Hexa- and octanuclear copper(II) complexes with tetraeicosaaza amine macrocycle
Gregoliński, Janusz; Fedorowicz, Dominka; Ślepokura, Katarzyna; Kłak, Julia; Witwicki, Maciej; Dalton Transactions  (2023) –; doi:10.1039/D3DT02993J

data_7714318
_publ_section_title
;
 Hexa- and octanuclear copper(II) complexes with tetraeicosaaza amine
 macrocycle
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02993J
_journal_year                    2023
_chemical_formula_moiety
'[Cu6 (C96 H136 N24) 2(OH) 2(H2 O)], 10(N O3), 7.5(H2 O)'
_chemical_formula_sum            'C96 H157 Cu6 N34 O41.5'
_chemical_formula_weight         2832.79
_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   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2023-08-22 deposited with the CCDC.	2023-10-25 downloaded from the CCDC.
;
_cell_angle_alpha                108.45(2)
_cell_angle_beta                 93.03(2)
_cell_angle_gamma                103.86(2)
_cell_formula_units_Z            1
_cell_length_a                   14.445(3)
_cell_length_b                   14.703(3)
_cell_length_c                   15.916(3)
_cell_measurement_reflns_used    71012
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.4710
_cell_measurement_theta_min      2.9200
_cell_volume                     3082.7(12)
_computing_cell_refinement       'CrysAlisPro 1.171.41.80a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.80a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.80a (Rigaku OD, 2020)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'Rigaku, XtaLAB Synergy R, DW system, HyPix-Arc 150'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0463
_diffrn_reflns_av_unetI/netI     0.0174
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            124554
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.680
_diffrn_reflns_theta_max         75.787
_diffrn_reflns_theta_min         2.956
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.948
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.09237
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.80a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.526
_exptl_crystal_description       column
_exptl_crystal_F_000             1477
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.773
_refine_diff_density_min         -0.575
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1127
_refine_ls_number_reflns         12402
_refine_ls_number_restraints     463
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0619
_refine_ls_R_factor_gt           0.0577
_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^)+(0.1015P)^2^+3.9527P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1681
_refine_ls_wR_factor_ref         0.1717
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11308
_reflns_number_total             12402
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02993j2.cif
_cod_data_source_block           1_cul88n
_cod_original_formula_sum        'C96 H157 Cu6 N34 O41.50'
_cod_database_code               7714318
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.685
_shelx_estimated_absorpt_t_max   0.962
_shelx_res_checksum              54472