Cyclopentadienyl Titanium Imido Compounds and Their Ethylene Polymerization Capability: Control of Molecular Weight Distributions by Imido N-Substituents
Owen, Christopher T.; Bolton, Paul D.; Cowley, Andrew R.; Mountford, Philip; Organometallics 26 (2007) 83–; doi:10.1021/om0608556

data_4072589
_publ_section_title
;
 Cyclopentadienyl Titanium Imido Compounds and Their Ethylene
 Polymerization Capability:&#x00A0; Control of Molecular Weight
 Distributions by Imido N-Substituents
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              83
_journal_paper_doi               10.1021/om0608556
_journal_volume                  26
_journal_year                    2007
_chemical_compound_source
;
synthesis as described
;
_chemical_formula_moiety         ' C24 H31 Cl1 N2 Ti1 '
_chemical_formula_sum            'C24 H31 Cl N2 Ti'
_chemical_formula_weight         430.88
_chemical_name_systematic
;                                      
Cp*Ti(N-2,6-C6H4iPr)Cl(py) 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                75.1960(9)
_cell_angle_beta                 82.9984(10)
_cell_angle_gamma                74.2354(12)
_cell_formula_units_Z            2
_cell_length_a                   8.3636(2)
_cell_length_b                   11.5408(3)
_cell_length_c                   12.7908(4)
_cell_measurement_reflns_used    19884
_cell_measurement_temperature    150
_cell_measurement_theta_max      28
_cell_measurement_theta_min      5
_cell_volume                     1146.89(5)
_computing_cell_refinement
; 
KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) 
;
_computing_data_collection
; 
KappaCCD software 'Collect' (Nonius, 2000) 
;
_computing_data_reduction
; 
KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) 
;
_computing_publication_material
; 
CRYSTALS (Watkin et al, 2001) 
;
_computing_structure_refinement
; 
CRYSTALS (Watkin et al, 2001) 
;
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1992)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type
; 
Nonius KappaCCD 
;
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.057
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            19884
_diffrn_reflns_theta_full        26.605
_diffrn_reflns_theta_max         27.428
_diffrn_reflns_theta_min         5.135
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.501
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_correction_T_min  0.88
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 Denzo/Scalepack (Otwinowski & Minor, 1996) 
;
_exptl_crystal_colour            ' brown-red '
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_description       ' fragment '
_exptl_crystal_F_000             456
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.26
_refine_diff_density_min         -0.23
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1242
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         3187
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0699
_refine_ls_R_factor_gt           0.0368
_refine_ls_shift/su_max          0.000219
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 0.284 0.101 0.064 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0711
_refine_ls_wR_factor_gt          0.0391
_refine_ls_wR_factor_ref         0.0391
_reflns_limit_h_max              10
_reflns_limit_h_min              -10
_reflns_limit_k_max              14
_reflns_limit_k_min              -14
_reflns_limit_l_max              16
_reflns_limit_l_min              0
_reflns_number_gt                3187
_reflns_number_total             5175
_reflns_threshold_expression     I>3.00u(I)
_cod_data_source_file            om0608556si20060918_031255.cif
_cod_data_source_block           COMPOUND_5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        ' C24 H31 Cl1 N2 Ti1 '
_cod_database_code               4072589
_refine_special_conditions
;
All hydrogen atoms were positioned geometrically, the preferred
orientations of the methyl H atoms having been previously identified
by examination of a difference Fourier map.
;