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_4319195
_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_compound_source        'J. Thorman / Prof. K. Woo - ISU'
_chemical_formula_analytical     'C96 H138 N4 O2 P2 Ti'
_chemical_formula_moiety         'C96 H138 N4 O2 P2 Ti'
_chemical_formula_structural     'C96 H138 N4 O2 P2 Ti'
_chemical_formula_sum            'C96 H138 N4 O2 P2 Ti'
_chemical_formula_weight         1489.94
_chemical_name_common            97310
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 96.169(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.2196(1)
_cell_length_b                   28.6024(5)
_cell_length_c                   15.4589(2)
_cell_measurement_temperature    173(2)
_cell_volume                     4492.55(11)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_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  0.0574
_diffrn_reflns_av_sigmaI/netI    0.0912
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            21423
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.42
_exptl_absorpt_coefficient_mu    0.179
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.487
_exptl_absorpt_correction_type   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            'Dark red'
_exptl_crystal_density_diffrn    1.101
_exptl_crystal_description       'Irregular block'
_exptl_crystal_F_000             1620
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.336
_refine_diff_density_min         -0.333
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.989
_refine_ls_goodness_of_fit_obs   1.096
_refine_ls_matrix_type           full
_refine_ls_number_parameters     475
_refine_ls_number_reflns         7800
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.995
_refine_ls_restrained_S_obs      1.096
_refine_ls_R_factor_all          0.1026
_refine_ls_R_factor_obs          0.0548
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0552P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1303
_refine_ls_wR_factor_obs         0.1138
_reflns_number_observed          5053
_reflns_number_total             7802
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic0003426_2.cif
_cod_data_source_block           97310
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0552P)^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^)+(0.0552P)^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_database_code               4319195