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_7244787
_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
'C91.58 H109.38 Br0.21 Co2.81 Li5.19 N1.79 O10, 4(C2 H3 N),Br1.37 Cl2.62, [+12 C2 H3 N]'
_chemical_formula_sum
'C123.58 H157.38 Br1.58 Cl2.62 Co2.81 Li5.19 N17.79 O10'
_chemical_formula_weight         2472.844
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   41.6832(5)
_cell_length_b                   41.6832(5)
_cell_length_c                   17.4818(3)
_cell_measurement_reflns_used    4099
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.918
_cell_measurement_theta_min      1.224
_cell_volume                     30374.4(7)
_computing_cell_refinement       'XIA2 0.5.53'
_computing_data_collection       'GDA http://www.opengda.org/OpenGDA.html'
_computing_data_reduction
;
XIA2 0.5.53 Winter, G. (2010) Journal of Applied Crystallography 43
;
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 5.81
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'three-circle diffractometer'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1200
_diffrn_reflns_av_unetI/netI     0.0619
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       49
_diffrn_reflns_limit_h_min       -49
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_k_min       -49
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            170311
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.028
_diffrn_reflns_theta_max         25.028
_diffrn_reflns_theta_min         1.872
_diffrn_source                   'synchrotron, DLS beamline I19'
_exptl_absorpt_coefficient_mu    0.805
_exptl_absorpt_correction_T_max  1.011
_exptl_absorpt_correction_T_min  0.9877
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
CCP4 7.0.018: AIMLESS, version 0.5.27 : 18/05/16
Scaling & analysis of unmerged intensities, absorption 
correction using spherical harmonics

Run via XIA2 0.5.53-gee81713-dials-1.3-patch135dmin, 
DIALS 1.3.4-g9f5e5cd-release, DIALS/i19 0.91-g03fbaed
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.082
_exptl_crystal_description       block
_exptl_crystal_F_000             8247
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.720
_refine_diff_density_min         -0.452
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     551
_refine_ls_number_reflns         13402
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.1571
_refine_ls_R_factor_gt           0.0968
_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^)+(0.1820P)^2^+45.7172P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2934
_refine_ls_wR_factor_ref         0.3319
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6984
_reflns_number_total             13402
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ra01009g2.cif
_cod_data_source_block           CoLi6
_cod_original_cell_volume        30374.4(9)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               7244787
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.889
_shelx_estimated_absorpt_t_max   0.961
_shelx_res_checksum              36824
_shelx_fab_checksum              95416