Rapid one-pot synthesis of pyrrole-appended isocorroles.
Larsen, Simon; McCormick, Laura J.; Ghosh, Abhik; Organic & biomolecular chemistry 17 (2019) 3159–3166; doi:10.1039/c9ob00168a

data_7156723
_publ_section_title
;
 Rapid one-pot synthesis of pyrrole-appended isocorroles.
;
_journal_issue                   12
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              3159
_journal_page_last               3166
_journal_paper_doi               10.1039/c9ob00168a
_journal_volume                  17
_journal_year                    2019
_chemical_formula_sum            'C45 H34 Cl3 Cu N5 O3'
_chemical_formula_weight         862.66
_chemical_name_systematic
'Copper(II) 5,10,15-tris(4'-methoxyphenyl)-10-(2''-pyrrolyl)isocorrole'
_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
_atom_sites_solution_primary     'dual space'
_atom_sites_solution_secondary   difmap
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_audit_update_record
;
2018-06-05 deposited with the CCDC.    2019-02-26 downloaded from the CCDC.
;
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_cell_angle_gamma                96.469(3)
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_cell_length_b                   11.6310(16)
_cell_length_c                   15.297(2)
_cell_measurement_reflns_used    9353
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.77
_cell_measurement_theta_min      3.01
_cell_volume                     1907.9(5)
_computing_cell_refinement       'SAINT V8.38A Bruker-AXS, Madison WI'
_computing_data_collection       'Bruker APEX3 Bruker-AXS, Madison WI'
_computing_data_reduction        'SAINT V8.38A Bruker-AXS, Madison WI'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT 2014/5 Bruker-AXS, Madison WI'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 7.39
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 with PHOTON II detector'
_diffrn_measurement_method       '\f and \w shutterless scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7749
_diffrn_reflns_av_R_equivalents  0.0568
_diffrn_reflns_av_unetI/netI     0.0285
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            94061
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        27.706
_diffrn_reflns_theta_max         31.849
_diffrn_reflns_theta_min         1.503
_diffrn_source
;
Advanced Light Source, station 11.3.1
;
_exptl_absorpt_coefficient_mu    1.050
_exptl_absorpt_correction_T_max  0.930
_exptl_absorpt_correction_T_min  0.776
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2016/2 - Bruker AXS, Madison WI'
_exptl_crystal_colour            'dark orange'
_exptl_crystal_density_diffrn    1.502
_exptl_crystal_description       block
_exptl_crystal_F_000             886
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.070
_refine_diff_density_max         1.383
_refine_diff_density_min         -1.674
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     570
_refine_ls_number_reflns         10084
_refine_ls_number_restraints     56
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0842
_refine_ls_R_factor_gt           0.0698
_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^)+(0.1191P)^2^+3.9013P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1939
_refine_ls_wR_factor_ref         0.2105
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8319
_reflns_number_total             10084
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ob00168a2.cif
_cod_data_source_block           CupMeO10pyr_a
_cod_depositor_comments
'Adding full bibliography for 7156722--7156723.cif.'
_cod_database_code               7156723
_shelx_estimated_absorpt_t_min   0.858
_shelx_estimated_absorpt_t_max   0.930
_shelxl_version_number           2014/6
_shelx_res_checksum              39090