Synthesis, Structure, and Single-Crystal EPR Study of [Cp(t-Bu3PN)Ti(μ-Cl)]2
Raymond C. W. Sung; Silke Courtenay; Bruce R. McGarvey; Douglas W. Stephan; Inorganic Chemistry 39 (2000) 2542–2546; doi:10.1021/ic991305l

data_4321030
_publ_section_title
;
 Synthesis, Structure, and Single-Crystal EPR Study of
 [Cp(t-Bu3PN)Ti(\m-Cl)]2
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2542
_journal_page_last               2546
_journal_paper_doi               10.1021/ic991305l
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C23 H40 Cl N P Ti'
_chemical_formula_weight         444.88
_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
_cell_angle_alpha                76.72(2)
_cell_angle_beta                 78.84(2)
_cell_angle_gamma                81.02(2)
_cell_formula_units_Z            2
_cell_length_a                   9.182(2)
_cell_length_b                   11.283(3)
_cell_length_c                   11.437(3)
_cell_measurement_temperature    293(2)
_cell_volume                     1123.6(5)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(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  0.0198
_diffrn_reflns_av_sigmaI/netI    0.0422
_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       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5698
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.85
_exptl_absorpt_coefficient_mu    0.580
_exptl_absorpt_correction_T_max  0.262640
_exptl_absorpt_correction_T_min  0.199798
_exptl_absorpt_correction_type   sadabs
_exptl_crystal_density_diffrn    1.315
_exptl_crystal_F_000             478
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.312
_refine_diff_density_min         -0.343
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.936
_refine_ls_goodness_of_fit_obs   0.957
_refine_ls_matrix_type           full
_refine_ls_number_parameters     212
_refine_ls_number_reflns         3760
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.966
_refine_ls_restrained_S_obs      0.957
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_obs          0.0438
_refine_ls_shift/esd_max         -0.480
_refine_ls_shift/esd_mean        0.024
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1403
_refine_ls_wR_factor_obs         0.1220
_reflns_number_observed          2928
_reflns_number_total             3765
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic991305l.cif
_cod_data_source_block           '[CpTi(NP(t-Bu)3)Cl]2'
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1000P)^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^)+(0.1000P)^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        1123.7(5)
_cod_database_code               4321030