Synthesis, Structure, and Properties of 9-Phospha-10-silatriptycenes and their Derivatives
Tsuji, Hayato; Inoue, Tomoyuki; Kaneta, Yasuhiro; Sase, Shohei; Kawachi, Atsushi; Tamao, Kohei; Organometallics 25 (2006) 6142–; doi:10.1021/om060681s

data_4074475
_publ_section_title
;
 Synthesis, Structure, and Properties of 9-Phospha-10-silatriptycenes and
 their Derivatives
;
_journal_issue                   26
_journal_name_full               Organometallics
_journal_page_first              6142
_journal_paper_doi               10.1021/om060681s
_journal_volume                  25
_journal_year                    2006
_chemical_formula_moiety         'C94 H130 N2 O14 P2 Pt Si2'
_chemical_formula_sum            'C94 H130 N2 O14 P2 Pt Si2'
_chemical_formula_weight         1825.21
_chemical_melting_point_gt       573
_chemical_name_common            cis-PtMe2(psit)2
_chemical_name_systematic
; 
cis-dimethybis(10-(4'-dimethylaminophenyl)-9-phsopha-
10-silatriptycene-kP)platinum 
;
_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                80.194(11)
_cell_angle_beta                 69.414(10)
_cell_angle_gamma                78.327(11)
_cell_formula_units_Z            2
_cell_length_a                   15.139(4)
_cell_length_b                   16.748(4)
_cell_length_c                   20.323(5)
_cell_measurement_temperature    173(2)
_cell_volume                     4696(2)
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_collection       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2000)'
_computing_molecular_graphics    'ORTEP III (Burnett & Johnson, 1996)'
_computing_publication_material  'SHELXL97 and Yadokari-XG (Wakita, 2005)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-97
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type
;
Saturn70 CCD (4x4 bin mode)
;
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0526
_diffrn_reflns_av_sigmaI/netI    0.0842
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            33086
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         3.22
_exptl_absorpt_coefficient_mu    1.614
_exptl_absorpt_correction_T_max  0.7938
_exptl_absorpt_correction_T_min  0.7385
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Jacobson, 1998)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.291
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1912
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.086
_refine_diff_density_min         -0.811
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1067
_refine_ls_number_reflns         17045
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0673
_refine_ls_R_factor_gt           0.0516
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0466P)^2^+3.2529P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1079
_refine_ls_wR_factor_ref         0.1161
_reflns_number_gt                14355
_reflns_number_total             17045
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060681ssi20060728_115005.cif
_cod_data_source_block           pt-1c
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' tag was changed to
'_chemical_melting_point_gt' since the value was specified 'more
than' ('>') a certain temperature. The value '> 573' was changed to
'573' - it should be numeric and without a unit
designator.

'_exptl_absorpt_correction_type' value 'Multi-scan'
changed to 'multi-scan' 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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        4696.4(19)
_cod_database_code               4074475