Neighboring Component Effect in a Tri-stable [2]Rotaxane.
Wang, Yuping; Cheng, Tao; Sun, Junling; Liu, Zhichang; Frasconi, Marco; Goddard, 3rd, William A; Stoddart, J. Fraser; Journal of the American Chemical Society 140 (2018) 13827–13834; doi:10.1021/jacs.8b08519

data_4133100
_publ_section_title
;
 Neighboring Component Effect in a Tri-stable [2]Rotaxane.
;
_journal_issue                   42
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13827
_journal_page_last               13834
_journal_paper_doi               10.1021/jacs.8b08519
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C54 H52 F8 N8 O2, 2(F6 P)'
_chemical_formula_sum            'C54 H52 F20 N8 O2 P2'
_chemical_formula_weight         1286.97
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-09-18
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 103.544(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   33.633(3)
_cell_length_b                   10.3014(11)
_cell_length_c                   33.059(3)
_cell_measurement_reflns_used    4196
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      58.204
_cell_measurement_theta_min      5.893
_cell_volume                     11135.3(19)
_computing_cell_refinement       'SAINT V8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 V2014.11-0 (Bruker, 2014)'
_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, 2015)'
_diffrn_ambient_temperature      99.99
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.584
_diffrn_measured_fraction_theta_max 0.979
_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  0.2437
_diffrn_reflns_av_unetI/netI     0.1763
_diffrn_reflns_Laue_measured_fraction_full 0.584
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            34474
_diffrn_reflns_point_group_measured_fraction_full 0.584
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         51.136
_diffrn_reflns_theta_min         5.422
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    1.767
_exptl_absorpt_correction_T_max  0.7516
_exptl_absorpt_correction_T_min  0.5086
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0843 before and 0.0554 after correction.
The Ratio of minimum to maximum transmission is 0.6767.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.535
_exptl_crystal_description       needle
_exptl_crystal_F_000             5264
_exptl_crystal_size_max          0.175
_exptl_crystal_size_mid          0.068
_exptl_crystal_size_min          0.015
_refine_diff_density_max         1.134
_refine_diff_density_min         -0.804
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1565
_refine_ls_number_reflns         11773
_refine_ls_number_restraints     1422
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.1922
_refine_ls_R_factor_gt           0.1162
_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^)+(0.1098P)^2^+112.6669P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2785
_refine_ls_wR_factor_ref         0.3297
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6411
_reflns_number_total             11773
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b08519_si_002.cif
_cod_data_source_block           cx0556
_cod_original_cell_volume        11135.2(19)
_cod_database_code               4133100
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.974
_shelx_estimated_absorpt_t_min   0.747
_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 body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10), C49(H49), C52(H52), C7A(H7A), C10A(H10A), C49A(H49A),
 C52A(H52A)
3.b Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C22(H22A,H22B), C33(H33A,H33B), C42(H42A,H42B), C13A(H13C,
 H13D), C22A(H22C,H22D), C33A(H33C,H33D), C42A(H42C,H42D)
3.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C15(H15), C23(H23), C24(H24), C26(H26), C27(H27),
 C29(H29), C30(H30), C31(H31), C32(H32), C40(H40), C45(H45), C46(H46), C47(H47),
  C3A(H3A), C4A(H4A), C5A(H5A), C15A(H15A), C23A(H23A), C24A(H24A), C26A(H26A),
 C27A(H27A), C29A(H29A), C30A(H30A), C31A(H31A), C32A(H32A), C40A(H40A),
 C45A(H45A), C46A(H46A), C47A(H47A)
3.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C53(H53A,H53B,H53C), C54(H54A,H54B,
 H54C), C8A(H8AA,H8AB,H8AC), C9A(H9AA,H9AB,H9AC), C11A(H11D,H11E,H11F),
 C12A(H12D,H12E,H12F), C50A(H50D,H50E,H50F), C51A(H51D,H51E,H51F), C53A(H53D,
 H53E,H53F), C54A(H54D,H54E,H54F)
;
_shelx_res_checksum              10031
_shelx_hkl_checksum              69932
_olex2_date_sample_data_collection 2015-09-11
_olex2_date_sample_submission    2015-09-01
_olex2_submission_original_sample_id cx0556
_olex2_submission_special_instructions 'No special instructions were received'