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_1557230
_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 H22 F40 N8 O3'
_chemical_formula_sum            'C89 H22 F40 N8 O3'
_chemical_formula_weight         2011.14
_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                82.937(6)
_cell_angle_beta                 77.650(8)
_cell_angle_gamma                70.954(9)
_cell_formula_units_Z            2
_cell_length_a                   11.6188(16)
_cell_length_b                   14.4030(11)
_cell_length_c                   26.7956(17)
_cell_measurement_reflns_used    4377
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      72.94
_cell_measurement_theta_min      3.23
_cell_volume                     4133.7(7)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics    'CrystalStructure 4.2.2 (Rigaku, 2016)'
_computing_publication_material  'CrystalStructure 4.2.2 (Rigaku, 2016)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'ShelXT (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 10.3271
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'GV1000 (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.1135
_diffrn_reflns_av_unetI/netI     0.1267
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            29600
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.687
_diffrn_reflns_theta_max         67.996
_diffrn_reflns_theta_min         3.252
_diffrn_source                   'rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    1.463
_exptl_absorpt_correction_T_max  0.925
_exptl_absorpt_correction_T_min  0.866
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.616
_exptl_crystal_F_000             1992
_exptl_crystal_size_max          0.166
_exptl_crystal_size_mid          0.123
_exptl_crystal_size_min          0.064
_refine_diff_density_max         0.427
_refine_diff_density_min         -0.368
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1262
_refine_ls_number_reflns         15002
_refine_ls_number_restraints     501
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.2486
_refine_ls_R_factor_gt           0.1453
_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^)+(0.0500P)^2^+16.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2787
_refine_ls_wR_factor_ref         0.3435
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5193
_reflns_number_total             15002
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc06197e2.cif
_cod_data_source_block           shelxl_CCDC2
_cod_depositor_comments
;Adding full bibliography for 1557228--1557232.cif.

 Adding full bibliography for 1557228--1557232.cif.
;
_cod_database_code               1557230
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.793
_shelx_estimated_absorpt_t_max   0.912
_shelx_res_checksum              42034
_shelx_fab_checksum              78519