Thiacrown PtII complexes with group 15 donor ligands: pentacoordination in Pt(II) complexes
Grant, Gregory J.; Benefield, Desirée A.; VanDerveer, Donald G.; Dalton Transactions  (2009) 8605–8615; doi:10.1039/b909875e

data_7002471
_publ_section_title
;
 Thiacrown PtII complexes with group 15 donor ligands:
 pentacoordination in Pt(II) complexes
;
_journal_coden_ASTM              DTARAF
_journal_issue                   40
_journal_name_full               'Dalton Transactions'
_journal_page_first              8605
_journal_page_last               8615
_journal_paper_doi               10.1039/b909875e
_journal_year                    2009
_chemical_formula_sum            'C44 H48 F12 N2 O4 P2 Pt S3 Sb2'
_chemical_formula_weight         1493.55
_chemical_name_common            (Pt(9S3)(SbPH3)2)(PF6)2
_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                93.67(3)
_cell_angle_beta                 93.94(3)
_cell_angle_gamma                91.84(3)
_cell_formula_units_Z            2
_cell_length_a                   12.893(3)
_cell_length_b                   13.110(3)
_cell_length_c                   15.374(3)
_cell_measurement_reflns_used    9578
_cell_measurement_temperature    163(2)
_cell_measurement_theta_max      26.7225
_cell_measurement_theta_min      2.9940
_cell_volume                     2585.4(10)
_computing_cell_refinement       'CrystalClear (Rigaku/MSC,2001)'
_computing_data_collection       'CrystalClear (Rigaku/MSC,2001)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC,2001)'
_computing_molecular_graphics    'SHELXTL 6.10 (Sheldrick,2008)'
_computing_publication_material  'SHELXTL 6.10 (Sheldrick,2008)'
_computing_structure_refinement  'SHELXTL 6.10 (Sheldrick,2008)'
_computing_structure_solution    'SHELXTL 6.10 (Sheldrick,2008)'
_diffrn_ambient_temperature      163(2)
_diffrn_detector_area_resol_mean 14.6306
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_details
;
scan:
Number of images: 260
Slice: -40.0000 - 90.0000
Image width: 0.5000
Exp time: 10.0000
Rotation axis: Omega
Omega: 0.0000
Chi: 45.0000
Phi: 0.0000
XTD: 27.6419
2theta: 0.8134
scan:
Number of images: 280
Slice: -60.0000 - 80.0000
Image width: 0.5000
Exp time: 10.0000
Rotation axis: Omega
Omega: 0.0000
Chi: 45.0000
Phi: 90.0000
XTD: 27.6419
2theta: 0.8134

;
_diffrn_measurement_device
;
Rigaku AFC8S Mercury CCD
;
_diffrn_measurement_device_details
;
AFC8: Eulerian 3 circle
;
_diffrn_measurement_method       omega
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_source         'Sealed Tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0219
_diffrn_reflns_av_sigmaI/netI    0.0350
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            23669
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        26.71
_diffrn_reflns_theta_max         26.71
_diffrn_reflns_theta_min         2.99
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.005
_exptl_absorpt_correction_T_max  0.4670
_exptl_absorpt_correction_T_min  0.3951
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R., (1998)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.918
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chip
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.19
_refine_diff_density_max         2.626
_refine_diff_density_min         -1.356
_refine_diff_density_rms         0.125
_refine_ls_extinction_coef       0.00117(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     634
_refine_ls_number_reflns         10830
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_gt           0.0341
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0332P)^2^+4.3404P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0729
_refine_ls_wR_factor_ref         0.0773
_reflns_number_gt                9559
_reflns_number_total             10830
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            B909875E.txt
_cod_data_source_block           pt9s3sbph32
_cod_original_cell_volume        2585.6(9)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7002471