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_1569318
_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         'C59 H40 Cl2 Mg N7 Sb'
_chemical_formula_sum            'C59 H40 Cl2 Mg N7 Sb'
_chemical_formula_weight         1063.94
_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             2022-06-05
_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                78.498(3)
_cell_angle_beta                 76.874(3)
_cell_angle_gamma                70.708(3)
_cell_formula_units_Z            2
_cell_length_a                   11.6920(4)
_cell_length_b                   13.9994(5)
_cell_length_c                   19.8328(5)
_cell_measurement_reflns_used    9110
_cell_measurement_temperature    293
_cell_measurement_theta_max      25.0420
_cell_measurement_theta_min      2.0430
_cell_volume                     2956.47(18)
_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      293(2)
_diffrn_detector_area_resol_mean 10.4757
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -12.00  30.00   1.00   17.55    --  -10.48 -99.00 -60.00   42
  2  \w    -46.00 -18.00   1.00   17.55    --   12.36 -77.00-180.00   28
  3  \w     19.00  45.00   1.00   17.55    --   12.36 -77.00-180.00   26
  4  \w    -12.00  85.00   1.00   17.55    --   12.36  37.00 -30.00   97
  5  \w    -52.00  32.00   1.00   17.55    --   12.36 -37.00 150.00   84
  6  \w     48.00  90.00   1.00   17.55    --   12.36 178.00 120.00   42
  7  \w     35.00 101.00   1.00   17.55    --   12.36 178.00-180.00   66
;
_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  0.0303
_diffrn_reflns_av_unetI/netI     0.0417
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            26850
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.207
_diffrn_reflns_theta_max         25.207
_diffrn_reflns_theta_min         1.762
_exptl_absorpt_coefficient_mu    0.608
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.566
_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    1.195
_exptl_crystal_description       block
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.315
_exptl_crystal_size_mid          0.173
_exptl_crystal_size_min          0.147
_refine_diff_density_max         0.609
_refine_diff_density_min         -0.760
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     634
_refine_ls_number_reflns         10623
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0369
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0348P)^2^+0.6214P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0786
_refine_ls_wR_factor_ref         0.0864
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8221
_reflns_number_total             10623
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc02151c2.cif
_cod_data_source_block           3Mg
_cod_original_cell_volume        2956.48(17)
_cod_database_code               1569318
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1.a 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), C41(H41), C42(H42), C47(H47),
  C48(H48), C49(H49), C50(H50), C51(H51), C54(H54), C55(H55), C56(H56),
 C57(H57), C58(H58), C60(H60), C61(H61), C71(H71), C72(H72), C76(H76), C77(H77),
  C78(H78), C79(H79), C80(H80), C82(H82), C83(H83), C87(H87), C88(H88),
 C89(H89), C90(H90), C91(H91)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 206 electrons were found in a volume of 685 cubic angstroms in 1 void per unit cell. 
The crystallization solvent was CHCl3/hexane and this is consistent with the presence of roughly 4CHCl3 per unit cell  which account for 232 electrons per unit cell
;
_smtbx_masks_void_probe_radius   1.25
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              29516
_shelx_hkl_checksum              73081
_shelx_fab_checksum              71398
_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
;