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_4514700
_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_formula_moiety         'C30 H41 Fe N4 P3'
_chemical_formula_sum            'C30 H41 Fe N4 P3'
_chemical_formula_weight         606.43
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_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     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                 98.630(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.626(2)
_cell_length_b                   10.7764(8)
_cell_length_c                   16.1774(19)
_cell_measurement_reflns_used    9991
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.72
_cell_measurement_theta_min      2.55
_cell_volume                     3038.0(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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      99.99
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0944
_diffrn_reflns_av_unetI/netI     0.0420
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            112007
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.081
_diffrn_reflns_theta_min         2.222
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.681
_exptl_absorpt_correction_T_max  0.950
_exptl_absorpt_correction_T_min  0.897
_exptl_absorpt_correction_type   cylinder
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1244 before'
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.326
_exptl_crystal_description       plate
_exptl_crystal_F_000             1280
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.076
_refine_diff_density_max         1.388
_refine_diff_density_min         -0.950
_refine_diff_density_rms         0.224
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     381
_refine_ls_number_reflns         10593
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0385
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0555P)^2^+1.4400P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1013
_refine_ls_wR_factor_ref         0.1167
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8444
_reflns_number_total             10593
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs9b00523_si_002.cif
_cod_data_source_block           p17278
_cod_database_code               4514700
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.950
_shelx_estimated_absorpt_t_min   0.899
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 N4, N3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(H22C)=
 Sof(C21)=Sof(H21)=1-FVAR(1)
 Sof(C24)=Sof(H24)=Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(H19C)=Sof(C23)=Sof(H23A)=
 Sof(H23B)=Sof(H23C)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C26(H26), C17(H17), C14(H14), C24(H24), C21(H21)
4.b Aromatic/amide H refined with riding coordinates:
 C32(H32), C9(H9), C8(H8), C4(H4), C10(H10), C6(H6), C3(H3), C31(H31), C5(H5),
 C11(H11), C29(H29), C2(H2), C30(H30)
4.c Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C13(H13A,H13B,H13C), C25(H25A,H25B,H25C), C18(H18A,H18B,
 H18C), C16(H16A,H16B,H16C), C15(H15A,H15B,H15C), C19(H19A,H19B,H19C), C20(H20A,
 H20B,H20C), C23(H23A,H23B,H23C), C22(H22A,H22B,H22C)
;
_shelx_res_checksum              37725
_shelx_hkl_checksum              43247
_olex2_submission_special_instructions 'No special instructions were received'