Catalytic Proton Coupled Electron Transfer from Metal Hydrides to Titanocene Amides, Hydrazides and Imides: Determination of Thermodynamic Parameters Relevant to Nitrogen Fixation.
Pappas, Iraklis; Chirik, Paul J.; Journal of the American Chemical Society 138 (2016) 13379–13389; doi:10.1021/jacs.6b08009

data_4130951
_publ_section_title
;
 Catalytic Proton Coupled Electron Transfer from Metal Hydrides to
 Titanocene Amides, Hydrazides and Imides: Determination of Thermodynamic
 Parameters Relevant to Nitrogen Fixation.
;
_journal_issue                   40
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13379
_journal_page_last               13389
_journal_paper_doi               10.1021/jacs.6b08009
_journal_volume                  138
_journal_year                    2016
_chemical_formula_sum            'C39 H55 Cl Cr O3 Si2 Ti'
_chemical_formula_weight         763.33
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                83.424(7)
_cell_angle_beta                 81.854(6)
_cell_angle_gamma                87.114(7)
_cell_formula_units_Z            2
_cell_length_a                   9.1532(7)
_cell_length_b                   12.5803(13)
_cell_length_c                   17.0067(12)
_cell_measurement_reflns_used    8301
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      63.72
_cell_measurement_theta_min      3.54
_cell_volume                     1924.6(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 'ACTA 50'
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0604
_diffrn_reflns_av_sigmaI/netI    0.0465
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            20986
_diffrn_reflns_theta_full        'ACTA 50'
_diffrn_reflns_theta_max         63.89
_diffrn_reflns_theta_min         3.54
_exptl_absorpt_coefficient_mu    5.594
_exptl_absorpt_correction_T_max  0.8501
_exptl_absorpt_correction_T_min  0.4162
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.317
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Columnar
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.913
_refine_diff_density_min         -0.456
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     439
_refine_ls_number_reflns         6065
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0644
_refine_ls_R_factor_gt           0.0490
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0763P)^2^+2.1683P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1232
_refine_ls_wR_factor_ref         0.1331
_reflns_number_gt                4941
_reflns_number_total             6065
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja6b08009_si_002.cif
_cod_data_source_block           ip48
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Triclinic' was changed to
'triclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      'P-1   '
_cod_original_formula_sum        'C39 H55 Cl1 Cr1 O3 Si2 Ti1'
_cod_database_code               4130951