Five-Membered Titanacyclocumulenes that Contain Linked Amido−Cyclopentadienyl Ligands
Spannenberg, Anke; Baumann, Wolfgang; Becke, Sigurd; Rosenthal, Uwe; Organometallics 21 (2002) 1512–; doi:10.1021/om0108954

data_4076665
_publ_section_title
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 Five-Membered Titanacyclocumulenes that Contain Linked
 Amido&#x2212;Cyclopentadienyl Ligands
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              1512
_journal_paper_doi               10.1021/om0108954
_journal_volume                  21
_journal_year                    2002
_chemical_formula_sum            'C27 H45 N Si Ti'
_chemical_formula_weight         459.63
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 98.65(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.233(2)
_cell_length_b                   11.790(2)
_cell_length_c                   20.887(4)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      4
_cell_volume                     2734.7(9)
_computing_cell_refinement       STOE-CELL
_computing_data_collection       STOE-EXPOSE
_computing_data_reduction        STOE-INTEGRATE
_computing_molecular_graphics    XP
_computing_publication_material  SHELXL-93
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       STOE-IPDS
_diffrn_measurement_method       'LASER SCANNED IMAGING PLATE'
_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  0.0543
_diffrn_reflns_av_sigmaI/netI    0.0865
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            6573
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.95
_diffrn_standards_interval_time  360
_diffrn_standards_number         50-200
_exptl_absorpt_coefficient_mu    0.370
_exptl_absorpt_correction_type   'MEAN IMAGING PLATE INTENSITY METHOD'
_exptl_crystal_colour            YELLOW
_exptl_crystal_density_diffrn    1.116
_exptl_crystal_description       PRISM
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.693
_refine_diff_density_min         -0.531
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.043
_refine_ls_goodness_of_fit_obs   1.188
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         3554
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.183
_refine_ls_restrained_S_obs      1.188
_refine_ls_R_factor_all          0.0976
_refine_ls_R_factor_obs          0.0705
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1177P)^2^+1.2043P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2235
_refine_ls_wR_factor_obs         0.1884
_reflns_number_observed          2533
_reflns_number_total             3567
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            om0108954.cif
_cod_data_source_block           224
_cod_depositor_comments
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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:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1177P)^2^+1.2043P] 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^)+(0.1177P)^2^+1.2043P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P21/N
_cod_database_code               4076665