Mechanical bonds and topological effects in radical dimer stabilization.
Frasconi, Marco; Kikuchi, Takashi; Cao, Dennis; Wu, Yilei; Liu, Wei-Guang; Dyar, Scott M.; Barin, Gokhan; Sarjeant, Amy A.; Stern, Charlotte L.; Carmieli, Raanan; Wang, Cheng; Wasielewski, Michael R.; Goddard, 3rd, William A; Stoddart, J. Fraser; Journal of the American Chemical Society 136 (2014) 11011–11026; doi:10.1021/ja504662a

data_4122355
_publ_section_title
;
 Mechanical bonds and topological effects in radical dimer stabilization.
;
_journal_issue                   31
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11011
_journal_page_last               11026
_journal_paper_doi               10.1021/ja504662a
_journal_volume                  136
_journal_year                    2014
_chemical_formula_moiety
'C68 H88 O20 S8, C46 H52 N12 Pt2, 7(F6 P), 2(Cl O4), 9(C2 H3 N)'
_chemical_formula_sum            'C132 H167 Cl2 F42 N21 O28 P7 Pt2 S8'
_chemical_formula_weight         4228.20
_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     dual
_audit_creation_date             2012-10-24
_audit_creation_method
;
  Olex2 1.2
  (compiled May  9 2012 12:37:22, GUI svn.r4230)
;
_cell_angle_alpha                104.377(2)
_cell_angle_beta                 102.420(2)
_cell_angle_gamma                99.953(2)
_cell_formula_units_Z            2
_cell_length_a                   17.1706(8)
_cell_length_b                   20.6416(10)
_cell_length_c                   27.7781(14)
_cell_measurement_reflns_used    9783
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      67.76
_cell_measurement_theta_min      2.40
_cell_volume                     9043.6(8)
_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
;
XLMP, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
XM, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      99.99
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'MX optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0324
_diffrn_reflns_av_unetI/netI     0.0230
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            179427
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.07
_diffrn_reflns_theta_min         2.28
_diffrn_source                   microsource
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.556
_exptl_absorpt_correction_T_max  0.7530
_exptl_absorpt_correction_T_min  0.4515
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0988 before and 0.0489 after correction.
The Ratio of minimum to maximum transmission is 0.5996.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.553
_exptl_crystal_description       block
_exptl_crystal_F_000             4262
_exptl_crystal_size_max          0.382
_exptl_crystal_size_mid          0.162
_exptl_crystal_size_min          0.094
_refine_diff_density_max         2.502
_refine_diff_density_min         -1.021
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2547
_refine_ls_number_reflns         32487
_refine_ls_number_restraints     3495
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0610
_refine_ls_R_factor_gt           0.0581
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0920P)^2^+31.7905P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1591
_refine_ls_wR_factor_ref         0.1617
_reflns_Friedel_coverage         0.000
_reflns_number_gt                29973
_reflns_number_total             32487
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja504662a_si_008.cif
_cod_data_source_block           n2151a_a
_cod_depositor_comments
'Adding full bibliography for 4122349--4122355.cif.'
_cod_database_code               4122355
_diffrn_reflns_sigmai/neti       0.0230
_refinement_special_details
;
All PF6 anions were subjected to various SADI restraints to preserve the 
octahedral environment around the P atoms. Chemically equivalent C-C, C-O, 
and 1,3 C-C distances in the disordered glycol chain and C-C and C-N distances 
in disordered acetonitrile molecules  were restrained to be equal (SADI).  
Global rigid bond (DELU) and similarity (SIMU) restraints were 
applied to keep displacement parameters reasonable. Six PF6 anion sites 
were determined to be partially occupied. Site occupancies for these were 
summed to equal a total of 3PF6 anions in order to account for charge 
balancing.
;
_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 = 755.9 Ang^3^ [8.4%]
Total electron count / cell = 206.8
;
_shelx_estimated_absorpt_t_max   0.623
_shelx_estimated_absorpt_t_min   0.225
_shelx_hkl_checksum              76010
_shelx_res_checksum              51819
_shelxl_version_number           2012-4