Threading-gated photochromism in [2]pseudorotaxanes
Baggi, Giorgio; Casimiro, Lorenzo; Baroncini, Massimo; Silvi, Serena; Credi, Alberto; Loeb, Stephen J.; Chemical Science  (2019) –; doi:10.1039/C9SC00913B

data_1550931
_publ_section_title
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 Threading-gated photochromism in [2]pseudorotaxanes
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C9SC00913B
_journal_year                    2019
_chemical_formula_moiety         'C27 H21 N2 S2, B F4'
_chemical_formula_sum            'C27 H21 B F4 N2 S2'
_chemical_formula_weight         524.39
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-10-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-11-06 deposited with the CCDC.    2019-04-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.410(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.1113(4)
_cell_length_b                   14.2082(7)
_cell_length_c                   19.2241(8)
_cell_measurement_reflns_used    9757
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      28.16
_cell_measurement_theta_min      2.95
_cell_volume                     2477.57(19)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      170.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0725
_diffrn_reflns_av_unetI/netI     0.0228
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            116870
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.354
_diffrn_reflns_theta_min         2.867
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.265
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.7003
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0650 before and 0.0609 after correction. The Ratio of minimum to maximum transmission is 0.9391. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            white
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_description       Needle
_exptl_crystal_F_000             1080
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: hexanes ethyl acetate'
_exptl_crystal_size_max          0.402
_exptl_crystal_size_mid          0.086
_exptl_crystal_size_min          0.059
_refine_diff_density_max         0.485
_refine_diff_density_min         -0.511
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     420
_refine_ls_number_reflns         6152
_refine_ls_number_restraints     146
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0676
_refine_ls_R_factor_gt           0.0467
_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^)+(0.0391P)^2^+1.8264P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1024
_refine_ls_wR_factor_ref         0.1130
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4793
_reflns_number_total             6152
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc00913b2.cif
_cod_data_source_block           mo_gb032_0m
_cod_database_code               1550931
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.985
_shelx_estimated_absorpt_t_min   0.901
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
B1A \\sim F1 \\sim B1 \\sim F2 \\sim F3 \\sim F4 \\sim F3A \\sim F1A \\sim F2A:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C13) = Uanis(C13A)
Uanis(C18) = Uanis(C18A)
Uanis(C15) = Uanis(C15A)
Uanis(C19) = Uanis(C19A)
Uanis(C21) = Uanis(C21A)
Uanis(C14) = Uanis(C14A)
3. Same fragment restrains
{C20A, C19A, C13A, C14A, C15A, C16A, C17A, C21A, C18A, S1A} sigma for 1-2:
0.02, 1-3: 0.02
as
{C20, C19, C13, C14, C15, C16, C17, C21, C18, S1}
4. Others
 Sof(F3A)=Sof(F1A)=Sof(F2A)=Sof(B1A)=1-FVAR(1)
 Sof(F1)=Sof(F2)=Sof(F3)=Sof(B1)=FVAR(1)
 Sof(C20A)=Sof(H20D)=Sof(H20E)=Sof(H20F)=Sof(C19A)=Sof(C13A)=Sof(C14A)=
 Sof(C15A)=Sof(H15A)=Sof(C16A)=Sof(H16A)=Sof(C17A)=Sof(H17A)=Sof(C21A)=
 Sof(H21A)=Sof(C18A)=Sof(S1A)=1-FVAR(2)
 Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=Sof(C19)=Sof(C13)=Sof(C14)=Sof(C15)=
 Sof(H15)=Sof(C16)=Sof(H16)=Sof(C17)=Sof(H17)=Sof(C21)=Sof(H21)=Sof(C18)=
 Sof(S1)=FVAR(2)
5.a Aromatic/amide H refined with riding coordinates:
 C15(H15), C16(H16), C17(H17), C21(H21), N1(H1), N2(H2), C1(H1A), C2(H2A),
 C3(H3), C9(H9), C10(H10), C11(H11), C25(H25), C26(H26), C27(H27), C15A(H15A),
 C16A(H16A), C17A(H17A), C21A(H21A)
5.b Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C23(H23A,H23B,H23C), C20A(H20D,H20E,H20F)
;
_shelx_res_checksum              41278
_olex2_submission_special_instructions 'No special instructions were received'