Continuous flow synthesis of a carbon-based molecular cage macrocycle via a three-fold homocoupling reaction
Melanie Kitchin; Kristina Konstas; Christopher J. Sumby; Milena L. Czyz; Peter Valente; Matthew R. Hill; Anastasios Polyzos; Christian J. Doonan; Chem.Commun. 51 (2015) 14231–; doi:10.1039/C5cc05181A

data_7117762
_publ_section_title
;
 Continuous flow synthesis of a carbon-based molecular cage macrocycle via
 a three-fold homocoupling reaction
;
_journal_name_full               Chem.Commun.
_journal_page_first              14231
_journal_paper_doi               10.1039/C5cc05181A
_journal_volume                  51
_journal_year                    2015
_chemical_formula_moiety         'C110 H56 Br2'
_chemical_formula_sum            'C110 H56 Br2'
_chemical_formula_weight         1537.36
_space_group_crystal_system      tetragonal
_space_group_IT_number           142
_space_group_name_Hall           '-I 4bd 2c'
_space_group_name_H-M_alt        'I 41/a c d'
_symmetry_space_group_name_Hall  '-I 4bd 2c'
_symmetry_space_group_name_H-M   'I 41/a c d :2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-06-24 deposited with the CCDC.
2015-08-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   39.709(6)
_cell_length_b                   39.709(6)
_cell_length_c                   39.724(8)
_cell_measurement_reflns_used    249
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      18.659
_cell_measurement_theta_min      1.026
_cell_volume                     62637(18)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.388
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'Phi Scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1152
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_Laue_measured_fraction_full 0.388
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            170819
_diffrn_reflns_point_group_measured_fraction_full 0.388
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         18.659
_diffrn_reflns_theta_min         1.026
_diffrn_source                   'MX1 Beamline Australian Synchrotron'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.544
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    0.652
_exptl_crystal_description       needle
_exptl_crystal_F_000             12576
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.275
_refine_diff_density_min         -1.084
_refine_diff_density_rms         0.069
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.325
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         5979
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.325
_refine_ls_R_factor_all          0.1305
_refine_ls_R_factor_gt           0.1092
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2968
_refine_ls_wR_factor_ref         0.3186
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4972
_reflns_number_total             5979
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc05181a2.cif
_cod_data_source_block           cage_C2
_cod_original_cell_volume        62636(22)
_cod_database_code               7117762
_shelx_estimated_absorpt_t_min   0.899
_shelx_estimated_absorpt_t_max   0.948
_shelxl_version_number           2013-4
_shelx_res_checksum              79766