Atom Transfer Reactions of (TTP)Ti(η2-3-hexyne): Synthesis and Molecular Structure of trans-(TTP)Ti[OP(Oct)3]2
Joseph L. Thorman; Victor G. Young,; Peter D. W. Boyd; Ilia A. Guzei; L. Keith Woo; Inorganic Chemistry 40 (2001) 499–506; doi:10.1021/ic0003426

data_4319194
_publ_section_title
;
 Atom Transfer Reactions of (TTP)Ti(\h2-3-hexyne): Synthesis and Molecular
 Structure of trans-(TTP)Ti[OP(Oct)3]2
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              499
_journal_page_last               506
_journal_paper_doi               10.1021/ic0003426
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C60 H66 N4 P2 Ti'
_chemical_formula_weight         953.01
_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                83.7470(10)
_cell_angle_beta                 78.9280(10)
_cell_angle_gamma                85.2520(10)
_cell_formula_units_Z            2
_cell_length_a                   10.9163(6)
_cell_length_b                   11.5404(6)
_cell_length_c                   20.7951(11)
_cell_measurement_temperature    293(2)
_cell_volume                     2550.5(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      293(2)
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1090
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7015
_diffrn_reflns_theta_full        23.25
_diffrn_reflns_theta_max         23.25
_diffrn_reflns_theta_min         1.00
_exptl_absorpt_coefficient_mu    0.274
_exptl_absorpt_correction_T_max  0.9784
_exptl_absorpt_correction_T_min  0.9032
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.241
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1012
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.033
_refine_diff_density_min         -1.557
_refine_diff_density_rms         0.162
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     267
_refine_ls_number_reflns         7015
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.1766
_refine_ls_R_factor_gt           0.1262
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1620P)^2^+36.9707P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3514
_refine_ls_wR_factor_ref         0.3795
_reflns_number_gt                4434
_reflns_number_total             7015
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0003426_1.cif
_cod_data_source_block           woo06tm
_cod_depositor_comments
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The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4319194