Low-Valent Pentafulvene Titanium Dinitrogen Complex as a Precursor for Cationic Titanium Complexes
Scherer, Axel; Haase, Detlev; Saak, Wolfgang; Beckhaus, Rüdiger; Meetsma, Auke; Bouwkamp, Marco W.; Organometallics 28 (2009) 6969–; doi:10.1021/om900875e

data_4070497
_publ_section_title
;
 Low-Valent Pentafulvene Titanium Dinitrogen Complex as a Precursor for
 Cationic Titanium Complexes
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              6969
_journal_paper_doi               10.1021/om900875e
_journal_volume                  28
_journal_year                    2009
_chemical_compound_source        'see text'
_chemical_formula_moiety
'C29 H41 O Ti, C24 H20 B, 0.5(C6 H12), 2(C4 H8 O)'
_chemical_formula_sum            'C64 H83 B O3 Ti'
_chemical_formula_weight         958.98
_chemical_name_systematic        ' ?'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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     heavy
_atom_sites_solution_secondary   direct
_audit_creation_date             '2004-02-06  08:25:40'
_audit_creation_method
;
 PLATON <TABLE ACC> option 
 SHELXL97-2 & Manual Editing 
;
_audit_update_record
;
?

2009-09-28 # Formatted by publCIF
;
_cell_angle_alpha                90
_cell_angle_beta                 99.080(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.7758(8)
_cell_length_b                   22.193(2)
_cell_length_c                   21.726(2)
_cell_measurement_reflns_used    6207
_cell_measurement_temperature    200(1)
_cell_measurement_theta_max      21.02
_cell_measurement_theta_min      2.54
_cell_volume                     5606.7(8)
_computing_cell_refinement       'SAINT-Plus, (Bruker, 2001'
_computing_data_collection       'SMART, (Bruker, 2001)'
_computing_data_reduction        SAINT-Pus
_computing_molecular_graphics
;
 PLUTO (Meetsma, 2003) 
 PLATON (Spek, 2003)
;
_computing_publication_material  'PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
;
 DIRDIF-99 (Beurskens et al., 1999)
;
_diffrn_ambient_temperature      200(1)
_diffrn_detector_area_resol_mean 66.06
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
;
  Bruker Smart Apex 
;
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_detector
;
  CCD area-detector
;
_diffrn_radiation_monochromator  'parallel mounted graphite'
_diffrn_radiation_source         'fine focus sealed Siemens Mo tube '
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0517
_diffrn_reflns_av_sigmaI/netI    0.0701
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            39473
_diffrn_reflns_reduction_process
;
 Intensity data were corrected for Lorentz and polarization
  effects, decay and absorption and reduced to F~o~^2^
  using SAINT-Plus & SADABS (Bruker, 2001)
;
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.31
_exptl_absorpt_coefficient_mu    0.196
_exptl_absorpt_correction_T_max  0.9599
_exptl_absorpt_correction_T_min  0.8176
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS, (Bruker, 2001))'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.136
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2072
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.302
_refine_diff_density_min         -0.292
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     627
_refine_ls_number_reflns         9881
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.1015
_refine_ls_R_factor_gt           0.0588
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0628P)^2^+3.5283P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1473
_refine_ls_wR_factor_ref         0.1699
_reflns_number_gt                6372
_reflns_number_total             9881
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om900875e_si_001.cif
_cod_data_source_block           global
_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 2.4.2 from
2011-04-26.

'_exptl_absorpt_correction_type' value 'Multi-Scan'
changed to 'multi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4070497
_vrn_publ_code_void_volume       106.4
_vrn_publ_code_frame_time_sec    10.0
_vrn_publ_code_meas_time_hour    8.0