Engineering entanglement: controlling the formation of polycatenanes and polyrotaxanes using π interactions
Boer, Stephanie A.; Hawes, Chris S.; Turner, David R.; Chemical Communications (Cambridge, United Kingdom) 50 (2014) 1125–1127; doi:10.1039/c3cc48802k

data_7110352
_publ_section_title
;
 Engineering entanglement: controlling the formation of polycatenanes and
 polyrotaxanes using \p interactions
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   9
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              1125
_journal_page_last               1127
_journal_paper_doi               10.1039/c3cc48802k
_journal_volume                  50
_journal_year                    2014
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C72 H64 Cd2 N4 O20, 3 (C3 H10 N O)'
_chemical_formula_sum            'C81 H94 Cd2 N7 O23'
_chemical_formula_weight         1758.43
_chemical_name_systematic        ?
_space_group_crystal_system      hexagonal
_space_group_IT_number           178
_space_group_name_Hall           'P 61 2 (0 0 5)'
_space_group_name_H-M_alt        'P 61 2 2'
_symmetry_space_group_name_Hall  'P 61 2 (0 0 5)'
_symmetry_space_group_name_H-M   'P 61 2 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            12
_cell_length_a                   19.928(3)
_cell_length_b                   19.928(3)
_cell_length_c                   78.862(16)
_cell_measurement_reflns_used    113556
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.70
_cell_measurement_theta_min      1.29
_cell_volume                     27122(8)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'Phi Scan'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.71080
_diffrn_reflns_av_R_equivalents  0.1084
_diffrn_reflns_av_unetI/netI     0.0418
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       81
_diffrn_reflns_limit_l_min       -81
_diffrn_reflns_number            113556
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        21.700
_diffrn_reflns_theta_max         21.698
_diffrn_reflns_theta_min         1.288
_diffrn_source                   'Australian Synchrotron'
_exptl_absorpt_coefficient_mu    0.541
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XScale within XDS'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.292
_exptl_crystal_description       block
_exptl_crystal_F_000             10908
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.020
_platon_squeeze_details
;
Approx. 3 DMF per ASU fits with squeeze value.
Correlates well with TGA and elemental analysis.
Solvent in UNIT instruction.
;
_refine_diff_density_max         0.437
_refine_diff_density_min         -0.551
_refine_diff_density_rms         0.081
_refine_ls_abs_structure_details
;
 Flack x determined using 3375 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.036(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     801
_refine_ls_number_reflns         10626
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0832
_refine_ls_R_factor_gt           0.0765
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.1732P)^2^+1.7652P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2101
_refine_ls_wR_factor_ref         0.2175
_reflns_Friedel_coverage         0.708
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                9176
_reflns_number_total             10626
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3cc48802k.txt
_cod_data_source_block           3
_cod_depositor_comments
;
The original supplementary material CIF (accessed 2015-02-03) provides the 
following  space group information:
_space_group_IT_number           178
_space_group_name_H-M_alt        'P 61 2 2'
_space_group_name_Hall           'P 61 2 (0 0 -1)

However, CIF uploaded to COD had the following spacegroup information (now 
stored in '_cod_cif_authors_sg_*' tags):
_space_group_IT_number           178
_space_group_name_H-M            'P 65 2 2'
_space_group_name_Hall           'P 65 2 (0 0 1)'

Either way, Hall space group 'P 61 2 (0 0 5)' was computed by COD deposition
scripts from the provided symmetry operators.

Antanas Vaitkus,
2015-02-03
;
_cod_original_cell_volume        27122(9)
_cod_original_sg_symbol_Hall     'P 65 2 (0 0 1)'
_cod_original_sg_symbol_H-M      'P 65 2 2'
_cod_database_code               7110352
_shelx_estimated_absorpt_t_min   0.973
_shelx_estimated_absorpt_t_max   0.989
_shelxl_version_number           2013-2