-AXS, 2008)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.235
_exptl_crystal_description       plate
_exptl_crystal_F_000             1058
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.931
_refine_diff_density_min         -0.418
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.161
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     654
_refine_ls_number_reflns         16055
_refine_ls_number_restraints     81
_refine_ls_restrained_S_all      1.160
_refine_ls_R_factor_all          0.0926
_refine_ls_R_factor_gt           0.0579
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0601P)^2^+1.8188P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1453
_refine_ls_wR_factor_ref         0.1598
_reflns_number_gt                11199
_reflns_number_total             16055
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja2020907_si_001_5.cif
_cod_data_source_block           ayt09
_cod_database_code               4106199