Aqua{μ-1,4-bis[(1,4,7,10-tetraazacyclododecan-1-yl)methyl]benzene}(nitrato-κO)dicopper(II) tris(nitrate) trihydrate
Ichimaru, Yoshimi; Kato, Koichi; Sugiura, Kirara; Ogawa, Sarina; Jin, Wanchun; Kurihara, Masaaki; Yamaguchi, Yoshihiro; Imai, Masanori; Kurosaki, Hiromasa; IUCrData 8 (2023) x230462–; doi:10.1107/S2414314623004625

data_1569378
_publ_section_title
;
 Aqua{\m-1,4-bis[(1,4,7,10-tetraazacyclododecan-1-yl)methyl]benzene}(nitrato-\kO)dicopper(II)
 tris(nitrate) trihydrate
;
_journal_coeditor_code           ZL4054
_journal_issue                   6
_journal_name_full               IUCrData
_journal_page_first              x230462
_journal_paper_doi               10.1107/S2414314623004625
_journal_volume                  8
_journal_year                    2023
_chemical_absolute_configuration syn
_chemical_formula_iupac
'[Cu2 (N O3) (C24 H46 N8) (H2 O)] (N O3)3, 3H2 O'
_chemical_formula_moiety         'C24 H48 Cu2 N9 O4 3+, 3(N O3 -), 3(H2 O)'
_chemical_formula_sum            'C24 H54 Cu2 N12 O16'
_chemical_formula_weight         893.87
_chemical_name_systematic
'Aqua{\m-1,4-bis[(1,4,7,10-tetraazacyclododecan-1-yl)methyl]benzene}(nitrato-\k<i>O</i>)dicopper(II) tris(nitrate) trihydrate'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.9788(2)
_cell_length_b                   15.3455(2)
_cell_length_c                   16.2948(2)
_cell_measurement_reflns_used    16388
_cell_measurement_temperature    93.25
_cell_measurement_theta_max      68.2240
_cell_measurement_theta_min      2.7200
_cell_volume                     3745.48(8)
_computing_cell_refinement
;
CrysAlisPro 1.171.42.55a (Rigaku OD, 2022)
;
_computing_data_collection
;
CrysAlisPro 1.171.42.55a (Rigaku OD, 2022)
;
_computing_data_reduction
;
CrysAlisPro 1.171.42.55a (Rigaku OD, 2022)
;
_computing_molecular_graphics
;
Olex2 1.3 (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
Olex2 1.3 (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
<i>SHELXL2018/3</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT2018/2</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      93.25
_diffrn_detector                 'Rigaku HyPix-3000 area detector'
_diffrn_detector_area_resol_mean 10.0
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB Synergy-i'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'multi-layer mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0465
_diffrn_reflns_av_unetI/netI     0.0416
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_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            19219
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.436
_diffrn_reflns_theta_min         3.957
_diffrn_source                   'microfocus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    2.144
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50473
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2022)
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.585
_exptl_crystal_description       block
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.083
_refine_diff_density_min         -0.526
_refine_ls_abs_structure_details
;
 Refined as an inversion twin
;
_refine_ls_abs_structure_Flack   0.36(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     530
_refine_ls_number_reflns         6617
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0535
_refine_ls_R_factor_gt           0.0458
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0781P)^2^+6.1629P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1219
_refine_ls_wR_factor_ref         0.1390
_reflns_number_gt                6227
_reflns_number_total             6617
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            zl4054.cif
_cod_data_source_block           I
_cod_database_code               1569378
_shelx_estimated_absorpt_t_min   0.385
_shelx_estimated_absorpt_t_max   0.712
_shelx_hkl_checksum              61555
_shelx_res_checksum              55711