Monocyclopentadienyl Chloro Bisphenoxo Ti(η5-C5H4SiMe2Cl)(η2-MBMP)Cl Derivative: Ti−Cl, Ti−O, and Si−Cl Reactivity. Crystal Structure of Ti(η5-C5H4SiMe3)(η2-MBMP)Cl and Ti(η5-C5H4SiMe2-η1-MBMP)(CH2Ph)2
González-Maupoey, Marta; Cuenca, Tomás; Herdtweck, Eberhardt; Organometallics 25 (2006) 4358–; doi:10.1021/om060368q

data_4075559
_publ_section_title
;
 Monocyclopentadienyl Chloro Bisphenoxo Ti(\h5-C5H4SiMe2Cl)(\h2-MBMP)Cl
 Derivative:&#x00A0; Ti&#x2212;Cl, Ti&#x2212;O, and Si&#x2212;Cl
 Reactivity. Crystal Structure of Ti(\h5-C5H4SiMe3)(\h2-MBMP)Cl and
 Ti(\h5-C5H4SiMe2-\h1-MBMP)(CH2Ph)2
;
_journal_issue                   18
_journal_name_full               Organometallics
_journal_page_first              4358
_journal_paper_doi               10.1021/om060368q
_journal_volume                  25
_journal_year                    2006
_chemical_formula_moiety         'C31 H43 Cl O2 Si Ti'
_chemical_formula_sum            'C31 H43 Cl O2 Si Ti'
_chemical_formula_weight         559.06
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 108.0383(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.7806(1)
_cell_length_b                   14.2076(1)
_cell_length_c                   17.5955(1)
_cell_measurement_reflns_used    5816
_cell_measurement_temperature    173(1)
_cell_measurement_theta_max      25.36
_cell_measurement_theta_min      1.88
_cell_volume                     3037.98(4)
_computing_cell_refinement       'DENZO (Nonius, 2001b)'
_computing_data_collection       'Kappa-CCD Control Software (Nonius, 2001a)'
_computing_data_reduction        'DENZO (Nonius, 2001b)'
_computing_molecular_graphics    'PLATON (Spek, 2001)'
_computing_publication_material  'PLATON (Spek, 2001)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1998)'
_computing_structure_solution    'SIR92 (Altomare, 1994)'
_diffrn_ambient_temperature      173(1)
_diffrn_detector                 ' CCD plate '
_diffrn_detector_area_resol_mean 18
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       ' \k-geometry diffractometer '
_diffrn_measurement_device_type  ' Nonius \k-CCD diffractometer'
_diffrn_measurement_method       ' phi- and omega-rotation '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'NONIUS FR 591 rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.049
_diffrn_reflns_av_sigmaI/netI    0.0193
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            67571
_diffrn_reflns_theta_full        25.36
_diffrn_reflns_theta_max         25.36
_diffrn_reflns_theta_min         1.88
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.434
_exptl_absorpt_correction_T_max  0.917
_exptl_absorpt_correction_T_min  0.770
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'(applied during the scaling procedure; Nonius, 2001b)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.222
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       plate
_exptl_crystal_F_000             1192
_exptl_crystal_size_max          0.61
_exptl_crystal_size_mid          0.48
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.267
_refine_diff_density_min         -0.297
_refine_diff_density_rms         0.042
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     497
_refine_ls_number_reflns         5560
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0388
_refine_ls_R_factor_gt           0.0306
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(Fo^2^)+(0.0371P)^2^+1.6964P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.0739
_refine_ls_wR_factor_ref         0.0773
_reflns_number_gt                4819
_reflns_number_total             5560
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om060368qsi20060428_093629.cif
_cod_data_source_block           TOMQ-4257-173
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4075559