Crystal structure of bis{μ-2-[bis(2-hydroxyethyl)amino]ethanolato}bis(μ-3,5-dimethylpyrazolato)tricopper(II) dibromide sesquihydrate
Vynohradov, Oleksandr S.; Pavlenko, Vadim A.; Naumova, Dina D.; Partsevska, Sofiia V.; Shova, Sergiu; Safarmamadov, Safarmamad M.; Acta Crystallographica Section E 76 (2020) 1641–1644; doi:10.1107/S2056989020012323

data_2243592
_publ_section_title
;
 Crystal structure of
 bis{\m-2-[bis(2-hydroxyethyl)amino]ethanolato}bis(\m-3,5-dimethylpyrazolato)tricopper(II)
 dibromide sesquihydrate
;
_journal_coeditor_code           DJ2014
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1641
_journal_page_last               1644
_journal_paper_doi               10.1107/S2056989020012323
_journal_volume                  76
_journal_year                    2020
_chemical_formula_iupac
'[Cu3 (C5 H7 N2 )2 (C6 H14 N O3 )2] Br2, 1.5H2 O'
_chemical_formula_moiety         'C22 H42 Cu3 N6 O6, 2(Br1), 1.5(H2 O)'
_chemical_formula_sum            'C22 H45 Br2 Cu3 N6 O7.5'
_chemical_formula_weight         864.08
_chemical_name_systematic
;
Bis{\m-2-[bis(2-hydroxyethyl)amino]ethanolato}-1:2\k^4^<i>O</i>,<i>O</i>',\
<i>O</i>'':<i>O</i>;2:3\k^4^<i>O</i>:<i>O</i>,<i>O</i>',<i>O</i>''-\
bis(\m-3,5-dimethylpyrazolato)-1:2\k^2^<i>N</i>^1^:<i>N</i>^2^;\
2:3<i>N</i>^1^:<i>N</i>^2^-tricopper(II) dibromide sesquihydrate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_cell_angle_alpha                90
_cell_angle_beta                 103.998(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.4930(7)
_cell_length_b                   8.8855(3)
_cell_length_c                   26.6017(11)
_cell_measurement_reflns_used    4599
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.9240
_cell_measurement_theta_min      1.5960
_cell_volume                     3324.0(2)
_computing_cell_refinement
;
CrysAlisPro (Rigaku OD, 2019)
;
_computing_data_collection
;
CrysAlisPro (Rigaku OD, 2019)
;
_computing_data_reduction
;
CrysAlisPro (Rigaku OD, 2019)
;
_computing_molecular_graphics
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
<i>SHELXL2018/3</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0797
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.865
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku Oxford Diffraction Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0243
_diffrn_reflns_av_unetI/netI     0.0317
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            10477
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.316
_diffrn_reflns_theta_min         2.424
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    4.354
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51440
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2019)
;
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.727
_exptl_crystal_description       block
_exptl_crystal_F_000             1744
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.607
_refine_diff_density_min         -0.517
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         3946
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0513
_refine_ls_R_factor_gt           0.0392
_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^)+(0.0485P)^2^+4.2091P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0976
_refine_ls_wR_factor_ref         0.1046
_reflns_number_gt                3296
_reflns_number_total             3946
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            dj2014sup1.cif
_cod_data_source_block           I
_cod_original_formula_sum        'C22 H45 Br2 Cu3 N6 O7.50'
_cod_database_code               2243592
_shelx_estimated_absorpt_t_min   0.409
_shelx_estimated_absorpt_t_max   0.561
_shelx_hkl_checksum              44842
_shelx_res_checksum              95088
_cod_database_fobs_code 2243592