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_7047069
_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 H22 Cu O4, C H Cl3'
_chemical_formula_sum            'C32 H23 Cl3 Cu O4'
_chemical_formula_weight         641.39
_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                111.662(5)
_cell_angle_beta                 96.458(5)
_cell_angle_gamma                100.561(5)
_cell_formula_units_Z            2
_cell_length_a                   9.9134(6)
_cell_length_b                   11.5595(7)
_cell_length_c                   13.3769(7)
_cell_measurement_reflns_used    4450
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      29.0510
_cell_measurement_theta_min      2.7940
_cell_volume                     1373.03(15)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector_area_resol_mean 16.1274
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details
;
  1 omega  -34.00   50.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.5219   57.0000  -30.0000 168

  2 omega  -10.00   22.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.5219  -99.0000  -60.0000 64

  3 omega    9.00   40.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5219  -38.0000  -30.0000 62

  4 omega   -9.00   88.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5219   77.0000 -120.0000 194

  5 omega  -49.00   -3.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5219  -38.0000  -30.0000 92

  6 omega  -53.00  -25.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5219  -27.0000 -175.0000 56

  7 omega    9.00   44.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5219  -27.0000 -175.0000 70

  8 omega  -25.00   60.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5219  -99.0000  120.0000 170
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0551062000
_diffrn_orient_matrix_UB_12      -0.0316706000
_diffrn_orient_matrix_UB_13      -0.0015776000
_diffrn_orient_matrix_UB_21      -0.0497270000
_diffrn_orient_matrix_UB_22      -0.0599953000
_diffrn_orient_matrix_UB_23      -0.0204396000
_diffrn_orient_matrix_UB_31      0.0014262000
_diffrn_orient_matrix_UB_32      -0.0055876000
_diffrn_orient_matrix_UB_33      -0.0544655000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_av_unetI/netI     0.0510
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11096
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.436
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.125
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77136
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.551
_exptl_crystal_description       needle
_exptl_crystal_F_000             654
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.100
_refine_diff_density_min         -1.841
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         5574
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.0887
_refine_ls_R_factor_gt           0.0732
_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^)+(0.1349P)^2^+3.2967P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2161
_refine_ls_wR_factor_ref         0.2332
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4567
_reflns_number_total             5574
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02693a2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7047069--7047074.cif.'
_cod_database_code               7047069
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'Cu2 O8 C20 H20 Cl3'
_chemical_oxdiff_usercomment     'Cu36 DCM/MeOH'
_shelx_estimated_absorpt_t_max   0.946
_shelx_estimated_absorpt_t_min   0.729
_reflns_odcompleteness_completeness 99.25
_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. Uiso/Uaniso restraints and constraints
Cl2 \\sim Cl3 \\sim C014 \\sim Cl1 \\sim H014: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
3. Rigid body (RIGU) restrains
 Cl2, Cl3, C014, Cl1, H014
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4.a Ternary CH refined with riding coordinates:
 C014(H014)
4.b Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B)
4.c Aromatic/amide H refined with riding coordinates:
 C14(H14), C15(H15), C21(H21), C8(H8), C19(H19), C24(H24), C27(H27), C31(H31),
 C6(H6), C22(H22), C2(H2), C18(H18), C3(H3), C30(H30), C11(H11), C29(H29),
 C4(H4), C12(H12), C28(H28), C5(H5)
;
_olex2_submission_special_instructions 'No special instructions were received'