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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/4/11/17/4111766.cif $
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#
# 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_4111766
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                 94.3240(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.0605(4)
_cell_length_b                   10.6978(2)
_cell_length_c                   17.3234(4)
_cell_measurement_reflns_used    7453
_cell_measurement_temperature    150
_cell_measurement_theta_max      38.25
_cell_measurement_theta_min      2.15
_cell_volume                     3522.28(13)
_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      150
_diffrn_measured_fraction_theta_full 0.798
_diffrn_measured_fraction_theta_max 0.798
_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    0.0303
_diffrn_reflns_limit_h_max       31
_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            8122
_diffrn_reflns_theta_full        38.90
_diffrn_reflns_theta_max         38.90
_diffrn_reflns_theta_min         2.14
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SMART 1k'
_exptl_absorpt_coefficient_mu    1.132
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.887024
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1997)'
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_density_diffrn    1.621
_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         1.323
_refine_diff_density_min         -1.903
_refine_diff_density_rms         0.220
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.210
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         8122
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.210
_refine_ls_R_factor_all          0.0908
_refine_ls_R_factor_gt           0.0510
_refine_ls_shift/su_max          0.035
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0770P)²+20.1005P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1308
_refine_ls_wR_factor_ref         0.2073
_reflns_number_gt                6046
_reflns_number_total             8122
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja051233zsi20050224_053323.cif
_cod_data_source_block           final150k
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_database_code               4111766
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 0.53202(6) 0.5000 0.01486(12) Uani 1 2 d S . .
Mn2 Mn 0.42569(2) 0.43140(4) 0.53520(2) 0.01624(10) Uani 1 1 d . . .
O1 O 0.46139(11) 0.5568(2) 0.43744(12) 0.0210(4) Uani 1 1 d . . .
O2 O 0.34860(11) 0.5196(2) 0.43488(11) 0.0198(4) Uani 1 1 d . A .
O8 O 0.29750(12) 0.6604(2) 0.58111(12) 0.0239(4) Uani 1 1 d . A .
O9 O 0.40823(12) 0.5908(3) 0.60019(14) 0.0297(5) Uani 1 1 d . A .
O11 O 0.30043(12) 0.3803(2) 0.56595(12) 0.0238(4) Uani 1 1 d . A .
O12 O 0.39643(13) 0.3134(3) 0.63090(15) 0.0361(6) Uani 1 1 d . A .
C1 C 0.40020(14) 0.5679(3) 0.40426(14) 0.0155(4) Uani 1 1 d . . .
C2 C 0.38970(15) 0.6351(3) 0.32878(15) 0.0196(5) Uani 1 1 d . A .
C3 C 0.44300(16) 0.7100(3) 0.30365(17) 0.0242(6) Uani 1 1 d . . .
H3 H 0.4860 0.7152 0.3326 0.029 Uiso 1 1 calc R A .
C4 C 0.43198(17) 0.7229(3) 0.73515(18) 0.0264(6) Uani 1 1 d . . .
H4 H 0.4670 0.6699 0.7196 0.032 Uiso 1 1 calc R . .
C5 C 0.36940(15) 0.7342(3) 0.68990(16) 0.0206(5) Uani 1 1 d . A .
C6 C 0.31716(17) 0.8117(3) 0.71384(18) 0.0268(6) Uani 1 1 d . . .
H6 H 0.2754 0.8210 0.6830 0.032 Uiso 1 1 calc R . .
C7 C 0.32672(17) 0.6240(3) 0.28374(18) 0.0266(6) Uani 1 1 d . . .
H7 H 0.2909 0.5737 0.3002 0.032 Uiso 1 1 calc R A .
C8 C 0.35720(16) 0.6565(3) 0.61736(16) 0.0213(5) Uani 1 1 d . . .
C11 C 0.33098(15) 0.3295(3) 0.62469(17) 0.0226(5) Uani 1 1 d . . .
C12 C 0.28888(15) 0.2869(3) 0.68914(16) 0.0200(5) Uani 1 1 d . A .
C13 C 0.21721(16) 0.3101(3) 0.68617(18) 0.0269(6) Uani 1 1 d . . .
H13 H 0.1951 0.3501 0.6433 0.032 Uiso 1 1 calc R A .
C14 C 0.32174(16) 0.2261(4) 0.75296(19) 0.0286(7) Uani 1 1 d . . .
H14 H 0.3698 0.2096 0.7549 0.034 Uiso 1 1 calc R A .
O21 O 0.4310(2) 0.2699(3) 0.46172(19) 0.0293(6) Uani 0.903(4) 1 d P A 1
N21 N 0.3910(3) 0.0889(4) 0.4073(3) 0.0587(12) Uani 1 1 d . A 1
C21 C 0.3866(3) 0.1850(4) 0.4545(3) 0.0384(9) Uani 0.903(4) 1 d P A 1
H21 H 0.3480 0.1893 0.4842 0.046 Uiso 1 1 calc R A 1
C22 C 0.4492(4) 0.0813(5) 0.3556(4) 0.0622(15) Uani 1 1 d . A 1
H22A H 0.4635 0.1656 0.3434 0.075 Uiso 1 1 calc R A 1
H22B H 0.4315 0.0421 0.3075 0.075 Uiso 1 1 calc R A 1
C23 C 0.5118(4) 0.0115(7) 0.3870(5) 0.081(2) Uani 1 1 d . A 1
H23A H 0.5345 0.0568 0.4298 0.121 Uiso 1 1 calc R A 1
H23B H 0.5439 0.0017 0.3473 0.121 Uiso 1 1 calc R A 1
H23C H 0.4977 -0.0693 0.4043 0.121 Uiso 1 1 calc R A 1
C24 C 0.3327(5) -0.0033(7) 0.3999(4) 0.084(2) Uani 1 1 d . A 1
H24A H 0.2889 0.0395 0.4077 0.101 Uiso 1 1 calc R A 1
H24B H 0.3292 -0.0364 0.3476 0.101 Uiso 1 1 calc R A 1
C25 C 0.3408(5) -0.1066(6) 0.4540(4) 0.079(2) Uani 1 1 d . A 1
H25A H 0.3862 -0.1442 0.4507 0.119 Uiso 1 1 calc R A 1
H25B H 0.3048 -0.1677 0.4414 0.119 Uiso 1 1 calc R A 1
H25C H 0.3367 -0.0765 0.5056 0.119 Uiso 1 1 calc R A 1
C31 C 0.451(2) 0.212(4) 0.421(2) 0.0384(9) Uani 0.097(4) 1 d P A 3
O31 O 0.429(2) 0.253(4) 0.483(2) 0.0293(6) Uani 0.097(4) 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 99.19(13) . 2_556
O8 Mn1 O11 170.19(9) . 2_556
O8 Mn1 O11 89.16(9) 2_556 2_556
O8 Mn1 O11 89.16(9) . .
O8 Mn1 O11 170.19(9) 2_556 .
O11 Mn1 O11 83.03(13) 2_556 .
O8 Mn1 O2 92.11(8) . 2_556
O8 Mn1 O2 92.24(8) 2_556 2_556
O11 Mn1 O2 82.37(8) 2_556 2_556
O11 Mn1 O2 92.59(8) . 2_556
O8 Mn1 O2 92.24(8) . .
O8 Mn1 O2 92.11(8) 2_556 .
O11 Mn1 O2 92.59(8) 2_556 .
O11 Mn1 O2 82.37(8) . .
O2 Mn1 O2 173.29(12) 2_556 .
O9 Mn2 O31 168.5(10) . .
O9 Mn2 O21 173.03(13) . .
O31 Mn2 O21 11.2(9) . .
O9 Mn2 O1 91.74(9) . 5_666
O31 Mn2 O1 95.0(13) . 5_666
O21 Mn2 O1 94.94(12) . 5_666
O9 Mn2 O12 90.14(12) . .
O31 Mn2 O12 79.6(9) . .
O21 Mn2 O12 90.64(12) . .
O1 Mn2 O12 99.97(9) 5_666 .
O9 Mn2 O1 89.35(10) . .
O31 Mn2 O1 101.1(9) . .
O21 Mn2 O1 90.17(10) . .
O1 Mn2 O1 77.51(9) 5_666 .
O12 Mn2 O1 177.41(9) . .
O9 Mn2 O2 87.42(9) . .
O31 Mn2 O2 94.6(12) . .
O21 Mn2 O2 86.57(12) . .
O1 Mn2 O2 133.00(7) 5_666 .
O12 Mn2 O2 127.02(8) . .
O1 Mn2 O2 55.49(7) . .
C1 O1 Mn2 163.12(18) . 5_666
C1 O1 Mn2 94.33(15) . .
Mn2 O1 Mn2 102.49(8) 5_666 .
C1 O2 Mn1 152.4(2) . .
C1 O2 Mn2 90.66(16) . .
Mn1 O2 Mn2 98.57(7) . .
C8 O8 Mn1 129.4(2) . .
C8 O9 Mn2 138.2(2) . .
C11 O11 Mn1 155.6(2) . .
C11 O12 Mn2 99.47(19) . .
O1 C1 O2 119.4(2) . .
O1 C1 C2 120.1(2) . .
O2 C1 C2 120.5(2) . .
C7 C2 C3 119.7(3) . .
C7 C2 C1 120.3(2) . .
C3 C2 C1 120.0(3) . .
C2 C3 C4 119.9(3) . 8_564
C2 C3 H3 120.0 . .
C4 C3 H3 120.0 8_564 .
C5 C4 C3 120.5(3) . 8_565
C5 C4 H4 119.8 . .
C3 C4 H4 119.8 8_565 .
C4 C5 C6 119.5(3) . .
C4 C5 C8 119.7(3) . .
C6 C5 C8 120.7(3) . .
C5 C6 C7 120.4(3) . 8_565
C5 C6 H6 119.8 . .
C7 C6 H6 119.8 8_565 .
C2 C7 C6 119.9(3) . 8_564
C2 C7 H7 120.1 . .
C6 C7 H7 120.1 8_564 .
O9 C8 O8 126.1(3) . .
O9 C8 C5 115.6(3) . .
O8 C8 C5 118.3(3) . .
O11 C11 O12 121.7(3) . .
O11 C11 C12 119.6(3) . .
O12 C11 C12 118.7(3) . .
C13 C12 C14 119.8(2) . .
C13 C12 C11 120.1(3) . .
C14 C12 C11 120.1(3) . .
C12 C13 C14 120.2(3) . 7_556
C12 C13 H13 119.9 . .
C14 C13 H13 119.9 7_556 .
C13 C14 C12 120.0(3) 7_556 .
C13 C14 H14 120.0 7_556 .
C12 C14 H14 120.0 . .
C21 O21 Mn2 125.8(3) . .
C21 N21 C22 120.3(4) . .
C21 N21 C24 119.2(6) . .
C22 N21 C24 120.1(5) . .
O21 C21 N21 123.8(5) . .
O21 C21 H21 118.1 . .
N21 C21 H21 118.1 . .
N21 C22 C23 115.3(6) . .
N21 C22 H22A 108.5 . .
C23 C22 H22A 108.5 . .
N21 C22 H22B 108.5 . .
C23 C22 H22B 108.5 . .
H22A C22 H22B 107.5 . .
C25 C24 N21 114.2(7) . .
C25 C24 H24A 108.7 . .
N21 C24 H24A 108.7 . .
C25 C24 H24B 108.7 . .
N21 C24 H24B 108.7 . .
H24A C24 H24B 107.6 . .
C31 O31 Mn2 134(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 O8 2.118(2) .
Mn1 O8 2.118(2) 2_556
Mn1 O11 2.167(2) 2_556
Mn1 O11 2.167(2) .
Mn1 O2 2.2676(19) 2_556
Mn1 O2 2.2676(19) .
Mn2 O9 2.084(2) .
Mn2 O31 2.12(4) .
Mn2 O21 2.153(3) .
Mn2 O1 2.172(2) 5_666
Mn2 O12 2.189(2) .
Mn2 O1 2.303(2) .
Mn2 O2 2.384(2) .
O1 C1 1.266(3) .
O1 Mn2 2.172(2) 5_666
O2 C1 1.263(3) .
O8 C8 1.258(4) .
O9 C8 1.253(4) .
O11 C11 1.257(4) .
O12 C11 1.256(4) .
C1 C2 1.492(4) .
C2 C7 1.387(4) .
C2 C3 1.390(4) .
C3 C4 1.389(4) 8_564
C3 H3 0.9300 .
C4 C5 1.382(4) .
C4 C3 1.389(4) 8_565
C4 H4 0.9300 .
C5 C6 1.383(4) .
C5 C8 1.510(4) .
C6 C7 1.393(4) 8_565
C6 H6 0.9300 .
C7 C6 1.393(4) 8_564
C7 H7 0.9300 .
C11 C12 1.494(4) .
C12 C13 1.386(4) .
C12 C14 1.391(4) .
C13 C14 1.390(4) 7_556
C13 H13 0.9300 .
C14 C13 1.390(4) 7_556
C14 H14 0.9300 .
O21 C21 1.241(5) .
N21 C21 1.321(6) .
N21 C22 1.479(8) .
N21 C24 1.484(7) .
C21 H21 0.9300 .
C22 C23 1.477(10) .
C22 H22A 0.9700 .
C22 H22B 0.9700 .
C23 H23A 0.9600 .
C23 H23B 0.9600 .
C23 H23C 0.9600 .
C24 C25 1.449(10) .
C24 H24A 0.9700 .
C24 H24B 0.9700 .
C25 H25A 0.9600 .
C25 H25B 0.9600 .
C25 H25C 0.9600 .
C31 O31 1.26(5) .
