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_1569317
_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 H95 Bi N15 Zn3, 3(C H Cl3)'
_chemical_formula_sum            'C150 H98 Bi Cl9 N15 Zn3'
_chemical_formula_weight         2834.57
_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     dual
_audit_creation_date             2022-05-26
_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                92.054(3)
_cell_angle_beta                 98.955(2)
_cell_angle_gamma                94.962(2)
_cell_formula_units_Z            2
_cell_length_a                   13.3955(3)
_cell_length_b                   21.5477(7)
_cell_length_c                   25.0484(8)
_cell_measurement_reflns_used    11686
_cell_measurement_temperature    180.00(14)
_cell_measurement_theta_max      24.9540
_cell_measurement_theta_min      2.8390
_cell_volume                     7106.2(4)
_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    'XT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      180.00(14)
_diffrn_detector_area_resol_mean 10.4757
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -34.00  18.00   1.00   25.00    --  -10.64  57.00 -60.00   52
  2  \w    -20.00  30.00   1.00   25.00    --  -10.64 -99.00-180.00   50
  3  \w     51.00  98.00   1.00   25.00    --   12.51 178.00  90.00   47
  4  \w    -12.00  87.00   1.00   25.00    --   12.51  37.00-180.00   99
  5  \w    -68.00  27.00   1.00   25.00    --   12.51 -19.00   0.00   95
;
_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  0.0498
_diffrn_reflns_av_unetI/netI     0.0882
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            56986
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.041
_diffrn_reflns_theta_max         25.041
_diffrn_reflns_theta_min         2.425
_exptl_absorpt_coefficient_mu    1.958
_exptl_absorpt_correction_T_max  0.908
_exptl_absorpt_correction_T_min  0.612
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
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    1.325
_exptl_crystal_description       needle
_exptl_crystal_F_000             2858
_exptl_crystal_size_max          0.437
_exptl_crystal_size_mid          0.113
_exptl_crystal_size_min          0.045
_refine_diff_density_max         1.649
_refine_diff_density_min         -1.505
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1603
_refine_ls_number_reflns         25082
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0910
_refine_ls_R_factor_gt           0.0566
_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^)+(0.0859P)^2^+1.2989P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1448
_refine_ls_wR_factor_ref         0.1588
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17315
_reflns_number_total             25082
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc02151c2.cif
_cod_data_source_block           2Zn-closed
_cod_database_code               1569317
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.917
_shelx_estimated_absorpt_t_min   0.482
_olex2_refinement_description
;
1.a Ternary CH refined with riding coordinates:
 C2S(H2S), C1S(H1S), C3S(H3S)
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), 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), C88(H88), C89(H89), C93(H93), C94(H94), C95(H95), C96(H96),
  C97(H97), C100(H100), C101(H101), C105(H105), C106(H106), C107(H107),
 C108(H108), C109(H109), C111(H111), C112(H112), C116(H116), C117(H117),
 C118(H118), C119(H119), C120(H120), C122(H122), C123(H123), C126(H126),
 C127(H127), C128(H128), C129(H129), C130(H130), C133(H133), C134(H134),
 C138(H138), C139(H139), C140(H140), C141(H141), C142(H142), C144(H144),
 C145(H145), C149(H149), C150(H150), C151(H151), C152(H152), C154(H154),
 C156(H156), C157(H157), C161(H161), C162(H162), C163(H163), C164(H164),
 C165(H165), C167(H167), C168(H168), C171(H171), C172(H172), C173(H173),
 C174(H174), C175(H175)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 435 electrons were found in a volume of 1176 cubic angstroms in 1 void per unit cell. 
The crystallization solvent was CHCl3/hexane and this is consistent with roughly 8 CHCl3 per unit cell (i.e, 4 CHCl3, per formula unit) which account for 464 electrons per unit cell.
The crystals were observed to lose solvent very quickly during the preparation of the sample, and therefore the exact amount of CHCl3 is expected to vary among crystals due to partial loss of CHCl3.
;
_smtbx_masks_void_probe_radius   1.25
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              40308
_shelx_hkl_checksum              28799
_shelx_fab_checksum              66725
_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
;