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_4345455
_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         'C40 H69 Cl N2 P2 Si Ti, C2.5 H5'
_chemical_formula_sum            'C42.5 H74 Cl N2 P2 Si Ti'
_chemical_formula_weight         786.42
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -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             2015-12-04
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                78.60(3)
_cell_angle_beta                 81.96(3)
_cell_angle_gamma                74.41(3)
_cell_formula_units_Z            2
_cell_length_a                   10.567(2)
_cell_length_b                   11.761(2)
_cell_length_c                   19.903(4)
_cell_measurement_reflns_used    27476
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.33
_cell_measurement_theta_min      1.95
_cell_volume                     2325.6(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      150(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0927
_diffrn_reflns_av_unetI/netI     0.1518
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            19081
_diffrn_reflns_theta_full        26
_diffrn_reflns_theta_max         26
_diffrn_reflns_theta_min         1.94
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_exptl_absorpt_coefficient_mu    0.365
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.123
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             852
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.068
_refine_diff_density_min         -0.517
_refine_diff_density_rms         0.07
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.943
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     459
_refine_ls_number_reflns         9048
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      0.942
_refine_ls_R_factor_all          0.1669
_refine_ls_R_factor_gt           0.0822
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0845P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1668
_refine_ls_wR_factor_ref         0.2014
_reflns_number_gt                4496
_reflns_number_total             9048
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic6b01929_si_001.cif
_cod_data_source_block           1a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/home/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_cell_volume        2325.6(8)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C42.50 H74 Cl N2 P2 Si Ti'
_cod_database_code               4345455