Simple Synthesis of (Triphenylphosphoniomethylidene)(pentamethylcyclopentadienyl)titanium(II) Dichloride and Its Unexpected Reduction To Form a Trinuclear Titanium Cluster
Wang, Aichen; Sun, Hongjian; Li, Xiaoyan; Organometallics 28 (2009) 5285–; doi:10.1021/om9005406

data_4069963
_publ_section_title
;
 Simple Synthesis of
 (Triphenylphosphoniomethylidene)(pentamethylcyclopentadienyl)titanium(II)
 Dichloride and Its Unexpected Reduction To Form a Trinuclear Titanium
 Cluster
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              5285
_journal_paper_doi               10.1021/om9005406
_journal_volume                  28
_journal_year                    2009
_chemical_formula_sum            'C29 H31 Cl2 N0 O0 P Ti'
_chemical_formula_weight         529.31
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.434(16)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.493(2)
_cell_length_b                   16.578(3)
_cell_length_c                   15.602(3)
_cell_measurement_reflns_used    1179
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      19.67
_cell_measurement_theta_min      2.46
_cell_volume                     2650.4(9)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.1420
_diffrn_reflns_av_sigmaI/netI    0.1419
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            22560
_diffrn_reflns_theta_full        27.39
_diffrn_reflns_theta_max         27.39
_diffrn_reflns_theta_min         1.82
_exptl_absorpt_coefficient_mu    0.601
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.327
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1104
_refine_diff_density_max         0.313
_refine_diff_density_min         -0.349
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.954
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     303
_refine_ls_number_reflns         5997
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.954
_refine_ls_R_factor_all          0.1667
_refine_ls_R_factor_gt           0.0602
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0573P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1152
_refine_ls_wR_factor_ref         0.1519
_reflns_number_gt                2747
_reflns_number_total             5997
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om9005406_si_002.cif
_cod_data_source_block           080103c
_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        2650.2(10)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4069963