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_1569310
_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         'C162 H108 Mg3 N18 Sb2, 5(C H Cl3)'
_chemical_formula_sum            'C167 H113 Cl15 Mg3 N18 Sb2'
_chemical_formula_weight         3219.93
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-06-05
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   20.9301(8)
_cell_length_b                   20.9301(8)
_cell_length_c                   37.6852(17)
_cell_measurement_reflns_used    2233
_cell_measurement_temperature    219.9(2)
_cell_measurement_theta_max      24.1020
_cell_measurement_theta_min      3.0070
_cell_volume                     14297.0(10)
_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      219.9(2)
_diffrn_detector_area_resol_mean 10.4757
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_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    -19.00  79.00   1.00   20.00    --   12.36  77.00-180.00   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  0.0464
_diffrn_reflns_av_unetI/netI     0.0952
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            10644
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        24.720
_diffrn_reflns_theta_max         24.720
_diffrn_reflns_theta_min         2.927
_exptl_absorpt_coefficient_mu    0.551
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.679
_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    1.122
_exptl_crystal_description       block
_exptl_crystal_F_000             4902
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.298
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.863
_refine_diff_density_min         -0.551
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.975
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     328
_refine_ls_number_reflns         5421
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      0.979
_refine_ls_R_factor_all          0.0968
_refine_ls_R_factor_gt           0.0583
_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^)+(0.1007P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1567
_refine_ls_wR_factor_ref         0.1727
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3404
_reflns_number_total             5421
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc02151c2.cif
_cod_data_source_block           1Mg
_cod_original_cell_volume        14297.0(13)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               1569310
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.932
_shelx_estimated_absorpt_t_min   0.822
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C2S-Cl3S \\sim C2S-Cl4S \\sim C2S-Cl2S
 with sigma of 0.02
 Cl3S-Cl4S \\sim Cl4S-Cl2S \\sim Cl2S-Cl3S
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Cl2S \\sim Cl3S \\sim Cl4S \\sim C2S: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
4. Rigid body (RIGU) restrains
 Cl2S, Cl3S, Cl4S, C2S
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: Cl2S(0.5) Cl3S(0.5) Cl4S(0.5) C2S(0.5) H2S(0.5)
6.a Ternary CH refined with riding coordinates:
 C2S(H2S), C1S(H1S)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C8(H8), C12(H12), C13(H13), C17(H17),
 C18(H18), C19(H19), C20(H20), C21(H21), C23(H23), C24(H24), C25(H25), C26(H26),
  C27(H27)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 537 electrons were found in a volume of 3105 cubic angstroms in 2 voids per unit cell. 
This is consistent with roughly 3 CHCl3 molecules per Formula Unit which account for 522 electrons (9 CHCl3 molecules 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   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              86217
_shelx_hkl_checksum              84933
_shelx_fab_checksum              55840
_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
;