Pseudo [M(ii)7] (M = Co, Ni and Zn) metallocalix[6]arene hosts encapsulate a range of organic guest molecules in the solid state
Slater-Parry, Mari; Meally, Seán T.; Ratanasakprakan, Chotima; Townrow, David E.; Ellaby, Rebecca J.; Page, Samuel J.; Jones, Leigh F.; CrystEngComm 27 (2025) 3823–3832; doi:10.1039/D5CE00341E

data_7250378
_publ_section_title
;
 Pseudo [M(ii)7] (M = Co, Ni and Zn) metallocalix[6]arene hosts
 encapsulate a range of organic guest molecules in the solid state
;
_journal_issue                   22
_journal_name_full               CrystEngComm
_journal_page_first              3823
_journal_page_last               3832
_journal_paper_doi               10.1039/D5CE00341E
_journal_volume                  27
_journal_year                    2025
_chemical_formula_sum            'C63 H78 N8 Ni7 O29'
_chemical_formula_weight         1822.19
_chemical_name_common            '[Cou-Ni7].3H2O'
_chemical_name_systematic        Coumarin-Ni7
_space_group_crystal_system      trigonal
_space_group_IT_number           165
_space_group_name_Hall           '-P 3 2"c'
_space_group_name_H-M_alt        'P -3 c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2024-11-19 deposited with the CCDC.	2025-05-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   13.82410(10)
_cell_length_b                   13.82410(10)
_cell_length_c                   23.4073(4)
_cell_measurement_reflns_used    29716
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      30.0400
_cell_measurement_theta_min      2.4130
_cell_volume                     3873.96(8)
_computing_cell_refinement       'crysalispro 1.171.40.84a (rigaku od, 2020)'
_computing_data_collection       'crysalispro 1.171.40.84a (rigaku od, 2020)'
_computing_data_reduction        'crysalispro 1.171.40.84a (rigaku od, 2020)'
_computing_molecular_graphics
'ORTEX - P. McArdle, J.Appl.Cryst.,1995,28,65-65.'
_computing_publication_material
'Oscail - P. McArdle, J.Appl.Cryst.,2017,50,320-326.'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution
'SHELXT - G.M.Sheldrick,Acta Crystallogr.A71(2015)3-8.'
_diffrn_ambient_temperature      100.0(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'xtalab afc12 (rcd3): kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0688
_diffrn_reflns_av_unetI/netI     0.0179
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            74054
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.347
_diffrn_reflns_theta_min         2.434
_diffrn_source                   'rotating-anode x-ray tube'
_exptl_absorpt_coefficient_mu    1.734
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.552
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
crysalispro 1.171.40.84a (rigaku oxford diffraction, 2020)
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            Green
_exptl_crystal_density_diffrn    1.391
_exptl_crystal_description       Parallelepiped
_exptl_crystal_F_000             1668
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: methanol'
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.598
_refine_diff_density_min         -0.440
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     143
_refine_ls_number_reflns         2379
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.132
_refine_ls_R_factor_all          0.0603
_refine_ls_R_factor_gt           0.0575
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1256P)^2^+6.6319P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1884
_refine_ls_wR_factor_ref         0.1923
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2200
_reflns_number_total             2379
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00341e2.cif
_cod_data_source_block           lfjoh1sq
_cod_depositor_comments
'Adding full bibliography for 7250376--7250384.cif.'
_cod_original_cell_volume        3873.96(9)
_cod_database_code               7250378
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              72830
_shelx_fab_checksum              28729
_platon_squeeze_void_probe_radius 1.20