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_4129352
_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            'C24 H42 Cl N Si2 Ti'
_chemical_formula_weight         484.11
_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   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                84.7470(10)
_cell_angle_beta                 84.9590(10)
_cell_angle_gamma                82.0550(10)
_cell_formula_units_Z            4
_cell_length_a                   8.8819(4)
_cell_length_b                   16.3974(8)
_cell_length_c                   18.2158(9)
_cell_measurement_reflns_used    9877
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.55
_cell_measurement_theta_min      2.49
_cell_volume                     2608.8(2)
_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 0.992
_diffrn_measurement_device_type  'BRUKER APEX2 CCD'
_diffrn_measurement_method       'Phi and Omega Scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0409
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            11926
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.577
_diffrn_reflns_theta_min         1.126
_exptl_absorpt_coefficient_mu    0.534
_exptl_absorpt_correction_T_max  0.745553
_exptl_absorpt_correction_T_min  0.637957
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.233
_exptl_crystal_description       Columnar
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.156
_exptl_crystal_size_mid          0.126
_exptl_crystal_size_min          0.119
_refine_diff_density_max         1.904
_refine_diff_density_min         -0.748
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.852
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     566
_refine_ls_number_reflns         11926
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      0.880
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.0493
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0910P)^2^+6.7218P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1289
_refine_ls_wR_factor_ref         0.1413
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10849
_reflns_number_total             11926
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b01047_si_001.cif
_cod_data_source_block           ip60
_cod_database_code               4129352
_shelx_estimated_absorpt_t_min   0.921
_shelx_estimated_absorpt_t_max   0.939
_shelxl_version_number           2014-3
_shelx_hkl_checksum              49881