Light Enhanced Fe-Mediated Nitrogen Fixation: Mechanistic Insights Regarding H<sub>2</sub> Elimination, HER, and NH<sub>3</sub> Generation.
Schild, Dirk J.; Peters, Jonas C.; ACS catalysis 9 (2019) 4286–4295; doi:10.1021/acscatal.9b00523

data_4514705
_publ_section_title
;
 Light Enhanced Fe-Mediated Nitrogen Fixation: Mechanistic Insights
 Regarding H<sub>2</sub> Elimination, HER, and NH<sub>3</sub> Generation.
;
_journal_issue                   5
_journal_name_full               'ACS catalysis'
_journal_page_first              4286
_journal_page_last               4295
_journal_paper_doi               10.1021/acscatal.9b00523
_journal_volume                  9
_journal_year                    2019
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C33 H50 Fe K N2 P3 Si'
_chemical_formula_sum            'C33 H50 Fe K N2 P3 Si'
_chemical_formula_weight         690.70
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-12-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.5863(9)
_cell_length_b                   16.3326(12)
_cell_length_c                   20.8095(17)
_cell_measurement_reflns_used    9403
_cell_measurement_temperature    125(2)
_cell_measurement_theta_max      77.36
_cell_measurement_theta_min      3.44
_cell_volume                     3598.0(5)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      124.99
_diffrn_detector                 'CMOS Area Detector'
_diffrn_detector_area_resol_mean 10.24
_diffrn_detector_type            'Bruker PHOTON 100 CMOS'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multilayer mirrors'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0728
_diffrn_reflns_av_unetI/netI     0.0653
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            38615
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         79.104
_diffrn_reflns_theta_min         3.440
_diffrn_source                   'I\mS HB micro-focus sealed tube'
_diffrn_source_current           1
_diffrn_source_power             0.05
_diffrn_source_type              'Incoatech I\mS HB'
_diffrn_source_voltage           50
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.154
_exptl_absorpt_correction_T_max  0.9741
_exptl_absorpt_correction_T_min  0.7068
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1244 before and 0.0956 after correction. The Ratio of minimum to maximum transmission is 0.7256. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'blackish orange'
_exptl_crystal_colour_modifier   blackish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_description       block
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.164
_exptl_crystal_size_mid          0.077
_exptl_crystal_size_min          0.059
_refine_diff_density_max         1.307
_refine_diff_density_min         -0.815
_refine_diff_density_rms         0.086
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.125(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     382
_refine_ls_number_reflns         7481
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0873
_refine_ls_R_factor_gt           0.0670
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0588P)^2^+7.1259P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1490
_refine_ls_wR_factor_ref         0.1606
_reflns_Friedel_coverage         0.793
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.981
_reflns_number_gt                6100
_reflns_number_total             7481
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs9b00523_si_002.cif
_cod_data_source_block           p17555
_cod_database_code               4514705
_shelx_shelxl_version_number     2018/1
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.875(11)
 0.125(11)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Ternary CH refined with riding coordinates:
 C32(H32), C5(H5), C29(H29), C8(H8)
3.b Aromatic/amide H refined with riding coordinates:
 C23(H23), C14(H14), C24(H24), C21(H21), C17(H17), C13(H13), C26(H26),
 C11(H11), C25(H25), C20(H20), C18(H18), C19(H19), C12(H12)
3.c Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C28(H28A,H28B,H28C), C33(H33A,H33B,H33C), C6(H6A,H6B,
 H6C), C30(H30A,H30B,H30C), C1(H1A,H1B,H1C), C9(H9A,H9B,H9C), C3(H3A,H3B,H3C),
 C7(H7A,H7B,H7C), C4(H4A,H4B,H4C), C2(H2A,H2B,H2C)
;
_shelx_res_checksum              26518
_shelx_hkl_checksum              92718
_olex2_submission_special_instructions 'No special instructions were received'