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_2243021
_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 Gd (C2 H4 N2 O2)5 (C O3) (N O3) (H2 O)5], 3.5H2 O'
_chemical_formula_moiety         'C11 H30 Cu5 Gd N11 O21, 3.5(H2 O)'
_chemical_formula_sum            'C11 H37 Cu5 Gd N11 O24.5'
_chemical_formula_weight         1190.49
_chemical_name_systematic
'Pentaaquacarbonatopentakis(glycine hydroxamato)nitratopentacopper(II)gadolinium(III) 3.5-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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                94.026(4)
_cell_angle_beta                 94.942(3)
_cell_angle_gamma                107.558(3)
_cell_formula_units_Z            2
_cell_length_a                   11.2057(15)
_cell_length_b                   11.5054(15)
_cell_length_c                   13.2983(10)
_cell_measurement_reflns_used    9949
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.4891
_cell_measurement_theta_min      3.0639
_cell_volume                     1620.2(3)
_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_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_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  0.0560
_diffrn_reflns_av_unetI/netI     0.0396
_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       -19
_diffrn_reflns_number            118155
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.234
_diffrn_reflns_theta_min         3.091
_diffrn_source                   'sealed tube X-ray source'
_exptl_absorpt_coefficient_mu    5.353
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.5988
_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    2.440
_exptl_crystal_description       rod
_exptl_crystal_F_000             1170
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         2.059
_refine_diff_density_min         -1.396
_refine_ls_extinction_coef       0.00141(15)
_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 2015)
;
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     570
_refine_ls_number_reflns         12399
_refine_ls_number_restraints     135
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0594
_refine_ls_R_factor_gt           0.0343
_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^)+(0.0346P)^2^+2.5135P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0681
_refine_ls_wR_factor_ref         0.0762
_reflns_number_gt                9545
_reflns_number_total             12399
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cq2031sup1.cif
_cod_data_source_block           Complex_1
_cod_original_formula_sum        'C11 H37 Cu5 Gd N11 O24.50'
_cod_database_code               2243021
_shelx_estimated_absorpt_t_min   0.501
_shelx_estimated_absorpt_t_max   0.776
_shelx_hkl_checksum              91577
_shelx_res_checksum              94263
_cod_database_fobs_code 2243021