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_2243395
_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_coeditor_code           MW2160
_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_formula_iupac
'[Mn4 Na2 (C7 H4 Cl O2)2 (C7 H4 N O3)4 (C3 H7 N O)6]'
_chemical_formula_moiety
'C59.23 H64.21 Cl2 Mn4 N9.74 Na2 O21.74, 0.258(C3H7 N O)'
_chemical_formula_sum            'C60 H66.01 Cl2 Mn4 N10 Na2 O22'
_chemical_formula_weight         1615.99
_chemical_name_systematic
Bis(\m-3-chlorobenzoato)hexakis(dimethylformamide)tetrakis(\m~4~-<i>N</i>,2-dioxidobenzene-1-carboximidato)tetramanganese(III)disodium(I)
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
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_atom_sites_solution_secondary   difmap
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_cell_angle_alpha                102.839(3)
_cell_angle_beta                 111.628(3)
_cell_angle_gamma                90.722(4)
_cell_formula_units_Z            1
_cell_length_a                   12.0423(8)
_cell_length_b                   12.3722(8)
_cell_length_c                   12.6875(9)
_cell_measurement_reflns_used    9922
_cell_measurement_temperature    150(2)
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_cell_measurement_theta_min      5.6966
_cell_volume                     1704.0(2)
_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)
;
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;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
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<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 7.4074
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.918
_diffrn_measurement_device_type
;
Bruker AXS D8 Quest CMOS diffractometer with PhotonII charge-integrating pixel
array detector (CPAD)
;
_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  0.0475
_diffrn_reflns_av_unetI/netI     0.0458
_diffrn_reflns_limit_h_max       13
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_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            22753
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_diffrn_reflns_theta_max         80.764
_diffrn_reflns_theta_min         5.130
_diffrn_source                   'I-mu-S microsource X-ray tube'
_diffrn_source_current           '1.0 mA'
_diffrn_source_voltage           '50 kV'
_exptl_absorpt_coefficient_mu    7.454
_exptl_absorpt_correction_T_max  0.7543
_exptl_absorpt_correction_T_min  0.5276
_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    1.575
_exptl_crystal_description       plate
_exptl_crystal_F_000             828
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.491
_refine_diff_density_min         -0.571
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     999
_refine_ls_number_reflns         6871
_refine_ls_number_restraints     2038
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0542
_refine_ls_R_factor_gt           0.0450
_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^)+(0.0687P)^2^+0.5540P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1233
_refine_ls_wR_factor_ref         0.1284
_reflns_number_gt                5590
_reflns_number_total             6871
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            mw2160sup1.cif
_cod_data_source_block           1
_cod_database_code               2243395
_shelx_estimated_absorpt_t_min   0.347
_shelx_estimated_absorpt_t_max   0.755
_shelx_hkl_checksum              39683
_shelx_res_checksum              61481
_cod_database_fobs_code 2243395