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_4130592
_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
'C36 H32 N4, C36 H44 O10, 3(F6 P), 2(C2 H3 N)'
_chemical_formula_sum            'C76 H82 F18 N6 O10 P3'
_chemical_formula_weight         1674.38
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-03-17
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.12 svn.r2899 for OlexSys, GUI svn.r4796)
;
_cell_angle_alpha                90
_cell_angle_beta                 113.1366(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.9335(5)
_cell_length_b                   13.4484(3)
_cell_length_c                   27.6224(6)
_cell_measurement_reflns_used    9608
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      65.048
_cell_measurement_theta_min      3.954
_cell_volume                     7492.5(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    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.03
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.939
_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  'Quazar optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0219
_diffrn_reflns_av_unetI/netI     0.0134
_diffrn_reflns_Laue_measured_fraction_full 0.939
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            56084
_diffrn_reflns_point_group_measured_fraction_full 0.939
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         65.116
_diffrn_reflns_theta_min         3.480
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    1.685
_exptl_absorpt_correction_T_max  0.7526
_exptl_absorpt_correction_T_min  0.6284
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0548 before and 0.0355 after correction.
The Ratio of minimum to maximum transmission is 0.8350.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.484
_exptl_crystal_description       hexangonal
_exptl_crystal_F_000             3468
_exptl_crystal_size_max          0.455
_exptl_crystal_size_mid          0.404
_exptl_crystal_size_min          0.162
_refine_diff_density_max         0.532
_refine_diff_density_min         -0.369
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     531
_refine_ls_number_reflns         6377
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0411
_refine_ls_R_factor_gt           0.0408
_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^)+(0.0455P)^2^+13.7324P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1037
_refine_ls_wR_factor_ref         0.1039
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6276
_reflns_number_total             6377
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b04982_si_004.cif
_cod_data_source_block           n3379a
_cod_database_code               4130592
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.772
_shelx_estimated_absorpt_t_min   0.514
_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. Rigid bond restraints
 C24, C25, C24A, C25A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C24 \\sim C25 \\sim C24A \\sim C25A: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.01
4. Others
 Sof(C24A)=Sof(H24C)=Sof(H24D)=Sof(C25A)=Sof(H25C)=Sof(H25D)=1-FVAR(1)
 Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(C25)=Sof(H25A)=Sof(H25B)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C13(H13A,H13B), C24(H24A,H24B), C25(H25A,H25B), C24A(H24C,H24D),
 C25A(H25C,H25D), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,
 H29B), C30(H30A,H30B), C31(H31A,H31B)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C8(H8), C9(H9), C11(H11), C12(H12), C14(H14),
 C15(H15), C17(H17), C18(H18), C20(H20), C21(H21), C22(H22), C34(H34), C35(H35),
  C36(H36)
5.c Idealised Me refined as rotating group:
 C38(H38A,H38B,H38C)
;
_shelx_res_checksum              47569
_shelx_hkl_checksum              89865
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'