Dinitrogen Reduction to Ammonium at Rhenium Utilizing Light and Proton-Coupled Electron Transfer.
Bruch, Quinton J.; Connor, Gannon P.; Chen, Chun-Hsing; Holland, Patrick L.; Mayer, James M.; Hasanayn, Faraj; Miller, Alexander J. M.; Journal of the American Chemical Society  (2019) –; doi:10.1021/jacs.9b10031

data_4133756
_publ_section_title
;
 Dinitrogen Reduction to Ammonium at Rhenium Utilizing Light and
 Proton-Coupled Electron Transfer.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.9b10031
_journal_year                    2019
_chemical_formula_moiety         'C17 H31 Cl2 N2 O2 P2 Re'
_chemical_formula_sum            'C17 H31 Cl2 N2 O2 P2 Re'
_chemical_formula_weight         614.48
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-08-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 99.3350(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.3593(2)
_cell_length_b                   16.8784(2)
_cell_length_c                   15.7289(2)
_cell_measurement_reflns_used    9841
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.05
_cell_measurement_theta_min      4.39
_cell_volume                     4547.49(10)
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0304
_diffrn_reflns_av_unetI/netI     0.0197
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            51233
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.111
_diffrn_reflns_theta_min         2.579
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    14.064
_exptl_absorpt_correction_T_max  0.3148
_exptl_absorpt_correction_T_min  0.0862
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0897 before and 0.0429 after correction. The Ratio of minimum to maximum transmission is 0.2738. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.795
_exptl_crystal_description       block
_exptl_crystal_F_000             2416
_exptl_crystal_size_max          0.254
_exptl_crystal_size_mid          0.194
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.569
_refine_diff_density_min         -1.667
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.229
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     485
_refine_ls_number_reflns         8561
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.229
_refine_ls_R_factor_all          0.0349
_refine_ls_R_factor_gt           0.0338
_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^)+(0.0148P)^2^+26.9414P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0729
_refine_ls_wR_factor_ref         0.0734
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8273
_reflns_number_total             8561
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b10031_si_002.cif
_cod_data_source_block           x1804003
_cod_database_code               4133756
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.186
_shelx_estimated_absorpt_t_min   0.124
_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.a Ternary CH refined with riding coordinates:
 C6(H6), C12(H12), C9(H9), C15(H15), C23(H23), C29(H29), C32(H32), C26(H26)
2.b Aromatic/amide H refined with riding coordinates:
 C21(H21), C20(H20), C3(H3), C2(H2), C19(H19), C4(H4)
2.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C8(H8A,H8B,H8C), C7(H7A,H7B,H7C), C24(H24A,H24B,H24C),
 C33(H33A,H33B,H33C), C10(H10A,H10B,H10C), C27(H27A,H27B,H27C), C34(H34A,H34B,
 H34C), C25(H25A,H25B,H25C), C13(H13A,H13B,H13C), C28(H28A,H28B,H28C), C11(H11A,
 H11B,H11C), C14(H14A,H14B,H14C), C17(H17A,H17B,H17C), C30(H30A,H30B,H30C),
 C31(H31A,H31B,H31C)
;
_shelx_res_checksum              92742
_shelx_hkl_checksum              94632
_olex2_submission_special_instructions 'No special instructions were received'