Mixed-Valence Superstructure Assembled from a Mixed-Valence Host-Guest Complex.
Liu, Zhichang; Frasconi, Marco; Liu, Wei-Guang; Zhang, Yu; Dyar, Scott M.; Shen, Dengke; Sarjeant, Amy A.; Goddard, 3rd, William A; Wasielewski, Michael R.; Stoddart, J. Fraser; Journal of the American Chemical Society 140 (2018) 9387–9391; doi:10.1021/jacs.8b05322

data_4132643
_publ_section_title
;
 Mixed-Valence Superstructure Assembled from a Mixed-Valence Host-Guest
 Complex.
;
_journal_issue                   30
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9387
_journal_page_last               9391
_journal_paper_doi               10.1021/jacs.8b05322
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety
'6(C36 H32 N4), 3(C12 H14 N2), 2(F6 P), 6(C2 H3 N)'
_chemical_formula_sum            'C264 H252 F12 N36 P2'
_chemical_formula_weight         4218.94
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2012-12-03
_audit_creation_method
;
  Olex2 1.2
  (compiled Nov  5 2012 18:25:38, GUI svn.r4372)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   33.494(3)
_cell_length_b                   33.494(3)
_cell_length_c                   17.2240(17)
_cell_measurement_reflns_used    9849
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.44
_cell_measurement_theta_min      2.64
_cell_volume                     16734(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
;
XM, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      100.01
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.901
_diffrn_measured_fraction_theta_max 0.997
_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  0.0414
_diffrn_reflns_av_unetI/netI     0.0255
_diffrn_reflns_Laue_measured_fraction_full 0.901
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            32335
_diffrn_reflns_point_group_measured_fraction_full 0.901
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        66.440
_diffrn_reflns_theta_max         62.350
_diffrn_reflns_theta_min         4.573
_diffrn_source                   microsource
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.786
_exptl_absorpt_correction_T_max  0.7378
_exptl_absorpt_correction_T_min  0.6422
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0748 before and 0.0585 after correction.
The Ratio of minimum to maximum transmission is 0.8704.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.256
_exptl_crystal_description       block
_exptl_crystal_F_000             6678
_exptl_crystal_size_max          0.161
_exptl_crystal_size_mid          0.109
_exptl_crystal_size_min          0.086
_refine_diff_density_max         0.631
_refine_diff_density_min         -0.321
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     527
_refine_ls_number_reflns         5902
_refine_ls_number_restraints     189
_refine_ls_restrained_S_all      2.172
_refine_ls_R_factor_all          0.0600
_refine_ls_R_factor_gt           0.0534
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.1061P)^2^+22.8543P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1722
_refine_ls_wR_factor_ref         0.1809
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5081
_reflns_number_total             5902
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b05322_si_001.cif
_cod_data_source_block           n2314
_cod_original_cell_volume        16734(4)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4132643
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  H9 of C9, H10 of C10, {H11A,H11B} of C11, H8 of C8, H4 of C4, H5 of C5, H2
  of C2, H1 of C1, H7 of C7, H34 of C34, H35 of C35, {H36A,H36B} of C36, H37 of
  C37, H38 of C38, H40 of C40, H41 of C41, H32 of C32, H31 of C31, {H29A,H29B}
  of C29, H28 of C28, H27 of C27, H26 of C26, H25 of C25, H23 of C23, H22 of
  C22, H20 of C20, H19 of C19, {H18A,H18B} of C18, H17 of C17, H16 of C16, H14
  of C14, H13 of C13
 At 1.5 times of:
  {H2SA,H2SB,H2SC} of C2S, {H42A,H42B,H42C} of C42
2. Restrained distances
 F8-F4 ~ F8-F3 ~ F8-F7 ~ F8-F2 ~ F4-F5 ~ F4-F3 ~ F4-F2 ~ F5-F3 ~ F5-F7 ~ F5-F2
 ~ F3-F7 ~ F7-F2 ~ F8-F5 ~ F4-F7 ~ F3-F2
 with sigma of 0.04
 P2-F8 ~ P2-F4 ~ P2-F5 ~ P2-F3 ~ P2-F7 ~ P2-F2
 with sigma of 0.02
3. Rigid bond restraints
 P2, F2, F3, F4, F5, F7, F8
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
P2 ~ F2 ~ F3 ~ F4 ~ F5 ~ F7 ~ F8: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
5. Others
 Fixed Sof: P2(0.16667) F2(0.16667) F3(0.16667) F4(0.16667) F5(0.16667)
 F7(0.16667) F8(0.16667)
6.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C18(H18A,H18B), C29(H29A,H29B), C36(H36A,H36B)
6.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C7(H7), C8(H8), C9(H9), C10(H10), C13(H13),
 C14(H14), C16(H16), C17(H17), C19(H19), C20(H20), C22(H22), C23(H23), C25(H25),
  C26(H26), C27(H27), C28(H28), C31(H31), C32(H32), C34(H34), C35(H35),
 C37(H37), C38(H38), C40(H40), C41(H41)
6.c Idealised Me refined as rotating group:
 C42(H42A,H42B,H42C), C2S(H2SA,H2SB,H2SC)
;
_shelx_estimated_absorpt_t_max   0.935
_shelx_estimated_absorpt_t_min   0.884
_shelx_hkl_checksum              94940
_shelx_res_checksum              1638
_shelxl_version_number           2012-6