Stable pseudo[3]rotaxanes with strong positive binding cooperativity based on shape-persistent aromatic oligoamide macrocycles.
Sobiech, Thomas A.; Zhong, Yulong; Sánchez B, Laura S; Kauffmann, Brice; McGrath, Jillian K.; Scalzo, Christina; Miller, Daniel P.; Huc, Ivan; Zurek, Eva; Ferrand, Yann; Gong, Bing; Chemical communications (Cambridge, England) 57 (2021) 11645–11648; doi:10.1039/d1cc05193h

data_7129195
_publ_section_title
;
 Stable pseudo[3]rotaxanes with strong positive binding cooperativity
 based on shape-persistent aromatic oligoamide macrocycles.
;
_journal_issue                   88
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              11645
_journal_page_last               11648
_journal_paper_doi               10.1039/d1cc05193h
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'F6 P, C90 H125 N6 O24, C13 H21 N, H2 O'
_chemical_formula_sum            'C103 H148 F6 N7 O25 P'
_chemical_formula_weight         2029.25
_chemical_name_systematic        macro1
_chemical_properties_physical    Air-sensitive
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-08-13
_audit_creation_method
;
Olex2 1.3
(compiled 2020.12.01 svn.r5f60950 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-08-13 deposited with the CCDC.	2021-10-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.9030(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.5642(2)
_cell_length_b                   21.6386(3)
_cell_length_c                   30.8946(3)
_cell_measurement_reflns_used    16184
_cell_measurement_temperature    130
_cell_measurement_theta_max      61.5770
_cell_measurement_theta_min      2.8680
_cell_volume                     10403.6(2)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      130
_diffrn_measured_fraction_theta_full 0.900
_diffrn_measured_fraction_theta_max 0.900
_diffrn_measurement_device_type  'Rigaku FRX'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0289
_diffrn_reflns_av_unetI/netI     0.0366
_diffrn_reflns_Laue_measured_fraction_full 0.900
_diffrn_reflns_Laue_measured_fraction_max 0.900
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            44426
_diffrn_reflns_point_group_measured_fraction_full 0.900
_diffrn_reflns_point_group_measured_fraction_max 0.900
_diffrn_reflns_theta_full        62.125
_diffrn_reflns_theta_max         62.125
_diffrn_reflns_theta_min         3.498
_diffrn_source                   'rotating anode'
_exptl_absorpt_coefficient_mu    0.929
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.24324
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            clear
_exptl_crystal_colour_lustre     clear
_exptl_crystal_density_diffrn    1.296
_exptl_crystal_description       block
_exptl_crystal_F_000             4336
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.596
_refine_diff_density_min         -0.662
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.917
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1301
_refine_ls_number_reflns         14786
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.917
_refine_ls_R_factor_all          0.1575
_refine_ls_R_factor_gt           0.1334
_refine_ls_shift/su_max          0.052
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4125
_refine_ls_wR_factor_ref         0.4392
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11106
_reflns_number_total             14786
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc05193h2.cif
_cod_data_source_block           macro_guest1_a
_cod_database_code               7129195
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1.a Free rotating group:
 O01H(H01Y,H)
1.b Ternary CH refined with riding coordinates:
 C022(H022), C02T(H02Y), C038(H038), C03N(H03), C03P(H4), C03V(H9)
1.c Secondary CH2 refined with riding coordinates:
 C01A(H01A,H01B), C01G(H01H,H01I), C01N(H01K,H01L), C01Q(H01M,H01N), C01R(H01O,
 H01P), C01V(H01Q,H01R), C01Z(H01V,H01X), C020(H02A,H02B), C028(H02L,H02M),
 C02E(H02O,H02P), C02G(H02R,H02S), C02I(H02T,H02U), C02J(H02V,H02W), C02V(H02Z,
 HA), C02X(H02,HB), C030(H17,HG), C031(H03A,H03B), C036(H03F,H03G), C03B(H18,
 HH), C03C(H03N,H03O), C03D(H19,HI), C03E(H20,HJ), C03F(H03P,H03Q), C03G(H03R,
 H03S), C03H(H21,HK), C03J(H22,HL), C03K(H23,HM), C03O(H3,HP), C03T(H7,HW),
 C03U(H8,HX)
1.d Aromatic/amide H refined with riding coordinates:
 N00E(H00E), N00M(H00M), N00P(H00P), N00Q(H00Q), N00R(H00R), N00S(H00S),
 C011(H011), C014(H014), C015(H015), C017(H017), C01B(H01C), C01C(H01D),
 C01I(H01J), C01W(H01W), C026(H026), C029(H029), C02A(H02N), C02D(H13),
 C02F(H02Q), C02L(H14), C02P(H15), C02Q(H02X), C02U(H16)
1.e Idealised Me refined as rotating group:
 C01D(H01E,H01F,H01G), C01Y(H01S,H01T,H01U), C021(H02C,H02D,H02E), C024(H02F,
 H02G,H02H), C025(H02I,H02J,H02K), C02Y(H1,HC,HD), C02Z(H2,HE,HF), C032(H03C,
 H03D,H03E), C039(H03H,H03I,H03J), C03A(H03K,H03L,H03M), C03I(H03T,H03U,H03V),
 C03L(H03W,H03X,H03Y), C03M(H03Z,HN,HO), C03Q(H24,HQ,HR), C03R(H5,HS,HT),
 C03S(H6,HU,HV), C03W(H10,HY,HZ), C03X(H11,H25,H26), C03Y(H12,H27,H28)
;
_shelx_res_checksum              87288
_olex2_submission_original_sample_id macro_guest1
_olex2_submission_special_instructions 'No special instructions were received'