Trinuclear zinc calix[4]arenes: synthesis, structure, and ring opening polymerization studies.
Xing, Tian; Frese, Josef W. A.; Derbyshire, Max; Glenister, Mollie A.; Elsegood, Mark R. J.; Redshaw, Carl; Dalton transactions (Cambridge, England : 2003)  (2022) –; doi:10.1039/d2dt01496c

data_7710708
_publ_section_title
;
 Trinuclear zinc calix[4]arenes: synthesis, structure, and ring opening
 polymerization studies.
;
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_paper_doi               10.1039/d2dt01496c
_journal_year                    2022
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C96 H125 O10 Zn3, 4(C2 H3 N)'
_chemical_formula_sum            'C104 H137 N4 O10 Zn3'
_chemical_formula_weight         1799.28
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-01-07 deposited with the CCDC.	2022-07-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.849(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.3700(15)
_cell_length_b                   22.934(3)
_cell_length_c                   18.132(2)
_cell_measurement_reflns_used    6881
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      22.62
_cell_measurement_theta_min      2.35
_cell_volume                     4923.1(10)
_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-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0515
_diffrn_reflns_av_unetI/netI     0.0758
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            39466
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.720
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.783
_exptl_absorpt_correction_T_max  0.962
_exptl_absorpt_correction_T_min  0.715
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2008/1, Sheldrick, G.M., (2008)'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.214
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1918
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile'
_exptl_crystal_size_max          0.460
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.547
_refine_diff_density_min         -0.295
_refine_diff_density_rms         0.060
_refine_ls_abs_structure_details
; 
 Flack x determined using 5099 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   -0.001(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1247
_refine_ls_number_reflns         17245
_refine_ls_number_restraints     730
_refine_ls_restrained_S_all      0.991
_refine_ls_R_factor_all          0.0697
_refine_ls_R_factor_gt           0.0489
_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^)+(0.0598P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1082
_refine_ls_wR_factor_ref         0.1183
_reflns_Friedel_coverage         0.934
_reflns_Friedel_fraction_full    0.987
_reflns_Friedel_fraction_max     0.987
_reflns_number_gt                13412
_reflns_number_total             17245
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01496c2.cif
_cod_data_source_block           3dot4MeCN
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7710708
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.715
_shelx_estimated_absorpt_t_max   0.962
_shelx_res_checksum              20281