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_4106198
_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            'C70 H104 Fe2 P4 S2 Si2'
_chemical_formula_weight         1301.41
_chemical_name_common            '[[SiPipr2S]Fe]2'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 90.993(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.2792(14)
_cell_length_b                   18.8853(18)
_cell_length_c                   14.6011(19)
_cell_measurement_reflns_used    6264
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.70
_cell_measurement_theta_min      2.40
_cell_volume                     3385.4(7)
_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 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.2393
_diffrn_reflns_av_sigmaI/netI    0.1868
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            47126
_diffrn_reflns_theta_full        26.05
_diffrn_reflns_theta_max         26.05
_diffrn_reflns_theta_min         1.98
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.660
_exptl_absorpt_correction_T_max  0.9309
_exptl_absorpt_correction_T_min  0.8471
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2008/1 (Bruker-AXS, 2008)'
_exptl_crystal_density_diffrn    1.277
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.881
_refine_diff_density_min         -1.043
_refine_diff_density_rms         0.168
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.613
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     348
_refine_ls_number_reflns         6631
_refine_ls_number_restraints     47
_refine_ls_restrained_S_all      1.611
_refine_ls_R_factor_all          0.2502
_refine_ls_R_factor_gt           0.1426
_refine_ls_shift/su_max          0.033
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3305
_refine_ls_wR_factor_ref         0.3619
_reflns_number_gt                3136
_reflns_number_total             6631
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja2020907_si_001_4.cif
_cod_data_source_block           ayt072
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_database_code               4106198