Reduction of Titanium Supported by aσ-/π-Bonded Tripyrrole Ligand: Ligand C−N Bond Cleavage and Coordination of Olefin and Arene with an Inverse Sandwich Structure
Nikiforov, Grigory B.; Crewdson, Patrick; Gambarotta, Sandro; Korobkov, Ilia; Budzelaar, Peter H. M.; Organometallics 26 (2007) 48–; doi:10.1021/om060908j

data_4072644
_publ_section_title
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 Reduction of Titanium Supported by a\s-/\p-Bonded Tripyrrole
 Ligand:&#x00A0; Ligand C&#x2212;N Bond Cleavage and Coordination of
 Olefin and Arene with an Inverse Sandwich Structure
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_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              48
_journal_paper_doi               10.1021/om060908j
_journal_volume                  26
_journal_year                    2007
_chemical_formula_sum            'C56 H50 K N3 O2 Ti'
_chemical_formula_weight         883.99
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.51(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.50(2)
_cell_length_b                   9.136(16)
_cell_length_c                   20.49(3)
_cell_measurement_reflns_used    217
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      24.80
_cell_measurement_theta_min      1.66
_cell_volume                     2293(6)
_computing_cell_refinement       'SMART, Bruker (2000)'
_computing_data_collection       'SMART, Bruker (2000)'
_computing_data_reduction        'XPREP, Bruker (2000)'
_computing_molecular_graphics    'SHELXTL, Bruker (2000)'
_computing_publication_material  'SHELXTL, Bruker (2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0378
_diffrn_reflns_av_sigmaI/netI    0.0570
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       10
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_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            16686
_diffrn_reflns_theta_full        24.80
_diffrn_reflns_theta_max         24.80
_diffrn_reflns_theta_min         1.66
_diffrn_standards_decay_%        <1
_exptl_absorpt_coefficient_mu    0.323
_exptl_absorpt_correction_T_max  0.9684
_exptl_absorpt_correction_T_min  0.9381
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker (2000)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.524
_refine_diff_density_min         -0.232
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
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_refine_ls_matrix_type           full
_refine_ls_number_parameters     569
_refine_ls_number_reflns         7740
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_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0690
_refine_ls_R_factor_gt           0.0527
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0694P)^2^+1.5336P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1226
_refine_ls_wR_factor_ref         0.1322
_reflns_number_gt                6476
_reflns_number_total             7740
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060908jsi20061004_121219.cif
_cod_data_source_block           sg3014
_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.

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 'n/a' 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_cell_volume        2293(7)
_cod_original_sg_symbol_H-M      P2(1)
_cod_database_code               4072644