Crystal structure of tetraaqua(dimethylformamide)tetrakis(μ-<i>N</i>,2-dioxidobenzene-1-carboximidato)tetrakis(μ-trimethylacetato)tetramanganese(III)sodiumyttrium‒dimethylformamide‒water (1/8.04/0.62)
Travis, Jordan R.; Zeller, Matthias; Zaleski, Curtis M.; Acta Crystallographica Section E 71 (2015) 1300–1306; doi:10.1107/S2056989015018216

data_2241197
_publ_section_title
;
 Crystal structure of
 tetraaqua(dimethylformamide)tetrakis(\m-<i>N</i>,2-dioxidobenzene-1-carboximidato)tetrakis(\m-trimethylacetato)tetramanganese(III)sodiumyttrium--dimethylformamide--water
 (1/8.04/0.62)
;
_journal_coeditor_code           BG2568
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1300
_journal_page_last               1306
_journal_paper_doi               10.1107/S2056989015018216
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac
;
[Y Na Mn4 (C7 H4 N O3)4 (C5 H9 O2)4 (C3 H7 N O)\
0.24 (H2 O)3.76], 8.04C3 H7 N O, 0.62H2 O
;
_chemical_formula_moiety
'C48.73 H61.21 Mn4 N4.24 Na O24 Y, 8.043(C3 H7 N O), 0.618(H2 O)'
_chemical_formula_sum            'C72.85 H118.75 Mn4 N12.29 Na O32.66 Y'
_chemical_formula_weight         2021.04
_chemical_name_systematic
'Tetraaqua(dimethylformamide)tetrakis(\m-<i>N</i>,2-dioxidobenzene-1-carboximidato)tetrakis(\m-trimethylacetato)tetramanganese(III)sodiumyttrium--dimethylformamide--water (1/8.04/0.62)'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                83.488(3)
_cell_angle_beta                 82.499(3)
_cell_angle_gamma                72.805(3)
_cell_formula_units_Z            2
_cell_length_a                   14.8659(9)
_cell_length_b                   17.3261(10)
_cell_length_c                   19.2709(11)
_cell_measurement_reflns_used    9921
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.8161
_cell_measurement_theta_min      2.6780
_cell_volume                     4686.4(5)
_computing_cell_refinement
;
SAINT (Bruker, 2014)
;
_computing_data_collection
;
APEX2 (Bruker, 2014)
;
_computing_data_reduction
;
SAINT (Bruker, 2014)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>,  2006)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2008) and
<i>SHELXLE Rev714</i> (H\"ubschle <i>et al.</i>,  2011)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker X8 Prospector CCD'
_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  0.0446
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            59383
_diffrn_reflns_theta_full        66.852
_diffrn_reflns_theta_max         66.852
_diffrn_reflns_theta_min         2.320
_exptl_absorpt_coefficient_mu    5.826
_exptl_absorpt_correction_T_max  0.7529
_exptl_absorpt_correction_T_min  0.5716
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2014)
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.432
_exptl_crystal_description       plate
_exptl_crystal_F_000             2106.3
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.727
_refine_diff_density_min         -0.577
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1537
_refine_ls_number_reflns         16375
_refine_ls_number_restraints     1505
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0578
_refine_ls_R_factor_gt           0.0525
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0737P)^2^+11.1250P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1384
_refine_ls_wR_factor_ref         0.1421
_reflns_number_gt                14639
_reflns_number_total             16375
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            bg2568sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        4686.5(5)
_cod_database_code               2241197
_shelx_estimated_absorpt_t_min   0.475
_shelx_estimated_absorpt_t_max   0.593
_shelx_hkl_checksum              33743
_shelx_res_checksum              58420
_cod_database_fobs_code 2241197