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_7046820
_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         'C36 H54 Cl N P4 Ti'
_chemical_formula_sum            'C36 H54 Cl N P4 Ti'
_chemical_formula_weight         708.03
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_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
_audit_creation_date             2017-04-05T10:19:24-00:00
_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                 99.206(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
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_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.5488
_cell_measurement_theta_min      2.1528
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        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
        (compiled Aug  3 2011,13:03:54)
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_computing_data_collection
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        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
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        CrysAlisPro, Agilent Technologies,
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        (compiled Aug  3 2011,13:03:54)
;
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
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_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8.1883
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_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0431441
_diffrn_orient_matrix_UB_12      -0.0083305
_diffrn_orient_matrix_UB_13      0.0188967
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_diffrn_orient_matrix_UB_32      -0.0439386
_diffrn_orient_matrix_UB_33      0.0006354
_diffrn_radiation_monochromator  graphite
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_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.997
_diffrn_reflns_theta_min         2.158
_exptl_absorpt_coefficient_mu    0.481
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.7741
_exptl_absorpt_correction_type   multi-scan
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        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
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        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
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_exptl_crystal_description       block
_exptl_crystal_F_000             1504
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_exptl_crystal_size_min          0.23
_refine_diff_density_max         1.273
_refine_diff_density_min         -0.724
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_refine_ls_extinction_method     none
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_refine_ls_number_reflns         8224
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_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.1175
_refine_ls_R_factor_gt           0.0726
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0894P)^2^+5.0935P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.177
_refine_ls_wR_factor_ref         0.2219
_reflns_Friedel_coverage         0
_reflns_number_gt                5308
_reflns_number_total             8224
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01833b2.cif
_cod_data_source_block           lp4_15
_cod_depositor_comments
'Adding full bibliography for 7046819--7046822.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7046820
_shelx_estimated_absorpt_t_min   0.893
_shelx_estimated_absorpt_t_max   0.898
_shelx_res_checksum              66176