Ammonolysis of Mono(pentamethylcyclopentadienyl) Titanium(IV) Derivatives
Angel Abarca; Pilar Gómez-Sal; Avelino Martín; Miguel Mena; Josep María Poblet; Carlos Yélamos; Inorganic Chemistry 39 (2000) 642–651; doi:10.1021/ic9907718

data_4300084
_publ_section_title
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Ammonolysis of Mono(pentamethylcyclopentadienyl) Titanium(IV) Derivatives
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              642
_journal_page_last               651
_journal_paper_doi               10.1021/ic9907718
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C20 H33 Cl3 N2 Ti2'
_chemical_formula_weight         503.63
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 111.85(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   28.272(6)
_cell_length_b                   8.452(2)
_cell_length_c                   22.260(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      13
_cell_measurement_theta_min      6
_cell_volume                     4937(2)
_computing_cell_refinement       'CAD4 EXPRESS'
_computing_data_collection       'CAD4 EXPRESS'
_computing_data_reduction        'XCAD4 (Harms, 1996)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf Nonius CAD4'
_diffrn_measurement_method       Omega-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MOKa
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  0.0418
_diffrn_reflns_av_sigmaI/netI    0.0571
_diffrn_refln_scan_mode_backgd   MO
_diffrn_refln_scan_width         .70
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            5999
_diffrn_reflns_theta_max         22.00
_diffrn_reflns_theta_min         3.00
_diffrn_standards_decay_%        11
_diffrn_standards_interval_time  120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.979
_exptl_absorpt_correction_type   N/A
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.355
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2096
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.277
_refine_diff_density_min         -0.224
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.966
_refine_ls_goodness_of_fit_obs   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     257
_refine_ls_number_reflns         3004
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.968
_refine_ls_restrained_S_obs      1.019
_refine_ls_R_factor_all          0.0756
_refine_ls_R_factor_obs          0.0333
_refine_ls_shift/esd_max         -0.262
_refine_ls_shift/esd_mean        0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0489P)^2^+7.4679P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0951
_refine_ls_wR_factor_obs         0.0806
_reflns_number_observed          2032
_reflns_number_total             3005
_reflns_observed_criterion       >2sigma(I)
_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^)+(0.0489P)^2^+7.4679P] 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^)+(0.0489P)^2^+7.4679P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_original_cell_volume        4937.0(18)
_cod_database_code               4300084