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_7047070
_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         'C36 H26 Cu N O4'
_chemical_formula_sum            'C36 H26 Cu N O4'
_chemical_formula_weight         600.12
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_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                63.589(6)
_cell_angle_beta                 70.337(5)
_cell_angle_gamma                76.509(5)
_cell_formula_units_Z            2
_cell_length_a                   9.7072(5)
_cell_length_b                   12.5827(7)
_cell_length_c                   13.7631(8)
_cell_measurement_reflns_used    2833
_cell_measurement_temperature    298.8(4)
_cell_measurement_theta_max      25.6480
_cell_measurement_theta_min      3.1640
_cell_volume                     1410.82(16)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (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      298.8(4)
_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     48.00  74.00   0.10   40.00    --   18.52 179.00-120.00  260
  2  \w     -6.00  83.00   0.10   40.00    --   18.52  38.00 120.00  890
  3  \w     37.00  95.00   0.10   40.00    --   18.52 179.00 -30.00  580
  4  \w    -41.00  63.00   0.10   40.00    --   18.52 -19.00 -90.00 1040
  5  \w    -25.00  22.00   0.10   40.00    --  -18.68 -99.00 -60.00  470
  6  \w    -21.00  21.00   0.10   40.00    --  -18.68 -99.00 120.00  420
  7  \w    -23.00   2.00   0.10   40.00    --  -18.68 -99.00-180.00  250
;
_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      0.0075043000
_diffrn_orient_matrix_UB_12      0.0602854000
_diffrn_orient_matrix_UB_13      -0.0142240000
_diffrn_orient_matrix_UB_21      0.0745327000
_diffrn_orient_matrix_UB_22      -0.0075131000
_diffrn_orient_matrix_UB_23      -0.0297325000
_diffrn_orient_matrix_UB_31      -0.0216608000
_diffrn_orient_matrix_UB_32      0.0176093000
_diffrn_orient_matrix_UB_33      -0.0497933000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0412
_diffrn_reflns_av_unetI/netI     0.0594
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10586
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.429
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.817
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81947
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light green'
_exptl_crystal_density_diffrn    1.413
_exptl_crystal_description       needle
_exptl_crystal_F_000             620
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.624
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     434
_refine_ls_number_reflns         5765
_refine_ls_number_restraints     331
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0915
_refine_ls_R_factor_gt           0.0657
_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^)+(0.0376P)^2^+1.0883P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1235
_refine_ls_wR_factor_ref         0.1366
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4309
_reflns_number_total             5765
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02693a2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7047069--7047074.cif.'
_cod_database_code               7047070
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'Cu O4 N C10 H10'
_chemical_oxdiff_usercomment     'CuL2bipy polirotaxano'
_shelx_estimated_absorpt_t_max   0.992
_shelx_estimated_absorpt_t_min   0.792
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C1A-C7 \\sim C7-C1B
 with sigma of 0.02
 C6B-C1B \\sim C6A-C1A \\sim C1A-C2A \\sim C2B-C1B \\sim C2A-C3A \\sim C3B-C2B
\\sim C3B-C4B \\sim C4A-C3A
 \\sim C4A-C5A \\sim C4B-C5B \\sim C5A-C6A \\sim C5B-C6B
 with sigma of 0.01
3. Restrained planarity
 C1A, C6A, C5A, C4A, C3A, C2A
 with sigma of 0.1
 C1B, C6B, C2B, C5B, C4B, C3B
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C1B \\sim C6B \\sim C2B \\sim C5B \\sim C4B \\sim C3B \\sim C1A \\sim C6A \\sim
C5A \\sim C4A \\sim C3A \\sim C2A: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
5. Rigid body (RIGU) restrains
 C1B, C6B, C2B, C5B, C4B, C3B, C1A, C6A, C5A, C4A, C3A, C2A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(C1B)=Sof(C6B)=Sof(H6B)=Sof(C2B)=Sof(H2B)=Sof(C5B)=Sof(H5B)=Sof(C4B)=
 Sof(H4B)=Sof(C3B)=Sof(H3B)=1-FVAR(1)
 Sof(C1A)=Sof(C6A)=Sof(H6A)=Sof(C5A)=Sof(H5A)=Sof(C4A)=Sof(H4A)=Sof(C3A)=
 Sof(H3A)=Sof(C2A)=Sof(H2A)=FVAR(1)
7.a Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B)
7.b Aromatic/amide H refined with riding coordinates:
 C24(H24), C33(H33), C32(H32), C21(H21), C8(H8), C36(H36), C31(H31), C35(H35),
 C14(H14), C15(H15), C22(H22), C30(H30), C27(H27), C29(H29), C19(H19), C11(H11),
  C18(H18), C28(H28), C12(H12), C6B(H6B), C2B(H2B), C5B(H5B), C4B(H4B),
 C3B(H3B), C6A(H6A), C5A(H5A), C4A(H4A), C3A(H3A), C2A(H2A)
;
_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 1.444
_oxdiff_exptl_absorpt_empirical_full_min 0.715