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_7130202
_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         'C101 H129 N2 Nb2 O20 V4, 7(C2 H3 N)'
_chemical_formula_sum            'C115 H152 N9 Nb2 O20 V4'
_chemical_formula_weight         2370.03
_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                86.3411(16)
_cell_angle_beta                 71.046(2)
_cell_angle_gamma                69.098(2)
_cell_formula_units_Z            2
_cell_length_a                   17.0576(5)
_cell_length_b                   17.8520(4)
_cell_length_c                   22.0610(4)
_cell_measurement_reflns_used    37210
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.12
_cell_measurement_theta_min      1.93
_cell_volume                     5925.2(3)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (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 0.999
_diffrn_measured_fraction_theta_max 0.830
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
; 
Rigaku FRE+ equipped with VHF Varimax confocal mirrors and an AFC12 
goniometer and HyPix 6000 detector
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_radiation_collimation    0.2
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0576
_diffrn_reflns_av_unetI/netI     0.0636
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.830
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            142891
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.830
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.793
_diffrn_reflns_theta_min         1.907
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    0.557
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.747
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2478
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile'
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.050
_refine_diff_density_max         2.097
_refine_diff_density_min         -1.338
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1339
_refine_ls_number_reflns         33588
_refine_ls_number_restraints     366
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.1092
_refine_ls_R_factor_gt           0.0718
_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^)+(0.0460P)^2^+26.4490P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1565
_refine_ls_wR_factor_ref         0.1744
_reflns_Friedel_coverage         0.000
_reflns_number_gt                23771
_reflns_number_total             33588
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc02236b2.cif
_cod_data_source_block           3dot7MeCN
_cod_database_code               7130202
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.967
_shelx_estimated_absorpt_t_max   0.973
_shelx_res_checksum              59955
_shelx_hkl_checksum              99592
_shelx_fab_checksum              33495