General Strategy for the Synthesis of Rigid Weak-Link Approach Platinum(II) Complexes: Tweezers, Triple-Layer Complexes, and Macrocycles
Robert D. Kennedy; Charles W. Machan; C. Michael McGuirk; Mari S. Rosen; Charlotte L. Stern; Amy A. Sarjeant; Chad A. Mirkin; Inorganic Chemistry 52 (2013) 5876–5888; doi:10.1021/ic302855f

data_4334856
_publ_contact_author_name
;
;
_publ_section_title
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 General Strategy for the Synthesis of Rigid Weak-Link Approach
 Platinum(II) Complexes: Tweezers, Triple-Layer Complexes, and Macrocycles
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5876
_journal_page_last               5888
_journal_paper_doi               10.1021/ic302855f
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C68 H64 P4 Pt2 S4, 4(B F4)'
_chemical_formula_sum            'C68 H64 B4 F16 P4 Pt2 S4'
_chemical_formula_weight         1870.73
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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
_audit_creation_date             2012-11-14
_audit_creation_method
;
  Olex2 1.2
  (compiled Nov  5 2012 18:25:38, GUI svn.r4372)
;
_cell_angle_alpha                89.9189(13)
_cell_angle_beta                 76.2852(12)
_cell_angle_gamma                70.1689(13)
_cell_formula_units_Z            2
_cell_length_a                   15.5695(4)
_cell_length_b                   16.0911(4)
_cell_length_c                   16.9236(5)
_cell_measurement_reflns_used    9929
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.40
_cell_measurement_theta_min      2.37
_cell_volume                     3860.21(18)
_computing_cell_refinement       'SAINT V7.23A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2.1-4 (Bruker, 2007)'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      99.98
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_av_unetI/netI     0.0359
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            107854
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.67
_diffrn_reflns_theta_min         1.24
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.888
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.6669
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0653 before and 0.0446 after correction.
The Ratio of minimum to maximum transmission is 0.8937.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.609
_exptl_crystal_description       prism
_exptl_crystal_F_000             1832
_exptl_crystal_size_max          0.305
_exptl_crystal_size_mid          0.193
_exptl_crystal_size_min          0.184
_refine_diff_density_max         3.349
_refine_diff_density_min         -1.834
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     911
_refine_ls_number_reflns         25483
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0517
_refine_ls_R_factor_gt           0.0344
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0398P)^2^+6.1017P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0847
_refine_ls_wR_factor_ref         0.0917
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19886
_reflns_number_total             25483
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic302855f_si_002_11.cif
_cod_data_source_block           39-BF4
_cod_database_code               4334856
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  H2 of C2, H3 of C3, H4 of C4, H5 of C5, H6 of C6, {H8A,H8B} of C8, H9 of C9,
   H10 of C10, H11 of C11, H9A of C9A, H10A of C10A, H11A of C11A, {H12,H12A}
  of C12, {H13A,H13B} of C13, {H14A,H14B} of C14, H16 of C16, H17 of C17, H54
  of C54, H53 of C53, H40 of C40, H42 of C42, H43 of C43, H44 of C44, H45 of
  C45, H46 of C46, {H47A,H47B} of C47, {H55A,H55B} of C55, {H56A,H56B} of C56,
  H58 of C58, H51 of C51, {H48A,H48B} of C48, H50 of C50, H60 of C60, H59 of
  C59, H39 of C39, H38 of C38, H37 of C37, H36 of C36, H34 of C34, H33 of C33,
  H32 of C32, H31 of C31, H30 of C30, H28 of C28, H27 of C27, H26 of C26, H25
  of C25, H24 of C24, {H22A,H22B} of C22, {H21A,H21B} of C21, H20 of C20, H19
  of C19, H68 of C68, H67 of C67, H66 of C66, H65 of C65, H64 of C64, H62 of
  C62, H61 of C61
2. others
 Sof(H8A)=1-Sof(H8B)=Sof(C9)=Sof(H9)=Sof(C10)=Sof(H10)=Sof(C11)=Sof(H11)=1-
 Sof(H8B)=1-Sof(H8B)=1-Sof(H8B)=1-Sof(H8B)=1-Sof(H8B)=1-Sof(H8B)=Sof(H12)=1-
 Sof(H8B)
3.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C14(H14A,H14B), C21(H21A,H21B), C22(H22A,H22B), C47(H47A,
 H47B), C48(H48A,H48B), C55(H55A,H55B), C56(H56A,H56B)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8A), C8(H8B), C9(H9), C10(H10),
 C11(H11), C9A(H9A), C10A(H10A), C11A(H11A), C12(H12), C12(H12A), C16(H16),
 C17(H17), C19(H19), C20(H20), C24(H24), C25(H25), C26(H26), C27(H27), C28(H28),
  C30(H30), C31(H31), C32(H32), C33(H33), C34(H34), C36(H36), C37(H37),
 C38(H38), C39(H39), C40(H40), C42(H42), C43(H43), C44(H44), C45(H45), C46(H46),
  C50(H50), C51(H51), C53(H53), C54(H54), C58(H58), C59(H59), C60(H60),
 C61(H61), C62(H62), C64(H64), C65(H65), C66(H66), C67(H67), C68(H68)
;
_smtbx_masks_special_details
;
The solvent masking procedure as implemented in Olex2 was used to remove the
electronic contribution of solvent molecules from the refinement.  As the exact
solvent content is not known, only the atoms used in the refinement model are
reported in the formula here.

Total solvent accessible volume / cell = 655.9 Ang^3^ [17.0%]
Total electron count / cell = 176.8
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