Mechanical insulation of aza-Pechmann dyes within [2]rotaxanes.
Cutillas-Font, Guillermo; Pastor, Aurelia; Alajarin, Mateo; Martinez-Cuezva, Alberto; Marin-Luna, Marta; Batanero, Belen; Berna, Jose; Chemical science 15 (2024) 13823–13831; doi:10.1039/d4sc03657c

data_1572220
_publ_section_title
;
 Mechanical insulation of aza-Pechmann dyes within [2]rotaxanes.
;
_journal_issue                   34
_journal_name_full               'Chemical science'
_journal_page_first              13823
_journal_page_last               13831
_journal_paper_doi               10.1039/d4sc03657c
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C40 H58 N2 O2 S2, C32 H28 N4 O4'
_chemical_formula_sum            'C72 H86 N6 O6 S2'
_chemical_formula_weight         1195.58
_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             2023-05-22
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-02-26 deposited with the CCDC.	2024-07-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.854(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.549(5)
_cell_length_b                   14.378(5)
_cell_length_c                   30.473(10)
_cell_measurement_reflns_used    9666
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      28.212
_cell_measurement_theta_min      2.280
_cell_volume                     6280(4)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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      100.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 QUEST PHOTON II CMOS'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0764
_diffrn_reflns_av_unetI/netI     0.0318
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            242329
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.332
_diffrn_reflns_theta_min         1.789
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.144
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6755
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1560 before and 0.0742 after correction.
The Ratio of minimum to maximum transmission is 0.9059.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.264
_exptl_crystal_description       lath
_exptl_crystal_F_000             2560
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.693
_refine_diff_density_min         -0.805
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.177
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     793
_refine_ls_number_reflns         15617
_refine_ls_number_restraints     215
_refine_ls_restrained_S_all      1.169
_refine_ls_R_factor_all          0.1174
_refine_ls_R_factor_gt           0.0666
_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^)+(0.0799P)^2^+9.6946P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1650
_refine_ls_wR_factor_ref         0.2205
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10340
_reflns_number_total             15617
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc03657c2.cif
_cod_data_source_block           ii_gcf23_0msp
_cod_depositor_comments
'Adding full bibliography for 1572219--1572220.cif.'
_cod_original_cell_volume        6281(4)
_cod_database_code               1572220
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.997
_shelx_estimated_absorpt_t_min   0.949
_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
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B),
 C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B),
  C19(H19A,H19B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,
 H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B),
 C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B), C49(H49A,H49B), C56(H56A,H56B),
  C65(H65A,H65B), C72(H72A,H72B)
3.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C7(H7), C8(H8), C24(H24), C26(H26), C27(H27), C28(H28),
 C43(H43), C44(H44), C45(H45), C47(H47), C51(H51), C52(H52), C54(H54), C55(H55),
  C59(H59), C60(H60), C61(H61), C63(H63), C67(H67), C68(H68), C70(H70), C71(H71)
3.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C40(H40A,H40B,H40C)
;
_shelx_res_checksum              72270
_shelx_hkl_checksum              70025
_olex2_submission_special_instructions 'No special instructions were received'