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_4129355
_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 H44 Cl N Si2 Zr'
_chemical_formula_weight         529.45
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 93.886(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
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_cell_length_b                   14.684(5)
_cell_length_c                   20.920(5)
_cell_measurement_reflns_used    9918
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      44.21
_cell_measurement_theta_min      4.64
_cell_volume                     2633.9(19)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0258
_diffrn_reflns_av_unetI/netI     0.0168
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            128654
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         44.274
_diffrn_reflns_theta_min         2.751
_exptl_absorpt_coefficient_mu    0.625
_exptl_absorpt_correction_T_max  0.7847
_exptl_absorpt_correction_T_min  0.6832
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_description       Shard
_exptl_crystal_F_000             1208
_exptl_crystal_size_max          0.392
_exptl_crystal_size_mid          0.148
_exptl_crystal_size_min          0.111
_refine_diff_density_max         3.638
_refine_diff_density_min         -2.800
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     291
_refine_ls_number_reflns         20817
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0375
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0420P)^2^+1.9939P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0933
_refine_ls_wR_factor_ref         0.0994
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18444
_reflns_number_total             20817
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b01047_si_001.cif
_cod_data_source_block           ip64
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4129355
_shelx_estimated_absorpt_t_min   0.764
_shelx_estimated_absorpt_t_max   0.924
_shelxl_version_number           2014-3
_shelx_hkl_checksum              67416