Synthesis and crystal structure of two manganese-based 12-metallacrown-4 complexes: Na~2~(3-chlorobenzoate)~2~[12-MC~Mn(III)N(shi)~-4](DMF)~6~ and MnNa(3-chlorobenzoate)~3~[12-MC~Mn(III)N(shi)~-4](DMF)(H~2~O)~4~·4DMF·0.72H~2~O
Zaleski, Curtis M.; Zeller, Matthias; Acta Crystallographica Section E 76 (2020) 848–856; doi:10.1107/S2056989020006362

data_2243396
_publ_section_title
;
 Synthesis and crystal structure of two manganese-based 12-metallacrown-4
 complexes: Na~2~(3-chlorobenzoate)~2~[12-MC~Mn(III)N(shi)~-4](DMF)~6~ and
 MnNa(3-chlorobenzoate)~3~[12-MC~Mn(III)N(shi)~-4](DMF)(H~2~O)~4~&#x00B7;4DMF&#x00B7;0.72H~2~O
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              848
_journal_page_last               856
_journal_paper_doi               10.1107/S2056989020006362
_journal_volume                  76
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_iupac
;
[Mn5 Na (C7 H4 Cl1 O2)3 (C7 H4 N1 O3)4 (C3 H7 N1 O1) (H2 O1)4],
4C3 H7 N O, 0.718H2 O
;
_chemical_formula_moiety
'C52 H43 Cl3 Mn5 N5 Na O23, 4(C3 H7 N O), 0.718(H2 O)'
_chemical_formula_sum            'C64 H72.44 Cl3 Mn5 N9 Na O27.72'
_chemical_formula_weight         1815.30
_chemical_name_systematic
;Tetra-\m-aqua-tris(\m-3-chlorobenzoato)(dimethylformamide)tetrakis(\m~4~-<i>N</i>,2-dioxidobenzene-1-carboximidato)pentamanganese(III)sodium(I)
dimethylformamide tetraolvate 0.72-hydrate
;
_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                 94.235(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.1955(9)
_cell_length_b                   16.3349(11)
_cell_length_c                   16.6144(10)
_cell_measurement_reflns_used    9812
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      33.1841
_cell_measurement_theta_min      2.7569
_cell_volume                     3842.1(4)
_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, 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 0.997
_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  0.0375
_diffrn_reflns_av_unetI/netI     0.0370
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            118654
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.249
_diffrn_reflns_theta_min         2.323
_diffrn_source                   'fine focus sealed tube X-ray source'
_diffrn_source_current           '30 mA'
_diffrn_source_voltage           '50 kV'
_exptl_absorpt_coefficient_mu    0.995
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.6358
_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    1.569
_exptl_crystal_description       plate
_exptl_crystal_F_000             1856
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.818
_refine_diff_density_min         -0.691
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 10010 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   0.000(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1079
_refine_ls_number_reflns         27291
_refine_ls_number_restraints     143
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0342
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0522P)^2^+0.9214P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0863
_refine_ls_wR_factor_ref         0.0913
_reflns_number_gt                24179
_reflns_number_total             27291
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            mw2160sup1.cif
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      'P n'
_cod_database_code               2243396
_shelx_estimated_absorpt_t_min   0.663
_shelx_estimated_absorpt_t_max   0.916
_shelx_hkl_checksum              44755
_shelx_res_checksum              25163
_cod_database_fobs_code 2243396