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_7047073
_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 H27 Cu N O4'
_chemical_formula_sum            'C36 H27 Cu N O4'
_chemical_formula_weight         601.12
_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
_atom_sites_solution_primary     dual
_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                70.823(2)
_cell_angle_beta                 89.045(2)
_cell_angle_gamma                64.357(2)
_cell_formula_units_Z            2
_cell_length_a                   9.5306(2)
_cell_length_b                   10.9270(2)
_cell_length_c                   15.9767(4)
_cell_measurement_reflns_used    2615
_cell_measurement_temperature    296.8(9)
_cell_measurement_theta_max      26.6340
_cell_measurement_theta_min      2.7200
_cell_volume                     1401.25(6)
_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)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      296.8(9)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1274
_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     -6.00  86.00   0.10   10.00    --   18.52  38.00 -90.00  920
  2  \w    -18.00  23.00   0.10   10.00    --  -18.52 -99.00-120.00  410
  3  \w    -20.00  16.00   0.10   10.00    --  -18.52 -99.00   0.00  360
  4  \w    -24.00   4.00   0.10   10.00    --  -18.52 -99.00 120.00  280
  5  \w     45.00  87.00   0.10   10.00    --   18.52 179.00 150.00  420
  6  \w    -51.00  44.00   0.10   10.00    --   18.52 -38.00  90.00  950
  7  \w    -47.00  25.00   0.10   10.00    --   18.52 -57.00 -30.00  720
;
_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      0.0289928000
_diffrn_orient_matrix_UB_12      0.0462240000
_diffrn_orient_matrix_UB_13      -0.0283679000
_diffrn_orient_matrix_UB_21      -0.0699152000
_diffrn_orient_matrix_UB_22      0.0616410000
_diffrn_orient_matrix_UB_23      -0.0009446000
_diffrn_orient_matrix_UB_31      0.0351823000
_diffrn_orient_matrix_UB_32      0.0016824000
_diffrn_orient_matrix_UB_33      0.0381160000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0405
_diffrn_reflns_av_unetI/netI     0.0490
_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       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11035
_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         26.371
_diffrn_reflns_theta_min         2.417
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.822
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83735
_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            'clear light green'
_exptl_crystal_density_diffrn    1.425
_exptl_crystal_description       plate
_exptl_crystal_F_000             622
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.889
_refine_diff_density_min         -0.396
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         5731
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0711
_refine_ls_R_factor_gt           0.0557
_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^)+(0.0922P)^2^+0.4498P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1533
_refine_ls_wR_factor_ref         0.1696
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4541
_reflns_number_total             5731
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02693a2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7047069--7047074.cif.'
_cod_database_code               7047073
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'Cu N2 O10 C20 H20'
_chemical_oxdiff_usercomment     'cristalli da soluzioni esi (Py/DMA)'
_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.a Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B)
2.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C13(H13), C11(H11), C8(H8), C19(H19), C18(H18), C12(H12), C21(H21),
 C32(H32), C30(H30), C5(H5), C20(H20), C27(H27), C33(H33), C24(H24), C34(H34),
 C3(H3), C4(H4), C36(H36), C1(H1), C2(H2), C28(H28), C35(H35), C29(H29),
 C31(H31)
;
_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 1.214
_oxdiff_exptl_absorpt_empirical_full_min 0.893