Simple Synthesis of (Triphenylphosphoniomethylidene)(pentamethylcyclopentadienyl) titanium(IV) Dichloride and Its Reaction with Carbon Monoxide
Liu, Nazhen; Wang, Aichen; Sun, Hongjian; Li, Xiaoyan; Organometallics 29 (2010) 1996–; doi:10.1021/om1001588

data_4065835
_publ_section_title
;
 Simple Synthesis of
 (Triphenylphosphoniomethylidene)(pentamethylcyclopentadienyl)
 titanium(IV) Dichloride and Its Reaction with Carbon Monoxide
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              1996
_journal_paper_doi               10.1021/om1001588
_journal_volume                  29
_journal_year                    2010
_chemical_formula_moiety         'C30 H31 Cl2 O P Ti '
_chemical_formula_sum            'C30 H31 Cl2 O P Ti'
_chemical_formula_weight         557.29
_chemical_name_systematic
; 
 ? 
;
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                88.518(15)
_cell_angle_beta                 73.931(14)
_cell_angle_gamma                63.486(14)
_cell_formula_units_Z            4
_cell_length_a                   14.517(11)
_cell_length_b                   15.480(11)
_cell_length_c                   17.133(13)
_cell_measurement_reflns_used    854
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      16.00
_cell_measurement_theta_min      2.49
_cell_volume                     3289(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  '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  0.0893
_diffrn_reflns_av_sigmaI/netI    0.2032
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14273
_diffrn_reflns_theta_full        23.45
_diffrn_reflns_theta_max         23.45
_diffrn_reflns_theta_min         1.24
_exptl_absorpt_coefficient_mu    0.489
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.125
_exptl_crystal_density_meas      1.125
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.823
_refine_diff_density_min         -0.576
_refine_diff_density_rms         0.211
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     641
_refine_ls_number_reflns         9600
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.2588
_refine_ls_R_factor_gt           0.1243
_refine_ls_shift/su_max          0.111
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3225
_refine_ls_wR_factor_ref         0.4114
_reflns_number_gt                3517
_reflns_number_total             9600
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om1001588_si_001.cif
_cod_data_source_block           test
_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        'C30 H31 Cl2 O P Ti '
_cod_database_code               4065835