Crystal structures of two dysprosium‒aluminium‒sodium [3.3.1] metallacryptates that form two-dimensional sheets
Travis, Jordan R.; Van Trieste III, Gerard P.; Zeller, Matthias; Zaleski, Curtis M.; Acta Crystallographica Section E 76 (2020) 1378–1390; doi:10.1107/S2056989020010130

data_2243518
_publ_section_title
;
 Crystal structures of two dysprosium--aluminium--sodium [3.3.1]
 metallacryptates that form two-dimensional sheets
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1378
_journal_page_last               1390
_journal_paper_doi               10.1107/S2056989020010130
_journal_volume                  76
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_iupac
;
[Dy2 Al12 Na10 (C7 H5 N O3)4 (C7 H4 N O3)14 (C2 H3 O2)2 (C3 H7 N O)17],
6.335C3 H7 N O
;
_chemical_formula_moiety
'C181 H201 Al12 Dy2 N35 Na10 O75, 6.335(C3 H7 N O)[+ solvent]'
_chemical_formula_sum            'C200.01 H245.35 Al12 Dy2 N41.34 Na10 O81.34'
_chemical_formula_weight         5408.50
_chemical_name_systematic
;Poly[[di-\m~4~-acetato-nonakis(\m-<i>N</i>,<i>N</i>-dimethylformamide)octakis(<i>N</i>,<i>N</i>-dimethylformamide)tetrakis[salicylhydroximato(2-)]tetradecakis[salicylhydroximato(3-)]dodecaaluminium(III)didysprosium(III)decasodium(I)]
<i>N</i>,<i>N</i>-dimethylformamide 6.335-solvate]
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yc'
_space_group_name_H-M_alt        'P 1 c 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                90
_cell_angle_beta                 106.461(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   28.1847(14)
_cell_length_b                   15.3683(8)
_cell_length_c                   30.7354(16)
_cell_measurement_reflns_used    9892
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.6949
_cell_measurement_theta_min      2.8716
_cell_volume                     12767.4(11)
_computing_cell_refinement
;
SAINT (Bruker, 2014)
;
_computing_data_collection
;
APEX2 (Bruker, 2014)
;
_computing_data_reduction
;
SAINT (Bruker, 2014)
;
_computing_molecular_graphics    'Mercury (Macrae et al., 20<0)'
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015),
<i>shelXle</i> (H\"ubschle <i>et al.</i>,  2011)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008a)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker X8 Prospector CCD'
_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  0.0500
_diffrn_reflns_av_unetI/netI     0.0710
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            154195
_diffrn_reflns_theta_full        66.854
_diffrn_reflns_theta_max         66.854
_diffrn_reflns_theta_min         2.875
_diffrn_source                   'I-mu-S microsource X-ray tube'
_exptl_absorpt_coefficient_mu    4.440
_exptl_absorpt_correction_T_max  0.7529
_exptl_absorpt_correction_T_min  0.4880
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2014)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_description       block
_exptl_crystal_F_000             5567
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.190
_refine_diff_density_max         2.278
_refine_diff_density_min         -1.568
_refine_ls_abs_structure_details
;
 Refined as an inversion twin
;
_refine_ls_abs_structure_Flack   0.097(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3599
_refine_ls_number_reflns         38274
_refine_ls_number_restraints     4954
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0557
_refine_ls_R_factor_gt           0.0527
_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^)+(0.0820P)^2^+21.8730P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1351
_refine_ls_wR_factor_ref         0.1374
_reflns_number_gt                36111
_reflns_number_total             38274
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            pk2639sup1.cif
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      'P c'
_cod_database_code               2243518
_shelx_estimated_absorpt_t_min   0.403
_shelx_estimated_absorpt_t_max   0.486
_shelx_hkl_checksum              46491
_shelx_res_checksum              1787
_shelx_fab_checksum              53271
_cod_database_fobs_code 2243518