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_4106197
_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            'C96 H120 Fe2 O P4 S2 Si4'
_chemical_formula_weight         1701.98
_chemical_name_common            '[SiPipr2SAd]FeCp'
_space_group_IT_number           82
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4'
_symmetry_space_group_name_H-M   'I -4'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   27.2245(6)
_cell_length_b                   27.2245(6)
_cell_length_c                   13.8202(4)
_cell_measurement_reflns_used    9935
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.85
_cell_measurement_theta_min      2.37
_cell_volume                     10243.2(4)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0639
_diffrn_reflns_av_sigmaI/netI    0.0521
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            78637
_diffrn_reflns_theta_full        30.05
_diffrn_reflns_theta_max         30.05
_diffrn_reflns_theta_min         2.12
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.474
_exptl_absorpt_correction_T_max  0.6213
_exptl_absorpt_correction_T_min  0.4859
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2008/1 (Bruker-AXS, 2008)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.104
_exptl_crystal_description       block
_exptl_crystal_F_000             3616
_exptl_crystal_size_max          1.78
_exptl_crystal_size_mid          1.41
_exptl_crystal_size_min          1.11
_refine_diff_density_max         1.316
_refine_diff_density_min         -0.475
_refine_diff_density_rms         0.112
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.018(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     533
_refine_ls_number_reflns         14977
_refine_ls_number_restraints     99
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0612
_refine_ls_R_factor_gt           0.0498
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0884P)^2^+6.3918P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1376
_refine_ls_wR_factor_ref         0.1455
_reflns_number_gt                13085
_reflns_number_total             14977
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja2020907_si_001_3.cif
_cod_data_source_block           ayt06
_cod_database_code               4106197