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_4129357
_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 Si2 Zr'
_chemical_formula_weight         513.42
_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
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_cell_measurement_reflns_used    9923
_cell_measurement_temperature    100(2)
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_cell_measurement_theta_min      2.59
_cell_volume                     1328.81(8)
_computing_cell_refinement       'Bruker SAINT'
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_computing_molecular_graphics    'ORTEP 3 (Farraguia, 1997)'
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_computing_structure_solution    'SIR 92 (Giacavazzo, 1993)'
_diffrn_ambient_temperature      100(2)
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_diffrn_measured_fraction_theta_max 0.996
_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
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_diffrn_reflns_Laue_measured_fraction_max 0.996
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_diffrn_reflns_limit_l_min       -27
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_diffrn_reflns_point_group_measured_fraction_max 0.996
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_diffrn_reflns_theta_max         31.055
_diffrn_reflns_theta_min         2.586
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_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.7042
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.283
_exptl_crystal_description       columnar
_exptl_crystal_F_000             542
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_exptl_crystal_size_min          0.100
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_refine_diff_density_min         -0.621
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_refine_ls_extinction_method     none
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_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         8486
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0278
_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^)+(0.0290P)^2^+0.5767P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0604
_refine_ls_wR_factor_ref         0.0635
_reflns_Friedel_coverage         0.000
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_reflns_number_total             8486
_reflns_threshold_expression     'I > 2\s(I)'
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_cod_data_source_block           ip68
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_shelxl_version_number           2014-3
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