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_1513725
_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         'C66 H58 N8, C44 H60 O14, 8(F6 P)'
_chemical_formula_sum            'C110 H118 F48 N8 O14 P8'
_chemical_formula_weight         2935.88
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2011-11-29
_audit_creation_method
;
Olex2 1.1
(compiled Nov 1 2011 20:42:30, GUI svn.r3906)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 94.0820(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.0951(4)
_cell_length_b                   31.3942(6)
_cell_length_c                   24.2862(5)
_cell_measurement_reflns_used    9840
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      65.71
_cell_measurement_theta_min      3.10
_cell_volume                     15282.6(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      100.0
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.951
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Quazar optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0398
_diffrn_reflns_av_unetI/netI     0.0344
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            111556
_diffrn_reflns_theta_full        67.11
_diffrn_reflns_theta_max         67.11
_diffrn_reflns_theta_min         1.41
_diffrn_source                   microsource
_diffrn_source_current           0.64
_diffrn_source_power             0.0285952
_diffrn_source_voltage           44.68
_exptl_absorpt_coefficient_mu    1.847
_exptl_absorpt_correction_T_max  0.7529
_exptl_absorpt_correction_T_min  0.6855
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
R(int) was 0.0559 before and 0.0496 after correction.
The Ratio of minimum to maximum transmission is 0.9105.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.276
_exptl_crystal_description       block
_exptl_crystal_F_000             5992
_exptl_crystal_size_max          0.191
_exptl_crystal_size_mid          0.174
_exptl_crystal_size_min          0.096
_refine_diff_density_max         0.860
_refine_diff_density_min         -1.056
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2117
_refine_ls_number_reflns         25954
_refine_ls_number_restraints     2800
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.1067
_refine_ls_R_factor_gt           0.0893
_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^)+(0.1299P)^2^+31.5913P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2511
_refine_ls_wR_factor_ref         0.2620
_reflns_number_gt                19769
_reflns_number_total             25954
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3sc52106k.txt
_cod_data_source_block           n1427
_cod_database_code               1513725
_smtbx_masks_special_details
;
The solvent masking procedure as implemented in Olex2 was used to remove the
electronic contribution of solvent molecules from the refinement. Only the
atoms used in the refinement model are reported in the formula here.

Total solvent accessible volume / cell = 4095.6 Ang^3^ [26.8%]
Total electron count / cell = 1029.7
;