The crystal structures of {<i>Ln</i>Cu~5~}^3+^ (<i>Ln</i> = Gd, Dy and Ho) 15-metallacrown-5 complexes and a reevaluation of the isotypic Eu^III^ analogue
Pavlishchuk, Anna; Naumova, Dina; Zeller, Matthias; Calderon Cazorla, Sebastian; Addison, Anthony W.; Acta Crystallographica Section E 75 (2019) 1215–1223; doi:10.1107/S205698901900999X

data_2243023
_publ_section_title
;
 The crystal structures of {<i>Ln</i>Cu~5~}^3+^ (<i>Ln</i> = Gd, Dy and
 Ho) 15-metallacrown-5 complexes and a reevaluation of the isotypic
 Eu^III^ analogue
;
_journal_coeditor_code           CQ2031
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1215
_journal_page_last               1223
_journal_paper_doi               10.1107/S205698901900999X
_journal_volume                  75
_journal_year                    2019
_chemical_formula_iupac
'[Cu5 Ho1 (C2 H4 N2 O2)5 (C O3) (N O3) (H2 O)5], 3.445H2 O'
_chemical_formula_moiety         'C11 H30 Cu5 Ho N11 O21, 3.445(H2 O)'
_chemical_formula_sum            'C11 H36.89 Cu5 Ho N11 O24.45'
_chemical_formula_weight         1197.21
_chemical_name_systematic
'Pentaaquacarbonatopentakis(glycine hydroxamato)nitratopentacopper(II)holmium(III) 3.445-hydrate'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     isomor
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                94.001(3)
_cell_angle_beta                 94.784(3)
_cell_angle_gamma                107.518(3)
_cell_formula_units_Z            2
_cell_length_a                   11.2027(9)
_cell_length_b                   11.4955(9)
_cell_length_c                   13.2467(10)
_cell_measurement_reflns_used    9995
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      33.2122
_cell_measurement_theta_min      2.3049
_cell_volume                     1613.0(2)
_computing_cell_refinement
;
SAINT (Bruker, 2017)
;
_computing_data_collection
;
APEX3 (Bruker, 2017)
;
_computing_data_reduction
;
SAINT (Bruker, 2017)
;
_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 10.4167
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker AXS D8 Quest CMOS'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  'Triumph curved graphite crystal'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0417
_diffrn_reflns_av_unetI/netI     0.0407
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            50443
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.243
_diffrn_reflns_theta_min         2.544
_diffrn_source                   'fine focus sealed tube X-ray source'
_diffrn_source_current           30
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    5.773
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.5475
_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    2.467
_exptl_crystal_description       prism
_exptl_crystal_F_000             1174.9
_exptl_crystal_size_max          0.440
_exptl_crystal_size_mid          0.420
_exptl_crystal_size_min          0.280
_refine_diff_density_max         2.801
_refine_diff_density_min         -2.274
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     563
_refine_ls_number_reflns         12306
_refine_ls_number_restraints     139
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0334
_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^)+(0.0289P)^2^+5.8810P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0769
_refine_ls_wR_factor_ref         0.0824
_reflns_number_gt                10012
_reflns_number_total             12306
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cq2031sup1.cif
_cod_data_source_block           Complex_3
_cod_database_code               2243023
_shelx_estimated_absorpt_t_min   0.186
_shelx_estimated_absorpt_t_max   0.295
_shelx_hkl_checksum              32662
_shelx_res_checksum              63929
_cod_database_fobs_code 2243023