Tripyrrin-armed isosmaragdyrins: synthesis, heterodinuclear coordination, and protonation-triggered helical inversion
Li, Chengjie; Zhang, Kai; Ishida, Masatoshi; Li, Qizhao; Shimomura, Keito; Baryshnikov, Glib; Li, Xin; Savage, Mathew; Wu, Xin-Yan; Yang, Sihai; Furuta, Hiroyuki; Xie, Yongshu; Chemical Science 11 (2020) 2790–2795; doi:10.1039/C9SC06197E

data_1557232
_publ_section_title
;
 Tripyrrin-armed isosmaragdyrins: synthesis, heterodinuclear coordination,
 and protonation-triggered helical inversion
;
_journal_issue                   10
_journal_name_full               'Chemical Science'
_journal_page_first              2790
_journal_page_last               2795
_journal_paper_doi               10.1039/C9SC06197E
_journal_volume                  11
_journal_year                    2020
_chemical_formula_moiety         'C89 H18 Cu F40 N8 Ni O3'
_chemical_formula_sum            'C89 H18 Cu F40 N8 Ni O3'
_chemical_formula_weight         2129.36
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-10-16 deposited with the CCDC.	2020-02-03 downloaded from the CCDC.
;
_cell_angle_alpha                91.9040(10)
_cell_angle_beta                 101.174(2)
_cell_angle_gamma                107.743(2)
_cell_formula_units_Z            2
_cell_length_a                   14.0363(12)
_cell_length_b                   14.1385(15)
_cell_length_c                   24.8547(18)
_cell_measurement_reflns_used    2540
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.1360
_cell_measurement_theta_min      2.9520
_cell_volume                     4586.3(7)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1011
_diffrn_reflns_av_unetI/netI     0.1883
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            33376
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.020
_diffrn_reflns_theta_max         25.020
_diffrn_reflns_theta_min         2.500
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.571
_exptl_absorpt_correction_T_max  0.8208
_exptl_absorpt_correction_T_min  0.7913
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.542
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2098
_exptl_crystal_size_max          0.430
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.360
_refine_diff_density_max         0.893
_refine_diff_density_min         -0.950
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.920
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1280
_refine_ls_number_reflns         16178
_refine_ls_number_restraints     477
_refine_ls_restrained_S_all      0.917
_refine_ls_R_factor_all          0.1813
_refine_ls_R_factor_gt           0.0890
_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^)+(0.0950P)^2^+0.0300P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2021
_refine_ls_wR_factor_ref         0.2477
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6710
_reflns_number_total             16178
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc06197e2.cif
_cod_data_source_block           shelxl_CCDC4
_cod_depositor_comments
;Adding full bibliography for 1557228--1557232.cif.

 Adding full bibliography for 1557228--1557232.cif.
;
_cod_database_code               1557232
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.791
_shelx_estimated_absorpt_t_max   0.821
_shelx_res_checksum              29477
_shelx_fab_checksum              31931