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_7115241
_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_formula_sum            'C20 H36 P6 Ti'
_chemical_formula_weight         510.21
_space_group_IT_number           20
_symmetry_space_group_name_Hall  'C 2c 2'
_symmetry_space_group_name_H-M   'C 2 2 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.632(6)
_cell_length_b                   16.114(5)
_cell_length_c                   13.920(4)
_cell_measurement_temperature    173(2)
_cell_volume                     2609.1(17)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       CAD4
_diffrn_measurement_method       'omega-2theta scan'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0348
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2112
_diffrn_reflns_theta_max         29.96
_diffrn_reflns_theta_min         2.16
_exptl_absorpt_coefficient_mu    0.701
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.95
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_density_diffrn    1.299
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.556
_refine_diff_density_min         -0.400
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.12(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.063
_refine_ls_goodness_of_fit_obs   1.066
_refine_ls_matrix_type           full
_refine_ls_number_parameters     195
_refine_ls_number_reflns         2112
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_restrained_S_obs      1.066
_refine_ls_R_factor_all          0.0260
_refine_ls_R_factor_obs          0.0245
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0211P)^2^+1.6906P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0630
_refine_ls_wR_factor_obs         0.0619
_reflns_number_observed          2036
_reflns_number_total             2112
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            905469c.txt
_cod_data_source_block           hanks
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'psiscan' changed to
'psi-scan' according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0211P)^2^+1.6906P] 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^)+(0.0211P)^2^+1.6906P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               7115241