Reactions of (Ph)tBuP-P(SiMe<sub>3</sub>)Li·3THF with [(PNP)TiCl<sub>2</sub>] and [<sup>Me</sup>NacNacTiCl<sub>2</sub>·THF]: synthesis of first PNP titanium(iv) complex with the phosphanylphosphinidene ligand [(PNP)Ti(Cl){η<sup>2</sup>-P-P(Ph)tBu}].
Ziółkowska, Aleksandra; Szynkiewicz, Natalia; Wiśniewska, Aleksandra; Pikies, Jerzy; Ponikiewski, Łukasz; Dalton transactions (Cambridge, England : 2003) 47 (2018) 9733–9741; doi:10.1039/c8dt01833b

data_7046822
_publ_section_title
;
 Reactions of (Ph)tBuP-P(SiMe<sub>3</sub>)Li&#x00B7;3THF with
 [(PNP)TiCl<sub>2</sub>] and
 [<sup>Me</sup>NacNacTiCl<sub>2</sub>&#x00B7;THF]: synthesis of first PNP
 titanium(iv) complex with the phosphanylphosphinidene ligand
 [(PNP)Ti(Cl){\h<sup>2</sup>-P-P(Ph)tBu}].
;
_journal_issue                   29
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9733
_journal_page_last               9741
_journal_paper_doi               10.1039/c8dt01833b
_journal_volume                  47
_journal_year                    2018
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C39 H55 Cl N2 P2 Ti'
_chemical_formula_sum            'C39 H55 Cl N2 P2 Ti'
_chemical_formula_weight         697.14
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2017-04-05T12:27:26-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2018-01-23 deposited with the CCDC.
2018-06-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.874(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.6073(5)
_cell_length_b                   16.8138(5)
_cell_length_c                   13.4071(8)
_cell_measurement_reflns_used    9820
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      29.63
_cell_measurement_theta_min      3.79
_cell_volume                     3836.1(3)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_monochromator  'parabolic x-ray mirror'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0371
_diffrn_reflns_av_unetI/netI     0.035
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            18986
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.995
_diffrn_reflns_theta_min         3.791
_diffrn_source                   'GeniX Mo, 0.05 x 0.05 mm2 microfocus'
_exptl_absorpt_coefficient_mu    0.405
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.207
_exptl_crystal_description       block
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.616
_refine_diff_density_min         -0.526
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     410
_refine_ls_number_reflns         8251
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0584
_refine_ls_R_factor_gt           0.0468
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0925P)^2^+2.3492P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1324
_refine_ls_wR_factor_ref         0.1497
_reflns_Friedel_coverage         0
_reflns_number_gt                6822
_reflns_number_total             8251
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01833b2.cif
_cod_data_source_block           za11a
_cod_depositor_comments
'Adding full bibliography for 7046819--7046822.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7046822
_shelx_estimated_absorpt_t_min   0.913
_shelx_estimated_absorpt_t_max   0.92