Synthesis, structure and reactivity of the hexaphospha-titanocene, bis-(η5-3,5-di-tert-butyl-1,2,4-triphosphacyclopentadienyl)titanium(II)
Cloke, F. Geoffrey N.; Hanks, John R.; Hitchcock, Peter B.; Nixon, John F.; Chemical Communications  (1999) 1731–; doi:10.1039/a905469c

data_7115242
_publ_section_title
;
 Synthesis, structure and reactivity of the hexaphospha-titanocene,
 bis-(\h5-3,5-di-tert-butyl-1,2,4-triphosphacyclopentadienyl)titanium(II)
;
_journal_issue                   17
_journal_name_full               'Chemical Communications'
_journal_page_first              1731
_journal_paper_doi               10.1039/a905469c
_journal_year                    1999
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C25 H39 P7 Ti1'
_chemical_formula_structural     'C25 H39 P7 TI'
_chemical_formula_sum            'C25 H45 P7 Ti'
_chemical_formula_weight         610.3
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_conform_dict_location     ftp://ftp.iucr.org/cifdics/cif_core2.1beta.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.1beta3
_audit_creation_date             1999-05-04T13:10:04-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                86.48(5)
_cell_angle_beta                 71.00(5)
_cell_angle_gamma                68.75(4)
_cell_formula_units_Z            2
_cell_length_a                   10.299(5)
_cell_length_b                   11.910(6)
_cell_length_c                   14.230(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      8.7
_cell_measurement_theta_min      7.4
_cell_measurement_wavelength     0.71073
_cell_volume                     1535.0(17)
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1998)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'scintillation LiI'
_diffrn_detector_dtime           1.195
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf Nonius TurboCAD4'
_diffrn_measurement_method       'non-profiled omega/2theta scans'
_diffrn_orient_matrix_type
;
  x-axis points to radiation source
  the matrix is specified in reciprocal space
;
_diffrn_orient_matrix_UB_11      -0.14476E-1
_diffrn_orient_matrix_UB_12      0.76409E-1
_diffrn_orient_matrix_UB_13      -0.03562
_diffrn_orient_matrix_UB_21      -0.101788
_diffrn_orient_matrix_UB_22      0.5963E-2
_diffrn_orient_matrix_UB_23      0.5872E-2
_diffrn_orient_matrix_UB_31      -0.40129E-1
_diffrn_orient_matrix_UB_32      0.47755E-1
_diffrn_orient_matrix_UB_33      0.65298E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0
_diffrn_reflns_av_sigmaI/netI    0.061
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5362
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.24
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.657
_exptl_absorpt_correction_T_max  0.9054
_exptl_absorpt_correction_T_min  0.2065
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
        Walker, N. & Stuart, D (1983) Acta. Cryst. A39, 158-166
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.32
_exptl_crystal_density_method    none
_exptl_crystal_description       plate
_exptl_crystal_F_000             644
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.306
_refine_diff_density_min         -1.023
_refine_diff_density_rms         0.15
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.007
_refine_ls_goodness_of_fit_gt    1.081
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         5362
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.007
_refine_ls_restrained_S_obs      1.081
_refine_ls_R_factor_all          0.0992
_refine_ls_R_factor_gt           0.0765
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1512P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.212
_refine_ls_wR_factor_gt          0.1964
_reflns_number_gt                4021
_reflns_number_total             5362
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            905469c.txt
_cod_data_source_block           may899
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1512P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1512P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1535.1(16)
_cod_database_code               7115242
_exptl_absorpt_factor_mur        0.099
_diffrn_standards_decay_corr_max 1.051
_diffrn_standards_decay_corr_min 0.993