Crystal structure of a Tb^III^–Cu^II^ glycinehydroxamate 15-metallacrown-5 sulfate complex
Pavlishchuk, Anna V.; Vasylenko, Inna V.; Zeller, Matthias; Addison, Anthony W.; Acta Crystallographica Section E 77 (2021) 1197–1202; doi:10.1107/S2056989021011907

data_2243985
_publ_section_title
;
 Crystal structure of a Tb^III^--Cu^II^ glycinehydroxamate
 15-metallacrown-5 sulfate complex
;
_journal_coeditor_code           YY2004
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1197
_journal_page_last               1202
_journal_paper_doi               10.1107/S2056989021011907
_journal_volume                  77
_journal_year                    2021
_chemical_formula_iupac
'[Tb Cu5 (C2 H4 N2 O2)5 (S O4) (H2 O)6.5]2 (S O4), 6H2 O'
_chemical_formula_moiety
'2(C10 H33 Cu5 N10 O20.50 S Tb +), O4 S 2-, 6(H2 O)'
_chemical_formula_sum            'C20 H78 Cu10 N20 O51 S3 Tb2'
_chemical_formula_weight         2464.44
_chemical_name_systematic
'Bis[hexaaquahemiaquapentakis(\m~3~-glycinehydroxamato)sulfatopentacopper(II)terbium(III)] sulfate hexahydrate'
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                99.6716(13)
_cell_angle_beta                 91.3031(12)
_cell_angle_gamma                105.3123(12)
_cell_formula_units_Z            1
_cell_length_a                   9.6370(4)
_cell_length_b                   11.5888(5)
_cell_length_c                   16.2367(6)
_cell_measurement_reflns_used    9965
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      79.9275
_cell_measurement_theta_min      4.0210
_cell_volume                     1719.81(12)
_computing_cell_refinement
;
SAINT (Bruker, 2018)
;
_computing_data_collection
;
APEX3 (Bruker, 2018)
;
_computing_data_reduction
;
SAINT (Bruker, 2018)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
<i>SHELXL2018/3</i> (Sheldrick, 2015),
<i>shelXle</i>  (H\"ubschle <i>et al.</i>,  2011)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 7.4074
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.933
_diffrn_measurement_device_type
;
Bruker AXS D8 Quest CMOS diffractometer with PhotonII charge-integrating pixel
array detector (CPAD)
;
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  'laterally graded multilayer (Goebel) mirror'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0498
_diffrn_reflns_av_unetI/netI     0.0617
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16278
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         80.280
_diffrn_reflns_theta_min         2.768
_diffrn_source                   'I-mu-S microsource X-ray tube'
_diffrn_source_current           '1.0 mA'
_diffrn_source_voltage           '50 kV'
_exptl_absorpt_coefficient_mu    15.108
_exptl_absorpt_correction_T_max  0.7543
_exptl_absorpt_correction_T_min  0.4537
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>,  2015
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.380
_exptl_crystal_description       plate
_exptl_crystal_F_000             1214
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.080
_refine_diff_density_max         1.590
_refine_diff_density_min         -1.342
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     562
_refine_ls_number_reflns         7029
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0414
_refine_ls_R_factor_gt           0.0406
_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^)+(0.0656P)^2^+1.8351P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1167
_refine_ls_wR_factor_ref         0.1175
_reflns_number_gt                6786
_reflns_number_total             7029
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            yy2004sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        1719.80(12)
_cod_database_code               2243985
_shelx_estimated_absorpt_t_min   0.152
_shelx_estimated_absorpt_t_max   0.378
_shelx_hkl_checksum              84841
_shelx_res_checksum              62354
_cod_database_fobs_code 2243985