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_4133757
_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         'C34 H62.00 Cl4 N4 O4 P4 Re2'
_chemical_formula_sum            'C34 H62 Cl4 N4 O4 P4 Re2'
_chemical_formula_weight         1229.00
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_creation_date             2019-06-06
_audit_creation_method           CRYSTALS_ver_14.61_build_6236
_cell_angle_alpha                90
_cell_angle_beta                 99.1846(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.8067(4)
_cell_length_b                   10.1615(2)
_cell_length_c                   22.6120(5)
_cell_measurement_reflns_used    9915
_cell_measurement_temperature    150
_cell_measurement_theta_max      73
_cell_measurement_theta_min      4
_cell_volume                     4492.67(16)
_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    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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     1.54178
_diffrn_reflns_av_R_equivalents  0.037
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            24690
_diffrn_reflns_theta_full        72.487
_diffrn_reflns_theta_max         72.487
_diffrn_reflns_theta_min         3.961
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    14.235
_exptl_absorpt_correction_T_max  0.49
_exptl_absorpt_correction_T_min  0.06
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.817
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2416.000
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.050
_refine_diff_density_max         2.27
_refine_diff_density_min         -1.60
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         4437
_refine_ls_number_restraints     543
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0505
_refine_ls_shift/su_max          0.0112073
_refine_ls_shift/su_mean         0.0013499
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.04P)^2^ +*****P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1159
_refine_ls_wR_factor_gt          0.1143
_refine_ls_wR_factor_ref         0.1159
_reflns_limit_h_max              23
_reflns_limit_h_min              -24
_reflns_limit_k_max              12
_reflns_limit_k_min              0
_reflns_limit_l_max              27
_reflns_limit_l_min              0
_reflns_number_gt                4197
_reflns_number_total             4455
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.97
_oxford_diffrn_Wilson_scale      678.75
_oxford_refine_ls_r_factor_ref   0.0526
_oxford_refine_ls_scale          0.042890(8)
_oxford_reflns_number_all        4437
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title '19011_0m in C2/c'
_cod_data_source_file            ja9b10031_si_002.cif
_cod_data_source_block           19011
_cod_original_sg_symbol_H-M      'C 2/c '
_cod_original_formula_sum        'C34 H62.00 Cl4 N4 O4 P4 Re2'
_cod_database_code               4133757