Ammonia Synthesis from a Pincer Ruthenium Nitride via Metal-Ligand Cooperative Proton-Coupled Electron Transfer.
Lindley, Brian M.; Bruch, Quinton J.; White, Peter S.; Hasanayn, Faraj; Miller, Alexander J. M.; Journal of the American Chemical Society 139 (2017) 5305–5308; doi:10.1021/jacs.7b01323

data_4125911
_publ_section_title
;
 Ammonia Synthesis from a Pincer Ruthenium Nitride via Metal-Ligand
 Cooperative Proton-Coupled Electron Transfer.
;
_journal_issue                   15
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5305
_journal_page_last               5308
_journal_paper_doi               10.1021/jacs.7b01323
_journal_volume                  139
_journal_year                    2017
_chemical_formula_moiety         'C28 H53 N2 O3 P2 Ru, B F4'
_chemical_formula_sum            'C28 H53 B F4 N2 O3 P2 Ru'
_chemical_formula_weight         715.54
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2016-08-29
_audit_creation_method
;
Olex2 1.2
(compiled 2016.08.25 svn.r3337 for OlexSys, GUI svn.r5221)
;
_cell_angle_alpha                113.1776(13)
_cell_angle_beta                 100.0148(15)
_cell_angle_gamma                92.8470(15)
_cell_formula_units_Z            2
_cell_length_a                   9.2072(2)
_cell_length_b                   13.6297(3)
_cell_length_c                   16.4432(3)
_cell_measurement_reflns_used    9948
_cell_measurement_temperature    100
_cell_measurement_theta_max      66.60
_cell_measurement_theta_min      3.56
_cell_volume                     1852.06(7)
_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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_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  0.0691
_diffrn_reflns_av_unetI/netI     0.0369
_diffrn_reflns_Laue_measured_fraction_full 0.966
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            47316
_diffrn_reflns_point_group_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        66.660
_diffrn_reflns_theta_max         66.660
_diffrn_reflns_theta_min         2.990
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.655
_exptl_absorpt_correction_T_max  0.8714
_exptl_absorpt_correction_T_min  0.4647
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0885 before and 0.0712 after correction.
The Ratio of minimum to maximum transmission is 0.5333.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.283
_exptl_crystal_description       plate
_exptl_crystal_F_000             748
_exptl_crystal_size_max          0.225
_exptl_crystal_size_mid          0.138
_exptl_crystal_size_min          0.052
_refine_diff_density_max         0.624
_refine_diff_density_min         -0.381
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     384
_refine_ls_number_reflns         6316
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0334
_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^)+(0.0445P)^2^+1.2889P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0810
_refine_ls_wR_factor_ref         0.0842
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5592
_reflns_number_total             6316
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b01323_si_003.cif
_cod_data_source_block           x1608007
_cod_depositor_comments
'Adding full bibliography for 4125910--4125911.cif.'
_cod_database_code               4125911
_shelx_estimated_absorpt_t_max   0.794
_shelx_estimated_absorpt_t_min   0.421
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C13(H13A,H13B), C16(H16A,H16B)
2.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C30(H30), C31(H31), C35(H35), C36(H36)
2.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C10(H10A,
 H10B,H10C), C11(H11A,H11B,H11C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C),
 C20(H20A,H20B,H20C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), N25(H25A,H25B,H25C), C34(H34A,H34B,H34C)
;
_shelx_fab_checksum              12310
_shelx_shelxl_version_number     2014/7
_olex2_submission_original_sample_id RuNH3
_olex2_submission_special_instructions 'No special instructions were received'