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_4122351
_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
'C46 H52 N12 Pt2, 2(C34 H44 O10 S4), 2(O4 S), 7(F6 P), 8(C2 H3 N)'
_chemical_formula_sum            'C130 H164 F42 N20 O28 P7 Pt2 S10'
_chemical_formula_weight         4180.37
_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             2012-11-15
_audit_creation_method
;
  Olex2 1.2
  (compiled Nov  5 2012 18:25:38, GUI svn.r4372)
;
_cell_angle_alpha                72.636(2)
_cell_angle_beta                 71.569(2)
_cell_angle_gamma                68.9620(10)
_cell_formula_units_Z            1
_cell_length_a                   13.8756(5)
_cell_length_b                   17.1561(7)
_cell_length_c                   21.5948(8)
_cell_measurement_reflns_used    9944
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      64.40
_cell_measurement_theta_min      4.64
_cell_volume                     4451.5(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
;
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      99.96
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.841
_diffrn_measured_fraction_theta_max 0.957
_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  0.0423
_diffrn_reflns_av_unetI/netI     0.0439
_diffrn_reflns_Laue_measured_fraction_full 0.841
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            40651
_diffrn_reflns_point_group_measured_fraction_full 0.841
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         62.38
_diffrn_reflns_theta_min         2.82
_diffrn_source                   microsource
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.579
_exptl_absorpt_correction_T_max  0.7525
_exptl_absorpt_correction_T_min  0.5197
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0992 before and 0.0541 after correction.
The Ratio of minimum to maximum transmission is 0.6906.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.559
_exptl_crystal_description       plate
_exptl_crystal_F_000             2107
_exptl_crystal_size_max          0.197
_exptl_crystal_size_mid          0.115
_exptl_crystal_size_min          0.011
_refine_diff_density_max         2.185
_refine_diff_density_min         -1.039
_refine_diff_density_rms         0.149
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1165
_refine_ls_number_reflns         13545
_refine_ls_number_restraints     978
_refine_ls_restrained_S_all      1.132
_refine_ls_R_factor_all          0.0753
_refine_ls_R_factor_gt           0.0645
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.1017P)^2^+23.0111P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1744
_refine_ls_wR_factor_ref         0.1857
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11716
_reflns_number_total             13545
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja504662a_si_007.cif
_cod_data_source_block           n2292
_cod_depositor_comments
'Adding full bibliography for 4122349--4122355.cif.'
_cod_database_code               4122351
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  {H35A,H35B} of C35, H21 of C21, {H37A,H37B} of C37, {H31A,H31B} of C31, H22
  of C22, {H32A,H32B} of C32, H25 of C25, {H33A,H33B} of C33, H28 of C28, {H30A,
  H30B} of C30, {H34A,H34B} of C34, {H36A,H36B} of C36, H23 of C23, H9 of C9,
  H10 of C10, H11 of C11, H12 of C12, {H1A,H1B} of N1, {H2A,H2B} of N2, {H1C,
  H1D} of C1, {H2C,H2D} of C2, H3 of C3, H4 of C4, H6 of C6, H7 of C7, {H38A,
  H38B} of C38, H40 of C40, H41 of C41, H42 of C42, H45 of C45, H46 of C46, H47
  of C47, {H49A,H49B} of C49, {H50A,H50B} of C50, {H51A,H51B} of C51, {H52A,
  H52B} of C52, {H53A,H53B} of C53, {H54A,H54B} of C54, {H55A,H55B} of C55,
  {H56A,H56B} of C56, {H57A,H57B} of C57, {H13A,H13B} of C13, H14 of C14, H15
  of C15, H17 of C17, H18 of C18, H20 of C20
 At 1.5 times of:
  {H59A,H59B,H59C} of C59, {H61A,H61B,H61C} of C61, {H63A,H63B,H63C} of C63,
  {H65A,H65B,H65C} of C65, {H67A,H67B,H67C} of C67
2. Same fragment restrains
{F1, F2, F3, F4, F5, F6}
as
{F7, F8, F9, F10, F11, F12}
{F1, F2, F3, F4, F5, F6}
as
{F7A, F8A, F9A, F10A, F11A, F12A}
3. Others
 Sof(F7)=Sof(F8)=Sof(F9)=Sof(F10)=Sof(F11)=Sof(F12)=1-Sof(F8)=1-Sof(F8)=1-
 Sof(F8)=1-Sof(F8)=1-Sof(F8)=1-Sof(F8)
 Fixed Sof: N8(0.5) C60(0.5) C61(0.5) H61A(0.5) H61B(0.5) H61C(0.5) N11(0.5)
 C66(0.5) C67(0.5) H67A(0.5) H67B(0.5) H67C(0.5)
4.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), N2(H2A,H2B), C1(H1C,H1D), C2(H2C,H2D), C13(H13A,H13B), C30(H30A,
 H30B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B),
 C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B), C49(H49A,H49B),
  C50(H50A,H50B), C51(H51A,H51B), C52(H52A,H52B), C53(H53A,H53B), C54(H54A,
 H54B), C55(H55A,H55B), C56(H56A,H56B), C57(H57A,H57B)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11), C12(H12),
 C14(H14), C15(H15), C17(H17), C18(H18), C20(H20), C21(H21), C22(H22), C23(H23),
  C25(H25), C28(H28), C40(H40), C41(H41), C42(H42), C45(H45), C46(H46), C47(H47)
4.c Idealised Me refined as rotating group:
 C59(H59A,H59B,H59C), C61(H61A,H61B,H61C), C63(H63A,H63B,H63C), C65(H65A,H65B,
 H65C), C67(H67A,H67B,H67C)
;
_smtbx_masks_special_details
;
Total solvent accessible volume / cell = 307.2 Ang^3^ [6.9%]
Total electron count / cell = 24.0

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.
;
_shelx_estimated_absorpt_t_max   0.941
_shelx_estimated_absorpt_t_min   0.406
_shelx_hkl_checksum              55256
_shelx_res_checksum              61715
_shelxl_version_number           2012-6