A Cu(ii) metallocycle for the reversible self-assembly of coordination-driven polyrotaxane-like architectures.
Truccolo, Giada; Tessari, Zeno; Tessarolo, Jacopo; Quici, Silvio; Armelao, Lidia; Rancan, Marzio; Dalton transactions (Cambridge, England : 2003) 47 (2018) 12079–12084; doi:10.1039/c8dt02693a

data_7047074
_publ_section_title
;
 A Cu(ii) metallocycle for the reversible self-assembly of
 coordination-driven polyrotaxane-like architectures.
;
_journal_issue                   35
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12079
_journal_page_last               12084
_journal_paper_doi               10.1039/c8dt02693a
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C38.5 H29 Cu N O4.5'
_chemical_formula_sum            'C38.5 H29 Cu N O4.5'
_chemical_formula_weight         641.17
_space_group_crystal_system      orthorhombic
_space_group_IT_number           36
_space_group_name_Hall           'C 2c -2'
_space_group_name_H-M_alt        'C m c 21'
_symmetry_space_group_name_Hall  'C 2c -2'
_symmetry_space_group_name_H-M   'C m c 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-05-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_audit_update_record
;
2018-05-18 deposited with the CCDC.
2018-07-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.2987(16)
_cell_length_b                   8.5438(5)
_cell_length_c                   30.614(3)
_cell_measurement_reflns_used    2187
_cell_measurement_temperature    298(1)
_cell_measurement_theta_max      18.7280
_cell_measurement_theta_min      3.1320
_cell_volume                     6355.6(8)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      298(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0637
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     -8.00  24.00   0.10   40.00    --    7.44 -57.00 -30.00  320
  2  \w     -5.00  22.00   0.10   40.00    --   -7.51 -77.00 150.00  270
  3  \w    -77.00 -19.00   0.10   40.00    --   -7.51 -77.00 150.00  580
  4  \w    -54.00  51.00   0.10   40.00    --   15.06 -19.00 -60.00 1050
  5  \w    -50.00   6.00   0.10   40.00    --  -15.21 -57.00 -60.00  560
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0229910000
_diffrn_orient_matrix_UB_12      -0.0181735000
_diffrn_orient_matrix_UB_13      -0.0133489000
_diffrn_orient_matrix_UB_21      0.0172134000
_diffrn_orient_matrix_UB_22      -0.0004315000
_diffrn_orient_matrix_UB_23      0.0187165000
_diffrn_orient_matrix_UB_31      -0.0052562000
_diffrn_orient_matrix_UB_32      -0.0809802000
_diffrn_orient_matrix_UB_33      0.0028896000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0608
_diffrn_reflns_av_unetI/netI     0.0886
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            14602
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.712
_diffrn_reflns_theta_max         24.712
_diffrn_reflns_theta_min         2.527
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.731
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91560
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear intense green'
_exptl_crystal_density_diffrn    1.340
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2656
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.516
_refine_diff_density_min         -0.404
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.46(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     409
_refine_ls_number_reflns         5085
_refine_ls_number_restraints     197
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.1354
_refine_ls_R_factor_gt           0.1001
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1009P)^2^+11.2203P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2015
_refine_ls_wR_factor_ref         0.2211
_reflns_Friedel_coverage         0.957
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                3681
_reflns_number_total             5085
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02693a2.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 7047069--7047074.cif.'
_cod_original_formula_sum        'C38.50 H29 Cu N O4.50'
_cod_database_code               7047074
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'Cu2 O8 N2 C20 H20'
_chemical_oxdiff_usercomment     'Cu2+phPy DMA vap iPr2O'
_shelx_estimated_absorpt_t_max   0.993
_shelx_estimated_absorpt_t_min   0.944
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.66
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.54(5)
 0.46(5)
2. 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
3. Restrained distances
 C24A-C20 \\sim C25A-C24A \\sim C25A-C21 \\sim C23A-C21 \\sim C23A-C22A \\sim
C22A-C20
 with sigma of 0.01
 C24B-C20 \\sim C25B-C24B \\sim C25B-C21 \\sim C23B-C21 \\sim C23B-C22B \\sim
C22B-C20
 with sigma of 0.01
 C30-C26B \\sim C27B-C31 \\sim C28B-C29B \\sim C26A-C27A \\sim C28A-C29A
 with sigma of 0.01
4. Restrained planarity
 C20, C24B, C25B, C21, C23B, C22B
 with sigma of 0.1
 C25A, C24A, C22A, C23A, C21, C20
 with sigma of 0.1
 C29B, C30, C28B, C26B, C31, C27B
 with sigma of 0.1
 C30, C31, C26A, C27A, C28A, C29A
 with sigma of 0.1
5. Uiso/Uaniso restraints and constraints
Uanis(C35B) = Uanis(C36B) = Uanis(C39B) = Uanis(C38B) = Uanis(C40B) =
Uanis(C42B) = Uanis(C45B) = Uanis(C43B) = Uanis(C41B) = Uanis(C44B) =
Uanis(C37B)
Uanis(C26B) = Uanis(C26A) = Uanis(C27A) = Uanis(C27B)
Uanis(C28B) = Uanis(C29B) = Uanis(C28A) = Uanis(C29A)
6. Rigid body (RIGU) restrains
 C20, C24B, C25B, C21, C23B, C22B, C25A, C24A, C22A, C23A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C30, C26B, C27B, C31, C28B, C29B, C26A, C27A, C28A, C29A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Others
 Sof(C24B)=Sof(H24B)=Sof(C25B)=Sof(H25B)=Sof(H21A)=Sof(C23B)=Sof(H23B)=
 Sof(C22B)=Sof(H22B)=1-FVAR(1)
 Sof(H21)=Sof(C25A)=Sof(H25A)=Sof(C24A)=Sof(H24A)=Sof(C22A)=Sof(H22A)=
 Sof(C23A)=Sof(H23A)=FVAR(1)
 Sof(C26B)=Sof(H26B)=Sof(C27B)=Sof(H27B)=Sof(H31A)=Sof(C28B)=Sof(H28B)=
 Sof(C29B)=Sof(H29B)=1-FVAR(2)
 Sof(H31)=Sof(C26A)=Sof(H26A)=Sof(C27A)=Sof(H27A)=Sof(C28A)=Sof(H28A)=
 Sof(C29A)=Sof(H29A)=FVAR(2)
 Fixed Sof: C35B(0.5) C36B(0.5) C39B(0.5) C38B(0.5) C37B(0.5) H34A(0.5)
 H34B(0.5) H34C(0.5) H33A(0.5) H33B(0.5) H33C(0.5) H32A(0.5) H32B(0.5) H32C(0.5)
8.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B)
8.b Aromatic/amide H refined with riding coordinates:
 C16(H16), C6(H6), C15(H15), C12(H12), C7(H7), C18(H18), C24B(H24B),
 C25B(H25B), C21(H21A), C21(H21), C23B(H23B), C22B(H22B), C8(H8), C26B(H26B),
 C27B(H27B), C31(H31A), C31(H31), C28B(H28B), C29B(H29B), C5(H5), C13(H13),
 C2(H2), C42B(H42B), C45B(H45B), C43B(H43B), C41B(H41B), C44B(H44B), C25A(H25A),
  C24A(H24A), C22A(H22A), C23A(H23A), C26A(H26A), C27A(H27A), C28A(H28A),
 C29A(H29A)
8.c Fitted hexagon refined as free rotating group:
 N1(C35B,C36B,C39B,C38B,C37B), C20(C24B,C25B,C21,C23B,C22B), C30(C26B,C27B,C31,
 C28B,C29B)
8.d Idealised Me refined as rotating group:
 C34B(H34A,H34B,H34C), C33B(H33A,H33B,H33C), C32B(H32A,H32B,H32C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.074
_oxdiff_exptl_absorpt_empirical_full_min 0.939