Titanoxycarbene complexes of Ti(iv) with O- and N-donor ligands
Nogai, Stefan D.; Schuster, Oliver; Bruce, Jocelyn; Raubenheimer, Helgard G.; New Journal of Chemistry 32 (2008) 540–; doi:10.1039/b715075j

data_7051829
_publ_section_title
;
 Titanoxycarbene complexes of Ti(iv) with O- and N-donor ligands
;
_journal_issue                   3
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              540
_journal_paper_doi               10.1039/b715075j
_journal_volume                  32
_journal_year                    2008
_chemical_formula_moiety         'C30 H30 N2 O14 Ti W2'
_chemical_formula_sum            'C30 H30 N2 O14 Ti W2'
_chemical_formula_weight         1058.16
_chemical_name_systematic
;
?
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 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                 100.7040(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            6
_cell_length_a                   23.5197(15)
_cell_length_b                   15.4154(10)
_cell_length_c                   14.9223(9)
_cell_measurement_reflns_used    5006
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      2.41
_cell_measurement_theta_min      26.36
_cell_volume                     5316.2(6)
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL-PLUS
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Bruker APEX CCD area-detector'
_diffrn_measurement_method       \w
_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  0.0318
_diffrn_reflns_av_sigmaI/netI    0.0388
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            31409
_diffrn_reflns_theta_full        26.86
_diffrn_reflns_theta_max         26.86
_diffrn_reflns_theta_min         1.59
_exptl_absorpt_coefficient_mu    6.763
_exptl_absorpt_correction_T_max  0.5512
_exptl_absorpt_correction_T_min  0.3755
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS, Blessing, Acta Cryst. A51 (1995) 33-38'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.983
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3036
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         3.152
_refine_diff_density_min         -4.027
_refine_diff_density_rms         0.165
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     702
_refine_ls_number_reflns         11164
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0490
_refine_ls_R_factor_gt           0.0380
_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^)+(0.0436P)^2^+16.2353P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0899
_refine_ls_wR_factor_ref         0.0955
_reflns_number_gt                9184
_reflns_number_total             11164
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b715075j.txt
_cod_data_source_block           (OC)5W=C(Me)OTi(OiPr)3(C5H5N)2
_cod_original_sg_symbol_H-M      P2/c
_cod_database_code               7051829