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_1557228
_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(C3 H7 N O)'
_chemical_formula_sum            'C101 H48 F40 N12 Ni O7'
_chemical_formula_weight         2360.22
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.571(3)
_cell_length_b                   19.7599(18)
_cell_length_c                   19.1951(18)
_cell_measurement_reflns_used    7114
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      20.49
_cell_measurement_theta_min      2.43
_cell_volume                     10457.5(18)
_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      213(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_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  0.0851
_diffrn_reflns_av_unetI/netI     0.0951
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            72138
_diffrn_reflns_point_group_measured_fraction_full 0.897
_diffrn_reflns_point_group_measured_fraction_max 0.883
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.933
_diffrn_reflns_theta_min         1.479
_exptl_absorpt_coefficient_mu    0.317
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.686
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.499
_exptl_crystal_description       block
_exptl_crystal_F_000             4728
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.650
_refine_diff_density_min         -0.381
_refine_diff_density_rms         0.060
_refine_ls_abs_structure_details
;
 Flack x determined using 3852 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.007(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1459
_refine_ls_number_reflns         20015
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0953
_refine_ls_R_factor_gt           0.0551
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0430P)^2^+1.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1074
_refine_ls_wR_factor_ref         0.1184
_reflns_Friedel_coverage         0.721
_reflns_Friedel_fraction_full    0.790
_reflns_Friedel_fraction_max     0.763
_reflns_number_gt                12141
_reflns_number_total             20015
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc06197e2.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
;Adding full bibliography for 1557228--1557232.cif.

 Adding full bibliography for 1557228--1557232.cif.
;
_cod_database_code               1557228
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.934
_shelx_estimated_absorpt_t_max   0.969
_shelx_res_checksum              17290
_shelx_fab_checksum              86071