Heterometallic cobalt(ii) calix[6 and 8]arenes: synthesis, structure and electrochemical activity
Ignaszak, Anna; Patterson, Nigel; O'Brien, Connor; True, Allison; Elsegood, Mark R. J.; Prior, Timothy J.; Redshaw, Carl; RSC Advances 12 (2022) 11672–11685; doi:10.1039/D2RA01009G

data_7244782
_publ_section_title
;
 Heterometallic cobalt(ii) calix[6 and 8]arenes: synthesis, structure and
 electrochemical activity
;
_journal_issue                   19
_journal_name_full               'RSC Advances'
_journal_page_first              11672
_journal_page_last               11685
_journal_paper_doi               10.1039/D2RA01009G
_journal_volume                  12
_journal_year                    2022
_chemical_formula_moiety
;

C154 H196 Br2 Co3 Li9 N7 O16, 10(C2 H3 N), 5[CH3CN]
;
_chemical_formula_sum            'C184 H239 Br2 Co3 Li9 N22 O16'
_chemical_formula_weight         3414.079
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/1
_audit_update_record
;
2021-06-15 deposited with the CCDC.	2022-03-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.986(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.6753(4)
_cell_length_b                   61.6021(17)
_cell_length_c                   18.8069(7)
_cell_measurement_reflns_used    26345
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.447
_cell_measurement_theta_min      2.23
_cell_volume                     19307.5(10)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
;
Rigaku FRE+ equipped with VHF Varimax confocal mirrors and an 
AFC10 goniometer and HG Saturn 724+ detector
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0904
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       71
_diffrn_reflns_limit_k_min       -73
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            79547
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.056
_diffrn_source                   'rotating anode'
_exptl_absorpt_coefficient_mu    0.726
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.71287
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.175
_exptl_crystal_description       block
_exptl_crystal_F_000             6748
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.015
_refine_diff_density_max         1.723
_refine_diff_density_min         -1.053
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2006
_refine_ls_number_reflns         79547
_refine_ls_number_restraints     3178
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.2373
_refine_ls_R_factor_gt           0.1766
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1119P)^2^+400.6648P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3987
_refine_ls_wR_factor_ref         0.4369
_reflns_Friedel_coverage         0.000
_reflns_number_gt                52688
_reflns_number_total             79547
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ra01009g2.cif
_cod_data_source_block           CoLi1
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7244782
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.857
_shelx_estimated_absorpt_t_max   0.989
_shelx_res_checksum              77708
_shelx_fab_checksum              34938