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_7710705
_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_formula_moiety         'C54 H76 O4, C2 H3 N'
_chemical_formula_sum            'C56 H79 N O4'
_chemical_formula_weight         830.20
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_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                 110.1060(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.6259(2)
_cell_length_b                   11.52628(9)
_cell_length_c                   23.5831(3)
_cell_measurement_reflns_used    21476
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.05
_cell_measurement_theta_min      3.58
_cell_volume                     5009.71(10)
_computing_cell_refinement       'CrysAlisPro 1.171.41.105a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.105a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.105a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_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 0.998
_diffrn_measurement_device       'four-circle diffractometer'
_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  0.0278
_diffrn_reflns_av_unetI/netI     0.0256
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            46943
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.246
_diffrn_reflns_theta_min         2.538
_diffrn_source                   'Rotating anode'
_exptl_absorpt_coefficient_mu    0.517
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.819
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlisPro 1.171.41.105a (Rigaku Oxford Diffraction, 2021) 
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.101
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1816
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile'
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.431
_refine_diff_density_min         -0.252
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     571
_refine_ls_number_reflns         9146
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0521
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0725P)^2^+2.7409P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1425
_refine_ls_wR_factor_ref         0.1471
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7991
_reflns_number_total             9146
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01496c2.cif
_cod_data_source_block           LigandMonoclinicdotMeCN
_cod_original_cell_volume        5009.70(10)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7710705
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.886
_shelx_estimated_absorpt_t_max   0.960
_shelx_res_checksum              66892