#------------------------------------------------------------------------------
#$Date: 2016-03-23 20:52:13 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179428 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/25/4332583.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# 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_4332583
loop_
_publ_author_name
'Rood, Jeffrey A.'
'Noll, Bruce C.'
'Henderson, Kenneth W.'
_publ_section_title
;
 Synthesis, Structural Characterization, Gas Sorption and Guest-Exchange
 Studies of the Lightweight, Porous Metal−Organic Framework
 α-[Mg3(O2CH)6]
;
_journal_issue                   14
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5521
_journal_page_last               5528
_journal_paper_doi               10.1021/ic060543v
_journal_volume                  45
_journal_year                    2006
_chemical_compound_source        Synthesized
_chemical_formula_moiety         'C6 H6 Mg3 O12, C3 H6 O1'
_chemical_formula_sum            'C9 H12 Mg3 O13'
_chemical_formula_weight         401.12
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.565(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.2790(8)
_cell_length_b                   9.8339(7)
_cell_length_c                   14.7660(11)
_cell_measurement_reflns_used    7564
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.5753
_cell_measurement_theta_min      2.7484
_cell_volume                     1637.2(2)
_computing_cell_refinement       'APEX2/SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2004; Sheldrick, 2003)'
_computing_molecular_graphics    'XP (Sheldrick, 1998)'
_computing_publication_material  'XCIF (Sheldrick, 2001)/enCIFer (CCDC, 2004)'
_computing_structure_refinement  'XL (Sheldrick, 2001)'
_computing_structure_solution    'XS (Sheldrick, 2001)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker x8-ApexII CCD diffractometer'
_diffrn_measurement_method       'φ and ω'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_sigmaI/netI    0.0202
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            41801
_diffrn_reflns_theta_full        31.64
_diffrn_reflns_theta_max         31.64
_diffrn_reflns_theta_min         2.24
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Siemens KFFMO2K-90'
_exptl_absorpt_coefficient_mu    0.251
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.92
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; Blessing, R.H. (1995) Acta Cryst. A51, 33-38.

Sheldrick, G.M. (2004) SADABS, University of G\:ottingen, Germany.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.627
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             824
_exptl_crystal_recrystallization_method 'From reaction at 110 °C in DMF'
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.875
_refine_diff_density_min         -0.679
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.154
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     229
_refine_ls_number_reflns         5480
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.154
_refine_ls_R_factor_all          0.0510
_refine_ls_R_factor_gt           0.0433
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0377P)²+2.9723P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1173
_refine_ls_wR_factor_ref         0.1213
_reflns_number_gt                4750
_reflns_number_total             5480
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060543vsup5.cif
_cod_data_source_block           jr30
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4332583
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Mg1 Mg 0.24326(5) 0.92502(6) 0.86507(4) 0.00828(12) Uani 1 1 d .
Mg2 Mg 0.5000 1.0000 1.0000 0.00973(16) Uani 1 2 d S
Mg3 Mg 0.23980(5) 0.61695(6) 0.80602(4) 0.00881(12) Uani 1 1 d .
Mg4 Mg 0.0000 1.0000 1.0000 0.01014(16) Uani 1 2 d S
O1 O 0.36967(11) 1.01166(13) 0.78332(8) 0.0102(2) Uani 1 1 d .
O2 O 0.53938(11) 1.00580(14) 0.86466(9) 0.0139(2) Uani 1 1 d .
O3 O 0.34203(11) 0.74711(13) 0.88678(8) 0.0105(2) Uani 1 1 d .
O4 O 0.47868(11) 0.79325(13) 0.99500(9) 0.0131(2) Uani 1 1 d .
O5 O 0.09979(11) 0.85055(12) 0.93410(8) 0.0104(2) Uani 1 1 d .
O6 O 0.10589(11) 0.63027(13) 0.89509(9) 0.0128(2) Uani 1 1 d .
O7 O 0.19191(11) 0.80530(13) 0.75232(8) 0.0103(2) Uani 1 1 d .
O8 O 0.30911(12) 0.44825(13) 0.86567(9) 0.0125(2) Uani 1 1 d .
O9 O 0.31654(11) 1.02833(13) 0.97435(8) 0.0103(2) Uani 1 1 d .
O10 O 0.15042(11) 1.10367(14) 1.03717(9) 0.0142(2) Uani 1 1 d .
O11 O 0.15027(11) 1.08614(13) 0.80524(8) 0.0104(2) Uani 1 1 d .
O12 O -0.01329(12) 1.11767(14) 0.88511(9) 0.0150(3) Uani 1 1 d .
C1 C 0.48165(15) 1.02363(18) 0.79336(12) 0.0120(3) Uani 1 1 d .
H1 H 0.5246 1.0485 0.7414 0.014 Uiso 1 1 calc R
C2 C 0.42266(15) 0.71342(18) 0.94530(12) 0.0115(3) Uani 1 1 d .
H2 H 0.4409 0.6194 0.9510 0.014 Uiso 1 1 calc R
C3 C 0.06471(15) 0.72709(18) 0.93781(12) 0.0121(3) Uani 1 1 d .
H3 H 0.0013 0.7078 0.9769 0.015 Uiso 1 1 calc R
C4 C 0.32723(15) 0.33574(18) 0.83069(12) 0.0118(3) Uani 1 1 d .
H4 H 0.3581 0.2661 0.8692 0.014 Uiso 1 1 calc R
C5 C 0.25923(15) 1.10256(18) 1.02967(12) 0.0119(3) Uani 1 1 d .
H5 H 0.3043 1.1617 1.0681 0.014 Uiso 1 1 calc R
C6 C 0.05075(15) 1.14304(18) 0.82073(12) 0.0123(3) Uani 1 1 d .
H6 H 0.0238 1.2107 0.7791 0.015 Uiso 1 1 calc R
C2S C 0.8195(2) 0.9824(4) 0.66166(17) 0.0410(7) Uani 1 1 d .
O1S O 0.8797(3) 1.0859(4) 0.66687(18) 0.0792(11) Uani 1 1 d .
C1S C 0.7151(3) 0.9826(5) 0.5984(2) 0.0580(11) Uani 1 1 d .
H1SA H 0.6677 1.0645 0.6084 0.087 Uiso 1 1 calc R
H1SB H 0.6667 0.9017 0.6091 0.087 Uiso 1 1 calc R
H1SC H 0.7420 0.9818 0.5358 0.087 Uiso 1 1 calc R
C3S C 0.8476(4) 0.8615(5) 0.7162(3) 0.0675(11) Uani 1 1 d .
H3SA H 0.8630 0.7845 0.6761 0.101 Uiso 1 1 calc R
H3SB H 0.7805 0.8399 0.7544 0.101 Uiso 1 1 calc R
H3SC H 0.9181 0.8793 0.7546 0.101 Uiso 1 1 calc R
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'
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O9 Mg1 O5 95.23(5) . .
O9 Mg1 O1 89.19(5) . .
O5 Mg1 O1 171.95(6) . .
O9 Mg1 O11 98.26(5) . .
O5 Mg1 O11 94.97(5) . .
O1 Mg1 O11 77.71(5) . .
O9 Mg1 O3 95.26(5) . .
O5 Mg1 O3 92.80(5) . .
O1 Mg1 O3 93.49(5) . .
O11 Mg1 O3 163.71(6) . .
O9 Mg1 O7 171.82(6) . .
O5 Mg1 O7 89.41(5) . .
O1 Mg1 O7 87.03(5) . .
O11 Mg1 O7 88.02(5) . .
O3 Mg1 O7 77.75(5) . .
O9 Mg1 Mg3 133.80(4) . .
O5 Mg1 Mg3 78.01(4) . .
O1 Mg1 Mg3 103.71(4) . .
O11 Mg1 Mg3 127.68(4) . .
O3 Mg1 Mg3 40.71(4) . .
O7 Mg1 Mg3 40.84(4) . .
O9 Mg1 Mg3 107.43(4) . 2_556
O5 Mg1 Mg3 132.02(4) . 2_556
O1 Mg1 Mg3 39.95(4) . 2_556
O11 Mg1 Mg3 41.26(4) . 2_556
O3 Mg1 Mg3 125.25(4) . 2_556
O7 Mg1 Mg3 73.96(4) . 2_556
Mg3 Mg1 Mg3 110.672(19) . 2_556
O9 Mg1 Mg4 75.83(4) . .
O5 Mg1 Mg4 33.04(4) . .
O1 Mg1 Mg4 143.43(4) . .
O11 Mg1 Mg4 71.88(4) . .
O3 Mg1 Mg4 120.60(4) . .
O7 Mg1 Mg4 111.30(4) . .
Mg3 Mg1 Mg4 110.771(19) . .
Mg3 Mg1 Mg4 113.13(2) 2_556 .
O9 Mg1 Mg2 32.21(3) . .
O5 Mg1 Mg2 115.73(4) . .
O1 Mg1 Mg2 71.23(4) . .
O11 Mg1 Mg2 118.28(4) . .
O3 Mg1 Mg2 70.43(4) . .
O7 Mg1 Mg2 139.68(4) . .
Mg3 Mg1 Mg2 111.03(2) . .
Mg3 Mg1 Mg2 104.970(19) 2_556 .
Mg4 Mg1 Mg2 106.027(16) . .
O4 Mg2 O4 180.0 3_677 .
O4 Mg2 O2 88.81(5) 3_677 .
O4 Mg2 O2 91.19(5) . .
O4 Mg2 O2 88.81(5) . 3_677
O2 Mg2 O2 180.000(1) . 3_677
O4 Mg2 O9 89.37(5) 3_677 .
O4 Mg2 O9 90.63(5) . .
O2 Mg2 O9 93.35(5) . .
O2 Mg2 O9 86.65(5) 3_677 .
O4 Mg2 O9 89.37(5) . 3_677
O2 Mg2 O9 86.65(5) . 3_677
O9 Mg2 O9 180.0 . 3_677
O4 Mg2 Mg1 108.65(4) 3_677 .
O4 Mg2 Mg1 71.35(4) . .
O2 Mg2 Mg1 69.83(4) . .
O2 Mg2 Mg1 110.17(4) 3_677 .
O9 Mg2 Mg1 31.34(3) . .
O9 Mg2 Mg1 148.66(3) 3_677 .
O4 Mg2 Mg1 108.65(4) . 3_677
O2 Mg2 Mg1 110.17(4) . 3_677
O9 Mg2 Mg1 148.66(3) . 3_677
Mg1 Mg2 Mg1 180.0 . 3_677
O8 Mg3 O6 93.22(6) . .
O8 Mg3 O1 94.84(6) . 2_546
O6 Mg3 O1 90.22(6) . 2_546
O8 Mg3 O3 93.06(6) . .
O6 Mg3 O3 89.97(6) . .
O1 Mg3 O3 172.08(6) 2_546 .
O8 Mg3 O7 171.20(6) . .
O6 Mg3 O7 89.97(6) . .
O1 Mg3 O7 93.36(5) 2_546 .
O3 Mg3 O7 78.72(5) . .
O8 Mg3 O11 89.60(5) . 2_546
O6 Mg3 O11 167.60(6) . 2_546
O3 Mg3 O11 101.94(5) . 2_546
O7 Mg3 O11 89.03(5) . 2_546
O8 Mg3 Mg1 131.69(5) . .
O6 Mg3 Mg1 76.29(4) . .
O1 Mg3 Mg1 131.49(4) 2_546 .
O3 Mg3 Mg1 41.11(4) . .
O7 Mg3 Mg1 41.49(4) . .
O11 Mg3 Mg1 110.53(4) 2_546 .
O8 Mg3 Mg1 80.07(4) . 2_546
O6 Mg3 Mg1 128.10(5) . 2_546
O3 Mg3 Mg1 141.39(4) . 2_546
O7 Mg3 Mg1 104.33(4) . 2_546
Mg1 Mg3 Mg1 142.53(2) . 2_546
O10 Mg4 O10 180.0 3_577 .
O10 Mg4 O12 91.02(6) 3_577 .
O10 Mg4 O12 88.98(6) . .
O10 Mg4 O12 91.02(6) . 3_577
O12 Mg4 O12 180.0 . 3_577
O10 Mg4 O5 88.74(5) . 3_577
O12 Mg4 O5 87.74(5) . 3_577
O10 Mg4 O5 88.74(5) 3_577 .
O10 Mg4 O5 91.26(5) . .
O12 Mg4 O5 92.26(5) . .
O12 Mg4 O5 87.74(5) 3_577 .
O5 Mg4 O5 180.00(6) 3_577 .
O10 Mg4 Mg1 113.51(4) . 3_577
O12 Mg4 Mg1 108.02(4) . 3_577
O5 Mg4 Mg1 147.59(3) . 3_577
O10 Mg4 Mg1 113.51(4) 3_577 .
O10 Mg4 Mg1 66.49(4) . .
O12 Mg4 Mg1 71.98(4) . .
O12 Mg4 Mg1 108.02(4) 3_577 .
O5 Mg4 Mg1 147.59(3) 3_577 .
O5 Mg4 Mg1 32.41(3) . .
Mg1 Mg4 Mg1 180.0 3_577 .
C1 O1 Mg3 127.10(11) . 2_556
C1 O1 Mg1 131.69(11) . .
Mg3 O1 Mg1 99.75(6) 2_556 .
C1 O2 Mg2 135.09(12) . .
C2 O3 Mg3 126.92(11) . .
C2 O3 Mg1 133.18(11) . .
Mg3 O3 Mg1 98.18(5) . .
C2 O4 Mg2 135.17(12) . .
C3 O5 Mg1 127.17(11) . .
C3 O5 Mg4 118.23(11) . .
Mg1 O5 Mg4 114.56(6) . .
C3 O6 Mg3 132.36(12) . .
C4 O7 Mg3 127.67(11) 2_556 .
C4 O7 Mg1 131.63(12) 2_556 .
Mg3 O7 Mg1 97.66(5) . .
C4 O8 Mg3 127.99(12) . .
C5 O9 Mg1 125.49(11) . .
C5 O9 Mg2 117.97(11) . .
Mg1 O9 Mg2 116.46(6) . .
C5 O10 Mg4 142.36(12) . .
C6 O11 Mg1 133.65(11) . .
C6 O11 Mg3 127.87(11) . 2_556
Mg1 O11 Mg3 98.04(5) . 2_556
C6 O12 Mg4 135.89(12) . .
O2 C1 O1 125.76(16) . .
O2 C1 H1 117.1 . .
O1 C1 H1 117.1 . .
O4 C2 O3 125.32(16) . .
O4 C2 H2 117.3 . .
O3 C2 H2 117.3 . .
O6 C3 O5 125.94(16) . .
O6 C3 H3 117.0 . .
O5 C3 H3 117.0 . .
O8 C4 O7 125.77(16) . 2_546
O8 C4 H4 117.1 . .
O7 C4 H4 117.1 2_546 .
O10 C5 O9 125.53(16) . .
O10 C5 H5 117.2 . .
O9 C5 H5 117.2 . .
O12 C6 O11 125.68(16) . .
O12 C6 H6 117.2 . .
O11 C6 H6 117.2 . .
O1S C2S C3S 121.9(3) . .
O1S C2S C1S 117.9(4) . .
C3S C2S C1S 120.2(3) . .
C2S C1S H1SA 109.5 . .
C2S C1S H1SB 109.5 . .
H1SA C1S H1SB 109.5 . .
C2S C1S H1SC 109.5 . .
H1SA C1S H1SC 109.5 . .
H1SB C1S H1SC 109.5 . .
C2S C3S H3SA 109.5 . .
C2S C3S H3SB 109.5 . .
H3SA C3S H3SB 109.5 . .
C2S C3S H3SC 109.5 . .
H3SA C3S H3SC 109.5 . .
H3SB C3S H3SC 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mg1 O9 2.0606(13) .
Mg1 O5 2.0697(13) .
Mg1 O1 2.0761(13) .
Mg1 O11 2.0834(13) .
Mg1 O3 2.0941(14) .
Mg1 O7 2.1074(14) .
Mg1 Mg3 3.1525(8) .
Mg1 Mg3 3.1634(8) 2_556
Mg1 Mg4 3.5128(6) .
Mg1 Mg2 3.5473(6) .
Mg2 O4 2.0484(13) 3_677
Mg2 O4 2.0484(13) .
Mg2 O2 2.0599(13) .
Mg2 O2 2.0599(13) 3_677
Mg2 O9 2.1118(12) .
Mg2 O9 2.1118(12) 3_677
Mg2 Mg1 3.5473(6) 3_677
Mg3 O8 2.0253(14) .
Mg3 O6 2.0339(14) .
Mg3 O1 2.0610(13) 2_546
Mg3 O3 2.0773(14) .
Mg3 O7 2.0804(14) .
Mg3 O11 2.1069(13) 2_546
Mg3 Mg1 3.1634(8) 2_546
Mg4 O10 2.0416(13) 3_577
Mg4 O10 2.0416(13) .
Mg4 O12 2.0556(14) .
Mg4 O12 2.0556(14) 3_577
Mg4 O5 2.1056(12) 3_577
Mg4 O5 2.1056(12) .
Mg4 Mg1 3.5128(6) 3_577
O1 C1 1.273(2) .
O1 Mg3 2.0610(13) 2_556
O2 C1 1.235(2) .
O3 C2 1.281(2) .
O4 C2 1.236(2) .
O5 C3 1.279(2) .
O6 C3 1.240(2) .
O7 C4 1.274(2) 2_556
O8 C4 1.240(2) .
O9 C5 1.283(2) .
O10 C5 1.235(2) .
O11 C6 1.280(2) .
O11 Mg3 2.1069(13) 2_556
O12 C6 1.235(2) .
C1 H1 0.9500 .
C2 H2 0.9500 .
C3 H3 0.9500 .
C4 O7 1.274(2) 2_546
C4 H4 0.9500 .
C5 H5 0.9500 .
C6 H6 0.9500 .
C2S O1S 1.225(4) .
C2S C3S 1.466(5) .
C2S C1S 1.483(4) .
C1S H1SA 0.9800 .
C1S H1SB 0.9800 .
C1S H1SC 0.9800 .
C3S H3SA 0.9800 .
C3S H3SB 0.9800 .
C3S H3SC 0.9800 .
