Crystal structure of diaqua(3,14-diethyl-2,6,13,17-tetraazatricyclo[16.4.0.0^7,12^]docosane)copper(II) dichloride tetrahydrate
Moon, Dohyun; Choi, Jong-Ha; Acta Crystallographica Section E 77 (2021) 569–572; doi:10.1107/S2056989021004382

data_2243820
_publ_section_title
;
 Crystal structure of
 diaqua(3,14-diethyl-2,6,13,17-tetraazatricyclo[16.4.0.0^7,12^]docosane)copper(II)
 dichloride tetrahydrate
;
_journal_coeditor_code           WM5607
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              569
_journal_page_last               572
_journal_paper_doi               10.1107/S2056989021004382
_journal_volume                  77
_journal_year                    2021
_chemical_formula_iupac          '[Cu (C22 H44 N4) (H2 O)2] Cl2, 4H2 O'
_chemical_formula_moiety         'C22 H48 Cu N4 O2 2+, 2(Cl -), 4(H2 O)'
_chemical_formula_sum            'C22 H56 Cl2 Cu N4 O6'
_chemical_formula_weight         607.14
_chemical_name_systematic
'Diaqua(3,14-diethyl-2,6,13,17-tetraazatricyclo[16.4.0.0^7,12^]docosane)copper(II) dichloride tetrahydrate'
_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                81.36(3)
_cell_angle_beta                 72.84(3)
_cell_angle_gamma                69.71(3)
_cell_formula_units_Z            1
_cell_length_a                   8.0220(16)
_cell_length_b                   10.020(2)
_cell_length_c                   10.354(2)
_cell_measurement_reflns_used    49370
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      33.679
_cell_measurement_theta_min      0.350
_cell_volume                     744.8(3)
_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</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 0.997
_diffrn_measured_fraction_theta_max 0.998
_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  0.0194
_diffrn_reflns_av_unetI/netI     0.0250
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8262
_diffrn_reflns_theta_full        21.469
_diffrn_reflns_theta_max         24.996
_diffrn_reflns_theta_min         1.769
_diffrn_source                   'PLSII 2D bending magnet'
_exptl_absorpt_coefficient_mu    0.627
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.597
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
(<i>HKL3000sm Scalepack</i>; Otwinowski <i>et al.</i>,  2003)
;
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.354
_exptl_crystal_description       plate
_exptl_crystal_F_000             327
_exptl_crystal_size_max          0.123
_exptl_crystal_size_mid          0.119
_exptl_crystal_size_min          0.043
_refine_diff_density_max         0.863
_refine_diff_density_min         -0.882
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         4141
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0390
_refine_ls_R_factor_gt           0.0386
_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^)+(0.0740P)^2^+0.2905P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1081
_refine_ls_wR_factor_ref         0.1086
_reflns_number_gt                4013
_reflns_number_total             4141
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm5607sup1.cif
_cod_data_source_block           I
_cod_database_code               2243820
_cod_database_fobs_code          2243820
_shelx_estimated_absorpt_t_min   0.927
_shelx_estimated_absorpt_t_max   0.974
_shelx_hkl_checksum              57209
_shelx_res_checksum              64621