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_4334848
_publ_contact_author_name
;
;
_publ_section_title
;
 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         '2(C40 H38 Cl O P2 Pt S), 2(F6 P), C H2 Cl2'
_chemical_formula_sum            'C81 H78 Cl4 F12 O2 P6 Pt2 S2'
_chemical_formula_weight         2093.35
_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
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-06-04
_audit_creation_method
;
  Olex2 1.2
  (compiled May  9 2012 12:37:22, GUI svn.r4230)
;
_cell_angle_alpha                67.4410(10)
_cell_angle_beta                 88.8570(10)
_cell_angle_gamma                82.232(2)
_cell_formula_units_Z            2
_cell_length_a                   13.0672(5)
_cell_length_b                   18.0102(7)
_cell_length_c                   18.8700(7)
_cell_measurement_reflns_used    9935
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      64.43
_cell_measurement_theta_min      2.68
_cell_volume                     4061.0(3)
_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
;
XL, 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      99.92
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Quazar optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0220
_diffrn_reflns_av_unetI/netI     0.0288
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            25931
_diffrn_reflns_theta_full        64.63
_diffrn_reflns_theta_max         64.63
_diffrn_reflns_theta_min         2.54
_diffrn_source                   microsource
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.795
_exptl_absorpt_correction_T_max  0.7525
_exptl_absorpt_correction_T_min  0.5291
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0662 before and 0.0324 after correction.
The Ratio of minimum to maximum transmission is 0.7031.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.712
_exptl_crystal_description       plate
_exptl_crystal_F_000             2068
_exptl_crystal_size_max          0.268
_exptl_crystal_size_mid          0.224
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.731
_refine_diff_density_min         -1.399
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.164
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1004
_refine_ls_number_reflns         13141
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.181
_refine_ls_R_factor_all          0.0370
_refine_ls_R_factor_gt           0.0364
_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^)+(0.0225P)^2^+20.7546P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0917
_refine_ls_wR_factor_ref         0.0921
_reflns_number_gt                12877
_reflns_number_total             13141
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302855f_si_002_03.cif
_cod_data_source_block           29b
_cod_database_code               4334848