Imido titanium compounds bearing the 6-dimethylamino-1,4,6-trimethyl-1,4-diazacycloheptane ligand: synthesis, structures, solution dynamics and ethylene polymerisation capability
Hayday, Gregory J.; Wang, Chao; Rees, Nicholas H.; Mountford, Philip; Dalton Transactions  (2008) 3301–3310; doi:10.1039/b802027b

data_7004016
_publ_section_title
;
 Imido titanium compounds bearing the
 6-dimethylamino-1,4,6-trimethyl-1,4-diazacycloheptane ligand:
 synthesis, structures, solution dynamics and ethylene polymerisation
 capability
;
_journal_issue                   25
_journal_name_full               'Dalton Transactions'
_journal_page_first              3301
_journal_page_last               3310
_journal_paper_doi               10.1039/b802027b
_journal_year                    2008
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C20 H36 Cl2 N4 Ti1'
_chemical_formula_sum            'C20 H36 Cl2 N4 Ti'
_chemical_formula_weight         451.34
_chemical_name_systematic
;
Ti(N-2-C6H4tBu)(Me4DACH)Cl2
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.3237(9)
_cell_length_b                   12.9435(4)
_cell_length_c                   7.7526(3)
_cell_measurement_reflns_used    2903
_cell_measurement_temperature    150
_cell_measurement_theta_max      28
_cell_measurement_theta_min      5
_cell_volume                     2340.43(15)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997-2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.986
_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  0.000
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            5186
_diffrn_reflns_theta_full        26.347
_diffrn_reflns_theta_max         27.445
_diffrn_reflns_theta_min         5.245
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.606
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_correction_T_min  0.93
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.281
_exptl_crystal_description       block
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.49
_refine_diff_density_min         -0.29
_refine_ls_abs_structure_details 'Flack (1983), 2167 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.56(5)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0876
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         2767
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1212
_refine_ls_R_factor_gt           0.0495
_refine_ls_shift/su_max          0.000341
_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:
0.994 0.259E-01 0.764
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1013
_refine_ls_wR_factor_gt          0.0478
_refine_ls_wR_factor_ref         0.0478
_reflns_limit_h_max              30
_reflns_limit_h_min              0
_reflns_limit_k_max              16
_reflns_limit_k_min              0
_reflns_limit_l_max              9
_reflns_limit_l_min              -9
_reflns_number_gt                2767
_reflns_number_total             4998
_reflns_threshold_expression     I>3.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.34
_oxford_diffrn_Wilson_scale      15.77
_oxford_refine_ls_scale          0.2643(6)
_cod_data_source_file            b802027b.txt
_cod_data_source_block           COMPOUND_4-trans
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
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_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'P n a 21 '
_cod_original_formula_sum        'C20 H36 Cl2 N4 Ti1'
_cod_database_code               7004016