Synthesis and crystal structure of a pentacopper(II) 12-metallacrown-4: <i>cis</i>-diaquatetrakis(dimethylformamide-κ<i>O</i>)manganese(II) tetrakis(μ~3~-<i>N</i>,2-dioxidobenzene-1-carboximidate)pentacopper(II) dimethylformamide monosolvate
Van Trieste III, Gerard P.; Zeller, Matthias; Zaleski, Curtis M.; Acta Crystallographica Section E 76 (2020) 747–751; doi:10.1107/S2056989020005770

data_2243377
_publ_section_title
;
 Synthesis and crystal structure of a pentacopper(II) 12-metallacrown-4:
 <i>cis</i>-diaquatetrakis(dimethylformamide-\k<i>O</i>)manganese(II)
 tetrakis(\m~3~-<i>N</i>,2-dioxidobenzene-1-carboximidate)pentacopper(II)
 dimethylformamide monosolvate
;
_journal_coeditor_code           YK2128
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              747
_journal_page_last               751
_journal_paper_doi               10.1107/S2056989020005770
_journal_volume                  76
_journal_year                    2020
_chemical_formula_iupac
'[Mn (C3 H7 N O)4 (H2 O)2] [Cu5 (C7 H4 N O3)4], C3 H7 N O'
_chemical_formula_moiety
'C12 H32 Mn N4 O6 2+, C28 H16 Cu5 N4 O12 2-, C3 H7 N O'
_chemical_formula_sum            'C43 H55 Cu5 Mn N9 O19'
_chemical_formula_weight         1374.60
_chemical_name_systematic
;<i>cis</i>-Diaquatetrakis(dimethylformamide-\k<i>O</i>)manganese(II)
tetrakis(\m~3~-<i>N</i>,2-dioxidobenzene-1-carboximidate)pentacopper(II) dimethylformamide monosolvate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/1
_cell_angle_alpha                90
_cell_angle_beta                 95.1476(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.0669(9)
_cell_length_b                   14.2943(6)
_cell_length_c                   19.3450(8)
_cell_measurement_reflns_used    9700
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      38.5773
_cell_measurement_theta_min      2.8382
_cell_volume                     5251.2(4)
_computing_cell_refinement
;
SAINT (Bruker, 2016)
;
_computing_data_collection
;
APEX3 (Bruker, 2016)
;
_computing_data_reduction
;
SAINT(Bruker, 2016)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>,  2020)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
<i>SHELXL2018/1</i> (Sheldrick, 2015),
<i>SHELXLE Rev859</i> (H\"ubschle <i>et al.</i>,  2011)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.961
_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  0.0432
_diffrn_reflns_av_unetI/netI     0.0526
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            87027
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         38.658
_diffrn_reflns_theta_min         2.692
_diffrn_source                   'sealed tube X-ray source'
_exptl_absorpt_coefficient_mu    2.304
_exptl_absorpt_correction_T_max  0.7476
_exptl_absorpt_correction_T_min  0.5820
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS2016/2</i>; Krause <i>et al.</i>,  2015)
;
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.739
_exptl_crystal_description       block
_exptl_crystal_F_000             2792
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.41
_exptl_crystal_size_min          0.25
_refine_diff_density_max         2.438
_refine_diff_density_min         -2.181
_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     1153
_refine_ls_number_reflns         28700
_refine_ls_number_restraints     1810
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.1115
_refine_ls_R_factor_gt           0.0648
_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^)+(0.0001P)^2^+29.7569P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1180
_refine_ls_wR_factor_ref         0.1434
_reflns_number_gt                18767
_reflns_number_total             28700
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            yk2128sup1.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2243377
_shelx_hkl_checksum              39429
_shelx_res_checksum              61074
_cod_database_fobs_code 2243377