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_4076666
_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            'C56 H90 N2 O4 Si2 Ti2'
_chemical_formula_weight         1007.28
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                85.00(3)
_cell_angle_beta                 79.14(3)
_cell_angle_gamma                83.65(3)
_cell_formula_units_Z            1
_cell_length_a                   10.382(2)
_cell_length_b                   11.219(2)
_cell_length_c                   12.817(3)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      4
_cell_volume                     1453.8(5)
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.2046
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3612
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.62
_diffrn_standards_interval_time  360
_diffrn_standards_number         50-250
_exptl_absorpt_coefficient_mu    0.358
_exptl_absorpt_correction_type   NO
_exptl_crystal_colour            YELLOW-ORANGE
_exptl_crystal_density_diffrn    1.151
_exptl_crystal_description       PRISM
_exptl_crystal_F_000             544
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.247
_refine_diff_density_min         -0.223
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.734
_refine_ls_goodness_of_fit_obs   0.981
_refine_ls_matrix_type           full
_refine_ls_number_parameters     295
_refine_ls_number_reflns         3611
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.267
_refine_ls_restrained_S_obs      0.975
_refine_ls_R_factor_all          0.1288
_refine_ls_R_factor_obs          0.0481
_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^)+(0.0173P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1505
_refine_ls_wR_factor_obs         0.0738
_reflns_number_observed          1624
_reflns_number_total             3612
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            om0108954.cif
_cod_data_source_block           231
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'TRICLINIC' changed to 'triclinic'
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^)+(0.0173P)^2^+0.0000P] 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^)+(0.0173P)^2^+0.0000P] 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      P-1
_cod_database_code               4076666