Mixed-metal calix[8]arene complexes: Structure, and ring opening polymerization studies
Xing, Tian; Derbyshire, Max; Elsegood, Mark Robert James; Redshaw, Carl; Chemical Communications  (2022) –; doi:10.1039/D2CC02236B

data_7130203
_publ_section_title
;
 Mixed-metal calix[8]arene complexes: Structure, and ring opening
 polymerization studies
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC02236B
_journal_year                    2022
_chemical_formula_moiety         'C98 H124 N2 O15 Ta2 V2, 6.5(C2 H3 N)'
_chemical_formula_sum            'C111 H143.5 N8.5 O15 Ta2 V2'
_chemical_formula_weight         2300.61
_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     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-03-06 deposited with the CCDC.	2022-06-08 downloaded from the CCDC.
;
_cell_angle_alpha                79.652(3)
_cell_angle_beta                 69.474(3)
_cell_angle_gamma                69.029(3)
_cell_formula_units_Z            2
_cell_length_a                   16.1718(5)
_cell_length_b                   19.5000(5)
_cell_length_c                   21.3597(8)
_cell_measurement_reflns_used    26130
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      69.89
_cell_measurement_theta_min      3.06
_cell_volume                     5879.0(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_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 0.989
_diffrn_measured_fraction_theta_max 0.969
_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  0.0803
_diffrn_reflns_av_unetI/netI     0.0495
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            97203
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.563
_diffrn_reflns_theta_min         3.080
_diffrn_source                   'Rotating anode'
_exptl_absorpt_coefficient_mu    5.106
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.648
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlisPro 1.171.40.82a (Rigaku Oxford Diffraction, 2020) 
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2362
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile'
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.020
_refine_diff_density_max         3.804
_refine_diff_density_min         -2.524
_refine_diff_density_rms         0.185
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1231
_refine_ls_number_reflns         21829
_refine_ls_number_restraints     563
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.1205
_refine_ls_R_factor_gt           0.0840
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1311P)^2^+33.9765P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2157
_refine_ls_wR_factor_ref         0.2513
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15116
_reflns_number_total             21829
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc02236b2.cif
_cod_data_source_block           2dot6andahalfMeCN
_cod_original_formula_sum        'C111 H143.50 N8.50 O15 Ta2 V2'
_cod_database_code               7130203
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.495
_shelx_estimated_absorpt_t_max   0.905
_shelx_res_checksum              9432
_shelx_hkl_checksum              51058
_shelx_fab_checksum              61681