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_4345456
_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         'C38 H64 Cl N2 P2 Si Ti'
_chemical_formula_sum            'C38 H64 Cl N2 P2 Si Ti'
_chemical_formula_weight         722.29
_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             2015-12-21
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 95.655(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.4471(12)
_cell_length_b                   18.809(3)
_cell_length_c                   20.693(2)
_cell_measurement_reflns_used    1580
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.83
_cell_measurement_theta_min      3.61
_cell_volume                     4046.4(9)
_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      120(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0553
_diffrn_reflns_av_unetI/netI     0.0564
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            21434
_diffrn_reflns_theta_full        28
_diffrn_reflns_theta_max         28
_diffrn_reflns_theta_min         4.51
_diffrn_source                   'GeniX Mo, 0.05 x 0.05 mm2 microfocus'
_exptl_absorpt_coefficient_mu    0.414
_exptl_absorpt_correction_T_max  0.9636
_exptl_absorpt_correction_T_min  0.8987
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.186
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1556
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.696
_refine_diff_density_min         -0.865
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     435
_refine_ls_number_reflns         9588
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0836
_refine_ls_R_factor_gt           0.0562
_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^)+(0.0923P)^2^+1.2216P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1462
_refine_ls_wR_factor_ref         0.1703
_reflns_number_gt                6743
_reflns_number_total             9588
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic6b01929_si_001.cif
_cod_data_source_block           1b
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4345456