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_1557231
_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 H20 F40 N8 Ni O3, 4(C2 H3 N)'
_chemical_formula_sum            'C97 H32 F40 N12 Ni O3'
_chemical_formula_weight         2232.05
_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                92.257(3)
_cell_angle_beta                 101.581(2)
_cell_angle_gamma                108.230(2)
_cell_formula_units_Z            2
_cell_length_a                   14.057(2)
_cell_length_b                   14.080(2)
_cell_length_c                   24.646(4)
_cell_measurement_reflns_used    9896
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.94
_cell_measurement_theta_min      2.41
_cell_volume                     4511.4(12)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0238
_diffrn_reflns_av_unetI/netI     0.0953
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            31515
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.999
_diffrn_reflns_theta_min         0.848
_exptl_absorpt_coefficient_mu    0.359
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.675
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.643
_exptl_crystal_description       block
_exptl_crystal_F_000             2220
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.340
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.213
_refine_diff_density_min         -0.803
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1379
_refine_ls_number_reflns         19290
_refine_ls_number_restraints     358
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.1020
_refine_ls_R_factor_gt           0.0744
_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^)+(0.1500P)^2^+6.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2149
_refine_ls_wR_factor_ref         0.2485
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13982
_reflns_number_total             19290
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc06197e2.cif
_cod_data_source_block           shelxl_CCDC3
_cod_depositor_comments
;Adding full bibliography for 1557228--1557232.cif.

 Adding full bibliography for 1557228--1557232.cif.
;
_cod_database_code               1557231
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.813
_shelx_estimated_absorpt_t_max   0.965
_shelx_res_checksum              48464