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_4334847
_publ_contact_author_name
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;
_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         'C40 H34 F4 P2 Pt S2, 2(B F4)'
_chemical_formula_sum            'C40 H34 B2 F12 P2 Pt S2'
_chemical_formula_weight         1085.44
_chemical_name_systematic
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 ? 
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_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-02-22
_audit_creation_method
;
  Olex2 1.1
  (compiled Nov  1 2011 20:42:30, GUI svn.r3906)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.4113(5)
_cell_length_b                   18.8566(5)
_cell_length_c                   26.4263(6)
_cell_measurement_reflns_used    9981
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      67.25
_cell_measurement_theta_min      3.75
_cell_volume                     9174.5(4)
_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
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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    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      99.99
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_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     1.54184
_diffrn_reflns_av_R_equivalents  0.0545
_diffrn_reflns_av_unetI/netI     0.0279
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            90169
_diffrn_reflns_theta_full        67.82
_diffrn_reflns_theta_max         67.82
_diffrn_reflns_theta_min         1.67
_diffrn_source                   microsource
_diffrn_source_current           0.65
_diffrn_source_power             0.02925
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    7.916
_exptl_absorpt_correction_T_max  0.7530
_exptl_absorpt_correction_T_min  0.5005
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
R(int) was 0.1065 before and 0.0642 after correction.
The Ratio of minimum to maximum transmission is 0.6647.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.572
_exptl_crystal_description       needle
_exptl_crystal_F_000             4256
_exptl_crystal_size_max          0.502
_exptl_crystal_size_mid          0.051
_exptl_crystal_size_min          0.026
_refine_diff_density_max         5.881
_refine_diff_density_min         -1.479
_refine_diff_density_rms         0.177
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.200
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     522
_refine_ls_number_reflns         8197
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.202
_refine_ls_R_factor_all          0.0848
_refine_ls_R_factor_gt           0.0778
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0267P)^2^+197.8434P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1660
_refine_ls_wR_factor_ref         0.1686
_reflns_number_gt                7232
_reflns_number_total             8197
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302855f_si_002_02.cif
_cod_data_source_block           24
_cod_database_code               4334847
_smtbx_masks_special_details
;
Total solvent accessible volume / cell = 1290.6 Ang^3^ [14.1%]
Total electron count / cell = 423.4

The solvent masking procedure as implemented in Olex2 was used to remove the
electronic contribution of solvent molecules from the refinement.  Only the
atoms used in the refinement model are reported in the formula here.
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