Crystal structure of diaqua(3,14-diethyl-2,6,13,17-tetraazatricyclo[16.4.0.0^7,12^]docosane)copper(II) (3,14-diethyl-2,6,13,17-tetraazatricyclo[16.4.0.0^7,12^]docosane)copper(II) tetrabromide dihydrate, [Cu(C~22~H~44~N~4~)(H~2~O)~2~][Cu(C~22~H~44~N~4~)]Br~4~·2H~2~O
Moon, Dohyun; Jeon, Sunghwan; Lim, Woo Taik; Ryoo, Keon Sang; Choi, Jong-Ha; Acta Crystallographica Section E 77 (2021) 677–680; doi:10.1107/S205698902100551X

data_2243844
_publ_section_title
;
 Crystal structure of
 diaqua(3,14-diethyl-2,6,13,17-tetraazatricyclo[16.4.0.0^7,12^]docosane)copper(II)
 (3,14-diethyl-2,6,13,17-tetraazatricyclo[16.4.0.0^7,12^]docosane)copper(II)
 tetrabromide dihydrate,
 [Cu(C~22~H~44~N~4~)(H~2~O)~2~][Cu(C~22~H~44~N~4~)]Br~4~&#x00B7;2H~2~O
;
_journal_coeditor_code           WM5611
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              677
_journal_page_last               680
_journal_paper_doi               10.1107/S205698902100551X
_journal_volume                  77
_journal_year                    2021
_chemical_formula_iupac
'[Cu (C22 H44 N4)] Br2, 2H2 O'
_chemical_formula_moiety
'C22 H44 Cu N4 2+, 2(Br -), 2(H2 O)'
_chemical_formula_sum            'C22 H48 Br2 Cu N4 O2'
_chemical_formula_weight         624.00
_chemical_name_systematic
'Diaqua(3,14-diethyl-2,6,13,17-tetraazatricyclo[16.4.0.0^7,12^]docosane)copper(II) (3,14-diethyl-2,6,13,17-tetraazatricyclo[16.4.0.0^7,12^]docosane)copper(II) tetrabromide dihydrate'
_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
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                97.02(3)
_cell_angle_beta                 92.91(3)
_cell_angle_gamma                111.31(3)
_cell_formula_units_Z            2
_cell_length_a                   8.0800(16)
_cell_length_b                   10.380(2)
_cell_length_c                   17.511(4)
_cell_measurement_reflns_used    74723
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      33.679
_cell_measurement_theta_min      0.350
_cell_volume                     1350.8(6)
_computing_cell_refinement
;
<i>HKL3000sm</i> (Otwinowski <i>et al.</i>,  2003)
;
_computing_data_collection
;
<i>PAL BL2D-SMDC</i> (Shin <i>et al.</i>,  2016)
;
_computing_data_reduction
;
<i>HKL3000sm</i> (Otwinowski <i>et al.</i>,  2003)
;
_computing_molecular_graphics
;
<i>DIAMOND 4</i> (Putz & Brandenburg, 2014)
;
_computing_publication_material
;
<i>publCIF</i> (Westrip, 2010)
;
_computing_structure_refinement
;
<i>SHELXL2018</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT2018</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      220(2)
_diffrn_measured_fraction_theta_full 0.954
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'Rayonix MX225HS CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.610
_diffrn_reflns_av_R_equivalents  0.0227
_diffrn_reflns_av_unetI/netI     0.0341
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            14201
_diffrn_reflns_theta_full        21.469
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.828
_diffrn_source                   'PLSII 2D bending magnet'
_exptl_absorpt_coefficient_mu    2.532
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.748
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
(<i>HKL3000sm Scalepack</i>; Otwinowski <i>et al.</i>,  2003)
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.534
_exptl_crystal_description       octahedron
_exptl_crystal_F_000             646
_exptl_crystal_size_max          0.075
_exptl_crystal_size_mid          0.074
_exptl_crystal_size_min          0.069
_refine_diff_density_max         0.831
_refine_diff_density_min         -1.030
_refine_ls_extinction_coef       0.013(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL-2018/3 (Sheldrick 2018)
;
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         7233
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0721
_refine_ls_R_factor_gt           0.0561
_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^)+(0.0966P)^2^+0.5261P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1655
_refine_ls_wR_factor_ref         0.1762
_reflns_number_gt                5311
_reflns_number_total             7233
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm5611sup1.cif
_cod_data_source_block           I
_cod_depositor_comments
;

2023-01-25
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C44 H96 Br4 Cu2 N8 O4'
_cod_original_formula_weight         1248.00
_cod_original_formula_moiety
'C22 H48 Cu N4 O2 2+, C22 H44 Cu N4 2+, 4(Br -), 2(H2 O)'
_cod_original_formula_iupac
'[Cu (C22 H44 N4) (H2 O)2] [Cu (C22 H44 N4)] Br4, 2H2 O'
_cod_original_formula_units_Z            1
_cod_original_cell_volume        1350.8(5)
_cod_database_code               2243844
_shelx_estimated_absorpt_t_min   0.833
_shelx_estimated_absorpt_t_max   0.845
_shelx_hkl_checksum              85368
_shelx_res_checksum              52545
_cod_database_fobs_code 2243844