Metallo-Wittig chemistry of an alkylidene to form a terminal titanium oxo complex.
Solowey, Douglas P.; Kurogi, Takashi; Manor, Brian C.; Carroll, Patrick J.; Mindiola, Daniel J.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 15894–15901; doi:10.1039/c6dt01534d

data_7039553
_publ_section_title
;
 Metallo-Wittig chemistry of an alkylidene to form a terminal titanium oxo
 complex.
;
_journal_issue                   40
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15894
_journal_page_last               15901
_journal_paper_doi               10.1039/c6dt01534d
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C40 H50 F3 N O4 P2 S Ti, 2.5(C4 H10 O1).'
_chemical_formula_sum            'C50 H75 F3 N O7.5 P2 S Ti'
_chemical_formula_weight         1009.01
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-05-10 deposited with the CCDC.
2016-06-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.271(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.5327(12)
_cell_length_b                   12.0477(8)
_cell_length_c                   27.564(2)
_cell_measurement_reflns_used    9703
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.42
_cell_measurement_theta_min      2.42
_cell_volume                     5446.1(7)
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics
'Yadokari-XG 2009 (Wakita Nemoto et al., 2009)'
_computing_publication_material
'Yadokari-XG 2009 (Wakita,Nemoto et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'ShelXS-1997 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(1)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'CCD Area Detector'
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0471
_diffrn_reflns_av_unetI/netI     0.0391
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            85632
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         1.489
_exptl_absorpt_coefficient_mu    0.312
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6834
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2014/4'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.231
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2148
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.13
_platon_squeeze_details
;
;
_refine_diff_density_max         1.400
_refine_diff_density_min         -0.779
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     536
_refine_ls_number_reflns         12515
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0758
_refine_ls_R_factor_gt           0.0539
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0927P)^2^+2.8904P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1519
_refine_ls_wR_factor_ref         0.1618
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9264
_reflns_number_total             12515
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt01534d2.cif
_cod_data_source_block           UP9182
_cod_depositor_comments
'Adding full bibliography for 7039553--7039554.cif.'
_cod_original_cell_volume        5446.2(7)
_cod_original_formula_sum        'C50 H75 F3 N O7.50 P2 S Ti'
_cod_database_code               7039553
_shelx_shelxl_version_number     2014/7
_solvent_exptl_crystal_recrystallization_method 'diethyl ether, pentane'