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_4106196
_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            'C72 H67 B Cl F24 Fe N2 P2 S Si'
_chemical_formula_weight         1640.48
_chemical_name_common            '[SiPipr2SAd]FeN2BArF'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.447(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.5522(7)
_cell_length_b                   15.7697(6)
_cell_length_c                   28.0672(11)
_cell_measurement_reflns_used    9895
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.69
_cell_measurement_theta_min      2.50
_cell_volume                     7154.0(5)
_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      296(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0573
_diffrn_reflns_av_sigmaI/netI    0.0497
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            78211
_diffrn_reflns_theta_full        26.38
_diffrn_reflns_theta_max         26.38
_diffrn_reflns_theta_min         1.49
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.446
_exptl_absorpt_correction_T_max  0.7336
_exptl_absorpt_correction_T_min  0.4907
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2008/1 (Bruker-AXS, 2008)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_description       block
_exptl_crystal_F_000             3348
_exptl_crystal_size_max          1.86
_exptl_crystal_size_mid          1.55
_exptl_crystal_size_min          0.74
_refine_diff_density_max         1.249
_refine_diff_density_min         -0.746
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1039
_refine_ls_number_reflns         14505
_refine_ls_number_restraints     120
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0835
_refine_ls_R_factor_gt           0.0547
_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^)+(0.0708P)^2^+11.2906P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1339
_refine_ls_wR_factor_ref         0.1503
_reflns_number_gt                10456
_reflns_number_total             14505
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja2020907_si_001_2.cif
_cod_data_source_block           ayt05
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_database_code               4106196