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_7110350
_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_sum            'C72 H93 Cd2 N9 O21'
_chemical_formula_weight         1645.35
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_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_method           SHELXL-2013
_cell_angle_alpha                73.28(3)
_cell_angle_beta                 79.44(3)
_cell_angle_gamma                80.24(3)
_cell_formula_units_Z            1
_cell_length_a                   10.239(2)
_cell_length_b                   13.283(3)
_cell_length_c                   15.851(3)
_cell_measurement_reflns_used    69001
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.526
_cell_measurement_theta_min      1.355
_cell_volume                     2014.0(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    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.919
_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  0.0565
_diffrn_reflns_av_unetI/netI     0.0524
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.919
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            69001
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.869
_diffrn_reflns_theta_full        27.500
_diffrn_reflns_theta_max         31.526
_diffrn_reflns_theta_min         1.355
_diffrn_source                   'Australian Synchrotron'
_exptl_absorpt_coefficient_mu    0.601
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XScale within XDS'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.357
_exptl_crystal_description       block
_exptl_crystal_F_000             852
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.040
_refine_diff_density_max         1.365
_refine_diff_density_min         -1.312
_refine_diff_density_rms         0.120
_refine_ls_abs_structure_details
;
 Flack x determined using 8099 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.060(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     931
_refine_ls_number_reflns         23372
_refine_ls_number_restraints     79
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0735
_refine_ls_R_factor_gt           0.0575
_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^)+(0.1133P)^2^+0.4403P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1565
_refine_ls_wR_factor_ref         0.1732
_reflns_Friedel_coverage         0.892
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.820
_reflns_number_gt                18857
_reflns_number_total             23372
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3cc48802k.txt
_cod_data_source_block           1
_cod_original_cell_volume        2014.1(8)
_cod_database_code               7110350
_shelx_estimated_absorpt_t_min   0.971
_shelx_estimated_absorpt_t_max   0.976
_shelxl_version_number           2013-2