Topological isomerism in a chiral handcuff catenane
Hartlieb, Karel J.; Blackburn, Anthea K.; Schneebeli, Severin T.; Forgan, Ross S.; Sarjeant, Amy A.; Stern, Charlotte L.; Cao, Dennis; Stoddart, J. Fraser; Chemical Science 5 (2014) 90–; doi:10.1039/c3sc52106k

data_1513723
_publ_section_title
;
 Topological isomerism in a chiral handcuff catenane
;
_journal_issue                   1
_journal_name_full               'Chemical Science'
_journal_page_first              90
_journal_paper_doi               10.1039/c3sc52106k
_journal_volume                  5
_journal_year                    2014
_chemical_formula_moiety         '8(F6 P), C66 H58 N8, 6.86(C2 H3 N)'
_chemical_formula_sum            'C79.72 H78.59 F48 N14.86 P8'
_chemical_formula_weight         2404.70
_chemical_name_systematic
;
?
;
_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
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-05-30
_audit_creation_method
;
Olex2 1.2
(compiled May 9 2012 12:37:22, GUI svn.r4230)
;
_cell_angle_alpha                71.154(2)
_cell_angle_beta                 78.075(2)
_cell_angle_gamma                73.175(2)
_cell_formula_units_Z            4
_cell_length_a                   16.6223(5)
_cell_length_b                   22.9236(6)
_cell_length_c                   29.6344(8)
_cell_measurement_reflns_used    9980
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      62.75
_cell_measurement_theta_min      3.18
_cell_volume                     10149.1(5)
_computing_cell_refinement       'SAINT V7.23A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2.1-4 (Bruker, 2007)'
_computing_data_reduction        'Bruker SAINT'
_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
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
XM, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      100.01
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'MX optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0913
_diffrn_reflns_av_unetI/netI     0.0943
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            59810
_diffrn_reflns_theta_full        54.24
_diffrn_reflns_theta_max         54.24
_diffrn_reflns_theta_min         1.59
_diffrn_source                   microsource
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.551
_exptl_absorpt_correction_T_max  0.7529
_exptl_absorpt_correction_T_min  0.5885
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1358 before and 0.0521 after correction.
The Ratio of minimum to maximum transmission is 0.7816.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.574
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             4852
_exptl_crystal_size_max          0.269
_exptl_crystal_size_mid          0.055
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.279
_refine_diff_density_min         -0.606
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2908
_refine_ls_number_reflns         24665
_refine_ls_number_restraints     1223
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.1562
_refine_ls_R_factor_gt           0.0983
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1660P)^2^+36.6454P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2597
_refine_ls_wR_factor_ref         0.3027
_reflns_number_gt                14699
_reflns_number_total             24665
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3sc52106k.txt
_cod_data_source_block           n1810
_cod_database_code               1513723
_refinement_special_details
'Disordered PF6 anions were subjected to SADI restraints to effect an equivalent coordination environment around the P atom. Disordered and partially occupied acetonitrile solvent molecules were refined with SADI restraints to keep affected bonds equivalent. A global rigid bond (DELU) restraint was applied, and various SIMU restraints were applied to disordered PF6 and ACN molecules. C24T C24S, N9S N9T C17T C18T C17S C18S, and N14S C27S C28S, were respectively refined with group displacement parameters. SOFs were allowed to refine freely, but were fixed (for the multiply-disordered PF6 and partially occupied ACN) during the final refinement stages.'