Supramolecular stacking in a high Z′ calix[8]arene‒porphyrin assembly
Alex, Jimi M.; McArdle, Patrick; Crowley, Peter B.; CrystEngComm 22 (2020) 14–17; doi:10.1039/C9CE01646E

data_7235142
_publ_section_title
;
 Supramolecular stacking in a high Z&#x2032; calix[8]arene--porphyrin
 assembly
;
_journal_issue                   1
_journal_name_full               CrystEngComm
_journal_page_first              14
_journal_page_last               17
_journal_paper_doi               10.1039/C9CE01646E
_journal_volume                  22
_journal_year                    2020
_chemical_formula_sum            'C313 H317 N24 O149.5 S16'
_chemical_formula_weight         7319.85
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-09-26 deposited with the CCDC.	2019-11-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.56(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   33.621(17)
_cell_length_b                   38.411(13)
_cell_length_c                   40.234(15)
_cell_measurement_reflns_used    70073
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.5
_cell_measurement_theta_min      2.5
_cell_volume                     50715(4)
_computing_cell_refinement       'XDS (Kabsch, 2017)'
_computing_data_collection       'MXCuBE(Gabadinho <i>et al.</i>, 2010)'
_computing_data_reduction        'XDS (Kabsch, 2017)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.788
_diffrn_measured_fraction_theta_max 0.788
_diffrn_measurement_device_type  'SOLEIL synchrotron'
_diffrn_measurement_method       'Phi Scan'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.82656
_diffrn_reflns_av_R_equivalents  0.0572
_diffrn_reflns_av_unetI/netI     0.0502
_diffrn_reflns_Laue_measured_fraction_full 0.788
_diffrn_reflns_Laue_measured_fraction_max 0.788
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            367899
_diffrn_reflns_point_group_measured_fraction_full 0.760
_diffrn_reflns_point_group_measured_fraction_max 0.760
_diffrn_reflns_theta_full        28.132
_diffrn_reflns_theta_max         28.132
_diffrn_reflns_theta_min         0.603
_exptl_absorpt_coefficient_mu    0.205
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    0.959
_exptl_crystal_description       block
_exptl_crystal_F_000             15260
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.375
_refine_diff_density_min         -0.517
_refine_diff_density_rms         0.143
_refine_ls_abs_structure_details
;
 Flack x determined using 23399 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.497(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.627
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     8137
_refine_ls_number_reflns         119907
_refine_ls_number_restraints     15387
_refine_ls_restrained_S_all      11.955
_refine_ls_R_factor_all          0.2282
_refine_ls_R_factor_gt           0.1837
_refine_ls_shift/su_max          3.978
_refine_ls_shift/su_mean         0.162
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4178
_refine_ls_wR_factor_ref         0.4651
_reflns_Friedel_coverage         0.897
_reflns_Friedel_fraction_full    0.731
_reflns_Friedel_fraction_max     0.731
_reflns_number_gt                65813
_reflns_number_total             119907
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce01646e2.cif
_cod_data_source_block           tmap_3aO
_cod_depositor_comments
;Adding full bibliography for 7235142--7235143.cif.

 Adding full bibliography for 7235142--7235143.cif.
;
_cod_original_cell_volume        50715(37)
_cod_original_sg_symbol_H-M      'P 21'
_cod_original_formula_sum        'C313 H317 N24 O149.50 S16'
_cod_database_code               7235142
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.960
_shelx_estimated_absorpt_t_max   0.990
_shelx_res_checksum              12578