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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/4/11/17/4111769.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_4111769
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                 94.4500(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.0977(4)
_cell_length_b                   10.7768(2)
_cell_length_c                   17.3233(4)
_cell_measurement_reflns_used    7775
_cell_measurement_temperature    225
_cell_measurement_theta_max      38.37
_cell_measurement_theta_min      2.14
_cell_volume                     3554.60(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      225
_diffrn_measured_fraction_theta_full 0.797
_diffrn_measured_fraction_theta_max 0.797
_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    0.0314
_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            8210
_diffrn_reflns_theta_full        38.95
_diffrn_reflns_theta_max         38.95
_diffrn_reflns_theta_min         2.23
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SMART 1k'
_exptl_absorpt_coefficient_mu    1.122
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.869449
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1997)'
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_density_diffrn    1.606
_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         1.222
_refine_diff_density_min         -1.669
_refine_diff_density_rms         0.182
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.228
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         8210
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.228
_refine_ls_R_factor_all          0.0911
_refine_ls_R_factor_gt           0.0473
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0787P)²+9.2590P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1246
_refine_ls_wR_factor_ref         0.1934
_reflns_number_gt                5783
_reflns_number_total             8210
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja051233zsi20050224_053414.cif
_cod_data_source_block           final225k
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_database_code               4111769
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 0.53416(5) 0.5000 0.01876(11) Uani 1 2 d S . .
Mn2 Mn 0.425528(18) 0.43346(4) 0.53591(2) 0.02061(10) Uani 1 1 d . . .
O1 O 0.46146(10) 0.55639(19) 0.43731(11) 0.0264(4) Uani 1 1 d . . .
O2 O 0.34875(9) 0.52129(18) 0.43502(10) 0.0245(3) Uani 1 1 d . A .
O8 O 0.29806(11) 0.6616(2) 0.58103(11) 0.0314(4) Uani 1 1 d . A .
O9 O 0.40850(11) 0.5932(2) 0.60007(13) 0.0377(5) Uani 1 1 d . A .
O11 O 0.29970(11) 0.3836(2) 0.56684(11) 0.0312(4) Uani 1 1 d . A .
O12 O 0.39565(11) 0.3173(3) 0.63172(14) 0.0468(7) Uani 1 1 d . A .
C1 C 0.40053(12) 0.5683(2) 0.40446(12) 0.0194(4) Uani 1 1 d . . .
C2 C 0.38993(13) 0.6357(2) 0.32910(13) 0.0241(4) Uani 1 1 d . A .
C3 C 0.44319(14) 0.7101(3) 0.30415(16) 0.0326(6) Uani 1 1 d . . .
H3 H 0.4861 0.7154 0.3333 0.039 Uiso 1 1 calc R A .
C4 C 0.43208(15) 0.7234(3) 0.73552(17) 0.0341(6) Uani 1 1 d . . .
H4 H 0.4671 0.6710 0.7200 0.041 Uiso 1 1 calc R . .
C5 C 0.36953(13) 0.7343(3) 0.69001(14) 0.0259(5) Uani 1 1 d . A .
C6 C 0.31733(15) 0.8114(3) 0.71402(16) 0.0334(6) Uani 1 1 d . . .
H6 H 0.2755 0.8205 0.6833 0.040 Uiso 1 1 calc R . .
C7 C 0.32719(15) 0.6248(3) 0.28406(16) 0.0331(6) Uani 1 1 d . . .
H7 H 0.2915 0.5749 0.3005 0.040 Uiso 1 1 calc R A .
C8 C 0.35750(14) 0.6576(3) 0.61734(14) 0.0266(5) Uani 1 1 d . . .
C11 C 0.33051(14) 0.3326(3) 0.62543(15) 0.0284(5) Uani 1 1 d . . .
C12 C 0.28852(13) 0.2887(3) 0.68956(14) 0.0261(5) Uani 1 1 d . A .
C13 C 0.21709(14) 0.3119(3) 0.68718(16) 0.0328(6) Uani 1 1 d . . .
H13 H 0.1948 0.3529 0.6449 0.039 Uiso 1 1 calc R A .
C14 C 0.32148(14) 0.2260(3) 0.75217(17) 0.0359(7) Uani 1 1 d . . .
H14 H 0.3693 0.2092 0.7536 0.043 Uiso 1 1 calc R A .
O21 O 0.4303(2) 0.2720(4) 0.4628(2) 0.0401(8) Uani 0.880(4) 1 d P A 1
N21 N 0.3919(3) 0.0907(4) 0.4103(3) 0.0849(16) Uani 1 1 d . A 1
C21 C 0.3864(3) 0.1877(4) 0.4563(3) 0.0538(11) Uani 0.880(4) 1 d P A 1
H21 H 0.3476 0.1925 0.4854 0.065 Uiso 1 1 calc R A 1
C22 C 0.4484(4) 0.0831(6) 0.3569(4) 0.0859(19) Uani 1 1 d . A 1
H22A H 0.4292 0.0450 0.3090 0.103 Uiso 1 1 calc R A 1
H22B H 0.4625 0.1668 0.3446 0.103 Uiso 1 1 calc R A 1
C23 C 0.5114(5) 0.0133(8) 0.3853(5) 0.119(3) Uani 1 1 d . A 1
H23A H 0.5374 0.0605 0.4248 0.178 Uiso 1 1 calc R A 1
H23B H 0.5402 -0.0015 0.3432 0.178 Uiso 1 1 calc R A 1
H23C H 0.4976 -0.0645 0.4064 0.178 Uiso 1 1 calc R A 1
C24 C 0.3316(5) 0.0003(7) 0.4022(5) 0.117(3) Uani 1 1 d . A 1
H24A H 0.2886 0.0438 0.4115 0.140 Uiso 1 1 calc R A 1
H24B H 0.3268 -0.0304 0.3494 0.140 Uiso 1 1 calc R A 1
C25 C 0.3392(5) -0.1006(8) 0.4525(5) 0.125(3) Uani 1 1 d . A 1
H25A H 0.3871 -0.1281 0.4561 0.188 Uiso 1 1 calc R A 1
H25B H 0.3092 -0.1670 0.4333 0.188 Uiso 1 1 calc R A 1
H25C H 0.3265 -0.0763 0.5029 0.188 Uiso 1 1 calc R A 1
C31 C 0.449(2) 0.213(3) 0.425(2) 0.0538(11) Uani 0.120(4) 1 d P A 3
O31 O 0.426(2) 0.259(4) 0.4834(19) 0.0401(8) Uani 0.120(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 99.30(12) . 2_556
O8 Mn1 O11 170.63(9) . 2_556
O8 Mn1 O11 88.98(8) 2_556 2_556
O8 Mn1 O11 88.98(8) . .
O8 Mn1 O11 170.63(9) 2_556 .
O11 Mn1 O11 83.12(12) 2_556 .
O8 Mn1 O2 91.96(7) . .
O8 Mn1 O2 92.57(7) 2_556 .
O11 Mn1 O2 92.03(7) 2_556 .
O11 Mn1 O2 82.72(7) . .
O8 Mn1 O2 92.57(7) . 2_556
O8 Mn1 O2 91.96(7) 2_556 2_556
O11 Mn1 O2 82.72(7) 2_556 2_556
O11 Mn1 O2 92.03(7) . 2_556
O2 Mn1 O2 173.01(10) . 2_556
O31 Mn2 O9 168.5(9) . .
O31 Mn2 O21 10.6(8) . .
O9 Mn2 O21 172.94(14) . .
O31 Mn2 O1 95.8(12) . 5_666
O9 Mn2 O1 92.17(8) . 5_666
O21 Mn2 O1 94.53(14) . 5_666
O31 Mn2 O12 80.0(8) . .
O9 Mn2 O12 90.42(11) . .
O21 Mn2 O12 90.55(12) . .
O1 Mn2 O12 100.36(8) 5_666 .
O31 Mn2 O1 100.5(8) . .
O9 Mn2 O1 89.32(9) . .
O21 Mn2 O1 89.98(10) . .
O1 Mn2 O1 77.40(7) 5_666 .
O12 Mn2 O1 177.73(8) . .
O31 Mn2 O2 93.5(11) . .
O9 Mn2 O2 87.17(8) . .
O21 Mn2 O2 86.65(13) . .
O1 Mn2 O2 132.76(6) 5_666 .
O12 Mn2 O2 126.87(7) . .
O1 Mn2 O2 55.37(6) . .
C1 O1 Mn2 163.02(16) . 5_666
C1 O1 Mn2 94.33(14) . .
Mn2 O1 Mn2 102.60(7) 5_666 .
C1 O2 Mn1 152.74(17) . .
C1 O2 Mn2 90.55(14) . .
Mn1 O2 Mn2 98.48(6) . .
C8 O8 Mn1 129.62(18) . .
C8 O9 Mn2 137.81(19) . .
C11 O11 Mn1 156.1(2) . .
C11 O12 Mn2 100.04(17) . .
O1 C1 O2 119.6(2) . .
O1 C1 C2 120.1(2) . .
O2 C1 C2 120.3(2) . .
C7 C2 C3 119.7(2) . .
C7 C2 C1 120.3(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(3) . 8_565
C5 C4 H4 119.6 . .
C3 C4 H4 119.6 8_565 .
C4 C5 C6 119.3(2) . .
C4 C5 C8 119.8(2) . .
C6 C5 C8 120.8(2) . .
C5 C6 C7 120.3(3) . 8_565
C5 C6 H6 119.8 . .
C7 C6 H6 119.8 8_565 .
C2 C7 C6 120.1(2) . 8_564
C2 C7 H7 119.9 . .
C6 C7 H7 119.9 8_564 .
O9 C8 O8 126.1(2) . .
O9 C8 C5 115.6(2) . .
O8 C8 C5 118.2(2) . .
O12 C11 O11 121.8(2) . .
O12 C11 C12 118.7(2) . .
O11 C11 C12 119.5(2) . .
C13 C12 C14 119.8(2) . .
C13 C12 C11 120.3(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 119.9(2) . 7_556
C12 C14 H14 120.0 . .
C13 C14 H14 120.0 7_556 .
C21 O21 Mn2 125.9(3) . .
C21 N21 C22 121.1(4) . .
C21 N21 C24 118.1(6) . .
C22 N21 C24 119.7(5) . .
O21 C21 N21 123.4(5) . .
O21 C21 H21 118.3 . .
N21 C21 H21 118.3 . .
C23 C22 N21 115.9(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 113.9(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 137(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 O8 2.1211(19) .
Mn1 O8 2.1211(19) 2_556
Mn1 O11 2.169(2) 2_556
Mn1 O11 2.169(2) .
Mn1 O2 2.2743(17) .
Mn1 O2 2.2743(17) 2_556
Mn2 O31 2.09(4) .
Mn2 O9 2.088(2) .
Mn2 O21 2.159(4) .
Mn2 O1 2.1748(19) 5_666
Mn2 O12 2.189(2) .
Mn2 O1 2.3078(18) .
Mn2 O2 2.3882(19) .
O1 C1 1.262(3) .
O1 Mn2 2.1748(19) 5_666
O2 C1 1.263(3) .
O8 C8 1.255(3) .
O9 C8 1.251(3) .
O11 C11 1.259(3) .
O12 C11 1.251(3) .
C1 C2 1.494(3) .
C2 C7 1.383(4) .
C2 C3 1.390(4) .
C3 C4 1.390(4) 8_564
C3 H3 0.9300 .
C4 C5 1.384(4) .
C4 C3 1.390(4) 8_565
C4 H4 0.9300 .
C5 C6 1.386(4) .
C5 C8 1.509(3) .
C6 C7 1.395(4) 8_565
C6 H6 0.9300 .
C7 C6 1.395(4) 8_564
C7 H7 0.9300 .
C11 C12 1.496(3) .
C12 C13 1.384(4) .
C12 C14 1.387(4) .
C13 C14 1.390(3) 7_556
C13 H13 0.9300 .
C14 C13 1.390(3) 7_556
C14 H14 0.9300 .
O21 C21 1.236(6) .
N21 C21 1.324(6) .
N21 C22 1.477(8) .
N21 C24 1.507(8) .
C21 H21 0.9300 .
C22 C23 1.471(11) .
C22 H22A 0.9700 .
C22 H22B 0.9700 .
C23 H23A 0.9600 .
C23 H23B 0.9600 .
C23 H23C 0.9600 .
C24 C25 1.394(11) .
C24 H24A 0.9700 .
C24 H24B 0.9700 .
C25 H25A 0.9600 .
C25 H25B 0.9600 .
C25 H25C 0.9600 .
C31 O31 1.23(5) .
