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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/4/11/17/4111764.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_4111764
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                 94.27(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.042(4)
_cell_length_b                   10.657(2)
_cell_length_c                   17.324(4)
_cell_measurement_reflns_used    7933
_cell_measurement_temperature    100
_cell_measurement_theta_max      38.24
_cell_measurement_theta_min      2.15
_cell_volume                     3505.8(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      100
_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    0.0391
_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            8132
_diffrn_reflns_theta_full        39.07
_diffrn_reflns_theta_max         39.07
_diffrn_reflns_theta_min         2.25
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SMART 1k'
_exptl_absorpt_coefficient_mu    1.137
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.874897
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1997)'
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_density_diffrn    1.628
_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         1.700
_refine_diff_density_min         -2.482
_refine_diff_density_rms         0.246
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.203
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         8132
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.203
_refine_ls_R_factor_all          0.1016
_refine_ls_R_factor_gt           0.0517
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0706P)²+24.9828P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1260
_refine_ls_wR_factor_ref         0.2060
_reflns_number_gt                5743
_reflns_number_total             8132
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja051233zsi20050224_053230.cif
_cod_data_source_block           final100k
_cod_original_cell_volume        3505.9(12)
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_database_code               4111764
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 0.53086(6) 0.5000 0.01283(12) Uani 1 2 d S . .
Mn2 Mn 0.42577(2) 0.43047(4) 0.53498(2) 0.01397(10) Uani 1 1 d . . .
O1 O 0.46128(11) 0.5571(2) 0.43751(12) 0.0179(4) Uani 1 1 d . . .
O2 O 0.34835(11) 0.5187(2) 0.43480(12) 0.0173(4) Uani 1 1 d . A .
O8 O 0.29717(12) 0.6600(2) 0.58103(12) 0.0197(4) Uani 1 1 d . A .
O9 O 0.40804(12) 0.5903(3) 0.60012(14) 0.0243(5) Uani 1 1 d . A .
O11 O 0.30077(12) 0.3784(2) 0.56546(12) 0.0197(4) Uani 1 1 d . A .
O12 O 0.39691(13) 0.3119(3) 0.63098(15) 0.0303(6) Uani 1 1 d . A .
C1 C 0.40014(14) 0.5675(3) 0.40434(14) 0.0136(4) Uani 1 1 d . . .
C2 C 0.38947(15) 0.6347(3) 0.32879(16) 0.0170(5) Uani 1 1 d . A .
C3 C 0.44292(16) 0.7099(3) 0.30343(17) 0.0206(6) Uani 1 1 d . . .
H3 H 0.4860 0.7152 0.3323 0.025 Uiso 1 1 calc R A .
C4 C 0.43186(17) 0.7228(3) 0.73493(18) 0.0220(6) Uani 1 1 d . . .
H4 H 0.4669 0.6696 0.7194 0.026 Uiso 1 1 calc R . .
C5 C 0.36918(16) 0.7343(3) 0.68968(16) 0.0173(5) Uani 1 1 d . A .
C6 C 0.31685(17) 0.8125(3) 0.71361(18) 0.0226(6) Uani 1 1 d . . .
H6 H 0.2751 0.8221 0.6828 0.027 Uiso 1 1 calc R . .
C7 C 0.32652(17) 0.6232(3) 0.28364(18) 0.0233(6) Uani 1 1 d . . .
H7 H 0.2908 0.5725 0.3001 0.028 Uiso 1 1 calc R A .
C8 C 0.35682(16) 0.6563(3) 0.61737(16) 0.0181(5) Uani 1 1 d . . .
C11 C 0.33148(16) 0.3277(3) 0.62464(17) 0.0194(5) Uani 1 1 d . . .
C12 C 0.28903(15) 0.2861(3) 0.68912(16) 0.0175(5) Uani 1 1 d . A .
C13 C 0.21722(17) 0.3089(4) 0.68572(18) 0.0236(6) Uani 1 1 d . . .
H13 H 0.1951 0.3481 0.6425 0.028 Uiso 1 1 calc R A .
C14 C 0.32196(16) 0.2267(4) 0.75331(19) 0.0247(7) Uani 1 1 d . . .
H14 H 0.3701 0.2107 0.7555 0.030 Uiso 1 1 calc R A .
O21 O 0.4311(2) 0.2688(3) 0.46158(18) 0.0238(6) Uani 0.908(4) 1 d P A 1
N21 N 0.3909(3) 0.0879(4) 0.4062(3) 0.0463(10) Uani 1 1 d . A 1
C21 C 0.3865(2) 0.1838(4) 0.4539(2) 0.0306(8) Uani 0.908(4) 1 d P A 1
H21 H 0.3478 0.1878 0.4835 0.037 Uiso 1 1 calc R A 1
C22 C 0.4496(3) 0.0801(5) 0.3552(3) 0.0492(12) Uani 1 1 d . A 1
H22A H 0.4640 0.1647 0.3430 0.059 Uiso 1 1 calc R A 1
H22B H 0.4324 0.0403 0.3071 0.059 Uiso 1 1 calc R A 1
C23 C 0.5123(4) 0.0101(6) 0.3879(4) 0.0624(16) Uani 1 1 d . A 1
H23A H 0.5339 0.0551 0.4314 0.094 Uiso 1 1 calc R A 1
H23B H 0.5454 0.0013 0.3490 0.094 Uiso 1 1 calc R A 1
H23C H 0.4982 -0.0715 0.4043 0.094 Uiso 1 1 calc R A 1
C24 C 0.3334(4) -0.0053(6) 0.3990(4) 0.0647(18) Uani 1 1 d . A 1
H24A H 0.2892 0.0372 0.4058 0.078 Uiso 1 1 calc R A 1
H24B H 0.3307 -0.0396 0.3470 0.078 Uiso 1 1 calc R A 1
C25 C 0.3412(4) -0.1097(5) 0.4547(3) 0.0581(15) Uani 1 1 d . A 1
H25A H 0.3858 -0.1500 0.4503 0.087 Uiso 1 1 calc R A 1
H25B H 0.3039 -0.1693 0.4437 0.087 Uiso 1 1 calc R A 1
H25C H 0.3388 -0.0778 0.5062 0.087 Uiso 1 1 calc R A 1
C31 C 0.453(2) 0.213(4) 0.421(2) 0.0306(8) Uani 0.092(4) 1 d P A 3
O31 O 0.431(2) 0.251(4) 0.483(2) 0.0238(6) Uani 0.092(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 98.92(14) . 2_556
O8 Mn1 O11 170.00(9) . 2_556
O8 Mn1 O11 89.42(9) 2_556 2_556
O8 Mn1 O11 89.42(9) . .
O8 Mn1 O11 170.00(9) 2_556 .
O11 Mn1 O11 82.87(13) 2_556 .
O8 Mn1 O2 91.85(8) . 2_556
O8 Mn1 O2 92.42(8) 2_556 2_556
O11 Mn1 O2 82.22(8) 2_556 2_556
O11 Mn1 O2 92.83(8) . 2_556
O8 Mn1 O2 92.42(9) . .
O8 Mn1 O2 91.85(8) 2_556 .
O11 Mn1 O2 92.83(8) 2_556 .
O11 Mn1 O2 82.22(8) . .
O2 Mn1 O2 173.42(12) 2_556 .
O9 Mn2 O31 169.2(10) . .
O9 Mn2 O21 172.94(12) . .
O31 Mn2 O21 11.1(9) . .
O9 Mn2 O1 91.66(9) . 5_666
O31 Mn2 O1 94.0(13) . 5_666
O21 Mn2 O1 95.13(12) . 5_666
O9 Mn2 O12 90.02(11) . .
O31 Mn2 O12 80.0(9) . .
O21 Mn2 O12 90.71(12) . .
O1 Mn2 O12 99.73(9) 5_666 .
O9 Mn2 O1 89.22(10) . .
O31 Mn2 O1 100.9(9) . .
O21 Mn2 O1 90.37(10) . .
O1 Mn2 O1 77.58(9) 5_666 .
O12 Mn2 O1 177.18(9) . .
O9 Mn2 O2 87.45(9) . .
O31 Mn2 O2 95.3(12) . .
O21 Mn2 O2 86.51(11) . .
O1 Mn2 O2 133.14(8) 5_666 .
O12 Mn2 O2 127.11(9) . .
O1 Mn2 O2 55.57(7) . .
C1 O1 Mn2 163.26(19) . 5_666
C1 O1 Mn2 94.26(16) . .
Mn2 O1 Mn2 102.42(9) 5_666 .
C1 O2 Mn1 152.3(2) . .
C1 O2 Mn2 90.39(17) . .
Mn1 O2 Mn2 98.58(8) . .
C8 O8 Mn1 129.3(2) . .
C8 O9 Mn2 138.2(2) . .
C11 O11 Mn1 155.1(2) . .
C11 O12 Mn2 99.20(19) . .
O1 C1 O2 119.6(2) . .
O1 C1 C2 120.1(2) . .
O2 C1 C2 120.3(3) . .
C7 C2 C3 119.6(3) . .
C7 C2 C1 120.5(3) . .
C3 C2 C1 119.9(3) . .
C4 C3 C2 119.9(3) 8_564 .
C4 C3 H3 120.0 8_564 .
C2 C3 H3 120.0 . .
C5 C4 C3 120.5(3) . 8_565
C5 C4 H4 119.7 . .
C3 C4 H4 119.7 8_565 .
C4 C5 C6 119.5(3) . .
C4 C5 C8 119.8(3) . .
C6 C5 C8 120.6(3) . .
C5 C6 C7 120.3(3) . 8_565
C5 C6 H6 119.8 . .
C7 C6 H6 119.8 8_565 .
C2 C7 C6 120.0(3) . 8_564
C2 C7 H7 120.0 . .
C6 C7 H7 120.0 8_564 .
O9 C8 O8 125.9(3) . .
O9 C8 C5 115.5(3) . .
O8 C8 C5 118.5(3) . .
O12 C11 O11 121.7(3) . .
O12 C11 C12 118.9(3) . .
O11 C11 C12 119.4(3) . .
C13 C12 C14 120.0(3) . .
C13 C12 C11 120.2(3) . .
C14 C12 C11 119.8(3) . .
C12 C13 C14 120.2(3) . 7_556
C12 C13 H13 119.9 . .
C14 C13 H13 119.9 7_556 .
C12 C14 C13 119.8(3) . 7_556
C12 C14 H14 120.1 . .
C13 C14 H14 120.1 7_556 .
C21 O21 Mn2 126.0(3) . .
C21 N21 C22 120.2(4) . .
C21 N21 C24 119.5(5) . .
C22 N21 C24 120.1(5) . .
O21 C21 N21 123.9(4) . .
O21 C21 H21 118.0 . .
N21 C21 H21 118.0 . .
N21 C22 C23 115.1(5) . .
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 114.6(5) . .
C25 C24 H24A 108.6 . .
N21 C24 H24A 108.6 . .
C25 C24 H24B 108.6 . .
N21 C24 H24B 108.6 . .
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 2.262(2) 2_556
Mn1 O2 2.262(2) .
Mn2 O9 2.084(2) .
Mn2 O31 2.12(4) .
Mn2 O21 2.148(3) .
Mn2 O1 2.172(2) 5_666
Mn2 O12 2.191(2) .
Mn2 O1 2.302(2) .
Mn2 O2 2.385(2) .
O1 C1 1.264(3) .
O1 Mn2 2.172(2) 5_666
O2 C1 1.265(3) .
O8 C8 1.258(4) .
O9 C8 1.256(4) .
O11 C11 1.263(4) .
O12 C11 1.254(4) .
C1 C2 1.492(4) .
C2 C7 1.387(4) .
C2 C3 1.392(4) .
C3 C4 1.389(4) 8_564
C3 H3 0.9300 .
C4 C5 1.384(4) .
C4 C3 1.389(4) 8_565
C4 H4 0.9300 .
C5 C6 1.386(4) .
C5 C8 1.507(4) .
C6 C7 1.394(4) 8_565
C6 H6 0.9300 .
C7 C6 1.394(4) 8_564
C7 H7 0.9300 .
C11 C12 1.494(4) .
C12 C13 1.386(4) .
C12 C14 1.388(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 1.242(5) .
N21 C21 1.321(6) .
N21 C22 1.477(7) .
N21 C24 1.477(6) .
C21 H21 0.9300 .
C22 C23 1.485(9) .
C22 H22A 0.9700 .
C22 H22B 0.9700 .
C23 H23A 0.9600 .
C23 H23B 0.9600 .
C23 H23C 0.9600 .
C24 C25 1.472(8) .
C24 H24A 0.9700 .
C24 H24B 0.9700 .
C25 H25A 0.9600 .
C25 H25B 0.9600 .
C25 H25C 0.9600 .
C31 O31 1.24(6) .
