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_1551415
_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
'C174 H114 Br6 Cl12 Fe6 N30, 5(Cl O4), 0.5(Br4 Fe), 10(C2 H3 N), (H2 O)'
_chemical_formula_sum            'C194 H146 Br8 Cl17 Fe6.5 N40 O21'
_chemical_formula_weight         4978.45
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                89.880(2)
_cell_angle_beta                 89.852(2)
_cell_angle_gamma                72.396(2)
_cell_formula_units_Z            2
_cell_length_a                   16.0089(7)
_cell_length_b                   25.8622(10)
_cell_length_c                   29.8790(11)
_cell_measurement_reflns_used    9776
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      50.909
_cell_measurement_theta_min      4.344
_cell_volume                     11791.3(8)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_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 0.972
_diffrn_measured_fraction_theta_max 0.961
_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  0.0402
_diffrn_reflns_av_unetI/netI     0.0616
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            124553
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        24.500
_diffrn_reflns_theta_max         25.535
_diffrn_reflns_theta_min         0.661
_exptl_absorpt_coefficient_mu    1.841
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6019
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_description       block
_exptl_crystal_F_000             4992
_exptl_crystal_size_max          0.010
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.010
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2515
_refine_ls_number_reflns         46520
_refine_ls_number_restraints     2083
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.1088
_refine_ls_R_factor_gt           0.0751
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.1557P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2218
_refine_ls_wR_factor_ref         0.2426
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                28726
_reflns_number_total             46520
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            nchem.2205-s2.cif
_cod_data_source_block           csw278
_cod_original_formula_sum        'C194 H146 Br8 Cl17 Fe6.50 N40 O21'
_cod_database_code               1551415
_shelx_estimated_absorpt_t_min   0.993
_shelx_estimated_absorpt_t_max   0.993