Crystal structures of two heterotrimetallic dysprosium‒manganese‒sodium 12-metallacrown-4 complexes with the bridging ligands 3-hydroxybenzoate and 4-hydroxybenzoate
Manickas, Elizabeth C.; Zeller, Matthias; Zaleski, Curtis M.; Acta Crystallographica Section E 76 (2020) 1213–1221; doi:10.1107/S2056989020008853

data_2243479
_publ_section_title
;
 Crystal structures of two heterotrimetallic dysprosium--manganese--sodium
 12-metallacrown-4 complexes with the bridging ligands 3-hydroxybenzoate
 and 4-hydroxybenzoate
;
_journal_coeditor_code           PK2637
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1213
_journal_page_last               1221
_journal_paper_doi               10.1107/S2056989020008853
_journal_volume                  76
_journal_year                    2020
_chemical_formula_iupac
'[Dy Mn4 Na (C7 H5 O3)4 (C7 H4 N O2)4 (H2 O)4], 4C3 H7 N O'
_chemical_formula_moiety         'C56 H44 Dy Mn4 N4 Na O28, 4(C3 H7 N O)'
_chemical_formula_sum            'C68 H72 Dy Mn4 N8 Na O32'
_chemical_formula_weight         1918.58
_chemical_name_systematic
;Tetra-\m-aqua-tetrakis{2-[azanidylene(oxido)methyl]phenolato}tetrakis(\m~2~-3-hydroxybenzoato)dysprosium(III)tetramanganese(III)sodium(I)
<i>N</i>,<i>N</i>-dimethylformamide tetrasolvate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yac'
_space_group_name_H-M_alt        'P 1 n 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                 92.347(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.3622(11)
_cell_length_b                   16.5258(11)
_cell_length_c                   16.8246(12)
_cell_measurement_reflns_used    9804
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      34.6325
_cell_measurement_theta_min      2.8387
_cell_volume                     3989.9(5)
_computing_cell_refinement
;
SAINT (Bruker, 2018)
;
_computing_data_collection
;
APEX3 (Bruker, 2018)
;
_computing_data_reduction
;
SAINT (Bruker, 2018)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>,  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, 2008a)
;
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.975
_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  0.084
_diffrn_reflns_av_unetI/netI     0.0960
_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       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            40158
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.282
_diffrn_reflns_theta_min         2.845
_diffrn_source                   'sealed tube X-ray source'
_exptl_absorpt_coefficient_mu    1.635
_exptl_absorpt_correction_T_max  0.109305
_exptl_absorpt_correction_T_min  0.052982
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>TWINABS</i>; Sheldrick, 2012)
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.597
_exptl_crystal_description       prism
_exptl_crystal_F_000             1938
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.190
_refine_diff_density_max         1.860
_refine_diff_density_min         -1.826
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 5372 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   -0.025(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1433
_refine_ls_number_reflns         40158
_refine_ls_number_restraints     1908
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.1100
_refine_ls_R_factor_gt           0.0733
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1018P)^2^+15.3803P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1916
_refine_ls_wR_factor_ref         0.2190
_reflns_number_gt                29137
_reflns_number_total             40158
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            pk2637sup1.cif
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      'P n'
_cod_database_code               2243479
_shelx_estimated_absorpt_t_min   0.640
_shelx_estimated_absorpt_t_max   0.746
_shelx_hkl_checksum              54288
_shelx_res_checksum              94878
_cod_database_fobs_code 2243479