An Fe-N2 Complex That Generates Hydrazine and Ammonia via Fe═NNH2: Demonstrating a Hybrid Distal-to-Alternating Pathway for N2 Reduction.
Rittle, Jonathan; Peters, Jonas C.; Journal of the American Chemical Society 138 (2016) 4243–; doi:10.1021/jacs.6b01230

data_4124950
_publ_section_title
;
 An Fe-N2 Complex That Generates Hydrazine and Ammonia via Fe&#x2550;NNH2:
 Demonstrating a Hybrid Distal-to-Alternating Pathway for N2 Reduction.
;
_journal_issue                   12
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4243
_journal_paper_doi               10.1021/jacs.6b01230
_journal_volume                  138
_journal_year                    2016
_chemical_formula_sum            'C76.3 H85 B F24 Fe N2 O2 P3 Si'
_chemical_formula_weight         1705.72
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
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_cell_angle_beta                 77.192(3)
_cell_angle_gamma                78.758(3)
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_cell_length_b                   16.5462(9)
_cell_length_c                   19.6878(12)
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_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.26
_cell_measurement_theta_min      2.22
_cell_volume                     3930.1(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker-AXS, 2013)'
_computing_data_collection       'APEX2 v2014.11-0 (Bruker-AXS, 2014)'
_computing_data_reduction        'SAINT v8.34A (Bruker-AXS, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
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_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker KAPPA APEXII'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0652
_diffrn_reflns_av_unetI/netI     0.0387
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
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_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
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_diffrn_reflns_limit_l_min       -26
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_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.950
_diffrn_reflns_theta_min         1.636
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.372
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2014/5 (Sheldrick, 2014)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_description       block
_exptl_crystal_F_000             1758
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
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_exptl_transmission_factor_max   0.7458
_exptl_transmission_factor_min   0.7134
_refine_diff_density_max         1.767
_refine_diff_density_min         -0.740
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1158
_refine_ls_number_reflns         20771
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0653
_refine_ls_R_factor_gt           0.0437
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0695P)^2^+0.4995P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1180
_refine_ls_wR_factor_ref         0.1256
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15045
_reflns_number_total             20771
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b01230_si_002.cif
_cod_data_source_block           a15182
_cod_depositor_comments
'Adding full bibliography for 4124949--4124953.cif.'
_cod_original_formula_sum        'C76.30 H85 B F24 Fe N2 O2 P3 Si'
_cod_database_code               4124950
_shelxl_version_number           2013-3
_shelx_res_checksum              34937
_shelx_hkl_checksum              61305