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_1569320
_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 Cl2 N15 Sb Zn3, 3(C H Cl3)'
_chemical_formula_sum            'C150 H99 Cl11 N15 Sb Zn3'
_chemical_formula_weight         2819.25
_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             2022-06-06
_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                95.529(2)
_cell_angle_beta                 93.028(2)
_cell_angle_gamma                90.230(2)
_cell_formula_units_Z            2
_cell_length_a                   13.5059(4)
_cell_length_b                   16.2547(4)
_cell_length_c                   30.3809(8)
_cell_measurement_reflns_used    14861
_cell_measurement_temperature    180.00(14)
_cell_measurement_theta_max      24.9920
_cell_measurement_theta_min      2.2700
_cell_volume                     6629.1(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    'XT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      180.0
_diffrn_detector_area_resol_mean 10.4757
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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     -8.00  18.00   1.00   12.50    --  -10.48 -99.00   0.00   26
  2  \w    -77.00  13.00   1.00   12.50    --  -10.48 -57.00-120.00   90
  3  \w      1.00  30.00   1.00   12.50    --  -10.48 -99.00  30.00   29
  4  \w    -39.00  62.00   1.00   12.50    --  -10.48  57.00  30.00  101
  5  \w    -20.00   5.00   1.00   12.50    --  -10.48 -99.00-180.00   25
  6  \w     38.00  64.00   1.00   12.50    --   12.36 178.00 -90.00   26
  7  \w     38.00  92.00   1.00   12.50    --   12.36 178.00-120.00   54
;
_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  0.0373
_diffrn_reflns_av_unetI/netI     0.0618
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            53489
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.081
_diffrn_reflns_theta_max         25.081
_diffrn_reflns_theta_min         2.083
_exptl_absorpt_coefficient_mu    1.018
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.478
_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    1.412
_exptl_crystal_description       block
_exptl_crystal_F_000             2864
_exptl_crystal_size_max          0.425
_exptl_crystal_size_mid          0.347
_exptl_crystal_size_min          0.235
_refine_diff_density_max         1.348
_refine_diff_density_min         -1.276
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1621
_refine_ls_number_reflns         23428
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0799
_refine_ls_R_factor_gt           0.0547
_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^)+(0.0683P)^2^+9.9677P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1326
_refine_ls_wR_factor_ref         0.1501
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17340
_reflns_number_total             23428
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc02151c2.cif
_cod_data_source_block           3Zn
_cod_database_code               1569320
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1.a Ternary CH refined with riding coordinates:
 C1S(H1S), C2S(H2S), C3S(H3S)
1.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C13(H13), C14(H14), C15(H15), C21(H21), C23(H23), C24(H24),
 C25(H25), C31(H31), C33(H33), C34(H34), C35(H35), C44(H44), C45(H45), C46(H46),
  C47(H47), C48(H48), C50(H50), C51(H51), C55(H55), C56(H56), C57(H57),
 C58(H58), C59(H59), C61(H61), C62(H62), C67(H67), C68(H68), C69(H69), C70(H70),
  C71(H71), C73(H73), C74(H74), C78(H78), C79(H79), C80(H80), C81(H81),
 C82(H82), C84(H84), C85(H85), C89(H89), C90(H90), C91(H91), C92(H92), C93(H93),
  C95(H95), C96(H96), C100(H100), C101(H101), C102(H102), C103(H103),
 C104(H104), C106(H106), C107(H107), C111(H111), C112(H112), C113(H113),
 C114(H114), C115(H115), C117(H117), C118(H118), C122(H122), C123(H123),
 C124(H124), C125(H125), C126(H126), C128(H128), C129(H129), C133(H133),
 C134(H134), C135(H135), C136(H136), C137(H137), C139(H139), C140(H140),
 C144(H144), C145(H145), C146(H146), C147(H147), C148(H148), C150(H150),
 C151(H151), C156(H156), C157(H157), C158(H158), C159(H159), C160(H160),
 C162(H162), C163(H163), C167(H167), C168(H168), C169(H169), C170(H170),
 C171(H171), C173(H173), C174(H174)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 121 electrons were found in a volume of 401 cubic angstroms in 1 void per unit cell. 
The crystallization solvent was CHCl3/hexane and this is consistent with the presence of roughly 2CHCl3 per unit cell which account for 116 electrons per unit cell
;
_smtbx_masks_void_probe_radius   1.3
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              8624
_shelx_hkl_checksum              2675
_shelx_fab_checksum              1470
_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
;