Phosphaazaallene and phosphinylimide complexes stemming from a terminal and four-coordinate titanium phosphinideneElectronic supplementary information (ESI) available: Complete experimental, spectroscopic, analytical, and crystallographic details for 2 and 3, as well as DFT computational details for the model complex of 1, namely (Nacnac*)Ti?PMes(Me). See http://www.rsc.org/suppdata/dt/b3/b311748k/
Basuli, Falguni; Watson, Lori A.; Huffman, John C.; Mindiola, Daniel J.; Dalton Transactions  (2003) 4228–; doi:10.1039/b311748k

data_7013674
_publ_section_title
;
 Phosphaazaallene and phosphinylimide complexes stemming from a
 terminal and four-coordinate titanium phosphinideneElectronic
 supplementary information (ESI) available: Complete experimental,
 spectroscopic, analytical, and crystallographic details for 2 and 3,
 as well as DFT computational details for the model complex of 1,
 namely (Nacnac*)Ti?PMes(Me). See
 http://www.rsc.org/suppdata/dt/b3/b311748k/
;
_journal_issue                   22
_journal_name_full               'Dalton Transactions'
_journal_page_first              4228
_journal_paper_doi               10.1039/b311748k
_journal_year                    2003
_chemical_formula_sum            'C77 H132 N5 P Ti'
_chemical_formula_weight         1206.75
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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_creation_method           SHELXL-97
_cell_angle_alpha                103.400(5)
_cell_angle_beta                 92.806(6)
_cell_angle_gamma                91.863(6)
_cell_formula_units_Z            2
_cell_length_a                   12.297(2)
_cell_length_b                   13.182(3)
_cell_length_c                   24.843(5)
_cell_measurement_reflns_used    957
_cell_measurement_temperature    127(2)
_cell_measurement_theta_max      23.76
_cell_measurement_theta_min      2.44
_cell_volume                     3908.7(13)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        'SAINT (Bruker, 1999), XTEL (local package)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      127(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 44.52
_diffrn_detector_type            'Bruker SMART 6000'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
'   0.30 degree frames measured for  10.17 seconds each'
_diffrn_measurement_device       'three-circle goniometer with fixed chi'
_diffrn_measurement_device_type  'Bruker Platform goniometer'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1163
_diffrn_reflns_av_sigmaI/netI    0.0933
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            47023
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.97
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    0.171
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red/purple
_exptl_crystal_density_diffrn    1.025
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular fragment'
_exptl_crystal_F_000             1332
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.629
_refine_diff_density_min         -0.586
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     767
_refine_ls_number_reflns         13721
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.1241
_refine_ls_R_factor_gt           0.0869
_refine_ls_shift/su_max          0.026
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1473P)^2^+3.7128P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2321
_refine_ls_wR_factor_ref         0.2567
_reflns_number_gt                9219
_reflns_number_total             13721
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b311748k.txt
_cod_data_source_block           03118
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        3908.8(13)
_cod_original_sg_symbol_H-M      'P-1   '
_cod_database_code               7013674