Crystal structure of di-μ-chloroacetato-hexakis(dimethylformamide)tetrakis(μ-<i>N</i>,2-dioxidobenzene-1-carboximidato)tetramanganese(III)disodium dimethylformamide disolvate
Daly, Connor I.; Zeller, Matthias; Zaleski, Curtis M.; Acta Crystallographica Section E 70 (2014) 494–498; doi:10.1107/S1600536814024441

data_2240200
_publ_section_title
;
 Crystal structure of
 di-\m-chloroacetato-hexakis(dimethylformamide)tetrakis(\m-<i>N</i>,2-dioxidobenzene-1-carboximidato)tetramanganese(III)disodium
 dimethylformamide disolvate
;
_journal_coeditor_code           PK2534
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              494
_journal_page_last               498
_journal_paper_doi               10.1107/S1600536814024441
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac
'[Na2 Mn4 (C2 H2 Cl O2)2 (C7 H4 N O3)4 (C3 H7 N O)6], 2C3 H7 N O'
_chemical_formula_moiety         'C50 H62 Cl2 Mn4 N10 Na2 O22, 2(C3 H7 N O)'
_chemical_formula_sum            'C56 H76 Cl2 Mn4 N12 Na2 O24'
_chemical_formula_weight         1637.92
_chemical_name_systematic
;Di-\m-chloroacetato-hexakis(dimethylformamide)tetrakis(\m-<i>N</i>,2-dioxidobenzene-1-carboximidato)tetramanganese(III)disodium
dimethylformamide disolvate
;
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                90
_cell_angle_beta                 101.8584(17)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.4457(7)
_cell_length_b                   14.7091(6)
_cell_length_c                   16.5663(8)
_cell_measurement_reflns_used    9986
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.5461
_cell_measurement_theta_min      2.5130
_cell_volume                     3444.9(3)
_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
;
SHELXL2013 (Sheldrick, 2008) and
<i>SHELXLE</i> (H\"ubschle <i>et al.</i>,  2011)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker AXS D8 Quest CMOS'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'laterally graded multilayer (Goebel) mirror'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0296
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            39712
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.571
_diffrn_reflns_theta_min         2.197
_exptl_absorpt_coefficient_mu    0.893
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.6449
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2014)
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.579
_exptl_crystal_description       block
_exptl_crystal_F_000             1688
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.210
_refine_diff_density_max         0.854
_refine_diff_density_min         -0.453
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     791
_refine_ls_number_reflns         12392
_refine_ls_number_restraints     748
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0654
_refine_ls_R_factor_gt           0.0462
_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^)+(0.0286P)^2^+3.6909P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0941
_refine_ls_wR_factor_ref         0.1015
_reflns_number_gt                9900
_reflns_number_total             12392
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            pk2534sup1.cf
_cod_data_source_block           I
_cod_database_code               2240200
_cod_database_fobs_code          2240200
_shelx_estimated_absorpt_t_min   0.763
_shelx_estimated_absorpt_t_max   0.835
_shelx_hkl_checksum              89789
_shelx_res_checksum              83977
_shelxl_version_number           .000002012