Synthesis and crystal structure of a heterobimetallic nickel‒manganese 12-metallacrown-4 methanol disolvate monohydrate compound
Hall, Abigail J.; Zeller, Matthias; Zaleski, Curtis M.; Acta Crystallographica Section E 76 (2020) 1720–1724; doi:10.1107/S205698902001316X

data_2243615
_publ_section_title
;
 Synthesis and crystal structure of a heterobimetallic nickel--manganese
 12-metallacrown-4 methanol disolvate monohydrate compound
;
_journal_coeditor_code           IS5558
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1720
_journal_page_last               1724
_journal_paper_doi               10.1107/S205698902001316X
_journal_volume                  76
_journal_year                    2020
_chemical_formula_iupac
'[Mn4 Ni1 (C7 H4 N1 O3)4 (C2 H3 O2)2 (C1 H4 O1)6], 2C H4 O, H2 O'
_chemical_formula_moiety         'C38 H46 Mn4 N4 Ni O22, 2(C H4 O), H2 O'
_chemical_formula_sum            'C40 H56 Mn4 N4 Ni O25'
_chemical_formula_weight         1271.35
_chemical_name_systematic
'Di-\m-acetato-tetrakis(\m~4~-<i>N</i>,2-dioxidobenzene-1-carboximidato)hexamethanoltetramanganese(III)nickel(II) methanol disolvate monohydrate'
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                85.318(3)
_cell_angle_beta                 86.231(3)
_cell_angle_gamma                77.583(3)
_cell_formula_units_Z            1
_cell_length_a                   10.3647(7)
_cell_length_b                   10.7781(8)
_cell_length_c                   11.8303(8)
_cell_measurement_reflns_used    9780
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.5600
_cell_measurement_theta_min      2.5896
_cell_volume                     1284.79(16)
_computing_cell_refinement
;
SAINT (Bruker, 2018)
;
_computing_data_collection
;
APEX3 (Bruker, 2018)
;
_computing_data_reduction
;
SAINT (Bruker, 2018)
;
_computing_molecular_graphics
;
Mercury (Macrae et al., 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 0.996
_diffrn_measured_fraction_theta_max 0.982
_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  0.0263
_diffrn_reflns_av_unetI/netI     0.0505
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13573
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.616
_diffrn_reflns_theta_min         2.508
_diffrn_source                   'fine focus sealed tube X-ray source'
_diffrn_source_current           '30 mA'
_diffrn_source_voltage           '50 kV'
_exptl_absorpt_coefficient_mu    1.404
_exptl_absorpt_correction_T_max  0.746067
_exptl_absorpt_correction_T_min  0.615857
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS2016/2</i>; Krause <i>et al.</i>, 2015)
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.643
_exptl_crystal_description       block
_exptl_crystal_F_000             652
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.130
_refine_diff_density_max         1.791
_refine_diff_density_min         -1.016
_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     355
_refine_ls_number_reflns         7767
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0642
_refine_ls_R_factor_gt           0.0495
_refine_ls_shift/su_max          0.030
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0720P)^2^+1.2905P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1308
_refine_ls_wR_factor_ref         0.1372
_reflns_number_gt                6204
_reflns_number_total             7767
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            is5558sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        1284.78(16)
_cod_database_code               2243615
_shelx_estimated_absorpt_t_min   0.729
_shelx_estimated_absorpt_t_max   0.839
_shelx_hkl_checksum              78636
_shelx_res_checksum              33966
_cod_database_fobs_code 2243615