Double-Circularly Connected Saloph-Belt Macrocycles Generated from a Bis-Armed Bifunctional Monomer.
Nakamura, Takashi; Tsukuda, Shinnosuke; Nabeshima, Tatsuya; Journal of the American Chemical Society 141 (2019) 6462–6467; doi:10.1021/jacs.9b00171

data_4128261
_publ_section_title
;
 Double-Circularly Connected Saloph-Belt Macrocycles Generated from a
 Bis-Armed Bifunctional Monomer.
;
_journal_issue                   16
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6462
_journal_page_last               6467
_journal_paper_doi               10.1021/jacs.9b00171
_journal_volume                  141
_journal_year                    2019
_chemical_formula_sum            'C168 H204 N6 O18'
_chemical_formula_weight         2595.36
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                61.056(2)
_cell_angle_beta                 68.264(2)
_cell_angle_gamma                88.742(3)
_cell_formula_units_Z            2
_cell_length_a                   20.7339(8)
_cell_length_b                   22.5701(9)
_cell_length_c                   22.5707(8)
_cell_measurement_reflns_used    5579
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      18.519
_cell_measurement_theta_min      2.167
_cell_volume                     8423.6(6)
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1541
_diffrn_reflns_av_unetI/netI     0.1156
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            59373
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        17.999
_diffrn_reflns_theta_max         17.999
_diffrn_reflns_theta_min         1.051
_exptl_absorpt_coefficient_mu    0.066
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5588
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;    
 SADABS-2014/5 - Bruker AXS area detector scaling and absorption correction 
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.023
_exptl_crystal_description       plate
_exptl_crystal_F_000             2796
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.856
_refine_diff_density_min         -0.478
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.961
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1735
_refine_ls_number_reflns         11589
_refine_ls_number_restraints     1539
_refine_ls_restrained_S_all      1.863
_refine_ls_R_factor_all          0.2214
_refine_ls_R_factor_gt           0.1384
_refine_ls_shift/su_max          0.166
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3468
_refine_ls_wR_factor_ref         0.3769
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6021
_reflns_number_total             11589
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b00171_si_002.cif
_cod_data_source_block           1202
_cod_database_code               4128261
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.993
_shelx_estimated_absorpt_t_max   0.999
_shelx_res_checksum              18542
_shelx_hkl_checksum              54946