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_7130206
_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         'C103.55 H135.73 Li N2 Nb O15 W2, 3(C2 H3 N)'
_chemical_formula_sum            'C109.55 H144.73 Li N5 Nb O15 W2'
_chemical_formula_weight         2239.21
_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                80.1717(12)
_cell_angle_beta                 85.4069(11)
_cell_angle_gamma                66.0269(14)
_cell_formula_units_Z            2
_cell_length_a                   15.4661(2)
_cell_length_b                   17.4102(3)
_cell_length_c                   22.4328(3)
_cell_measurement_reflns_used    66442
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.07
_cell_measurement_theta_min      2.85
_cell_volume                     5437.97(15)
_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 0.995
_diffrn_measured_fraction_theta_max 0.981
_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  0.0590
_diffrn_reflns_av_unetI/netI     0.0271
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            180640
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.595
_diffrn_reflns_theta_min         2.810
_diffrn_source                   'Rotating anode'
_exptl_absorpt_coefficient_mu    5.159
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.716
_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            orange
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2298
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile'
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.595
_refine_diff_density_min         -2.463
_refine_diff_density_rms         0.105
_refine_ls_extinction_coef       0.000128(15)
_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   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1396
_refine_ls_number_reflns         20452
_refine_ls_number_restraints     899
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0474
_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^)+(0.0693P)^2^+11.7579P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1251
_refine_ls_wR_factor_ref         0.1317
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17807
_reflns_number_total             20452
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc02236b2.cif
_cod_data_source_block           5dot3MeCN
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_atom_sites_solution_primary' value 'Iterative' was
changed to 'iterative' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_database_code               7130206
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.626
_shelx_estimated_absorpt_t_max   0.904
_shelx_res_checksum              52614
_shelx_hkl_checksum              54220