Cu(ii) templated formation of [n]pseudorotaxanes (n = 2, 3, 4) using a tris-amino ether macrocyclic wheel and multidentate axles.
Bej, Somnath; Nandi, Mandira; Ghosh, Tamal Kanti; Ghosh, Pradyut; Dalton transactions (Cambridge, England : 2003) 48 (2019) 6853–6862; doi:10.1039/c9dt01067j

data_7049609
_publ_section_title
;
 Cu(ii) templated formation of [n]pseudorotaxanes (n = 2, 3, 4) using a
 tris-amino ether macrocyclic wheel and multidentate axles.
;
_journal_issue                   20
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6853
_journal_page_last               6862
_journal_paper_doi               10.1039/c9dt01067j
_journal_volume                  48
_journal_year                    2019
_chemical_absolute_configuration unk
_chemical_formula_moiety
'C49 H49 Cu N5 O4, 2(C F3 O3 S), C2 H3 N, 1[C2H3N]'
_chemical_formula_sum            'C55 H55 Cu F6 N7 O10 S2'
_chemical_formula_weight         1215.72
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-04-02
_audit_creation_method
;
Olex2 1.3-dev
(compiled 2019.03.18 svn.r3573 for OlexSys, GUI svn.r5585)
;
_audit_update_record
;
2019-04-03 deposited with the CCDC.    2019-04-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.701(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.630(4)
_cell_length_b                   15.523(4)
_cell_length_c                   24.015(7)
_cell_measurement_reflns_used    9252
_cell_measurement_temperature    127(2)
_cell_measurement_theta_max      24.98
_cell_measurement_theta_min      2.19
_cell_volume                     5391(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_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, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      127.56
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0917
_diffrn_reflns_av_unetI/netI     0.1190
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            45000
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        25.026
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_min         2.192
_exptl_absorpt_coefficient_mu    0.570
_exptl_absorpt_correction_T_max  .989
_exptl_absorpt_correction_T_min  .980
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            GREEN
_exptl_crystal_density_diffrn    1.498
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             2516
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.661
_refine_diff_density_min         -0.462
_refine_diff_density_rms         0.092
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.474(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1488
_refine_ls_number_reflns         18637
_refine_ls_number_restraints     285
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0851
_refine_ls_R_factor_gt           0.0688
_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^)+(0.1059P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1748
_refine_ls_wR_factor_ref         0.1909
_reflns_Friedel_coverage         0.884
_reflns_Friedel_fraction_full    0.956
_reflns_Friedel_fraction_max     0.956
_reflns_number_gt                14949
_reflns_number_total             18637
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01067j2.cif
_cod_data_source_block           '[2]pseudorotaxane'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'MULTI-SCAN' changed to
'multi-scan' according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7049609.cif.
;
_cod_original_cell_volume        5391(2)
_cod_database_code               7049609
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.526(17)
 0.474(17)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C1A-F4 \\sim C1A-F5 \\sim C1A-F6
 with sigma of 0.02
 F4-F5 \\sim F5-F6 \\sim F6-F4
 with sigma of 0.04
 S6-F4 \\sim S6-F5 \\sim S6-F6
 with sigma of 0.04
 S6-O18 \\sim S6-O19 \\sim S6-O1A
 with sigma of 0.02
 O18-O19 \\sim O19-O1A \\sim O18-O1A
 with sigma of 0.04
 C1A-O18 \\sim C1A-O19 \\sim C1A-O1A
 with sigma of 0.04
 C1A-F4 \\sim C1B-F4A
 with sigma of 0.02
 C1A-F5 \\sim C1B-F5A
 with sigma of 0.02
 C1A-F6 \\sim C1B-F6A
 with sigma of 0.02
 S6-O19 \\sim S6A-O19A
 with sigma of 0.02
 C1A-S6 \\sim C1B-S6A
 with sigma of 0.04
 C1A-O18 \\sim C1B-O18A
 with sigma of 0.04
 C1A-O19 \\sim C1B-O19A
 with sigma of 0.04
 C1A-O1A \\sim C1B-O1B
 with sigma of 0.04
 F4-F5 \\sim F4A-F5A
 with sigma of 0.04
 F4-F6 \\sim F4A-F6A
 with sigma of 0.04
 F4-S6 \\sim F4A-S6A
 with sigma of 0.04
 F5-F6 \\sim F5A-F6A
 with sigma of 0.04
 F5-S6 \\sim F5A-S6A
 with sigma of 0.04
 F6-S6 \\sim F6A-S6A
 with sigma of 0.04
 S6-O18 \\sim S6A-O18A
 with sigma of 0.04
 S6-O1A \\sim S6A-O1B
 with sigma of 0.04
 O18-O19 \\sim O18A-O19A
 with sigma of 0.04
 O18-O1A \\sim O18A-O1B
 with sigma of 0.04
 O19-O1A \\sim O19A-O1B
 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
C1A \\sim F4 \\sim F5 \\sim F6 \\sim S6 \\sim O18 \\sim O19 \\sim O1A: within
2A with sigma of 0.04 and sigma for terminal atoms of 0.08
5. Rigid body (RIGU) restrains
 C1A, F4, F5, F6, S6, O18, O19, O1A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S6, C1A, F4, F5, F6, O18, O19, O1A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 S6A, C1B, O18A, O19A, O1B, F4A, F5A, F6A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C99, S1, O9, O11, O10, F2, F3, F1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Others
 Sof(S6A)=Sof(C1B)=Sof(F4A)=Sof(F5A)=Sof(F6A)=Sof(O18A)=Sof(O19A)=Sof(O1B)=1-
 FVAR(1)
 Sof(C1A)=Sof(F4)=Sof(F5)=Sof(F6)=Sof(S6)=Sof(O18)=Sof(O19)=Sof(O1A)=FVAR(1)
 Fixed Sof: S1(0.8) C99(0.8) S4(0.2) C100(0.2)
 Fixed X: Cu1(0.72462)
 Fixed Y: Cu1(0.439679)
 Fixed Z: Cu1(0.61861)
7.a Ternary CH refined with riding coordinates:
 N1(H1), N8(H8), N2(H2), N6(H6), N7(H7), N3(H3)
7.b Secondary CH2 refined with riding coordinates:
 C35(H35A,H35B), C7(H7A,H7B), C85(H85A,H85B), C70(H70A,H70B), C72(H72A,H72B),
 C19(H19A,H19B), C69(H69A,H69B), C68(H68A,H68B), C71(H71A,H71B), C8(H8A,H8B),
 C20(H20A,H20B), C36(H36A,H36B), C22(H22A,H22B), C56(H56A,H56B), C57(H57A,H57B),
  C73(H73A,H73B), C84(H84A,H84B), C21(H21A,H21B), C24(H24A,H24B), C23(H23A,H23B)
7.c Aromatic/amide H refined with riding coordinates:
 C91(H91), C38(H38), C90(H90), C27(H27), C75(H75), C11(H11), C43(H43),
 C45(H45), C2(H2A), C79(H79), C26(H26), C86(H86), C96(H96), C37(H37), C87(H87),
 C76(H76), C95(H95), C59(H59), C47(H47), C82(H82), C3(H3A), C51(H51), C46(H46),
 C88(H88), C15(H15), C42(H42), C10(H10), C81(H81), C80(H80), C66(H66), C54(H54),
  C5(H5), C31(H31), C63(H63), C17(H17), C4(H4), C34(H34), C60(H60), C65(H65),
 C52(H52), C53(H53), C14(H14), C33(H33), C64(H64), C16(H16), C32(H32)
7.d Idealised Me refined as rotating group:
 C94(H94A,H94B,H94C), C40(H40A,H40B,H40C), C103(H10A,H10B,H10C), C105(H10D,
 H10E,H10F)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 86 electrons were 
found in a volume of 348\%A^3 in 1 void. 
This is consistent with the presence of 
1[C2H3N] per formula unit 
which account for 88 electrons.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              17999
_shelx_fab_checksum              53646
_olex2_submission_special_instructions 'No special instructions were received'