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_4125910
_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
'2(C20 H45 N2 P2 Ru0.94), 2(B F4), C4 H8 O, 0.12(Ru)'
_chemical_formula_sum            'C44 H98 B2 F8 N4 O P4 Ru2'
_chemical_formula_weight         1198.90
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2017-01-11
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5289)
;
_cell_angle_alpha                90
_cell_angle_beta                 96.8021(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   28.0407(4)
_cell_length_b                   14.5457(2)
_cell_length_c                   14.2999(2)
_cell_measurement_reflns_used    9964
_cell_measurement_temperature    100
_cell_measurement_theta_max      66.59
_cell_measurement_theta_min      3.17
_cell_volume                     5791.47(14)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0991
_diffrn_reflns_av_unetI/netI     0.0569
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            35736
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        66.601
_diffrn_reflns_theta_max         66.601
_diffrn_reflns_theta_min         3.174
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.774
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.5371
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1038 before and 0.0847 after correction.
The Ratio of minimum to maximum transmission is 0.7135.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.375
_exptl_crystal_description       block
_exptl_crystal_F_000             2512
_exptl_crystal_size_max          0.142
_exptl_crystal_size_mid          0.056
_exptl_crystal_size_min          0.023
_refine_diff_density_max         1.343
_refine_diff_density_min         -0.494
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         5108
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0618
_refine_ls_R_factor_gt           0.0471
_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^)+(0.0709P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1091
_refine_ls_wR_factor_ref         0.1177
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4105
_reflns_number_total             5108
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b01323_si_003.cif
_cod_data_source_block           x1609003
_cod_depositor_comments
'Adding full bibliography for 4125910--4125911.cif.'
_cod_database_code               4125910
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.879
_shelx_estimated_absorpt_t_min   0.494
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(Ru1) = Uanis(Ru1A)
3. Others
 Sof(Ru1A)=1-FVAR(1)
 Sof(Ru1)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 N15(H15)
4.b Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C14(H14A,H14B), C16(H16A,H16B), C17(H17A,H17B), C32(H32A,
 H32B), C33(H33A,H33B)
4.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C),
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C19(H19A,H19B,H19C), C20(H20A,H20B,
 H20C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C25(H25A,
 H25B,H25C)
;
_olex2_date_sample_data_collection 2016-09-07
_olex2_date_sample_submission    2016-09-07
_olex2_submission_original_sample_id RuNBF4
_olex2_submission_special_instructions 'No special instructions were received'