Self-sorting in dynamic disulfide assembly: new biphenyl-bridged “nanohoops” and unsymmetrical cyclophanes
Phan, Ngoc-Minh; Choy, Emma P. K. L.; Zakharov, Lev N.; Johnson, Darren W.; Chemical Communications  (2019) –; doi:10.1039/C9CC06503B

data_7124160
_publ_section_title
;
 Self-sorting in dynamic disulfide assembly: new biphenyl-bridged
 &#x201C;nanohoops&#x201D; and unsymmetrical cyclophanes
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC06503B
_journal_year                    2019
_chemical_formula_sum            'C45 H42 Cl2 S4'
_chemical_formula_weight         781.92
_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
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-12-09 deposited with the CCDC.    2019-09-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.429(15)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.152(4)
_cell_length_b                   5.5339(12)
_cell_length_c                   22.599(5)
_cell_measurement_reflns_used    410
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.60
_cell_measurement_theta_min      5.74
_cell_volume                     1927.2(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker apex II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1651
_diffrn_reflns_av_unetI/netI     0.1639
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            10516
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        49.781
_diffrn_reflns_theta_max         49.781
_diffrn_reflns_theta_min         2.984
_diffrn_source                   'Incoatec I\mS'
_exptl_absorpt_coefficient_mu    3.781
_exptl_absorpt_correction_T_max  0.7498
_exptl_absorpt_correction_T_min  0.5458
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.347
_exptl_crystal_description       needle
_exptl_crystal_F_000             820
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.010
_platon_squeeze_details
; 
Solvent molecule CH2Cl2, 42 electrons, is highly disordered 
around an inversion center and was treated by SQUEEZE. 
;
_refine_diff_density_max         0.262
_refine_diff_density_min         -0.251
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         1960
_refine_ls_number_restraints     180
_refine_ls_restrained_S_all      0.972
_refine_ls_R_factor_all          0.1667
_refine_ls_R_factor_gt           0.0864
_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^)+(0.0760P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1787
_refine_ls_wR_factor_ref         0.2086
_reflns_Friedel_coverage         0.000
_reflns_number_gt                908
_reflns_number_total             1960
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc06503b2.cif
_cod_data_source_block           cu_dwj250_0m_a_sqd
_cod_original_cell_volume        1927.2(7)
_cod_database_code               7124160
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.752
_shelx_estimated_absorpt_t_max   0.963
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              89396