Zirconium and Titanium Propylene Polymerization Precatalysts Supported by a FluxionalC2-Symmetric Bis(anilide)pyridine Ligand
Tonks, Ian A.; Tofan, Daniel; Weintrob, Edward C.; Agapie, Theodor; Bercaw, John E.; Organometallics 31 (2012) 1965–; doi:10.1021/om201262h

data_4076495
_publ_section_title
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 Zirconium and Titanium Propylene Polymerization Precatalysts Supported by
 a FluxionalC2-Symmetric Bis(anilide)pyridine Ligand
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1965
_journal_paper_doi               10.1021/om201262h
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C35 H33 Cl2 N3 Ti, C4 H8 O'
_chemical_formula_sum            'C39 H41 Cl2 N3 O Ti'
_chemical_formula_weight         686.55
_chemical_name_systematic
;

 ?

;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 109.665(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   36.2843(15)
_cell_length_b                   11.6553(5)
_cell_length_c                   16.9710(8)
_cell_measurement_reflns_used    9047
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.08
_cell_measurement_theta_min      2.52
_cell_volume                     6758.5(5)
_computing_cell_refinement       'Bruker SAINT-Plus v7.34A'
_computing_data_collection       'Bruker APEX2 v2.1-0'
_computing_data_reduction        'Bruker SAINT-Plus v7.34A'
_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 0.944
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measurement_device_type  'Bruker KAPPA APEX II'
_diffrn_measurement_method       '\w scans; 17 settings'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0527
_diffrn_reflns_av_sigmaI/netI    0.0524
_diffrn_reflns_limit_h_max       55
_diffrn_reflns_limit_h_min       -55
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            99635
_diffrn_reflns_theta_full        33.19
_diffrn_reflns_theta_max         33.19
_diffrn_reflns_theta_min         1.85
_exptl_absorpt_coefficient_mu    0.448
_exptl_absorpt_correction_T_max  0.9780
_exptl_absorpt_correction_T_min  0.8555
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Red-brown
_exptl_crystal_density_diffrn    1.349
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Blade
_exptl_crystal_F_000             2880
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.441
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_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    Unrestrained
_refine_ls_matrix_type           'Full matrix'
_refine_ls_number_parameters     579
_refine_ls_number_reflns         12205
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.938
_refine_ls_R_factor_all          0.0703
_refine_ls_R_factor_gt           0.0420
_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          0.0523
_refine_ls_wR_factor_ref         0.0533
_reflns_number_gt                8505
_reflns_number_total             12205
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om201262h_si_002.cif
_cod_data_source_block           complex4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_refine_ls_weighting_scheme' value 'Sigma' changed to
'sigma' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

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

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

'_atom_sites_solution_hydrogens' value 'Difference Fourier map' was
changed to 'difmap'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4076495