Di-μ-chloro-bis[(<i>N</i>-<i>tert</i>-butylimido)chlorobis(pyridine-κ<i>N</i>)titanium(IV)] perdeuterobenzene disolvate
Nilay Hazari; Andrew R. Cowley; Philip Mountford; Acta Crystallographica Section E 60 (2004) m1844–m1846; doi:10.1107/S160053680402865X

data_2204708
_publ_section_title
;Di-\m-chloro-bis[(<i>N</i>-<i>tert</i>-butylimido)chlorobis(pyridine-\k<i>N</i>)titanium(IV)]
 perdeuterobenzene disolvate
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1844
_journal_page_last               m1846
_journal_paper_doi               10.1107/S160053680402865X
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          '[Ti2 (C4 H9 N)2 Cl2 (C5 H5 N)4], 2C6 D6'
_chemical_formula_moiety         'C28 H38 Cl4 N6 Ti2, 2C6 D6'
_chemical_formula_sum            'C40 H38 Cl4 D12 N6 Ti2'
_chemical_formula_weight         864.58
_chemical_name_systematic
;
Di-\m-chloro-bis[(N-tert-butylimido)chlorobis(pyridine-\kN)titanium(IV)]
benzene disolvate
;
_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                101.6259(9)
_cell_angle_beta                 90.1675(10)
_cell_angle_gamma                103.4005(11)
_cell_formula_units_Z            1
_cell_length_a                   8.0662(2)
_cell_length_b                   11.0937(2)
_cell_length_c                   12.7589(3)
_cell_measurement_reflns_used    18502
_cell_measurement_temperature    150
_cell_measurement_theta_max      28
_cell_measurement_theta_min      5
_cell_volume                     1086.37(4)
_computing_cell_refinement
;
DENZO
;
_computing_data_collection
;
COLLECT (Nonius, 2000)
;
_computing_data_reduction
;
DENZO (Otwinowski & Minor, 1996)
;
_computing_molecular_graphics
;
CAMERON (Watkin et al., 1996)
;
_computing_publication_material
;
CRYSTALS
;
_computing_structure_refinement
;
CRYSTALS (Watkin et al., 2003)
;
_computing_structure_solution
;
SIR92 (Altomare et al., 1994)
;
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
;
Nonius KappaCCD
;
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.028
_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            18502
_diffrn_reflns_theta_full        27.417
_diffrn_reflns_theta_max         27.417
_diffrn_reflns_theta_min         5.103
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.648
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.82
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(DENZO/SCALEPACK; Otwinowski & Minor, 1996)'
_exptl_crystal_colour            'pale orange'
_exptl_crystal_density_diffrn    1.321
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             444
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.24
_refine_diff_density_min         -0.42
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0289
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     252
_refine_ls_number_reflns         3925
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0301
_refine_ls_shift/su_max          0.018808
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial (Watkin, 1994; Prince, 1983):
[weight] = 1/[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, 1983):
W = [weight][1-(\dF/6\sF)^2^]^2^, where A~i~ are
1.08, 0.471 and 0.742
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0455
_refine_ls_wR_factor_gt          0.0365
_refine_ls_wR_factor_ref         0.0365
_reflns_number_gt                3925
_reflns_number_total             4933
_reflns_threshold_expression     I>3\s(I)
_cod_data_source_file            hg6108.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               2204708