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_4345457
_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         'C37 H59 Cl N2 P2 Ti'
_chemical_formula_sum            'C37 H59 Cl N2 P2 Ti'
_chemical_formula_weight         677.15
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_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   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                 104.503(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.5957(9)
_cell_length_b                   17.4527(6)
_cell_length_c                   12.8529(7)
_cell_measurement_reflns_used    25719
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      59.53
_cell_measurement_theta_min      2.29
_cell_volume                     3821.3(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                 Pilatus100K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_av_unetI/netI     0.0439
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            21680
_diffrn_reflns_theta_full        89.75
_diffrn_reflns_theta_max         89.75
_diffrn_reflns_theta_min         3.63
_diffrn_source                   'Cu LFF Sealed Tube'
_exptl_absorpt_coefficient_mu    3.518
_exptl_absorpt_correction_T_max  0.5253
_exptl_absorpt_correction_T_min  0.4733
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.177
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.93
_refine_diff_density_min         -0.452
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         8705
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0727
_refine_ls_R_factor_gt           0.0457
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0785P)^2^+0.0457P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1133
_refine_ls_wR_factor_ref         0.1261
_reflns_number_gt                6310
_reflns_number_total             8705
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic6b01929_si_001.cif
_cod_data_source_block           2a1
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4345457