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_2243517
_publ_section_title
;
 Crystal structures of two dysprosium--aluminium--sodium [3.3.1]
 metallacryptates that form two-dimensional sheets
;
_journal_coeditor_code           PK2639
_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_formula_iupac
;
[Dy Al6 Na5 (C7 H5 N O3)2 (C7 H4 N O3)7 (C2 H3 O2) (C3 H7 N O)8], 4C3 H7 N O,
H2 O
;
_chemical_formula_moiety
'C89 H97 Al6 Dy N17 Na5 O37, 4(C3 H7 N O), O H2'
_chemical_formula_sum            'C101 H127 Al6 Dy N21 Na5 O42'
_chemical_formula_weight         2746.57
_chemical_name_systematic
;Poly[[\m~3~-acetato-hexakis(\m-<i>N</i>,<i>N</i>-dimethylformamide)bis(<i>N</i>,<i>N</i>-dimethylformamide)bis[salicylhydroximato(2-)]heptakis[salicylhydroximato(3-)]hexaaluminium(III)dysprosium(III)pentasodium(I)] <i>N</i>,<i>N</i>-dimethylformamide tetrasolvate
monohydrate]
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 101.590(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.6809(13)
_cell_length_b                   20.5788(11)
_cell_length_c                   27.6206(16)
_cell_measurement_reflns_used    9947
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.3630
_cell_measurement_theta_min      2.9214
_cell_volume                     12628.9(12)
_computing_cell_refinement
;
SAINT (Bruker, 2014)
;
_computing_data_collection
;
APEX2 (Bruker, 2014)
;
_computing_data_reduction
;
SAINT (Bruker, 2014)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>,  2020)
;
_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 0.973
_diffrn_measured_fraction_theta_max 0.715
_diffrn_measurement_device_type  'Bruker D8 Quest CMOS'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  'laterally graded multilayer (Goebel) mirror'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.071
_diffrn_reflns_av_unetI/netI     0.0907
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            40899
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.655
_diffrn_reflns_theta_min         2.467
_diffrn_source                   'I-mu-S microsource X-ray tube'
_exptl_absorpt_coefficient_mu    0.740
_exptl_absorpt_correction_T_max  0.746246
_exptl_absorpt_correction_T_min  0.628084
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2014)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.445
_exptl_crystal_description       block
_exptl_crystal_F_000             5660
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.140
_refine_diff_density_max         1.375
_refine_diff_density_min         -2.042
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 7452 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   0.026(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1634
_refine_ls_number_reflns         40899
_refine_ls_number_restraints     393
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0718
_refine_ls_R_factor_gt           0.0561
_refine_ls_shift/su_max          0.034
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0559P)^2^+94.4342P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1463
_refine_ls_wR_factor_ref         0.1588
_reflns_number_gt                36071
_reflns_number_total             40899
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            pk2639sup1.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               2243517
_shelx_estimated_absorpt_t_min   0.897
_shelx_estimated_absorpt_t_max   0.903
_shelx_hkl_checksum              3397
_shelx_res_checksum              60004
_shelx_fab_checksum              46940
_cod_database_fobs_code 2243517