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#$Date: 2016-03-22 11:11:11 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178888 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/17/4111771.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4111771
loop_
_publ_author_name
'Rasmus D. Poulsen'
'Anders Bentien'
'Marie Chevalier'
'Bo B. Iversen'
_publ_contact_author_address
;University of Aarhus
Department of Chemistry
Laboratory of Inorganic Chemistry
Langelandsgade 140
DK-8000 Aarhus C
Denmark
;
_publ_contact_author_email       bo@chem.au.dk
_publ_contact_author_fax         '+458619 6199'
_publ_contact_author_name        'Professor Bo B. Iversen'
_publ_contact_author_phone       +4589423969
_publ_section_title
;
 Synthesis, Physical Properties, Multitemperature Crystal Structure, and
 20 K Synchrotron X-ray Charge Density of a Magnetic Metal Organic
 Framework Structure, Mn₃[C₈O₄H₄]₃(C₅H₁₁ON)₂
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9156
_journal_page_last               9166
_journal_paper_doi               10.1021/ja051233z
_journal_volume                  127
_journal_year                    2005
_chemical_formula_moiety         'C34 H34 Mn3 N2 O14'
_chemical_formula_sum            'C34 H34 Mn3 N2 O14'
_chemical_formula_weight         859.45
_chemical_name_common            MnDEF
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 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                 94.5510(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.1084(5)
_cell_length_b                   10.8267(3)
_cell_length_c                   17.3100(4)
_cell_measurement_reflns_used    7371
_cell_measurement_temperature    275
_cell_measurement_theta_max      38.41
_cell_measurement_theta_min      2.24
_cell_volume                     3569.82(16)
_computing_cell_refinement       'SMART (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      275
_diffrn_measured_fraction_theta_full 0.794
_diffrn_measured_fraction_theta_max 0.794
_diffrn_measurement_device_type  'Bruker SMART 1K CCD area-detector'
_diffrn_measurement_method       'ω and π'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0340
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8232
_diffrn_reflns_theta_full        38.95
_diffrn_reflns_theta_max         38.95
_diffrn_reflns_theta_min         2.22
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SMART 1k'
_exptl_absorpt_coefficient_mu    1.117
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.860466
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1997)'
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_density_diffrn    1.599
_exptl_crystal_description       trapezshaped
_exptl_crystal_F_000             1756
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.175
_exptl_crystal_size_rad          0.184
_refine_diff_density_max         1.013
_refine_diff_density_min         -1.402
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.192
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         8232
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.192
_refine_ls_R_factor_all          0.0908
_refine_ls_R_factor_gt           0.0454
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0755P)²+6.6708P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1186
_refine_ls_wR_factor_ref         0.1799
_reflns_number_gt                5653
_reflns_number_total             8232
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja051233zsi20050224_053454.cif
_cod_data_source_block           final275k
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_database_code               4111771
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.2500 0.53555(5) 0.5000 0.02065(11) Uani 1 2 d S . .
Mn2 Mn 0.425403(17) 0.43496(3) 0.536470(18) 0.02275(9) Uani 1 1 d . . .
O1 O 0.46157(9) 0.55607(18) 0.43712(10) 0.0295(4) Uani 1 1 d . . .
O2 O 0.34892(9) 0.52221(17) 0.43519(9) 0.0269(3) Uani 1 1 d . A .
O8 O 0.29837(10) 0.6622(2) 0.58094(11) 0.0355(4) Uani 1 1 d . A .
O9 O 0.40878(10) 0.5948(2) 0.60007(12) 0.0425(5) Uani 1 1 d . A .
O11 O 0.29923(10) 0.38600(19) 0.56753(10) 0.0348(4) Uani 1 1 d . A .
O12 O 0.39517(11) 0.3205(3) 0.63237(14) 0.0529(7) Uani 1 1 d . A .
C1 C 0.40060(11) 0.5686(2) 0.40454(11) 0.0211(4) Uani 1 1 d . . .
C2 C 0.38997(12) 0.6359(2) 0.32924(12) 0.0261(4) Uani 1 1 d . A .
C3 C 0.44310(13) 0.7102(3) 0.30448(16) 0.0374(6) Uani 1 1 d . . .
H3 H 0.4859 0.7157 0.3338 0.045 Uiso 1 1 calc R A .
C4 C 0.43215(14) 0.7239(3) 0.73589(16) 0.0389(6) Uani 1 1 d . . .
H4 H 0.4672 0.6719 0.7204 0.047 Uiso 1 1 calc R . .
C5 C 0.36964(13) 0.7346(2) 0.69020(13) 0.0291(5) Uani 1 1 d . A .
C6 C 0.31751(14) 0.8111(3) 0.71412(15) 0.0375(6) Uani 1 1 d . . .
H6 H 0.2757 0.8203 0.6833 0.045 Uiso 1 1 calc R . .
C7 C 0.32729(14) 0.6256(3) 0.28415(15) 0.0368(6) Uani 1 1 d . . .
H7 H 0.2915 0.5762 0.3006 0.044 Uiso 1 1 calc R A .
C8 C 0.35778(13) 0.6586(2) 0.61738(13) 0.0296(5) Uani 1 1 d . . .
C11 C 0.33005(13) 0.3351(3) 0.62590(14) 0.0319(5) Uani 1 1 d . . .
C12 C 0.28826(12) 0.2897(2) 0.68985(13) 0.0290(5) Uani 1 1 d . A .
C13 C 0.21702(13) 0.3129(3) 0.68783(15) 0.0362(6) Uani 1 1 d . . .
H13 H 0.1947 0.3548 0.6459 0.043 Uiso 1 1 calc R A .
C14 C 0.32127(13) 0.2262(3) 0.75187(16) 0.0396(7) Uani 1 1 d . . .
H14 H 0.3691 0.2096 0.7531 0.047 Uiso 1 1 calc R A .
O21 O 0.4296(3) 0.2731(5) 0.4634(2) 0.0465(9) Uani 0.850(3) 1 d P A 1
N21 N 0.3930(3) 0.0917(4) 0.4124(3) 0.1021(17) Uani 1 1 d . A 1
C21 C 0.3868(3) 0.1891(4) 0.4578(3) 0.0628(12) Uani 0.850(3) 1 d P A 1
H21 H 0.3479 0.1938 0.4868 0.075 Uiso 1 1 calc R A 1
C22 C 0.4480(4) 0.0836(6) 0.3576(5) 0.106(2) Uani 1 1 d . A 1
H22A H 0.4277 0.0459 0.3102 0.128 Uiso 1 1 calc R A 1
H22B H 0.4620 0.1668 0.3450 0.128 Uiso 1 1 calc R A 1
C23 C 0.5110(5) 0.0144(8) 0.3839(6) 0.145(4) Uani 1 1 d . A 1
H23A H 0.5388 0.0622 0.4216 0.218 Uiso 1 1 calc R A 1
H23B H 0.5379 -0.0025 0.3405 0.218 Uiso 1 1 calc R A 1
H23C H 0.4977 -0.0620 0.4068 0.218 Uiso 1 1 calc R A 1
C24 C 0.3309(6) 0.0024(7) 0.4036(5) 0.138(3) Uani 1 1 d . A 1
H24A H 0.2885 0.0465 0.4138 0.166 Uiso 1 1 calc R A 1
H24B H 0.3255 -0.0268 0.3505 0.166 Uiso 1 1 calc R A 1
C25 C 0.3385(6) -0.0965(8) 0.4519(6) 0.158(4) Uani 1 1 d . A 1
H25A H 0.3870 -0.1206 0.4578 0.237 Uiso 1 1 calc R A 1
H25B H 0.3108 -0.1640 0.4305 0.237 Uiso 1 1 calc R A 1
H25C H 0.3232 -0.0748 0.5016 0.237 Uiso 1 1 calc R A 1
C31 C 0.4468(16) 0.216(3) 0.4254(17) 0.0628(12) Uani 0.150(3) 1 d P A 3
O31 O 0.427(2) 0.264(3) 0.4843(16) 0.0465(9) Uani 0.150(3) 1 d P A 3
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'
Mn Mn 0.3368 0.7283 '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
O8 Mn1 O8 99.35(12) . 2_556
O8 Mn1 O11 170.98(8) . 2_556
O8 Mn1 O11 88.80(8) 2_556 2_556
O8 Mn1 O11 88.80(8) . .
O8 Mn1 O11 170.98(8) 2_556 .
O11 Mn1 O11 83.34(12) 2_556 .
O8 Mn1 O2 92.92(7) . 2_556
O8 Mn1 O2 91.79(7) 2_556 2_556
O11 Mn1 O2 82.92(6) 2_556 2_556
O11 Mn1 O2 91.64(7) . 2_556
O8 Mn1 O2 91.79(7) . .
O8 Mn1 O2 92.92(7) 2_556 .
O11 Mn1 O2 91.64(7) 2_556 .
O11 Mn1 O2 82.92(6) . .
O2 Mn1 O2 172.73(10) 2_556 .
O31 Mn2 O9 169.4(9) . .
O31 Mn2 O21 10.0(8) . .
O9 Mn2 O21 172.79(17) . .
O31 Mn2 O1 95.0(12) . 5_666
O9 Mn2 O1 92.42(8) . 5_666
O21 Mn2 O1 94.40(17) . 5_666
O31 Mn2 O12 80.6(7) . .
O9 Mn2 O12 90.51(11) . .
O21 Mn2 O12 90.54(12) . .
O1 Mn2 O12 100.58(7) 5_666 .
O31 Mn2 O1 99.7(7) . .
O9 Mn2 O1 89.37(8) . .
O21 Mn2 O1 89.84(11) . .
O1 Mn2 O1 77.32(7) 5_666 .
O12 Mn2 O1 177.89(7) . .
O31 Mn2 O2 93.4(11) . .
O9 Mn2 O2 87.09(8) . .
O21 Mn2 O2 86.56(15) . .
O1 Mn2 O2 132.61(6) 5_666 .
O12 Mn2 O2 126.80(7) . .
O1 Mn2 O2 55.30(6) . .
C1 O1 Mn2 163.05(15) . 5_666
C1 O1 Mn2 94.23(13) . .
Mn2 O1 Mn2 102.68(7) 5_666 .
C1 O2 Mn1 152.81(16) . .
C1 O2 Mn2 90.71(13) . .
Mn1 O2 Mn2 98.45(6) . .
C8 O8 Mn1 129.93(17) . .
C8 O9 Mn2 137.57(17) . .
C11 O11 Mn1 156.6(2) . .
C11 O12 Mn2 100.47(16) . .
O1 C1 O2 119.68(19) . .
O1 C1 C2 120.01(19) . .
O2 C1 C2 120.30(19) . .
C7 C2 C3 119.7(2) . .
C7 C2 C1 120.4(2) . .
C3 C2 C1 120.0(2) . .
C4 C3 C2 119.8(2) 8_564 .
C4 C3 H3 120.1 8_564 .
C2 C3 H3 120.1 . .
C5 C4 C3 120.7(2) . 8_565
C5 C4 H4 119.6 . .
C3 C4 H4 119.6 8_565 .
C6 C5 C4 119.2(2) . .
C6 C5 C8 120.9(2) . .
C4 C5 C8 119.8(2) . .
C5 C6 C7 120.3(2) . 8_565
C5 C6 H6 119.8 . .
C7 C6 H6 119.8 8_565 .
C2 C7 C6 120.2(2) . 8_564
C2 C7 H7 119.9 . .
C6 C7 H7 119.9 8_564 .
O9 C8 O8 126.0(2) . .
O9 C8 C5 115.7(2) . .
O8 C8 C5 118.3(2) . .
O12 C11 O11 121.8(2) . .
O12 C11 C12 118.5(2) . .
O11 C11 C12 119.7(2) . .
C13 C12 C14 119.8(2) . .
C13 C12 C11 120.2(2) . .
C14 C12 C11 119.9(2) . .
C12 C13 C14 120.2(2) . 7_556
C12 C13 H13 119.9 . .
C14 C13 H13 119.9 7_556 .
C12 C14 C13 120.0(2) . 7_556
C12 C14 H14 120.0 . .
C13 C14 H14 120.0 7_556 .
C21 O21 Mn2 126.3(4) . .
C21 N21 C22 122.1(5) . .
C21 N21 C24 117.2(6) . .
C22 N21 C24 119.0(5) . .
O21 C21 N21 123.2(5) . .
O21 C21 H21 118.4 . .
N21 C21 H21 118.4 . .
C23 C22 N21 116.3(7) . .
C23 C22 H22A 108.2 . .
N21 C22 H22A 108.2 . .
C23 C22 H22B 108.2 . .
N21 C22 H22B 108.2 . .
H22A C22 H22B 107.4 . .
C25 C24 N21 113.1(9) . .
C25 C24 H24A 108.9 . .
N21 C24 H24A 108.9 . .
C25 C24 H24B 108.9 . .
N21 C24 H24B 108.9 . .
H24A C24 H24B 107.8 . .
C31 O31 Mn2 139(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 O8 2.1197(18) .
Mn1 O8 2.1197(18) 2_556
Mn1 O11 2.1676(19) 2_556
Mn1 O11 2.1676(19) .
Mn1 O2 2.2779(15) 2_556
Mn1 O2 2.2779(15) .
Mn2 O31 2.06(4) .
Mn2 O9 2.089(2) .
Mn2 O21 2.167(5) .
Mn2 O1 2.1741(17) 5_666
Mn2 O12 2.185(2) .
Mn2 O1 2.3114(17) .
Mn2 O2 2.3865(17) .
O1 C1 1.261(3) .
O1 Mn2 2.1741(17) 5_666
O2 C1 1.262(2) .
O8 C8 1.255(3) .
O9 C8 1.250(3) .
O11 C11 1.256(3) .
O12 C11 1.250(3) .
C1 C2 1.493(3) .
C2 C7 1.381(3) .
C2 C3 1.389(3) .
C3 C4 1.387(3) 8_564
C3 H3 0.9300 .
C4 C5 1.384(4) .
C4 C3 1.387(3) 8_565
C4 H4 0.9300 .
C5 C6 1.384(3) .
C5 C8 1.507(3) .
C6 C7 1.392(3) 8_565
C6 H6 0.9300 .
C7 C6 1.392(3) 8_564
C7 H7 0.9300 .
C11 C12 1.498(3) .
C12 C13 1.382(3) .
C12 C14 1.384(3) .
C13 C14 1.387(3) 7_556
C13 H13 0.9300 .
C14 C13 1.387(3) 7_556
C14 H14 0.9300 .
O21 C21 1.222(7) .
N21 C21 1.326(6) .
N21 C22 1.474(9) .
N21 C24 1.528(9) .
C21 H21 0.9300 .
C22 C23 1.459(11) .
C22 H22A 0.9700 .
C22 H22B 0.9700 .
C23 H23A 0.9600 .
C23 H23B 0.9600 .
C23 H23C 0.9600 .
C24 C25 1.360(12) .
C24 H24A 0.9700 .
C24 H24B 0.9700 .
C25 H25A 0.9600 .
C25 H25B 0.9600 .
C25 H25C 0.9600 .
C31 O31 1.24(4) .
