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_4072587
_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         ' C21 H23 Br2 Cl N2 Ti '
_chemical_formula_sum            'C21 H23 Br2 Cl N2 Ti'
_chemical_formula_weight         546.59
_chemical_name_systematic
;                                      
Cp*Ti(N-2,6-C6H3Br2)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                97.8878(12)
_cell_angle_beta                 90.4074(12)
_cell_angle_gamma                111.1461(14)
_cell_formula_units_Z            2
_cell_length_a                   8.6809(2)
_cell_length_b                   9.7070(3)
_cell_length_c                   13.8311(5)
_cell_measurement_reflns_used    18043
_cell_measurement_temperature    150
_cell_measurement_theta_max      28
_cell_measurement_theta_min      5
_cell_volume                     1074.70(6)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.040
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            18043
_diffrn_reflns_theta_full        27.485
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         5.173
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.249
_exptl_absorpt_correction_T_max  0.65
_exptl_absorpt_correction_T_min  0.55
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 Denzo/Scalepack (Otwinowski & Minor, 1996) 
;
_exptl_crystal_colour            ' brown '
_exptl_crystal_density_diffrn    1.689
_exptl_crystal_description       ' fragment '
_exptl_crystal_F_000             544
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.55
_refine_diff_density_min         -0.70
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0423
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         3791
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0460
_refine_ls_R_factor_gt           0.0331
_refine_ls_shift/su_max          0.006466
_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: 
 0.856 0.384 0.504 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0534
_refine_ls_wR_factor_gt          0.0387
_refine_ls_wR_factor_ref         0.0387
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              12
_reflns_limit_k_min              -12
_reflns_limit_l_max              17
_reflns_limit_l_min              0
_reflns_number_gt                3791
_reflns_number_total             4860
_reflns_threshold_expression     I>3.00u(I)
_cod_data_source_file            om0608556si20060918_031255.cif
_cod_data_source_block           COMPOUND_3
_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        ' C21 H23 Br2 Cl N2 Ti '
_cod_database_code               4072587