Multinuclear Ni(II) and Cu(II) complexes of meso 6+6 macrocyclic amine derived from trans-1,2-diaminocyclopentane and 2,6-diformylpyridine
Gregoliński, Janusz; Ślepokura, Katarzyna; Kłak, Julia; Witwicki, Maciej; Dalton Transactions  (2022) –; doi:10.1039/D2DT01329K

data_7710381
_publ_section_title
;
 Multinuclear Ni(II) and Cu(II) complexes of meso 6+6 macrocyclic amine
 derived from trans-1,2-diaminocyclopentane and 2,6-diformylpyridine
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01329K
_journal_year                    2022
_chemical_formula_moiety
'[Cu4 (C72 H102 N18) 2(H2 O)], 8(N O3), 4(H2 O)'
_chemical_formula_sum            'C72 H114 Cu4 N26 O30'
_chemical_formula_weight         2078.05
_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   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2022-04-25 deposited with the CCDC.	2022-05-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 116.22(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.257(3)
_cell_length_b                   24.388(3)
_cell_length_c                   14.846(3)
_cell_measurement_reflns_used    4185
_cell_measurement_temperature    80(2)
_cell_measurement_theta_max      33.90
_cell_measurement_theta_min      3.02
_cell_volume                     4306.0(18)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT-2014/7 (Sheldrick, 2015)'
_diffrn_ambient_temperature      80(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3456
_diffrn_detector_type            Ruby
_diffrn_measured_fraction_theta_full 0.906
_diffrn_measured_fraction_theta_max 0.902
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Agilent Technologies Xcalibur, Ruby'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0348
_diffrn_reflns_av_unetI/netI     0.0564
_diffrn_reflns_Laue_measured_fraction_full 0.906
_diffrn_reflns_Laue_measured_fraction_max 0.902
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            11804
_diffrn_reflns_point_group_measured_fraction_full 0.906
_diffrn_reflns_point_group_measured_fraction_max 0.902
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_min         2.936
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.073
_exptl_absorpt_correction_T_max  0.938
_exptl_absorpt_correction_T_min  0.826
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark blue'
_exptl_crystal_density_diffrn    1.603
_exptl_crystal_description       plate
_exptl_crystal_F_000             2168
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.508
_refine_diff_density_min         -0.371
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     602
_refine_ls_number_reflns         7374
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0623
_refine_ls_R_factor_gt           0.0392
_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^)+(0.0405P)^2^+2.0628P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0834
_refine_ls_wR_factor_ref         0.0933
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5655
_reflns_number_total             7374
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01329k2.cif
_cod_data_source_block           3''_cul28nab
_cod_original_cell_volume        4306.0(17)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7710381
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.806
_shelx_estimated_absorpt_t_max   0.938
_shelx_res_checksum              83623
_shelx_hkl_checksum              39361