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_1557229
_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, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C89.5 H19 Cl Cu F40 N8 Ni O3'
_chemical_formula_weight         2171.83
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 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                90
_cell_angle_beta                 119.602(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   47.886(3)
_cell_length_b                   13.8742(13)
_cell_length_c                   28.061(3)
_cell_measurement_reflns_used    2457
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      46.71
_cell_measurement_theta_min      3.16
_cell_volume                     16210(3)
_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           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.1229
_diffrn_reflns_av_unetI/netI     0.2250
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -55
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            26628
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        62.700
_diffrn_reflns_theta_max         62.700
_diffrn_reflns_theta_min         3.167
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.307
_exptl_absorpt_correction_T_max  0.7091
_exptl_absorpt_correction_T_min  0.5644
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.780
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             8560
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.160
_refine_diff_density_max         0.620
_refine_diff_density_min         -0.520
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.863
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1294
_refine_ls_number_reflns         12994
_refine_ls_number_restraints     159
_refine_ls_restrained_S_all      0.861
_refine_ls_R_factor_all          0.2124
_refine_ls_R_factor_gt           0.0782
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0083P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1032
_refine_ls_wR_factor_ref         0.1598
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3942
_reflns_number_total             12994
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc06197e2.cif
_cod_data_source_block           shelxl_CCDC1
_cod_depositor_comments
;Adding full bibliography for 1557228--1557232.cif.

 Adding full bibliography for 1557228--1557232.cif.
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C89.50 H19 Cl Cu F40 N8 Ni O3'
_cod_database_code               1557229
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.564
_shelx_estimated_absorpt_t_max   0.709
_shelx_res_checksum              94620