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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/4/11/17/4111763.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_4111763
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                 94.24(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.117(4)
_cell_length_b                   10.657(2)
_cell_length_c                   17.412(4)
_cell_measurement_reflns_used    8460
_cell_measurement_temperature    20
_cell_measurement_theta_max      29.17
_cell_measurement_theta_min      2.68
_cell_volume                     3537.6(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      20
_diffrn_measured_fraction_theta_full 0.777
_diffrn_measured_fraction_theta_max 0.777
_diffrn_measurement_device_type  'four-circle diffractometer'
_diffrn_measurement_method       π
_diffrn_radiation_source         'synchrotron Brookhaven'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.39400
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0836
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            25778
_diffrn_reflns_theta_full        31.02
_diffrn_reflns_theta_max         31.02
_diffrn_reflns_theta_min         1.18
_exptl_absorpt_coefficient_mu    0.192
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.170341
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1997)'
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_density_diffrn    1.614
_exptl_crystal_description       trapezshaped
_exptl_crystal_F_000             1756
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.070
_refine_diff_density_max         5.078
_refine_diff_density_min         -6.097
_refine_diff_density_rms         0.374
_refine_ls_extinction_coef       0.193(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     243
_refine_ls_number_reflns         25778
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.1337
_refine_ls_R_factor_gt           0.0841
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1688P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2229
_refine_ls_wR_factor_ref         0.2724
_reflns_number_gt                16018
_reflns_number_total             25778
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja051233zsi20050224_053159.cif
_cod_data_source_block           final20k
_cod_original_cell_volume        3537.7(12)
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_database_code               4111763
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
Mn1 Mn 0.2500 1.03017(2) 1.0000 0.00768(4) Uani 1 2 d S
Mn2 Mn 0.425842(9) 0.929917(16) 1.034999(10) 0.00844(4) Uani 1 1 d .
O1 O 0.46126(5) 1.05716(9) 0.93733(5) 0.01093(12) Uani 1 1 d .
O2 O 0.34823(5) 1.01771(9) 0.93484(5) 0.01037(11) Uani 1 1 d .
O8 O 0.29688(5) 1.16017(10) 1.08129(6) 0.01314(13) Uani 1 1 d .
O9 O 0.40802(5) 1.09048(11) 1.09994(7) 0.01686(17) Uani 1 1 d .
O11 O 0.30114(5) 0.87698(10) 1.06504(6) 0.01390(14) Uani 1 1 d .
O12 O 0.39714(6) 0.81115(14) 1.13117(8) 0.0222(2) Uani 1 1 d .
C1 C 0.39991(6) 1.06681(10) 0.90445(6) 0.00875(12) Uani 1 1 d .
C2 C 0.38928(6) 1.13402(11) 0.82874(6) 0.01003(13) Uani 1 1 d .
C3 C 0.44262(6) 1.20996(12) 0.80363(8) 0.01350(17) Uani 1 1 d .
H3 H 0.4854 1.2155 0.8326 0.016 Uiso 1 1 calc R
C4 C 0.43183(6) 1.22259(13) 1.23513(8) 0.01367(17) Uani 1 1 d .
H4 H 0.4668 1.1695 1.2197 0.016 Uiso 1 1 calc R
C5 C 0.36875(6) 1.23432(11) 1.18955(7) 0.01072(14) Uani 1 1 d .
C6 C 0.31644(7) 1.31411(14) 1.21341(8) 0.0158(2) Uani 1 1 d .
H6 H 0.2750 1.3244 1.1826 0.019 Uiso 1 1 calc R
C7 C 0.32618(7) 1.12147(14) 0.78337(8) 0.0156(2) Uani 1 1 d .
H7 H 0.2907 1.0704 0.7997 0.019 Uiso 1 1 calc R
C8 C 0.35692(6) 1.15619(11) 1.11726(7) 0.01104(14) Uani 1 1 d .
C11 C 0.33158(6) 0.82699(12) 1.12460(7) 0.01307(17) Uani 1 1 d .
C12 C 0.28923(6) 0.78571(12) 1.18912(7) 0.01154(15) Uani 1 1 d .
C13 C 0.21710(7) 0.80829(15) 1.18527(8) 0.0168(2) Uani 1 1 d .
H13 H 0.1952 0.8471 1.1421 0.020 Uiso 1 1 calc R
C14 C 0.32223(7) 0.72741(16) 1.25377(9) 0.0181(2) Uani 1 1 d .
H14 H 0.3703 0.7123 1.2563 0.022 Uiso 1 1 calc R
O21 O 0.43132(7) 0.76688(11) 0.96244(8) 0.01935(19) Uani 1 1 d .
N21 N 0.39110(12) 0.58679(15) 0.90479(12) 0.0299(4) Uani 1 1 d .
C21 C 0.38647(11) 0.68279(17) 0.95340(11) 0.0231(3) Uani 1 1 d .
H21 H 0.3474 0.6870 0.9821 0.028 Uiso 1 1 calc R
C22 C 0.44983(16) 0.5792(2) 0.85493(14) 0.0331(5) Uani 1 1 d .
H22A H 0.4641 0.6638 0.8427 0.040 Uiso 1 1 calc R
H22B H 0.4333 0.5391 0.8070 0.040 Uiso 1 1 calc R
C23 C 0.51334(19) 0.5088(3) 0.8885(2) 0.0433(7) Uani 1 1 d .
H23A H 0.5352 0.5553 0.9310 0.065 Uiso 1 1 calc R
H23B H 0.5460 0.4982 0.8498 0.065 Uiso 1 1 calc R
H23C H 0.4992 0.4280 0.9062 0.065 Uiso 1 1 calc R
C24 C 0.3342(2) 0.4923(2) 0.89709(17) 0.0457(8) Uani 1 1 d .
H24A H 0.3331 0.4560 0.8459 0.055 Uiso 1 1 calc R
H24B H 0.2898 0.5343 0.9019 0.055 Uiso 1 1 calc R
C25 C 0.34166(18) 0.3885(2) 0.95543(16) 0.0372(6) Uani 1 1 d .
H25A H 0.3875 0.3520 0.9550 0.056 Uiso 1 1 calc R
H25B H 0.3068 0.3254 0.9429 0.056 Uiso 1 1 calc R
H25C H 0.3354 0.4217 1.0057 0.056 Uiso 1 1 calc R
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 98.86(6) . 2_557
O8 Mn1 O11 169.72(4) . 2_557
O8 Mn1 O11 89.51(5) 2_557 2_557
O8 Mn1 O11 89.51(5) . .
O8 Mn1 O11 169.72(4) 2_557 .
O11 Mn1 O11 82.84(6) 2_557 .
O8 Mn1 O2 91.65(4) . 2_557
O8 Mn1 O2 92.71(4) 2_557 2_557
O11 Mn1 O2 81.94(4) 2_557 2_557
O11 Mn1 O2 93.01(4) . 2_557
O8 Mn1 O2 92.71(4) . .
O8 Mn1 O2 91.65(4) 2_557 .
O11 Mn1 O2 93.01(4) 2_557 .
O11 Mn1 O2 81.94(4) . .
O2 Mn1 O2 173.29(5) 2_557 .
O9 Mn2 O21 173.10(5) . .
O9 Mn2 O1 91.54(4) . 5_677
O21 Mn2 O1 95.17(5) . 5_677
O9 Mn2 O12 89.96(6) . .
O21 Mn2 O12 90.46(6) . .
O1 Mn2 O12 99.59(4) 5_677 .
O9 Mn2 O1 89.21(5) . .
O21 Mn2 O1 90.69(5) . .
O1 Mn2 O1 77.70(4) 5_677 .
O12 Mn2 O1 177.14(4) . .
O9 Mn2 O2 87.55(4) . .
O21 Mn2 O2 86.70(5) . .
O1 Mn2 O2 133.31(4) 5_677 .
O12 Mn2 O2 127.08(4) . .
O1 Mn2 O2 55.62(3) . .
C1 O1 Mn2 163.72(8) . 5_677
C1 O1 Mn2 93.90(7) . .
Mn2 O1 Mn2 102.30(4) 5_677 .
C1 O2 Mn1 152.14(8) . .
C1 O2 Mn2 90.29(7) . .
Mn1 O2 Mn2 98.62(4) . .
C8 O8 Mn1 128.89(8) . .
C8 O9 Mn2 138.22(9) . .
C11 O11 Mn1 154.36(10) . .
C11 O12 Mn2 98.97(8) . .
O2 C1 O1 120.03(10) . .
O2 C1 C2 120.29(10) . .
O1 C1 C2 119.66(10) . .
C3 C2 C7 119.84(10) . .
C3 C2 C1 119.78(10) . .
C7 C2 C1 120.38(10) . .
C4 C3 C2 120.06(11) 8_574 .
C4 C3 H3 120.0 8_574 .
C2 C3 H3 120.0 . .
C3 C4 C5 120.38(11) 8_575 .
C3 C4 H4 119.8 8_575 .
C5 C4 H4 119.8 . .
C6 C5 C4 119.39(10) . .
C6 C5 C8 121.05(10) . .
C4 C5 C8 119.50(10) . .
C7 C6 C5 120.33(11) 8_575 .
C7 C6 H6 119.8 8_575 .
C5 C6 H6 119.8 . .
C6 C7 C2 119.92(11) 8_574 .
C6 C7 H7 120.0 8_574 .
C2 C7 H7 120.0 . .
O9 C8 O8 126.30(11) . .
O9 C8 C5 115.82(10) . .
O8 C8 C5 117.86(10) . .
O12 C11 O11 121.54(12) . .
O12 C11 C12 118.74(11) . .
O11 C11 C12 119.72(11) . .
C14 C12 C13 120.09(11) . .
C14 C12 C11 119.91(11) . .
C13 C12 C11 119.98(11) . .
C12 C13 C14 120.07(12) . 7_567
C12 C13 H13 120.0 . .
C14 C13 H13 120.0 7_567 .
C12 C14 C13 119.83(12) . 7_567
C12 C14 H14 120.1 . .
C13 C14 H14 120.1 7_567 .
C21 O21 Mn2 126.36(13) . .
C21 N21 C22 120.36(17) . .
C21 N21 C24 119.7(2) . .
C22 N21 C24 119.8(2) . .
O21 C21 N21 123.8(2) . .
O21 C21 H21 118.1 . .
N21 C21 H21 118.1 . .
N21 C22 C23 115.2(2) . .
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 . .
C22 C23 H23A 109.5 . .
C22 C23 H23B 109.5 . .
H23A C23 H23B 109.5 . .
C22 C23 H23C 109.5 . .
H23A C23 H23C 109.5 . .
H23B C23 H23C 109.5 . .
N21 C24 C25 114.1(2) . .
N21 C24 H24A 108.7 . .
C25 C24 H24A 108.7 . .
N21 C24 H24B 108.7 . .
C25 C24 H24B 108.7 . .
H24A C24 H24B 107.6 . .
C24 C25 H25A 109.5 . .
C24 C25 H25B 109.5 . .
H25A C25 H25B 109.5 . .
C24 C25 H25C 109.5 . .
H25A C25 H25C 109.5 . .
H25B C25 H25C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 O8 2.1304(10) .
Mn1 O8 2.1304(10) 2_557
Mn1 O11 2.1771(10) 2_557
Mn1 O11 2.1771(10) .
Mn1 O2 2.2684(11) 2_557
Mn1 O2 2.2685(11) .
Mn2 O9 2.0928(11) .
Mn2 O21 2.1554(12) .
Mn2 O1 2.1807(10) 5_677
Mn2 O12 2.2008(12) .
Mn2 O1 2.3151(10) .
Mn2 O2 2.3950(11) .
O1 C1 1.2705(14) .
O1 Mn2 2.1807(10) 5_677
O2 C1 1.2678(14) .
O8 C8 1.2670(15) .
O9 C8 1.2566(16) .
O11 C11 1.2683(15) .
O12 C11 1.2614(17) .
C1 C2 1.5009(15) .
C2 C3 1.3971(17) .
C2 C7 1.3987(17) .
C3 C4 1.3949(17) 8_574
C3 H3 0.9300 .
C4 C3 1.3949(17) 8_575
C4 C5 1.3994(17) .
C4 H4 0.9300 .
C5 C6 1.3990(17) .
C5 C8 1.5122(15) .
C6 C7 1.3987(17) 8_575
C6 H6 0.9300 .
C7 C6 1.3987(17) 8_574
C7 H7 0.9300 .
C11 C12 1.4984(16) .
C12 C14 1.3950(17) .
C12 C13 1.3965(18) .
C13 C14 1.3982(19) 7_567
C13 H13 0.9300 .
C14 C13 1.3982(19) 7_567
C14 H14 0.9300 .
O21 C21 1.2423(19) .
N21 C21 1.335(3) .
N21 C22 1.471(4) .
N21 C24 1.480(3) .
C21 H21 0.9300 .
C22 C23 1.508(4) .
C22 H22A 0.9700 .
C22 H22B 0.9700 .
C23 H23A 0.9600 .
C23 H23B 0.9600 .
C23 H23C 0.9600 .
C24 C25 1.502(4) .
C24 H24A 0.9700 .
C24 H24B 0.9700 .
C25 H25A 0.9600 .
C25 H25B 0.9600 .
C25 H25C 0.9600 .
