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_2243538
_publ_section_title
;
 Crystal structures of three anionic lanthanide--aluminium [3.3.1]
 metallacryptate complexes
;
_journal_coeditor_code           MW2167
_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 [Gd Al6 (C7 H6 N O3)2 (C7 H4 N O3)7 (C5 H5 N)1.855 (H2 O)2],
7.396C5 H5 N, H2 O
;
_chemical_formula_moiety
'C72.27 H53.28 Al6 Gd N10.86 O29, 2(C5 H6 N), 7.396(C5 H5 N), H2'
_chemical_formula_sum            'C119.25 H104.26 Al6 Gd N20.25 O30'
_chemical_formula_weight         2620.19
_chemical_name_systematic
;Bis(pyridinium)
diaquadipyridinehexakis[\m~3~-salicylhydroximato(3-)]bis[\m~2~-salicylhydroximato(1-)]hexaaluminiumgadolinium--pyridine--water (1/7.396/1)
;
_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     isomor
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                80.675(2)
_cell_angle_beta                 84.459(2)
_cell_angle_gamma                71.757(2)
_cell_formula_units_Z            2
_cell_length_a                   13.7267(10)
_cell_length_b                   16.0458(11)
_cell_length_c                   28.2591(18)
_cell_measurement_reflns_used    9126
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.6609
_cell_measurement_theta_min      2.4991
_cell_volume                     5826.3(7)
_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 0.996
_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  0.0555
_diffrn_reflns_av_unetI/netI     0.0387
_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       39
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            284595
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.626
_diffrn_reflns_theta_min         2.193
_diffrn_source                   'fine focus sealed tube X-ray source'
_diffrn_source_current           '30 mA'
_diffrn_source_voltage           '50 kV'
_exptl_absorpt_coefficient_mu    0.703
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6839
_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    1.493
_exptl_crystal_description       block
_exptl_crystal_F_000             2687.1
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.130
_refine_diff_density_max         1.444
_refine_diff_density_min         -0.983
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2119
_refine_ls_number_reflns         35792
_refine_ls_number_restraints     2173
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0766
_refine_ls_R_factor_gt           0.0543
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0552P)^2^+12.4814P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1339
_refine_ls_wR_factor_ref         0.1456
_reflns_number_gt                28478
_reflns_number_total             35792
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            mw2167sup1.cif
_cod_data_source_block           1
_cod_database_code               2243538
_shelx_estimated_absorpt_t_min   0.838
_shelx_estimated_absorpt_t_max   0.914
_shelx_hkl_checksum              54773
_shelx_res_checksum              65512
_cod_database_fobs_code 2243538