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_7130204
_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         'C96 H116 Li N4 Nb O13 W2, 4(C2 H3 N)'
_chemical_formula_sum            'C104 H128 Li N8 Nb O13 W2'
_chemical_formula_weight         2165.69
_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                108.9456(6)
_cell_angle_beta                 102.2931(5)
_cell_angle_gamma                110.7940(6)
_cell_formula_units_Z            4
_cell_length_a                   20.98734(13)
_cell_length_b                   22.70548(17)
_cell_length_c                   25.64355(11)
_cell_measurement_reflns_used    130275
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.27
_cell_measurement_theta_min      2.30
_cell_volume                     10033.28(14)
_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 0.995
_diffrn_measured_fraction_theta_max 0.988
_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  0.0580
_diffrn_reflns_av_unetI/netI     0.0291
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            219603
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.070
_diffrn_reflns_theta_min         2.316
_diffrn_source                   'Rotating anode'
_exptl_absorpt_coefficient_mu    5.568
_exptl_absorpt_correction_T_max  0.909
_exptl_absorpt_correction_T_min  0.771
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
; 
CrysAlisPro 1.171.40.82a (Rigaku Oxford Diffraction, 2020) 
Numerical absorption correction based on gaussian integration over 
a multifaceted crystal model 
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4416
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile'
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.040
_refine_diff_density_max         2.231
_refine_diff_density_min         -2.569
_refine_diff_density_rms         0.108
_refine_ls_extinction_coef       0.000067(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2528
_refine_ls_number_reflns         37666
_refine_ls_number_restraints     876
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0497
_refine_ls_R_factor_gt           0.0457
_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^)+(0.0594P)^2^+31.5393P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1169
_refine_ls_wR_factor_ref         0.1200
_reflns_Friedel_coverage         0.000
_reflns_number_gt                34182
_reflns_number_total             37666
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc02236b2.cif
_cod_data_source_block           4dot4MeCN
_cod_original_cell_volume        10033.27(12)
_cod_database_code               7130204
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.697
_shelx_estimated_absorpt_t_max   0.808
_shelx_res_checksum              69922
_shelx_hkl_checksum              25717