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_1551418
_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
'C234 H234 Br6 Fe6 N30 O36, 6(Br), 6.25(H2O), 0.75(KBr)'
_chemical_formula_sum            'C234 H234 Br12.75 Fe6 K0.75 N30 O42.25'
_chemical_formula_weight         5525.78
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 116.189(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
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_cell_length_b                   16.8956(15)
_cell_length_c                   62.436(5)
_cell_measurement_reflns_used    9375
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.089
_cell_measurement_theta_min      4.359
_cell_volume                     56290(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SUPERFLIP (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type
'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'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.1276
_diffrn_reflns_av_unetI/netI     0.0653
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       47
_diffrn_reflns_limit_h_min       -47
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            159461
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        16.490
_diffrn_reflns_theta_max         16.491
_diffrn_reflns_theta_min         0.705
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.019
_exptl_absorpt_correction_T_max  0.7440
_exptl_absorpt_correction_T_min  0.5461
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.304
_exptl_crystal_description       block
_exptl_crystal_F_000             22420
_exptl_crystal_size_max          0.031
_exptl_crystal_size_mid          0.025
_exptl_crystal_size_min          0.011
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.392
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2605
_refine_ls_number_reflns         15975
_refine_ls_number_restraints     5926
_refine_ls_restrained_S_all      1.287
_refine_ls_R_factor_all          0.1586
_refine_ls_R_factor_gt           0.1243
_refine_ls_shift/su_max          0.007
_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          0.3352
_refine_ls_wR_factor_ref         0.3586
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10664
_reflns_number_total             15975
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            nchem.2205-s5.cif
_cod_data_source_block           csw351_sq_d
_cod_original_cell_volume        56289(8)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               1551418
_shelx_estimated_absorpt_t_min   0.986
_shelx_estimated_absorpt_t_max   0.995