Cyclopentadienyl-Amido Ligands with a Pendant “−NHR” Amino Functionality in Titanium Chemistry. Molecular Structure of [Ti{η5-C5H4SiMe2-η-N(CH2)2-η-NHCHMe2}Cl2]
Jiménez, Gerardo; Royo, Pascual; Cuenca, Tomás; Herdtweck, Eberhardt; Organometallics 21 (2002) 2189–; doi:10.1021/om0110890

data_4076773
_publ_section_title
;
 Cyclopentadienyl-Amido Ligands with a Pendant &#x201C;&#x2212;NHR&#x201D;
 Amino Functionality in Titanium Chemistry. Molecular Structure of
 [Ti{\h5-C5H4SiMe2-\h-N(CH2)2-\h-NHCHMe2}Cl2]
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              2189
_journal_paper_doi               10.1021/om0110890
_journal_volume                  21
_journal_year                    2002
_chemical_compound_source        'see text'
_chemical_formula_moiety         'C12 H22 Cl2 N2 Si Ti'
_chemical_formula_sum            'C12 H22 Cl2 N2 Si Ti'
_chemical_formula_weight         341.18
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 98.633(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.5785(4)
_cell_length_b                   15.0383(12)
_cell_length_c                   16.4637(14)
_cell_measurement_reflns_used    4973
_cell_measurement_temperature    293(1)
_cell_measurement_theta_max      25.8
_cell_measurement_theta_min      8.2
_cell_volume                     1610.3(2)
_computing_cell_refinement       'IPDS (STOE, 1997)'
_computing_data_collection       'IPDS (STOE, 1997)'
_computing_data_reduction        'IPDS (STOE, 1997)'
_computing_molecular_graphics    'PLATON PLUTON (Spek, 2001)'
_computing_publication_material  'PLATON (Spek, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1998)'
_computing_structure_solution    'SIR-92 (Giacovazzo, 1994)'
_diffrn_ambient_temperature      293(1)
_diffrn_detector                 'image plate'
_diffrn_detector_area_resol_mean 67
_diffrn_measured_fraction_theta_full 0.942
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_device       'one-circle diffractometer'
_diffrn_measurement_device_type  'IPDS (STOE&CIE)'
_diffrn_measurement_method       'phi-oscillation '
_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  0.0413
_diffrn_reflns_av_sigmaI/netI    0.0241
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            21864
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.50
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    0.923
_exptl_absorpt_correction_T_max  0.7821
_exptl_absorpt_correction_T_min  0.5218
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
 none
;
_exptl_crystal_colour            ' yellow '
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       ' fragment '
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.81
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.254
_refine_diff_density_min         -0.157
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.946
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     251
_refine_ls_number_reflns         2866
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.946
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_gt           0.0239
_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^)+( 0.0407P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.0579
_refine_ls_wR_factor_ref         0.0602
_reflns_number_gt                2195
_reflns_number_total             2866
_reflns_threshold_expression     >2sigma(i)
_cod_data_source_file            om0110890.cif
_cod_data_source_block           TOMA-3085-293
_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.

'_exptl_absorpt_correction_type' value ' none ' changed
to 'none' 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/c'
_cod_database_code               4076773