Ammonia synthesis by hydrogenolysis of titanium-nitrogen bonds using proton coupled electron transfer.
Pappas, Iraklis; Chirik, Paul J.; Journal of the American Chemical Society 137 (2015) 3498–3501; doi:10.1021/jacs.5b01047

data_4129354
_publ_section_title
;
 Ammonia synthesis by hydrogenolysis of titanium-nitrogen bonds using
 proton coupled electron transfer.
;
_journal_issue                   10
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3498
_journal_page_last               3501
_journal_paper_doi               10.1021/jacs.5b01047
_journal_volume                  137
_journal_year                    2015
_chemical_formula_sum            'C56 H57 B F24 N Si2 Ti'
_chemical_formula_weight         1314.91
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                96.383(2)
_cell_angle_beta                 92.742(2)
_cell_angle_gamma                95.117(2)
_cell_formula_units_Z            2
_cell_length_a                   13.9923(9)
_cell_length_b                   14.3520(9)
_cell_length_c                   14.8495(8)
_cell_measurement_reflns_used    9008
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.00
_cell_measurement_theta_min      2.41
_cell_volume                     2946.7(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP 3 (Farraguia, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR 92 (Giacavazzo, 1993)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'BRUKER APEX2 CCD'
_diffrn_measurement_method       'Phi and Omega Scans'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2238
_diffrn_reflns_av_unetI/netI     0.0691
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            157607
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         2.145
_exptl_absorpt_coefficient_mu    0.300
_exptl_absorpt_correction_T_max  0.917
_exptl_absorpt_correction_T_min  0.825
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_description       Columnar
_exptl_crystal_F_000             1342
_exptl_crystal_size_max          0.616
_exptl_crystal_size_mid          0.435
_exptl_crystal_size_min          0.262
_refine_diff_density_max         1.590
_refine_diff_density_min         -1.406
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     807
_refine_ls_number_reflns         13506
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0960
_refine_ls_R_factor_gt           0.0795
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1122P)^2^+7.2062P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1982
_refine_ls_wR_factor_ref         0.2237
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10969
_reflns_number_total             13506
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b01047_si_001.cif
_cod_data_source_block           ip63
_cod_database_code               4129354
_shelx_estimated_absorpt_t_min   0.837
_shelx_estimated_absorpt_t_max   0.926
_shelxl_version_number           2014-3
_shelx_res_checksum              53051
_shelx_hkl_checksum              52147