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_4075560
_publ_section_title
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 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
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_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         'C44 H54 O2 Si Ti'
_chemical_formula_sum            'C44 H54 O2 Si Ti'
_chemical_formula_weight         690.83
_chemical_name_systematic        ?
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.2785(2)
_cell_length_b                   16.9519(2)
_cell_length_c                   27.6714(5)
_cell_measurement_reflns_used    7311
_cell_measurement_temperature    173(1)
_cell_measurement_theta_max      25.34
_cell_measurement_theta_min      1.88
_cell_volume                     7635.96(19)
_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 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.062
_diffrn_reflns_av_sigmaI/netI    0.0428
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            39965
_diffrn_reflns_theta_full        25.34
_diffrn_reflns_theta_max         25.34
_diffrn_reflns_theta_min         1.88
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.291
_exptl_absorpt_correction_T_max  0.981
_exptl_absorpt_correction_T_min  0.945
_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    1.202
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       fragment
_exptl_crystal_F_000             2960
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.471
_refine_diff_density_min         -0.374
_refine_diff_density_rms         0.052
_refine_ls_goodness_of_fit_ref   1.204
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     443
_refine_ls_number_reflns         6928
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.204
_refine_ls_R_factor_all          0.0783
_refine_ls_R_factor_gt           0.0610
_refine_ls_shift/su_max          0.000
_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^)+(0.0226P)^2^+8.7896P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.1089
_refine_ls_wR_factor_ref         0.1146
_reflns_number_gt                5822
_reflns_number_total             6928
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om060368qsi20060428_093629.cif
_cod_data_source_block           TOMT-4264-173
_cod_depositor_comments
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The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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 
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_cod_database_code               4075560