Mixed-magnesium/zinc calix[4]arene complexes: structure, and ring opening polymerisation studies.
Banks, Henry J. S.; Frese, Josef W. A.; Elsegood, Mark R. J.; Redshaw, Carl; Chemical communications (Cambridge, England) 60 (2024) 304–307; doi:10.1039/d3cc04899c

data_7132569
_publ_section_title
;
 Mixed-magnesium/zinc calix[4]arene complexes: structure, and ring opening
 polymerisation studies.
;
_journal_issue                   3
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              304
_journal_page_last               307
_journal_paper_doi               10.1039/d3cc04899c
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety
'C102 H132 Br3.42 Cl0.58 Mg2 N4 O10 Zn4, 5.19(C2 H3 N)'
_chemical_formula_sum
'C112.37 H147.56 Br3.42 Cl0.58 Mg2 N9.19 O10 Zn4'
_chemical_formula_weight         2390.84
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2023-11-18 deposited with the CCDC.	2023-12-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.3869(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.81378(8)
_cell_length_b                   25.56149(11)
_cell_length_c                   24.42596(10)
_cell_measurement_reflns_used    168989
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.23
_cell_measurement_theta_min      2.88
_cell_volume                     11739.45(9)
_computing_cell_refinement       'CrysAlisPro 1.171.40.18b (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.18b (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.18b (Rigaku OD, 2018)'
_computing_molecular_graphics    'Bruker SHLEXTL'
_computing_publication_material  'Bruker SHLEXTL'
_computing_structure_refinement  'SHELXL-2019/3 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_details 'Rigaku, AFC11 quarter \c goniometer'
_diffrn_measurement_device_type
; 
Rigaku 007HF equipped with Varimax confocal mirrors 
and an AFC11 goniometer and HyPix 6000 detector 
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_radiation_collimation    0.3
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0554
_diffrn_reflns_av_unetI/netI     0.0208
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            304295
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.241
_diffrn_reflns_theta_min         2.573
_diffrn_source                   'Rotating anode'
_exptl_absorpt_coefficient_mu    2.970
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.463
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlisPro 1.171.40.18b (Rigaku Oxford Diffraction, 2018) 
Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             4958
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile'
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.015
_refine_diff_density_max         1.886
_refine_diff_density_min         -1.862
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1487
_refine_ls_number_reflns         21421
_refine_ls_number_restraints     905
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0622
_refine_ls_R_factor_gt           0.0580
_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^)+(0.0822P)^2^+31.2491P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1622
_refine_ls_wR_factor_ref         0.1652
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19525
_reflns_number_total             21421
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc04899c2.cif
_cod_data_source_block           cr607
_cod_original_cell_volume        11739.44(9)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7132569
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.602
_shelx_estimated_absorpt_t_max   0.957
_shelx_res_checksum              43771
_shelx_hkl_checksum              4954