Sliding-Ring Catenanes.
Fernando, Isurika R.; Frasconi, Marco; Wu, Yilei; Liu, Wei-Guang; Wasielewski, Michael R.; Goddard, 3rd, William A; Stoddart, J. Fraser; Journal of the American Chemical Society 138 (2016) 10214–10225; doi:10.1021/jacs.6b04982

data_4130590
_publ_section_title
;
 Sliding-Ring Catenanes.
;
_journal_issue                   32
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10214
_journal_page_last               10225
_journal_paper_doi               10.1021/jacs.6b04982
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety
'2(C28 H40 O10), 2(C36 H32 N4), 6(F6 P), 11(C2 H3 N)'
_chemical_formula_sum            'C150 H177 F36 N19 O20 P6'
_chemical_formula_weight         3435.92
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2014-03-31
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_cell_angle_alpha                90
_cell_angle_beta                 93.421(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.1189(5)
_cell_length_b                   19.7795(6)
_cell_length_c                   45.0588(12)
_cell_measurement_reflns_used    9804
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      67.128
_cell_measurement_theta_min      3.405
_cell_volume                     17009.2(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    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XM (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.938
_diffrn_measured_fraction_theta_max 0.994
_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  0.0307
_diffrn_reflns_av_unetI/netI     0.0268
_diffrn_reflns_Laue_measured_fraction_full 0.938
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       53
_diffrn_reflns_limit_l_min       -53
_diffrn_reflns_number            128195
_diffrn_reflns_point_group_measured_fraction_full 0.938
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         65.084
_diffrn_reflns_theta_min         1.964
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    1.509
_exptl_absorpt_correction_T_max  0.7530
_exptl_absorpt_correction_T_min  0.6747
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0511 before and 0.0418 after correction.
The Ratio of minimum to maximum transmission is 0.8960.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_description       block
_exptl_crystal_F_000             7136
_exptl_crystal_size_max          0.196
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.046
_refine_diff_density_max         1.710
_refine_diff_density_min         -0.492
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2161
_refine_ls_number_reflns         28831
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0916
_refine_ls_R_factor_gt           0.0749
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0908P)^2^+47.2778P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2042
_refine_ls_wR_factor_ref         0.2130
_reflns_Friedel_coverage         0.000
_reflns_number_gt                22524
_reflns_number_total             28831
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b04982_si_005.cif
_cod_data_source_block           n3424
_cod_database_code               4130590
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.934
_shelx_estimated_absorpt_t_min   0.756
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 1*[Sof(P1)+Sof(F1)+Sof(F2)+Sof(F3)+Sof(F4)+Sof(F5)+Sof(F6)]+1*[Sof(P2)+
 Sof(F7)+Sof(F8)+Sof(F9)+Sof(F10)+Sof(F11)+Sof(F12)]+1*[Sof(P3)+Sof(F13)+
 Sof(F14)+Sof(F15)+Sof(F16)+Sof(F17)+Sof(F18)]+1*[Sof(P4)+Sof(F19)+Sof(F20)+
 Sof(F21)+Sof(F22)+Sof(F23)+Sof(F24)]+1*[Sof(P5)+Sof(F25)+Sof(F26)+Sof(F27)+
 Sof(F28)+Sof(F29)+Sof(F30)]+1*[Sof(P6)+Sof(F31)+Sof(F32)+Sof(F33)+Sof(F34)+
 Sof(F35)+Sof(F36)]+1*[Sof(P7)+Sof(F37)+Sof(F38)+Sof(F39)+Sof(F40)+Sof(F41)+
 Sof(F42)]=6 with esd of 0.0001
 Sof(P1)=Sof(F1)=Sof(F2)=Sof(F3)=Sof(F4)=Sof(F5)=Sof(F6)=FVAR(1)
 Sof(P2)=Sof(F7)=Sof(F8)=Sof(F9)=Sof(F10)=Sof(F11)=Sof(F12)=FVAR(2)
 Sof(P3)=Sof(F13)=Sof(F14)=Sof(F15)=Sof(F16)=Sof(F17)=Sof(F18)=FVAR(3)
 Sof(P4)=Sof(F19)=Sof(F20)=Sof(F21)=Sof(F22)=Sof(F23)=Sof(F24)=FVAR(4)
 Sof(P5)=Sof(F25)=Sof(F26)=Sof(F27)=Sof(F28)=Sof(F29)=Sof(F30)=FVAR(5)
 Sof(P6)=Sof(F31)=Sof(F32)=Sof(F33)=Sof(F34)=Sof(F35)=Sof(F36)=FVAR(6)
 Sof(P7)=Sof(F37)=Sof(F38)=Sof(F39)=Sof(F40)=Sof(F41)=Sof(F42)=FVAR(7)
3.a Secondary CH2 refined with riding coordinates:
 C79(H79A,H79B), C80(H80A,H80B), C81(H81A,H81B), C82(H82A,H82B), C83(H83A,
 H83B), C84(H84A,H84B), C85(H85A,H85B), C86(H86A,H86B), C93(H93A,H93B),
 C94(H94A,H94B), C95(H95A,H95B), C96(H96A,H96B), C97(H97A,H97B), C98(H98A,H98B),
  C99(H99A,H99B), C100(H10A,H10B), C1A(H1AA,H1AB), C18(H18A,H18B), C29(H29A,
 H29B), C36(H36A,H36B), C5(H5A,H5B), C107(H10C,H10D), C108(H10E,H10F),
 C109(H10G,H10H), C110(H11A,H11B), C111(H11C,H11D), C112(H11E,H11F), C113(H11G,
 H11H), C114(H11I,H11J), C121(H12A,H12B), C122(H12C,H12D), C123(H12E,H12F),
 C124(H12G,H12H), C125(H12I,H12J), C127(H12K,H12L), C128(H12M,H12N), C47(H47A,
 H47B), C54(H54A,H54B), C65(H65A,H65B), C72(H72A,H72B)
3.b Aromatic/amide H refined with riding coordinates:
 C74(H74), C75(H75), C77(H77), C78(H78), C88(H88), C89(H89), C91(H91),
 C92(H92), C1(H1), C2(H2), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11),
 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), C102(H102), C103(H103), C105(H105), C106(H106), C116(H116),
 C117(H117), C119(H119), C120(H120), C37(H37), C38(H38), C40(H40), C41(H41),
 C43(H43), C44(H44), C45(H45), C46(H46), C49(H49), C50(H50), C52(H52), C53(H53),
  C55(H55), C56(H56), C58(H58), C59(H59), C61(H61), C62(H62), C63(H63),
 C64(H64), C67(H67), C68(H68), C70(H70), C71(H71)
3.c Idealised Me refined as rotating group:
 C2S(H2SA,H2SB,H2SC), C4S(H4SA,H4SB,H4SC), C6S(H6SA,H6SB,H6SC), C8S(H8SA,H8SB,
 H8SC), C10S(H10I,H10J,H10K), C12S(H12O,H12P,H12Q), C14S(H14A,H14B,H14C),
 C16S(H16A,H16B,H16C), C18S(H18C,H18D,H18E), C20S(H20A,H20B,H20C), C22S(H22A,
 H22B,H22C)
;
_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 = 995.7 Ang^3^ [5.9%]
Total electron count / cell = 209.5
;
_shelx_res_checksum              13994
_shelx_hkl_checksum              64240