Crystal structure of a heterotrimetallic 12-metallacrown-4 with 2-propylvalerate anion bridges
Aziz, Ozha A.; Zeller, Matthias; Zaleski, Curtis M.; Acta Crystallographica Section E 78 (2022) –; doi:10.1107/S2056989022010489

data_2244213
_publ_section_title
;
 Crystal structure of a heterotrimetallic 12-metallacrown-4 with
 2-propylvalerate anion bridges
;
_journal_coeditor_code           EX2062
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2056989022010489
_journal_volume                  78
_journal_year                    2022
_chemical_formula_iupac
'[Dy Mn4 Na (C7 H4 N O3)4 (C8 H15 O2)4 (H2 O1)4], 4C3 H7 N O'
_chemical_formula_moiety
'C34.72 H29.83 Dy Mn4 N4 Na O24, 3.612(C7 H15), 4(C3 H7 N O)'
_chemical_formula_sum            'C72 H112 Dy Mn4 N8 Na O28'
_chemical_formula_weight         1942.94
_chemical_name_systematic
'Tetraaquatetrakis(\m-2-propylvalerato)tetrakis(\m~4~-salicylhydroximato)dysprosiumtetramanganesesodium dimethylformamide tetrasolvate,'
_space_group_crystal_system      tetragonal
_space_group_IT_number           85
_space_group_name_Hall           '-P 4a'
_space_group_name_H-M_alt        'P 4/n :2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   18.2654(9)
_cell_length_b                   18.2654(9)
_cell_length_c                   13.4219(9)
_cell_measurement_reflns_used    9870
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.0081
_cell_measurement_theta_min      2.4956
_cell_volume                     4477.9(4)
_computing_cell_refinement
;
SAINT (Bruker, 2022)
;
_computing_data_collection
;
APEX4 (Bruker, 2022)
;
_computing_data_reduction
;
SAINT (Bruker, 2022)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>,  2020)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
<i>SHELXL2018/3</i> (Sheldrick, 2015b),
<i>ShelXle</i> (H\"ubschle <i>et al.</i>,  2011)
;
_computing_structure_solution    'SHELXT (Sheldrick, 2015a)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 7.4074
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'three circle diffractometer'
_diffrn_measurement_device_type  'Bruker AXS D8 Quest'
_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  0.0699
_diffrn_reflns_av_unetI/netI     0.0433
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            87812
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.076
_diffrn_reflns_theta_min         2.188
_diffrn_source                   'fine focus sealed tube X-ray source'
_diffrn_source_current           '30 mA'
_diffrn_source_voltage           '50 kV'
_exptl_absorpt_coefficient_mu    1.454
_exptl_absorpt_correction_T_max  0.0596
_exptl_absorpt_correction_T_min  0.0195
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>,  2015)
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_description       plate
_exptl_crystal_F_000             2002.2
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.430
_exptl_crystal_size_min          0.150
_refine_diff_density_max         1.360
_refine_diff_density_min         -1.962
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     708
_refine_ls_number_reflns         7801
_refine_ls_number_restraints     2628
_refine_ls_restrained_S_all      0.949
_refine_ls_R_factor_all          0.1023
_refine_ls_R_factor_gt           0.0722
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1326P)^2^+7.8338P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2125
_refine_ls_wR_factor_ref         0.2571
_reflns_number_gt                5435
_reflns_number_total             7801
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ex2062sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        4477.9(5)
_cod_original_sg_symbol_H-M      'P 4/n'
_cod_database_code               2244213
_shelx_estimated_absorpt_t_min   0.561
_shelx_estimated_absorpt_t_max   0.811
_shelx_hkl_checksum              45278
_shelx_res_checksum              3190
_cod_database_fobs_code 2244213