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_4133758
_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         'C37.50 H66 Cl4 N4 O4 P4 Re2'
_chemical_formula_sum            'C37.5 H66 Cl4 N4 O4 P4 Re2'
_chemical_formula_weight         1275.07
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2019-08-13
_audit_creation_method           CRYSTALS_ver_14.61_build_6236
_cell_angle_alpha                90
_cell_angle_beta                 104.8380(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.2061(3)
_cell_length_b                   13.5815(2)
_cell_length_c                   20.4559(4)
_cell_measurement_reflns_used    9890
_cell_measurement_temperature    150
_cell_measurement_theta_max      72
_cell_measurement_theta_min      3
_cell_volume                     4889.38(15)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SHELXS 86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.054
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            67075
_diffrn_reflns_theta_full        72.361
_diffrn_reflns_theta_max         72.361
_diffrn_reflns_theta_min         2.511
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    13.106
_exptl_absorpt_correction_T_max  0.27
_exptl_absorpt_correction_T_min  0.07
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.732
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'block fragment'
_exptl_crystal_F_000             2516
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.28
_refine_diff_density_min         -0.86
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0199
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     532
_refine_ls_number_reflns         9613
_refine_ls_number_restraints     48
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0312
_refine_ls_shift/su_max          0.0123894
_refine_ls_shift/su_mean         0.0005498
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.03P)^2^ +14.08P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0750
_refine_ls_wR_factor_gt          0.0717
_refine_ls_wR_factor_ref         0.0750
_reflns_limit_h_max              21
_reflns_limit_h_min              -22
_reflns_limit_k_max              16
_reflns_limit_k_min              0
_reflns_limit_l_max              25
_reflns_limit_l_min              0
_reflns_number_gt                8337
_reflns_number_total             9653
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0389
_oxford_refine_ls_scale          0.11893(2)
_oxford_reflns_number_all        9613
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title '19024_a.res in P2(1)/c'
_cod_data_source_file            ja9b10031_si_002.cif
_cod_data_source_block           19024
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_original_formula_sum        'C37.50 H66 Cl4 N4 O4 P4 Re2'
_cod_database_code               4133758