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_4129353
_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            'C62 H62 B Cl F25 N Si2 Ti'
_chemical_formula_weight         1446.44
_space_group_crystal_system      orthorhombic
_space_group_IT_number           37
_space_group_name_Hall           'C 2 -2c'
_space_group_name_H-M_alt        'C c c 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   27.6821(6)
_cell_length_b                   27.6929(7)
_cell_length_c                   34.0662(8)
_cell_measurement_reflns_used    9761
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.47
_cell_measurement_theta_min      3.19
_cell_volume                     26115.1(11)
_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 'ACTA 50'
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type  'BRUKER APEX2 CCD'
_diffrn_measurement_method       'Phi and Omega Scans'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0305
_diffrn_reflns_av_unetI/netI     0.0269
_diffrn_reflns_Laue_measured_fraction_full 0.934
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            89998
_diffrn_reflns_point_group_measured_fraction_full 0.935
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        'ACTA 50'
_diffrn_reflns_theta_max         66.587
_diffrn_reflns_theta_min         2.257
_exptl_absorpt_coefficient_mu    2.840
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.5803
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.471
_exptl_crystal_description       Block
_exptl_crystal_F_000             11792
_exptl_crystal_size_max          0.273
_exptl_crystal_size_mid          0.157
_exptl_crystal_size_min          0.116
_refine_diff_density_max         1.628
_refine_diff_density_min         -1.045
_refine_diff_density_rms         0.138
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.460(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.598
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1520
_refine_ls_number_reflns         17631
_refine_ls_number_restraints     97
_refine_ls_restrained_S_all      1.607
_refine_ls_R_factor_all          0.0994
_refine_ls_R_factor_gt           0.0991
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3063
_refine_ls_wR_factor_ref         0.3078
_reflns_Friedel_coverage         0.965
_reflns_Friedel_fraction_full    0.936
_reflns_Friedel_fraction_max     0.960
_reflns_number_gt                17465
_reflns_number_total             17631
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b01047_si_001.cif
_cod_data_source_block           ip61
_cod_database_code               4129353
_shelx_estimated_absorpt_t_min   0.511
_shelx_estimated_absorpt_t_max   0.734
_shelxl_version_number           2014-3
_shelx_res_checksum              95076
_shelx_hkl_checksum              93878