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_7132566
_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
'C54 H70 Br2.94 Cl1.06 Mg1 N4 O4 Zn2, 1.5(C2 H3 N)'
_chemical_formula_sum            'C57 H74.5 Br2.94 Cl1.06 Mg N5.5 O4 Zn2'
_chemical_formula_weight         1328.13
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2023-11-16 deposited with the CCDC.	2023-12-01 downloaded from the CCDC.
;
_cell_angle_alpha                96.6727(19)
_cell_angle_beta                 97.5170(19)
_cell_angle_gamma                107.5764(19)
_cell_formula_units_Z            4
_cell_length_a                   13.4199(15)
_cell_length_b                   20.874(2)
_cell_length_c                   23.345(3)
_cell_measurement_reflns_used    2978
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.18
_cell_measurement_theta_min      2.18
_cell_volume                     6096.2(12)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX 2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'SHELXL-2019/3 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Bruker APEX 2 CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0620
_diffrn_reflns_av_unetI/netI     0.0783
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            101114
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.406
_diffrn_reflns_theta_min         1.037
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.816
_exptl_absorpt_correction_T_max  0.702
_exptl_absorpt_correction_T_min  0.219
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS v2008/2, Sheldrick, G.M., (2008)'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Rod
_exptl_crystal_F_000             2719
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile'
_exptl_crystal_size_max          0.630
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.110
_refine_diff_density_max         1.187
_refine_diff_density_min         -0.697
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1391
_refine_ls_number_reflns         29963
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.1022
_refine_ls_R_factor_gt           0.0512
_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^)+(0.0554P)^2^+0.3580P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1040
_refine_ls_wR_factor_ref         0.1213
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19044
_reflns_number_total             29963
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc04899c2.cif
_cod_data_source_block           cr398
_cod_original_formula_sum        'C57 H74.50 Br2.94 Cl1.06 Mg N5.50 O4 Zn2'
_cod_database_code               7132566
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.270
_shelx_estimated_absorpt_t_max   0.747
_shelx_res_checksum              48846
_shelx_hkl_checksum              93112