Crystal structures of three anionic lanthanide‒aluminium [3.3.1] metallacryptate complexes
Rheam, Rachel E.; Zeller, Matthias; Zaleski, Curtis M.; Acta Crystallographica Section E 76 (2020) 1458–1466; doi:10.1107/S2056989020010725

data_2243539
_publ_section_title
;
 Crystal structures of three anionic lanthanide--aluminium [3.3.1]
 metallacryptate complexes
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1458
_journal_page_last               1466
_journal_paper_doi               10.1107/S2056989020010725
_journal_volume                  76
_journal_year                    2020
_chemical_formula_iupac
;
(C5 H6 N)2 [Dy Al6 (C7 H6 N O3)2 (C7 H4 N O3)7 (C5 H5 N)1.855 (H2 O)2],
7.429C5 H5 N, H2 O
;
_chemical_formula_moiety
'C72.45 H53.45 Al6 Dy N10.89 O29, 2(C5 H6 N), 7.429(C5 H5 N), H2'
_chemical_formula_sum            'C119.6 H104.6 Al6 Dy N20.32 O30'
_chemical_formula_weight         2630.90
_chemical_name_systematic
;Bis(pyridinium)
diaquadipyridinehexakis[\m~3~-salicylhydroximato(3-)]bis[\m~2~-salicylhydroximato(1-)]hexaaluminiumdysprosium--pyridine--water (1/7.429/1)
;
_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                80.632(2)
_cell_angle_beta                 83.989(2)
_cell_angle_gamma                71.660(2)
_cell_formula_units_Z            2
_cell_length_a                   13.7232(6)
_cell_length_b                   16.0871(7)
_cell_length_c                   28.2946(13)
_cell_measurement_reflns_used    9221
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.8266
_cell_measurement_theta_min      2.4349
_cell_volume                     5840.6(5)
_computing_cell_refinement
;
SAINT (Bruker, 2018)
;
_computing_data_collection
;
APEX3  (Bruker, 2018)
;
_computing_data_reduction
;
SAINT (Bruker, 2018)
;
_computing_molecular_graphics
;
Mercury (Macrae et al., 2020)
;
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker AXS D8 Quest CMOS diffractometer'
_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  0.0448
_diffrn_reflns_av_unetI/netI     0.0327
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            209417
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.508
_diffrn_reflns_theta_min         2.192
_diffrn_source                   'fine focus sealed tube X-ray source'
_diffrn_source_current           '30 mA'
_diffrn_source_voltage           '50 kV'
_exptl_absorpt_coefficient_mu    0.773
_exptl_absorpt_correction_T_max  0.2694
_exptl_absorpt_correction_T_min  0.2249
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>,  2015)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_description       block
_exptl_crystal_F_000             2696.9
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.323
_refine_diff_density_min         -1.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2107
_refine_ls_number_reflns         35615
_refine_ls_number_restraints     2161
_refine_ls_restrained_S_all      1.122
_refine_ls_R_factor_all          0.0572
_refine_ls_R_factor_gt           0.0478
_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^)+(0.0312P)^2^+11.5040P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1117
_refine_ls_wR_factor_ref         0.1158
_reflns_number_gt                31175
_reflns_number_total             35615
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            mw2167sup1.cif
_cod_data_source_block           2
_cod_original_formula_sum        'C119.60 H104.60 Al6 Dy N20.32 O30'
_cod_database_code               2243539
_shelx_estimated_absorpt_t_min   0.854
_shelx_estimated_absorpt_t_max   0.927
_shelx_hkl_checksum              13729
_shelx_res_checksum              7538
_cod_database_fobs_code 2243539