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_1513724
_publ_section_title
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 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, 2.5(C18 H24 O6), 8(F6 P), 7(C2 H3 N)'
_chemical_formula_sum            'C125 H139 F48 N15 O15 P8'
_chemical_formula_weight         3251.27
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-07-09
_audit_creation_method
;
Olex2 1.2
(compiled May 9 2012 12:37:22, GUI svn.r4230)
;
_cell_angle_alpha                105.106(8)
_cell_angle_beta                 99.281(7)
_cell_angle_gamma                93.008(6)
_cell_formula_units_Z            2
_cell_length_a                   16.475(4)
_cell_length_b                   18.609(5)
_cell_length_c                   25.278(6)
_cell_measurement_reflns_used    9812
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      64.25
_cell_measurement_theta_min      4.79
_cell_volume                     7348(3)
_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
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      99.97
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0304
_diffrn_reflns_av_unetI/netI     0.0369
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            58131
_diffrn_reflns_theta_full        64.64
_diffrn_reflns_theta_max         64.64
_diffrn_reflns_theta_min         3.87
_diffrn_source                   microsource
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.999
_exptl_absorpt_correction_T_max  0.7525
_exptl_absorpt_correction_T_min  0.6632
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0491 before and 0.0381 after correction.
The Ratio of minimum to maximum transmission is 0.8813.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.469
_exptl_crystal_description       tabular
_exptl_crystal_F_000             3332
_exptl_crystal_size_max          0.153
_exptl_crystal_size_mid          0.115
_exptl_crystal_size_min          0.066
_refine_diff_density_max         2.075
_refine_diff_density_min         -0.717
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2151
_refine_ls_number_reflns         23976
_refine_ls_number_restraints     195
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0814
_refine_ls_R_factor_gt           0.0668
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1006P)^2^+10.9944P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1811
_refine_ls_wR_factor_ref         0.1899
_reflns_number_gt                19177
_reflns_number_total             23976
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3sc52106k.txt
_cod_data_source_block           n1900
_cod_database_code               1513724
_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 = 487.7 Ang^3 [6.6%]
Total electron count / cell = 77.2
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