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_7047072
_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         'C31 H24 O4'
_chemical_formula_sum            'C31 H24 O4'
_chemical_formula_weight         460.50
_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             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                 98.150(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.7464(12)
_cell_length_b                   5.2568(3)
_cell_length_c                   19.2835(13)
_cell_measurement_reflns_used    4232
_cell_measurement_temperature    296.6(3)
_cell_measurement_theta_max      25.9630
_cell_measurement_theta_min      3.4110
_cell_volume                     1178.70(16)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43b (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      296.6(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1274
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -46.00  92.00   1.00    3.50    --   18.68   0.00 -30.00  138
  2  \w     43.00  94.00   1.00    3.50    --   18.68 179.00 -30.00   51
  3  \w    -29.00  31.00   1.00    3.50    --   18.68 -57.00 -60.00   60
  4  \w     -1.00  55.00   1.00    3.50    --   18.68  57.00-150.00   56
  5  \w    -24.00   1.00   1.00    3.50    --  -18.76 -99.00 120.00   25
  6  \w    -12.00  18.00   1.00    3.50    --  -18.76 -99.00-180.00   30
  7  \w    -85.00 -59.00   1.00    3.50    --  -18.76 146.00 140.00   26
  8  \w    -46.00  35.00   1.00    3.50    --   18.68 -19.00 120.00   81
  9  \w     25.00  61.00   1.00    3.50    --   18.68 -99.00  90.00   36
 10  \w    -24.00  82.00   1.00    3.50    --   18.68  19.00 150.00  106
 11  \w      4.00  77.00   1.00    3.50    --   18.68  57.00   0.00   73
 12  \w    -24.00  23.00   1.00    3.50    --  -18.76 -99.00-120.00   47
 13  \w    -75.00 -34.00   1.00    3.50    --  -18.76 125.00 -25.00   41
;
_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      -0.0504277000
_diffrn_orient_matrix_UB_12      0.0155534000
_diffrn_orient_matrix_UB_13      0.0159113000
_diffrn_orient_matrix_UB_21      -0.0326809000
_diffrn_orient_matrix_UB_22      0.0184416000
_diffrn_orient_matrix_UB_23      -0.0334689000
_diffrn_orient_matrix_UB_31      -0.0104236000
_diffrn_orient_matrix_UB_32      -0.1327569000
_diffrn_orient_matrix_UB_33      -0.0027722000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0236
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            17085
_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         26.366
_diffrn_reflns_theta_min         2.562
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.085
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70012
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.297
_exptl_crystal_description       plate
_exptl_crystal_F_000             484
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.110
_refine_diff_density_min         -0.110
_refine_diff_density_rms         0.026
_refine_ls_abs_structure_details
;
 Flack x determined using 1268 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.1(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         4816
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0650
_refine_ls_R_factor_gt           0.0416
_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^)+(0.0382P)^2^+0.0950P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0868
_refine_ls_wR_factor_ref         0.0995
_reflns_Friedel_coverage         0.796
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                3557
_reflns_number_total             4816
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02693a2.cif
_cod_data_source_block           l
_cod_depositor_comments
'Adding full bibliography for 7047069--7047074.cif.'
_cod_database_code               7047072
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C31 H24 O4'
_chemical_oxdiff_usercomment     'DPM-Ph TPPO DCM/Tol'
_shelx_estimated_absorpt_t_max   0.993
_shelx_estimated_absorpt_t_min   0.959
_reflns_odcompleteness_completeness 99.81
_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
 At 1.5 times of:
  All O(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B)
2.b Aromatic/amide H refined with riding coordinates:
 C24(H24), C9(H9), C3(H3A), C4(H4), C6(H6), C21(H21), C22(H22), C16(H16),
 C19(H19), C7(H7), C31(H31), C18(H18), C12(H12), C15(H15), C13(H13), C14(H14),
 C27(H27), C29(H29), C30(H30), C28(H28)
2.c Idealised tetrahedral OH refined as rotating group:
 O2(H2), O3(H3)
;
_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 1.255
_oxdiff_exptl_absorpt_empirical_full_min 0.666