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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/4/11/17/4111770.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_4111770
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                 94.4960(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.0942(4)
_cell_length_b                   10.7964(3)
_cell_length_c                   17.3098(4)
_cell_measurement_reflns_used    7602
_cell_measurement_temperature    250
_cell_measurement_theta_max      38.41
_cell_measurement_theta_min      2.14
_cell_volume                     3557.41(15)
_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      250
_diffrn_measured_fraction_theta_full 0.796
_diffrn_measured_fraction_theta_max 0.796
_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    0.0325
_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            8233
_diffrn_reflns_theta_full        38.99
_diffrn_reflns_theta_max         38.99
_diffrn_reflns_theta_min         2.14
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SMART 1k'
_exptl_absorpt_coefficient_mu    1.121
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.866342
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1997)'
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_density_diffrn    1.605
_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         1.053
_refine_diff_density_min         -1.494
_refine_diff_density_rms         0.169
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.238
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         8233
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.238
_refine_ls_R_factor_all          0.0915
_refine_ls_R_factor_gt           0.0458
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0838P)²+5.4579P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1248
_refine_ls_wR_factor_ref         0.1905
_reflns_number_gt                5679
_reflns_number_total             8233
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja051233zsi20050224_053433.cif
_cod_data_source_block           final250k
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_database_code               4111770
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 0.53488(5) 0.5000 0.02014(11) Uani 1 2 d S . .
Mn2 Mn 0.425479(17) 0.43420(3) 0.536177(18) 0.02214(10) Uani 1 1 d . . .
O1 O 0.46151(9) 0.55632(18) 0.43720(10) 0.0284(4) Uani 1 1 d . . .
O2 O 0.34889(9) 0.52176(17) 0.43520(9) 0.0260(3) Uani 1 1 d . A .
O8 O 0.29818(10) 0.66204(19) 0.58097(10) 0.0338(4) Uani 1 1 d . A .
O9 O 0.40861(10) 0.5941(2) 0.60006(12) 0.0403(5) Uani 1 1 d . A .
O11 O 0.29950(10) 0.38481(19) 0.56719(10) 0.0334(4) Uani 1 1 d . A .
O12 O 0.39548(11) 0.3190(3) 0.63205(13) 0.0503(6) Uani 1 1 d . A .
C1 C 0.40056(11) 0.5683(2) 0.40449(11) 0.0207(4) Uani 1 1 d . . .
C2 C 0.38989(12) 0.6358(2) 0.32909(13) 0.0257(4) Uani 1 1 d . A .
C3 C 0.44318(13) 0.7100(3) 0.30432(15) 0.0355(6) Uani 1 1 d . . .
H3 H 0.4861 0.7152 0.3336 0.043 Uiso 1 1 calc R A .
C4 C 0.43220(14) 0.7236(3) 0.73568(16) 0.0371(6) Uani 1 1 d . . .
H4 H 0.4672 0.6713 0.7202 0.045 Uiso 1 1 calc R . .
C5 C 0.36964(12) 0.7347(2) 0.69019(13) 0.0280(4) Uani 1 1 d . A .
C6 C 0.31745(14) 0.8114(3) 0.71413(15) 0.0363(6) Uani 1 1 d . . .
H6 H 0.2757 0.8207 0.6833 0.044 Uiso 1 1 calc R . .
C7 C 0.32721(14) 0.6252(3) 0.28417(15) 0.0358(6) Uani 1 1 d . . .
H7 H 0.2915 0.5756 0.3007 0.043 Uiso 1 1 calc R A .
C8 C 0.35772(13) 0.6580(2) 0.61732(13) 0.0285(4) Uani 1 1 d . . .
C11 C 0.33023(13) 0.3339(3) 0.62571(14) 0.0304(5) Uani 1 1 d . . .
C12 C 0.28851(12) 0.2891(2) 0.68976(13) 0.0278(4) Uani 1 1 d . A .
C13 C 0.21697(13) 0.3121(3) 0.68735(15) 0.0348(6) Uani 1 1 d . . .
H13 H 0.1947 0.3533 0.6451 0.042 Uiso 1 1 calc R A .
C14 C 0.32140(13) 0.2261(3) 0.75212(16) 0.0380(6) Uani 1 1 d . . .
H14 H 0.3693 0.2093 0.7534 0.046 Uiso 1 1 calc R A .
O21 O 0.4300(3) 0.2724(4) 0.46289(19) 0.0433(8) Uani 0.864(3) 1 d P A 1
N21 N 0.3928(3) 0.0910(4) 0.4115(3) 0.0949(16) Uani 1 1 d . A 1
C21 C 0.3868(3) 0.1883(4) 0.4572(3) 0.0588(12) Uani 0.864(3) 1 d P A 1
H21 H 0.3480 0.1930 0.4862 0.071 Uiso 1 1 calc R A 1
C22 C 0.4484(4) 0.0828(6) 0.3572(4) 0.0959(19) Uani 1 1 d . A 1
H22A H 0.4287 0.0443 0.3097 0.115 Uiso 1 1 calc R A 1
H22B H 0.4624 0.1662 0.3444 0.115 Uiso 1 1 calc R A 1
C23 C 0.5110(5) 0.0141(8) 0.3848(5) 0.131(3) Uani 1 1 d . A 1
H23A H 0.5383 0.0627 0.4226 0.196 Uiso 1 1 calc R A 1
H23B H 0.5386 -0.0037 0.3421 0.196 Uiso 1 1 calc R A 1
H23C H 0.4975 -0.0622 0.4081 0.196 Uiso 1 1 calc R A 1
C24 C 0.3319(5) 0.0005(7) 0.4029(5) 0.127(3) Uani 1 1 d . A 1
H24A H 0.2890 0.0441 0.4123 0.152 Uiso 1 1 calc R A 1
H24B H 0.3272 -0.0296 0.3499 0.152 Uiso 1 1 calc R A 1
C25 C 0.3393(5) -0.0993(8) 0.4522(5) 0.145(4) Uani 1 1 d . A 1
H25A H 0.3877 -0.1242 0.4578 0.218 Uiso 1 1 calc R A 1
H25B H 0.3110 -0.1667 0.4313 0.218 Uiso 1 1 calc R A 1
H25C H 0.3243 -0.0765 0.5019 0.218 Uiso 1 1 calc R A 1
C31 C 0.4477(17) 0.214(3) 0.4233(18) 0.0588(12) Uani 0.136(3) 1 d P A 3
O31 O 0.427(2) 0.263(3) 0.4844(16) 0.0433(8) Uani 0.136(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 99.27(12) . 2_556
O8 Mn1 O11 170.84(8) . 2_556
O8 Mn1 O11 88.91(8) 2_556 2_556
O8 Mn1 O11 88.91(8) . .
O8 Mn1 O11 170.84(8) 2_556 .
O11 Mn1 O11 83.26(11) 2_556 .
O8 Mn1 O2 91.85(7) . .
O8 Mn1 O2 92.77(7) 2_556 .
O11 Mn1 O2 91.88(7) 2_556 .
O11 Mn1 O2 82.77(6) . .
O8 Mn1 O2 92.77(7) . 2_556
O8 Mn1 O2 91.85(7) 2_556 2_556
O11 Mn1 O2 82.77(6) 2_556 2_556
O11 Mn1 O2 91.88(7) . 2_556
O2 Mn1 O2 172.86(9) . 2_556
O31 Mn2 O9 169.0(8) . .
O31 Mn2 O21 10.4(8) . .
O9 Mn2 O21 172.82(15) . .
O31 Mn2 O1 95.2(11) . 5_666
O9 Mn2 O1 92.33(8) . 5_666
O21 Mn2 O1 94.47(14) . 5_666
O31 Mn2 O12 80.3(7) . .
O9 Mn2 O12 90.46(10) . .
O21 Mn2 O12 90.59(11) . .
O1 Mn2 O12 100.41(7) 5_666 .
O31 Mn2 O1 100.2(7) . .
O9 Mn2 O1 89.32(8) . .
O21 Mn2 O1 89.90(10) . .
O1 Mn2 O1 77.40(7) 5_666 .
O12 Mn2 O1 177.79(8) . .
O31 Mn2 O2 93.6(10) . .
O9 Mn2 O2 87.09(8) . .
O21 Mn2 O2 86.60(13) . .
O1 Mn2 O2 132.72(6) 5_666 .
O12 Mn2 O2 126.86(7) . .
O1 Mn2 O2 55.32(6) . .
C1 O1 Mn2 163.12(15) . 5_666
C1 O1 Mn2 94.23(13) . .
Mn2 O1 Mn2 102.60(7) 5_666 .
C1 O2 Mn1 152.84(16) . .
C1 O2 Mn2 90.68(13) . .
Mn1 O2 Mn2 98.53(6) . .
C8 O8 Mn1 129.62(17) . .
C8 O9 Mn2 137.69(17) . .
C11 O11 Mn1 156.3(2) . .
C11 O12 Mn2 100.29(16) . .
O1 C1 O2 119.66(19) . .
O1 C1 C2 120.02(19) . .
O2 C1 C2 120.3(2) . .
C7 C2 C3 119.9(2) . .
C7 C2 C1 120.3(2) . .
C3 C2 C1 119.8(2) . .
C4 C3 C2 119.8(2) 8_564 .
C4 C3 H3 120.1 8_564 .
C2 C3 H3 120.1 . .
C5 C4 C3 120.5(2) . 8_565
C5 C4 H4 119.7 . .
C3 C4 H4 119.7 8_565 .
C4 C5 C6 119.4(2) . .
C4 C5 C8 119.6(2) . .
C6 C5 C8 120.9(2) . .
C5 C6 C7 120.3(2) . 8_565
C5 C6 H6 119.8 . .
C7 C6 H6 119.8 8_565 .
C2 C7 C6 120.0(2) . 8_564
C2 C7 H7 120.0 . .
C6 C7 H7 120.0 8_564 .
O9 C8 O8 126.2(2) . .
O9 C8 C5 115.7(2) . .
O8 C8 C5 118.1(2) . .
O12 C11 O11 121.7(2) . .
O12 C11 C12 118.5(2) . .
O11 C11 C12 119.8(2) . .
C14 C12 C13 119.8(2) . .
C14 C12 C11 120.1(2) . .
C13 C12 C11 120.0(2) . .
C12 C13 C14 120.1(2) . 7_556
C12 C13 H13 120.0 . .
C14 C13 H13 120.0 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 126.0(3) . .
C21 N21 C22 121.8(4) . .
C21 N21 C24 117.9(6) . .
C22 N21 C24 118.9(5) . .
O21 C21 N21 123.2(5) . .
O21 C21 H21 118.4 . .
N21 C21 H21 118.4 . .
C23 C22 N21 115.8(7) . .
C23 C22 H22A 108.3 . .
N21 C22 H22A 108.3 . .
C23 C22 H22B 108.3 . .
N21 C22 H22B 108.3 . .
H22A C22 H22B 107.4 . .
C25 C24 N21 113.8(8) . .
C25 C24 H24A 108.8 . .
N21 C24 H24A 108.8 . .
C25 C24 H24B 108.8 . .
N21 C24 H24B 108.8 . .
H24A C24 H24B 107.7 . .
C31 O31 Mn2 138(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 O8 2.1198(18) .
Mn1 O8 2.1198(18) 2_556
Mn1 O11 2.1677(19) 2_556
Mn1 O11 2.1677(19) .
Mn1 O2 2.2750(15) .
Mn1 O2 2.2750(15) 2_556
Mn2 O31 2.06(3) .
Mn2 O9 2.089(2) .
Mn2 O21 2.165(4) .
Mn2 O1 2.1734(17) 5_666
Mn2 O12 2.186(2) .
Mn2 O1 2.3091(17) .
Mn2 O2 2.3846(17) .
O1 C1 1.260(3) .
O1 Mn2 2.1734(17) 5_666
O2 C1 1.261(3) .
O8 C8 1.256(3) .
O9 C8 1.247(3) .
O11 C11 1.257(3) .
O12 C11 1.253(3) .
C1 C2 1.495(3) .
C2 C7 1.380(3) .
C2 C3 1.389(3) .
C3 C4 1.390(3) 8_564
C3 H3 0.9300 .
C4 C5 1.383(4) .
C4 C3 1.390(3) 8_565
C4 H4 0.9300 .
C5 C6 1.384(3) .
C5 C8 1.511(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 1.495(3) .
C12 C14 1.384(3) .
C12 C13 1.386(3) .
C13 C14 1.388(3) 7_556
C13 H13 0.9300 .
C14 C13 1.388(3) 7_556
C14 H14 0.9300 .
O21 C21 1.225(6) .
N21 C21 1.325(6) .
N21 C22 1.475(8) .
N21 C24 1.517(8) .
C21 H21 0.9300 .
C22 C23 1.455(10) .
C22 H22A 0.9700 .
C22 H22B 0.9700 .
C23 H23A 0.9600 .
C23 H23B 0.9600 .
C23 H23C 0.9600 .
C24 C25 1.375(11) .
C24 H24A 0.9700 .
C24 H24B 0.9700 .
C25 H25A 0.9600 .
C25 H25B 0.9600 .
C25 H25C 0.9600 .
C31 O31 1.27(4) .
