Control over the macrocyclisation pathway and product topology in a copper-templated catenane synthesis
Yee, Chi-Chung; Ng, Antony, Wing Hung; Au-Yeung, Ho Yu; Chemical Communications  (2019) –; doi:10.1039/C9CC02263E

data_7123350
_publ_section_title
;
 Control over the macrocyclisation pathway and product topology in a
 copper-templated catenane synthesis
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC02263E
_journal_year                    2019
_chemical_formula_moiety         'C56 H40 Cu N4 O8, F6 P, 2(C2 H3 N)'
_chemical_formula_sum            'C60 H46 Cu F6 N6 O8 P'
_chemical_formula_weight         1187.54
_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'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-03-10 deposited with the CCDC.    2019-04-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.952(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.376(3)
_cell_length_b                   11.9418(12)
_cell_length_c                   16.4539(16)
_cell_measurement_reflns_used    9704
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.20
_cell_measurement_theta_min      2.48
_cell_volume                     5359.0(10)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2014)'
_computing_data_collection       'APEX2 v2014.11-0 (Bruker, 2014)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2014)'
_computing_molecular_graphics    'Mercury (Macrae et. al, 2008)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 1024
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
'Bruker D8 Venture with Photon100 CMOS detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0500
_diffrn_reflns_av_unetI/netI     0.0234
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            59902
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.787
_diffrn_source                   'microfocus I\mS'
_exptl_absorpt_coefficient_mu    0.522
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6974
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2014/5)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.472
_exptl_crystal_description       rod
_exptl_crystal_F_000             2440
_exptl_crystal_size_max          0.392
_exptl_crystal_size_mid          0.131
_exptl_crystal_size_min          0.076
_refine_diff_density_max         0.852
_refine_diff_density_min         -0.348
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     439
_refine_ls_number_reflns         4742
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_gt           0.0473
_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^)+(0.0747P)^2^+11.0211P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1216
_refine_ls_wR_factor_ref         0.1325
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3823
_reflns_number_total             4742
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc02263e2.cif
_cod_data_source_block           mo_CHEM0023_C0m
_cod_original_cell_volume        5359.1(9)
_cod_database_code               7123350
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.821
_shelx_estimated_absorpt_t_max   0.961
_shelx_res_checksum              15495