#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/47/2214777.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2214777
loop_
_publ_author_name
'Stadie, Nicholas P.'
'Sanchez-Smith, Rebeca'
'Groy, Thomas L.'
_publ_section_title
;Di-μ-acetato-κ⁴O:O'-μ-oxido-κ²O:O-bis[(acetic
 acid-κO)bis(1H-imidazole-κN³)magnesium(II)]
;
_journal_coeditor_code           LH2433
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2153
_journal_page_last               m2154
_journal_paper_doi               10.1107/S1600536807033818
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[Mg2 (C2 H3 O2)2 O (C3 H4 N2)4 (C2 H4 O2)2]'
_chemical_formula_moiety         'C20 H30 Mg2 N8 O9'
_chemical_formula_sum            'C20 H30 Mg2 N8 O9'
_chemical_formula_weight         575.14
_chemical_name_systematic
;
Di-μ-acetato-κ⁴O:O'-μ-oxido-κ²O:O-bis[(acetic
acid-\kO)bis(1H-imidazole-\kN³)magnesium(II)]
;
_space_group_IT_number           41
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'A 2 -2ab'
_symmetry_space_group_name_H-M   'A b a 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.6927(14)
_cell_length_b                   19.106(3)
_cell_length_c                   16.834(3)
_cell_measurement_reflns_used    1685
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      22.2
_cell_measurement_theta_min      2.4
_cell_volume                     2795.8(8)
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_collection       'SMART (Bruker, 2003)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL (Bruker, 2001)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART APEX'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1118
_diffrn_reflns_av_sigmaI/netI    0.0564
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            10414
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.13
_diffrn_standards_decay_%        0.00
_exptl_absorpt_coefficient_mu    0.147
_exptl_absorpt_correction_T_max  0.994
_exptl_absorpt_correction_T_min  0.986
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2004)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.366
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1208
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.242
_refine_diff_density_min         -0.247
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.167
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         1287
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.166
_refine_ls_R_factor_all          0.0934
_refine_ls_R_factor_gt           0.0705
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0579P)²+3.9683P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1379
_refine_ls_wR_factor_ref         0.1469
_reflns_number_gt                1034
_reflns_number_total             1287
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            lh2433.cif
_cod_data_source_block           I
_cod_original_sg_symbol_Hall     'A 2 -2ac'
_cod_database_code               2214777
_cod_database_fobs_code          2214777
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'x+1/2, -y+1, z+1/2'
'-x+1/2, y+1, z+1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
Mg Mg1 0.3999(3) 0.08395(10) 0.18240(17) 0.0326(6) Uani d . 1
O O1A 0.5000 0.0000 0.2501(4) 0.0333(17) Uani d S 1
O O2A 0.2900(6) 0.0160(2) 0.1101(4) 0.0469(15) Uani d . 1
C C2B 0.3038(8) -0.0453(3) 0.0872(4) 0.0298(16) Uani d . 1
O O2C 0.4045(6) -0.0881(2) 0.1118(4) 0.0438(14) Uani d . 1
C C2D 0.1915(12) -0.0706(4) 0.0281(7) 0.073(3) Uani d . 1
H H2D1 0.1459 -0.1134 0.0466 0.109 Uiso calc R 1
H H2D2 0.2429 -0.0789 -0.0215 0.109 Uiso calc R 1
H H2D3 0.1128 -0.0360 0.0207 0.109 Uiso calc R 1
O O3A 0.5018(6) 0.1576(2) 0.2544(3) 0.0436(14) Uani d . 1
C C3B 0.6049(8) 0.1524(4) 0.3047(5) 0.0383(18) Uani d . 1
O O3C 0.6644(6) 0.0947(3) 0.3253(4) 0.0529(16) Uani d . 1
H H3CA 0.6183 0.0625 0.3038 0.079 Uiso calc R 1
C C3D 0.6620(11) 0.2178(4) 0.3447(6) 0.059(2) Uani d . 1
H H3D1 0.7089 0.2479 0.3060 0.089 Uiso calc R 1
H H3D2 0.7364 0.2056 0.3845 0.089 Uiso calc R 1
H H3D3 0.5771 0.2417 0.3691 0.089 Uiso calc R 1
N N4A 0.2875(7) 0.1689(3) 0.1191(4) 0.0374(16) Uani d . 1
C C4E 0.1930(9) 0.1640(4) 0.0553(5) 0.044(2) Uani d . 1
H H4E 0.1779 0.1237 0.0254 0.053 Uiso calc R 1
C C4D 0.1237(10) 0.2263(4) 0.0416(6) 0.056(2) Uani d . 1
H H4D 0.0547 0.2370 0.0012 0.067 Uiso calc R 1
N N4C 0.1753(7) 0.2691(3) 0.0985(4) 0.0426(17) Uani d . 1
H H4CA 0.1477 0.3119 0.1055 0.051 Uiso calc R 1
C C4B 0.2761(9) 0.2343(4) 0.1422(5) 0.045(2) Uani d . 1
H H4B 0.3318 0.2537 0.1839 0.054 Uiso calc R 1
N N5A 0.2107(6) 0.0828(3) 0.2699(4) 0.0400(16) Uani d . 1
C C5B 0.0607(9) 0.0839(4) 0.2574(7) 0.054(2) Uani d . 1
H H5B 0.0150 0.0823 0.2075 0.065 Uiso calc R 1
N N5C -0.0174(7) 0.0874(4) 0.3264(5) 0.0530(19) Uani d . 1
H H5CA -0.1158 0.0897 0.3314 0.064 Uiso calc R 1
C C5E 0.2252(9) 0.0836(4) 0.3508(5) 0.050(2) Uani d . 1
H H5E 0.3181 0.0821 0.3782 0.060 Uiso calc R 1
C C5D 0.0842(10) 0.0868(5) 0.3855(6) 0.059(2) Uani d . 1
H H5D 0.0630 0.0884 0.4396 0.070 Uiso calc R 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
O2A Mg1 O3A . . 176.5(2)
O2A Mg1 O2C . 2_655 93.8(2)
O3A Mg1 O2C . 2_655 87.6(2)
O2A Mg1 O1A . . 91.78(19)
O3A Mg1 O1A . . 91.4(2)
O2C Mg1 O1A 2_655 . 90.1(2)
O2A Mg1 N4A . . 88.4(2)
O3A Mg1 N4A . . 88.4(2)
O2C Mg1 N4A 2_655 . 93.4(2)
O1A Mg1 N4A . . 176.6(3)
O2A Mg1 N5A . . 92.5(3)
O3A Mg1 N5A . . 86.3(2)
O2C Mg1 N5A 2_655 . 173.0(3)
O1A Mg1 N5A . . 86.6(2)
N4A Mg1 N5A . . 90.0(2)
O2A Mg1 Mg1 . 2_655 70.15(14)
O3A Mg1 Mg1 . 2_655 113.34(17)
O2C Mg1 Mg1 2_655 2_655 69.12(15)
O1A Mg1 Mg1 . 2_655 31.98(19)
N4A Mg1 Mg1 . 2_655 150.55(18)
N5A Mg1 Mg1 . 2_655 110.26(16)
Mg1 O1A Mg1 . 2_655 116.0(4)
C2B O2A Mg1 . . 138.5(5)
O2A C2B O2C . . 125.2(7)
O2A C2B C2D . . 117.1(6)
O2C C2B C2D . . 117.8(6)
C2B O2C Mg1 . 2_655 136.7(4)
C2B C2D H2D1 . . 109.5
C2B C2D H2D2 . . 109.5
H2D1 C2D H2D2 . . 109.5
C2B C2D H2D3 . . 109.5
H2D1 C2D H2D3 . . 109.5
H2D2 C2D H2D3 . . 109.5
C3B O3A Mg1 . . 131.2(5)
O3A C3B O3C . . 123.7(7)
O3A C3B C3D . . 118.5(7)
O3C C3B C3D . . 117.8(7)
C3B O3C H3CA . . 109.5
C3B C3D H3D1 . . 109.5
C3B C3D H3D2 . . 109.5
H3D1 C3D H3D2 . . 109.5
C3B C3D H3D3 . . 109.5
H3D1 C3D H3D3 . . 109.5
H3D2 C3D H3D3 . . 109.5
C4B N4A C4E . . 104.7(7)
C4B N4A Mg1 . . 126.9(6)
C4E N4A Mg1 . . 127.5(5)
N4A C4E C4D . . 110.1(7)
N4A C4E H4E . . 125.0
C4D C4E H4E . . 125.0
N4C C4D C4E . . 105.5(7)
N4C C4D H4D . . 127.3
C4E C4D H4D . . 127.3
C4B N4C C4D . . 108.2(6)
C4B N4C H4CA . . 125.9
C4D N4C H4CA . . 125.9
N4A C4B N4C . . 111.4(7)
N4A C4B H4B . . 124.3
N4C C4B H4B . . 124.3
C5B N5A C5E . . 104.4(8)
C5B N5A Mg1 . . 129.0(7)
C5E N5A Mg1 . . 126.5(5)
N5A C5B N5C . . 111.2(9)
N5A C5B H5B . . 124.4
N5C C5B H5B . . 124.4
C5D N5C C5B . . 108.0(7)
C5D N5C H5CA . . 126.0
C5B N5C H5CA . . 126.0
C5D C5E N5A . . 110.2(8)
C5D C5E H5E . . 124.9
N5A C5E H5E . . 124.9
N5C C5D C5E . . 106.2(8)
N5C C5D H5D . . 126.9
C5E C5D H5D . . 126.9
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Mg1 O2A . 2.021(6)
Mg1 O3A . 2.058(6)
Mg1 O2C 2_655 2.076(6)
Mg1 O1A . 2.151(5)
Mg1 N4A . 2.173(6)
Mg1 N5A . 2.208(7)
Mg1 Mg1 2_655 3.649(4)
O1A Mg1 2_655 2.151(5)
O2A C2B . 1.239(8)
C2B O2C . 1.267(8)
C2B C2D . 1.475(11)
O2C Mg1 2_655 2.076(6)
C2D H2D1 . 0.9600
C2D H2D2 . 0.9600
C2D H2D3 . 0.9600
O3A C3B . 1.237(9)
C3B O3C . 1.265(9)
C3B C3D . 1.505(10)
O3C H3CA . 0.8200
C3D H3D1 . 0.9600
C3D H3D2 . 0.9600
C3D H3D3 . 0.9600
N4A C4B . 1.312(9)
N4A C4E . 1.355(10)
C4E C4D . 1.354(10)
C4E H4E . 0.9300
C4D N4C . 1.337(11)
C4D H4D . 0.9300
N4C C4B . 1.323(10)
N4C H4CA . 0.8600
C4B H4B . 0.9300
N5A C5B . 1.320(10)
N5A C5E . 1.368(11)
C5B N5C . 1.347(12)
C5B H5B . 0.9300
N5C C5D . 1.330(11)
N5C H5CA . 0.8600
C5E C5D . 1.359(12)
C5E H5E . 0.9300
C5D H5D . 0.9300
