Two-stage directed self-assembly of a cyclic [3]catenane
Christopher S. Wood; Tanya K. Ronson; Ana M. Belenguer; Julian J. Holstein; Jonathan R. Nitschke; Nature Chemistry 7 (2015) 354–358; doi:10.1038/nchem.2205

data_1551417
_publ_section_title
;
 Two-stage directed self-assembly of a cyclic [3]catenane
;
_journal_name_full               'Nature Chemistry'
_journal_page_first              354
_journal_page_last               358
_journal_paper_doi               10.1038/nchem.2205
_journal_volume                  7
_journal_year                    2015
_chemical_formula_moiety         'C192 H150 Fe6 N36 O12 S6, 4(F6 P)'
_chemical_formula_sum            'C192 H150 F24 Fe6 N36 O12 P4 S6'
_chemical_formula_weight         4260.81
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 107.763(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   42.114(3)
_cell_length_b                   54.516(3)
_cell_length_c                   14.0878(9)
_cell_measurement_reflns_used    154080
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.502
_cell_measurement_theta_min      0.611
_cell_volume                     30802(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'shelXle (Huebschle et al., 2011)'
_computing_publication_material  'enCIFer 1.3, CCDC, 2008'
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_computing_structure_solution
;
Palatinus L., Chapuis G. (2007): Superflip - a computer program for
the solution of crystal structures by charge flipping in
arbitrary dimensions. J. Appl. Cryst. 40, 786-790
;
_diffrn_ambient_temperature      100(2)
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_diffrn_measured_fraction_theta_max 0.947
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'Rigaku Saturn 724+ detector on Crystal Logic diffractometer'
_diffrn_measurement_method       '\w  scans'
_diffrn_radiation_monochromator  'silicon double crystal'
_diffrn_radiation_source         'Diamond beamline I19'
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_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.2479
_diffrn_reflns_av_unetI/netI     0.2458
_diffrn_reflns_Laue_measured_fraction_full 0.947
_diffrn_reflns_Laue_measured_fraction_max 0.947
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       60
_diffrn_reflns_limit_k_min       -60
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            154080
_diffrn_reflns_point_group_measured_fraction_full 0.877
_diffrn_reflns_point_group_measured_fraction_max 0.877
_diffrn_reflns_theta_full        22.500
_diffrn_reflns_theta_max         22.502
_diffrn_reflns_theta_min         0.611
_exptl_absorpt_coefficient_mu    0.360
_exptl_absorpt_correction_T_max  0.4267
_exptl_absorpt_correction_T_min  0.2730
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2008, Bruker AXS, 2008'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    0.919
_exptl_crystal_description       block
_exptl_crystal_F_000             8712
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.020
_refine_diff_density_max         2.488
_refine_diff_density_min         -0.899
_refine_diff_density_rms         0.169
_refine_ls_abs_structure_details
;
 Flack x determined using 6198 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.540(16)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.231
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2521
_refine_ls_number_reflns         38792
_refine_ls_number_restraints     7373
_refine_ls_restrained_S_all      1.164
_refine_ls_R_factor_all          0.2051
_refine_ls_R_factor_gt           0.1411
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3353
_refine_ls_wR_factor_ref         0.3902
_reflns_Friedel_coverage         0.850
_reflns_Friedel_fraction_full    0.806
_reflns_Friedel_fraction_max     0.806
_reflns_number_gt                22362
_reflns_number_total             38792
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            nchem.2205-s4.cif
_cod_data_source_block           csw296_sq
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               1551417
_shelx_estimated_absorpt_t_min   0.982
_shelx_estimated_absorpt_t_max   0.993
_computing_refinement_gui        'shelXle (Huebschle et al, 2011)'
_platon_squeeze_void_probe_radius 1.20
_shelxl_version_number           2014/6
_shelx_res_checksum              23966
_shelx_hkl_checksum              45120
_shelx_fab_checksum              60830