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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/4/11/17/4111772.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_4111772
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                 94.6030(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.1115(5)
_cell_length_b                   10.8542(3)
_cell_length_c                   17.2982(4)
_cell_measurement_reflns_used    7228
_cell_measurement_temperature    300
_cell_measurement_theta_max      38.20
_cell_measurement_theta_min      2.21
_cell_volume                     3576.77(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      300
_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    0.0342
_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            8272
_diffrn_reflns_theta_full        38.93
_diffrn_reflns_theta_max         38.93
_diffrn_reflns_theta_min         2.14
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SMART 1k'
_exptl_absorpt_coefficient_mu    1.115
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.861913
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1997)'
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_density_diffrn    1.596
_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         0.837
_refine_diff_density_min         -1.253
_refine_diff_density_rms         0.145
_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         8272
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.192
_refine_ls_R_factor_all          0.0895
_refine_ls_R_factor_gt           0.0439
_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)+(0.0774P)²+3.6808P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1191
_refine_ls_wR_factor_ref         0.1716
_reflns_number_gt                5561
_reflns_number_total             8272
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja051233zsi20050224_053513.cif
_cod_data_source_block           final300k
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_database_code               4111772
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 0.53621(4) 0.5000 0.02197(10) Uani 1 2 d S . .
Mn2 Mn 0.425344(15) 0.43564(3) 0.536723(17) 0.02428(9) Uani 1 1 d . . .
O1 O 0.46160(8) 0.55593(16) 0.43702(9) 0.0314(3) Uani 1 1 d . . .
O2 O 0.34903(8) 0.52277(15) 0.43529(8) 0.0285(3) Uani 1 1 d . A .
O8 O 0.29852(9) 0.66262(18) 0.58100(10) 0.0379(4) Uani 1 1 d . A .
O9 O 0.40889(9) 0.5954(2) 0.60012(11) 0.0450(5) Uani 1 1 d . A .
O11 O 0.29899(9) 0.38727(18) 0.56790(9) 0.0375(4) Uani 1 1 d . A .
O12 O 0.39506(10) 0.3220(2) 0.63267(12) 0.0561(6) Uani 1 1 d . A .
C1 C 0.40062(10) 0.56874(18) 0.40458(10) 0.0225(3) Uani 1 1 d . . .
C2 C 0.39005(11) 0.6361(2) 0.32924(11) 0.0277(4) Uani 1 1 d . A .
C3 C 0.44306(12) 0.7101(3) 0.30465(14) 0.0396(6) Uani 1 1 d . . .
H3 H 0.4858 0.7156 0.3341 0.048 Uiso 1 1 calc R A .
C4 C 0.43221(13) 0.7240(3) 0.73598(15) 0.0419(6) Uani 1 1 d . . .
H4 H 0.4673 0.6723 0.7205 0.050 Uiso 1 1 calc R . .
C5 C 0.36975(11) 0.7344(2) 0.69030(12) 0.0312(4) Uani 1 1 d . A .
C6 C 0.31770(13) 0.8109(3) 0.71418(14) 0.0401(6) Uani 1 1 d . . .
H6 H 0.2759 0.8200 0.6833 0.048 Uiso 1 1 calc R . .
C7 C 0.32744(12) 0.6259(3) 0.28411(14) 0.0392(6) Uani 1 1 d . . .
H7 H 0.2917 0.5766 0.3005 0.047 Uiso 1 1 calc R A .
C8 C 0.35795(12) 0.6590(2) 0.61738(12) 0.0314(4) Uani 1 1 d . . .
C11 C 0.32977(12) 0.3362(2) 0.62609(13) 0.0336(5) Uani 1 1 d . . .
C12 C 0.28831(11) 0.2902(2) 0.69008(12) 0.0305(4) Uani 1 1 d . A .
C13 C 0.21698(12) 0.3137(3) 0.68802(14) 0.0380(5) Uani 1 1 d . . .
H13 H 0.1947 0.3560 0.6463 0.046 Uiso 1 1 calc R A .
C14 C 0.32122(12) 0.2261(3) 0.75169(15) 0.0414(6) Uani 1 1 d . . .
H14 H 0.3690 0.2095 0.7528 0.050 Uiso 1 1 calc R A .
O21 O 0.4292(3) 0.2735(5) 0.4633(2) 0.0499(9) Uani 0.825(3) 1 d P A 1
N21 N 0.3939(3) 0.0921(4) 0.4134(3) 0.1101(17) Uani 1 1 d . A 1
C21 C 0.3870(3) 0.1902(4) 0.4585(3) 0.0663(12) Uani 0.825(3) 1 d P A 1
H21 H 0.3481 0.1948 0.4874 0.080 Uiso 1 1 calc R A 1
C22 C 0.4483(4) 0.0835(6) 0.3579(4) 0.116(2) Uani 1 1 d . A 1
H22A H 0.4274 0.0462 0.3106 0.139 Uiso 1 1 calc R A 1
H22B H 0.4624 0.1664 0.3451 0.139 Uiso 1 1 calc R A 1
C23 C 0.5106(5) 0.0146(8) 0.3831(6) 0.158(4) Uani 1 1 d . A 1
H23A H 0.5390 0.0622 0.4204 0.237 Uiso 1 1 calc R A 1
H23B H 0.5368 -0.0028 0.3394 0.237 Uiso 1 1 calc R A 1
H23C H 0.4973 -0.0613 0.4064 0.237 Uiso 1 1 calc R A 1
C24 C 0.3319(5) 0.0027(7) 0.4044(5) 0.151(3) Uani 1 1 d . A 1
H24A H 0.2894 0.0466 0.4146 0.181 Uiso 1 1 calc R A 1
H24B H 0.3265 -0.0260 0.3511 0.181 Uiso 1 1 calc R A 1
C25 C 0.3390(6) -0.0946(8) 0.4515(6) 0.173(4) Uani 1 1 d . A 1
H25A H 0.3878 -0.1157 0.4601 0.259 Uiso 1 1 calc R A 1
H25B H 0.3135 -0.1632 0.4281 0.259 Uiso 1 1 calc R A 1
H25C H 0.3207 -0.0750 0.5001 0.259 Uiso 1 1 calc R A 1
C31 C 0.4464(13) 0.218(2) 0.4272(13) 0.0663(12) Uani 0.175(3) 1 d P A 3
O31 O 0.4268(19) 0.268(3) 0.4845(13) 0.0499(9) Uani 0.175(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 99.37(11) . 2_556
O8 Mn1 O11 171.14(8) . 2_556
O8 Mn1 O11 88.71(7) 2_556 2_556
O8 Mn1 O11 88.71(7) . .
O8 Mn1 O11 171.14(8) 2_556 .
O11 Mn1 O11 83.47(11) 2_556 .
O8 Mn1 O2 93.05(6) . 2_556
O8 Mn1 O2 91.69(6) 2_556 2_556
O11 Mn1 O2 83.04(6) 2_556 2_556
O11 Mn1 O2 91.48(6) . 2_556
O8 Mn1 O2 91.69(6) . .
O8 Mn1 O2 93.05(6) 2_556 .
O11 Mn1 O2 91.48(6) 2_556 .
O11 Mn1 O2 83.04(6) . .
O2 Mn1 O2 172.66(9) 2_556 .
O31 Mn2 O9 169.9(8) . .
O31 Mn2 O1 94.7(11) . 5_666
O9 Mn2 O1 92.54(7) . 5_666
O31 Mn2 O21 9.5(7) . .
O9 Mn2 O21 172.64(18) . .
O1 Mn2 O21 94.39(18) 5_666 .
O31 Mn2 O12 81.2(7) . .
O9 Mn2 O12 90.55(10) . .
O1 Mn2 O12 100.64(6) 5_666 .
O21 Mn2 O12 90.61(13) . .
O31 Mn2 O1 99.0(7) . .
O9 Mn2 O1 89.40(8) . .
O1 Mn2 O1 77.28(6) 5_666 .
O21 Mn2 O1 89.71(12) . .
O12 Mn2 O1 177.92(7) . .
O31 Mn2 O2 93.2(9) . .
O9 Mn2 O2 87.02(7) . .
O1 Mn2 O2 132.52(5) 5_666 .
O21 Mn2 O2 86.47(16) . .
O12 Mn2 O2 126.84(6) . .
O1 Mn2 O2 55.24(5) . .
C1 O1 Mn2 163.09(13) . 5_666
C1 O1 Mn2 94.17(11) . .
Mn2 O1 Mn2 102.72(6) 5_666 .
C1 O2 Mn1 152.92(15) . .
C1 O2 Mn2 90.81(12) . .
Mn1 O2 Mn2 98.45(5) . .
C8 O8 Mn1 129.91(16) . .
C8 O9 Mn2 137.50(16) . .
C11 O11 Mn1 156.92(19) . .
C11 O12 Mn2 100.64(14) . .
O2 C1 O1 119.72(17) . .
O2 C1 C2 120.40(18) . .
O1 C1 C2 119.87(17) . .
C7 C2 C3 119.67(19) . .
C7 C2 C1 120.31(18) . .
C3 C2 C1 120.02(19) . .
C2 C3 C4 119.9(2) . 8_564
C2 C3 H3 120.1 . .
C4 C3 H3 120.1 8_564 .
C5 C4 C3 120.7(2) . 8_565
C5 C4 H4 119.7 . .
C3 C4 H4 119.7 8_565 .
C4 C5 C6 119.1(2) . .
C4 C5 C8 119.9(2) . .
C6 C5 C8 120.9(2) . .
C5 C6 C7 120.4(2) . 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 115.7(2) . .
O8 C8 C5 118.17(19) . .
O12 C11 O11 121.77(19) . .
O12 C11 C12 118.3(2) . .
O11 C11 C12 119.9(2) . .
C14 C12 C13 119.94(19) . .
C14 C12 C11 120.2(2) . .
C13 C12 C11 119.85(19) . .
C12 C13 C14 120.0(2) . 7_556
C12 C13 H13 120.0 . .
C14 C13 H13 120.0 7_556 .
C12 C14 C13 120.1(2) . 7_556
C12 C14 H14 120.0 . .
C13 C14 H14 120.0 7_556 .
C21 O21 Mn2 126.2(4) . .
C21 N21 C22 122.7(5) . .
C21 N21 C24 116.9(6) . .
C22 N21 C24 118.3(5) . .
O21 C21 N21 122.6(5) . .
O21 C21 H21 118.7 . .
N21 C21 H21 118.7 . .
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 113.5(9) . .
C25 C24 H24A 108.9 . .
N21 C24 H24A 108.9 . .
C25 C24 H24B 108.9 . .
N21 C24 H24B 108.9 . .
H24A C24 H24B 107.7 . .
C31 O31 Mn2 141(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 O8 2.1207(16) .
Mn1 O8 2.1207(16) 2_556
Mn1 O11 2.1664(17) 2_556
Mn1 O11 2.1664(17) .
Mn1 O2 2.2795(14) 2_556
Mn1 O2 2.2795(14) .
Mn2 O31 2.03(3) .
Mn2 O9 2.0892(18) .
Mn2 O1 2.1739(16) 5_666
Mn2 O21 2.175(5) .
Mn2 O12 2.1827(18) .
Mn2 O1 2.3132(15) .
Mn2 O2 2.3852(16) .
O1 C1 1.260(2) .
O1 Mn2 2.1739(16) 5_666
O2 C1 1.260(2) .
O8 C8 1.254(3) .
O9 C8 1.249(3) .
O11 C11 1.254(3) .
O12 C11 1.253(3) .
C1 C2 1.494(3) .
C2 C7 1.380(3) .
C2 C3 1.386(3) .
C3 C4 1.388(3) 8_564
C3 H3 0.9300 .
C4 C5 1.382(3) .
C4 C3 1.388(3) 8_565
C4 H4 0.9300 .
C5 C6 1.383(3) .
C5 C8 1.506(3) .
C6 C7 1.390(3) 8_565
C6 H6 0.9300 .
C7 C6 1.390(3) 8_564
C7 H7 0.9300 .
C11 C12 1.498(3) .
C12 C14 1.381(3) .
C12 C13 1.384(3) .
C13 C14 1.389(3) 7_556
C13 H13 0.9300 .
C14 C13 1.389(3) 7_556
C14 H14 0.9300 .
O21 C21 1.211(7) .
N21 C21 1.333(6) .
N21 C22 1.473(8) .
N21 C24 1.531(8) .
C21 H21 0.9300 .
C22 C23 1.443(10) .
C22 H22A 0.9700 .
C22 H22B 0.9700 .
C23 H23A 0.9600 .
C23 H23B 0.9600 .
C23 H23C 0.9600 .
C24 C25 1.335(11) .
C24 H24A 0.9700 .
C24 H24B 0.9700 .
C25 H25A 0.9600 .
C25 H25B 0.9600 .
C25 H25C 0.9600 .
C31 O31 1.22(3) .
