Preparation of Ti(IV) Fluoride N-Heterocyclic Carbene Complexes
Grigory B. Nikiforov; Herbert W. Roesky; Peter G. Jones; Jörg Magull; Arne Ringe; Rainer B. Oswald; Inorganic Chemistry 47 (2008) 2171–2179; doi:10.1021/ic701751r

data_4304269
_publ_contact_author_address
;Institut fuer Anorganische Chemie
Universitaet Goettingen
Tammannstr. 4
37077 Goettingen
Germany
;
_publ_contact_author_email       hroesky@gwdg.de
_publ_contact_author_fax         '0049 /551 /39-3373'
_publ_contact_author_name        'Herbert W. Roesky'
_publ_contact_author_phone       '0049/ 551/ 39-3001'
_publ_section_title
;
Preparation of Ti(IV) Fluoride N-Heterocyclic Carbene Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2171
_journal_page_last               2179
_journal_paper_doi               10.1021/ic701751r
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C22 H40 F4 N4 Ti'
_chemical_formula_weight         484.48
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     Patterson
_atom_sites_solution_secondary   'tangent expansion'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 104.688(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.3210(6)
_cell_length_b                   12.2112(4)
_cell_length_c                   15.0316(4)
_cell_measurement_reflns_used    9847
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.43
_cell_measurement_theta_min      2.18
_cell_volume                     2542.77(16)
_computing_cell_refinement       'Bruker APEX2'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Siemens XP'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX2 CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0437
_diffrn_reflns_av_sigmaI/netI    0.0323
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            70374
_diffrn_reflns_theta_full        31.00
_diffrn_reflns_theta_max         31.00
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    0.381
_exptl_absorpt_correction_T_max  0.9702
_exptl_absorpt_correction_T_min  0.8321
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.266
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       prism
_exptl_crystal_F_000             1032
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.378
_refine_diff_density_min         -0.424
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    'rigid methyls, others riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     292
_refine_ls_number_reflns         8091
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0540
_refine_ls_R_factor_gt           0.0357
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0464P)^2^+0.8743P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0894
_refine_ls_wR_factor_ref         0.0983
_reflns_number_gt                6274
_reflns_number_total             8091
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic701751r-file005.cif
_cod_data_source_block           goegg
_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.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        2542.77(15)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4304269