Reactions of Lithiated Diphosphanes R2P-P(SiMe3)Li (R = tBu and iPr) with [(Me)NacnacTiCl2·THF] and [(Me)NacnacTiCl3]. Formation and Structure of Titanium(III) and Titanium(IV) β-Diketiminato Complexes Bearing the Side-on Phosphanylphosphido and Phosphanylphosphinidene Functionalities.
Ponikiewski, Ł; Ziółkowska, A; Pikies, J.; Inorganic chemistry 56 (2017) 1094–1103; doi:10.1021/acs.inorgchem.6b01929

data_4345459
_publ_section_title
;
 Reactions of Lithiated Diphosphanes R2P-P(SiMe3)Li (R = tBu and iPr) with
 [(Me)NacnacTiCl2&#x00B7;THF] and [(Me)NacnacTiCl3]. Formation and
 Structure of Titanium(III) and Titanium(IV) \b-Diketiminato Complexes
 Bearing the Side-on Phosphanylphosphido and Phosphanylphosphinidene
 Functionalities.
;
_journal_issue                   3
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1094
_journal_page_last               1103
_journal_paper_doi               10.1021/acs.inorgchem.6b01929
_journal_volume                  56
_journal_year                    2017
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C35 H55 Cl N2 P2 Ti'
_chemical_formula_sum            'C35 H55 Cl N2 P2 Ti'
_chemical_formula_weight         649.1
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_date             2015-11-18
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 108.142(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.6082(5)
_cell_length_b                   21.4838(7)
_cell_length_c                   16.8009(7)
_cell_measurement_reflns_used    19596
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.76
_cell_measurement_theta_min      1.76
_cell_volume                     3638.7(3)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0377
_diffrn_reflns_av_unetI/netI     0.064
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19268
_diffrn_reflns_theta_full        25.69
_diffrn_reflns_theta_max         25.69
_diffrn_reflns_theta_min         1.59
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_exptl_absorpt_coefficient_mu    0.421
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.185
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.458
_refine_diff_density_min         -0.465
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.869
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         6850
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.869
_refine_ls_R_factor_all          0.0655
_refine_ls_R_factor_gt           0.0358
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0414P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.073
_refine_ls_wR_factor_ref         0.0786
_reflns_number_gt                4576
_reflns_number_total             6850
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic6b01929_si_001.cif
_cod_data_source_block           2b
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4345459