Structural and dimensional control of porphyrin capsules using Group 15 tris(3-pyridyl) linkers.
García-Romero, Álvaro; Miguel, Daniel; Wright, Dominic S.; Álvarez, Celedonio M; García-Rodríguez, Raúl; Chemical science 14 (2023) 6522–6530; doi:10.1039/d3sc02151c

data_1569313
_publ_section_title
;
 Structural and dimensional control of porphyrin capsules using Group 15
 tris(3-pyridyl) linkers.
;
_journal_issue                   24
_journal_name_full               'Chemical science'
_journal_page_first              6522
_journal_page_last               6530
_journal_paper_doi               10.1039/d3sc02151c
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C147 H96 N15 Sb Zn3, C H Cl3'
_chemical_formula_sum            'C148 H97 Cl3 N15 Sb Zn3'
_chemical_formula_weight         2509.61
_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     iterative
_audit_creation_date             2022-05-31
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-08-10 deposited with the CCDC.	2023-05-17 downloaded from the CCDC.
;
_cell_angle_alpha                86.6057(18)
_cell_angle_beta                 79.266(2)
_cell_angle_gamma                77.064(2)
_cell_formula_units_Z            2
_cell_length_a                   11.5963(3)
_cell_length_b                   21.0912(5)
_cell_length_c                   28.0154(6)
_cell_measurement_reflns_used    17567
_cell_measurement_temperature    180.1(2)
_cell_measurement_theta_max      25.0270
_cell_measurement_theta_min      2.4050
_cell_volume                     6560.2(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      180.1(2)
_diffrn_detector_area_resol_mean 10.4757
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -56.00  37.00   1.00   19.53    --   12.36 -57.00 150.00   93
  2  \w    -14.00  76.00   1.00   19.53    --   12.36  77.00  60.00   90
  3  \w    -13.00  85.00   1.00   19.53    --   12.36  57.00 -60.00   98
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_av_unetI/netI     0.0579
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            43227
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.058
_diffrn_reflns_theta_max         25.058
_diffrn_reflns_theta_min         2.173
_exptl_absorpt_coefficient_mu    0.862
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.343
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
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_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.270
_exptl_crystal_description       block
_exptl_crystal_F_000             2564
_exptl_crystal_size_max          0.594
_exptl_crystal_size_mid          0.283
_exptl_crystal_size_min          0.202
_refine_diff_density_max         1.596
_refine_diff_density_min         -1.090
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1531
_refine_ls_number_reflns         23158
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0704
_refine_ls_R_factor_gt           0.0530
_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^)+(0.0601P)^2^+12.6027P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1297
_refine_ls_wR_factor_ref         0.1409
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18212
_reflns_number_total             23158
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc02151c2.cif
_cod_data_source_block           1Zn-open
_cod_original_cell_volume        6560.1(3)
_cod_database_code               1569313
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1.a Ternary CH refined with riding coordinates:
 C1S(H1S)
1.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C14(H14), C15(H15), C22(H22), C23(H23), C24(H24),
 C25(H25), C32(H32), C33(H33), C34(H34), C35(H35), C42(H42), C43(H43), C47(H47),
  C48(H48), C49(H49), C50(H50), C51(H51), C53(H53), C54(H54), C58(H58),
 C59(H59), C60(H60), C61(H61), C62(H62), C64(H64), C65(H65), C69(H69), C70(H70),
  C71(H71), C72(H72), C73(H73), C75(H75), C76(H76), C80(H80), C81(H81),
 C82(H82), C83(H83), C84(H84), C86(H86), C87(H87), C91(H91), C92(H92), C93(H93),
  C94(H94), C95(H95), C97(H97), C98(H98), C102(H102), C103(H103), C104(H104),
 C105(H105), C106(H106), C108(H108), C109(H109), C113(H113), C114(H114),
 C115(H115), C116(H116), C117(H117), C119(H119), C120(H120), C124(H124),
 C125(H125), C126(H126), C127(H127), C128(H128), C130(H130), C131(H131),
 C135(H135), C136(H136), C137(H137), C138(H138), C139(H139), C141(H141),
 C143(H143), C147(H147), C148(H148), C149(H149), C150(H150), C151(H151),
 C153(H153), C154(H154), C158(H158), C159(H159), C160(H160), C161(H161),
 C162(H162), C164(H164), C165(H165), C169(H169), C170(H170), C171(H171),
 C172(H172), C173(H173)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 259 electrons were found in a volume of 1016cubic angstroms in 2 voids per unit cell, with poorly defined molecules of solvent (CHCl3 and hexane).
The crystallization solvent was CHCl3/hexane and NMR spectroscopy indicated the presence of both CHCl3 and hexane in the bulk crystalline sample. Although this could be consistent with the presence of roughly 3 molecules of hexane and 2 molecules of CHCl3 in the unit cell (which account for 266 electrons per unit cell), the exact proportion of the solvents in the crystal is difficult to determine due to their similar electron count
Moreover, the crystals were observed to lose solvent very quickly during the preparation of the sample, and therefore the exact amount of hexane or CHCl3 is expected to vary among crystals due to their partial loss
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              42717
_shelx_hkl_checksum              93625
_shelx_fab_checksum              44391
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;