Alkyne Hydroamination and Trimerization with Titanium Bis(phenolate)pyridine Complexes: Evidence for Low-Valent Titanium Intermediates and Synthesis of an Ethylene Adduct of Titanium(II)
Tonks, Ian A.; Meier, Josef C.; Bercaw, John E.; Organometallics 32 (2013) 3451–; doi:10.1021/om400080g

data_4089418
_publ_section_title
;
 Alkyne Hydroamination and Trimerization with Titanium
 Bis(phenolate)pyridine Complexes: Evidence for Low-Valent Titanium
 Intermediates and Synthesis of an Ethylene Adduct of Titanium(II)
;
_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              3451
_journal_paper_doi               10.1021/om400080g
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C37 H53 N2 O2 Ti, 0.5(C5 H12)'
_chemical_formula_sum            'C39.5 H59 N2 O2 Ti'
_chemical_formula_weight         641.79
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 104.343(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.7536(5)
_cell_length_b                   10.5239(3)
_cell_length_c                   20.7880(6)
_cell_measurement_reflns_used    9906
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.01
_cell_measurement_theta_min      2.18
_cell_volume                     3762.91(19)
_computing_cell_refinement       'Bruker SAINT-Plus v7.66A'
_computing_data_collection       'Bruker APEX2 v2009.7-0'
_computing_data_reduction        'Bruker SAINT-Plus v7.66A'
_computing_molecular_graphics    'Bruker XP v5.1'
_computing_publication_material  'Bruker XCIF 2008'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.932
_diffrn_measured_fraction_theta_max 0.932
_diffrn_measurement_device_type  'Bruker KAPPA APEX II'
_diffrn_measurement_method       '\w scans; 14 settings'
_diffrn_radiation_monochromator  graphite
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_diffrn_radiation_type           MoK\a
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_diffrn_reflns_av_sigmaI/netI    0.0906
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            109497
_diffrn_reflns_theta_full        29.99
_diffrn_reflns_theta_max         29.99
_diffrn_reflns_theta_min         2.02
_exptl_absorpt_coefficient_mu    0.261
_exptl_absorpt_correction_T_max  0.9794
_exptl_absorpt_correction_T_min  0.9472
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'Dark red'
_exptl_crystal_density_diffrn    1.133
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Blade
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.13
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_refine_ls_matrix_type           'Full matrix'
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_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      2.097
_refine_ls_R_factor_all          0.1167
_refine_ls_R_factor_gt           0.0612
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     w=1/s^2^(Fo^2^)
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.0614
_refine_ls_wR_factor_ref         0.0627
_reflns_number_gt                5835
_reflns_number_total             10215
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400080g_si_002.cif
_cod_data_source_block           7
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_refine_ls_weighting_scheme' value 'Sigma' was changed to
'sigma' 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.

data item '_symmetry_cell_setting' value 'Monoclinic' was changed to
'monoclinic' 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.

data item '_atom_sites_solution_primary' value 'Direct methods' was
changed to 'direct'.

data item '_atom_sites_solution_secondary' value 'Difference Fourier
map' was changed to 'difmap'.

data item '_atom_sites_solution_hydrogens' value 'Geometric
positions' was changed to 'geom'.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_original_formula_sum        'C39.50 H59 N2 O2 Ti'
_cod_database_code               4089418