#------------------------------------------------------------------------------
#$Date: 2016-03-21 17:04:53 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178767 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/21/4102138.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_4102138
loop_
_publ_author_name
'Guohai Xu'
'Xiaoguang Zhang'
'Peng Guo'
'Chengling Pan'
'Hongjie Zhang'
'Cheng Wang'
_publ_section_title
;
 MnII-based MIL-53 Analogues: Synthesis Using Neutral Bridging μ2-Ligands
 and Application in Liquid-Phase Adsorption and Separation of C6-C8
 Aromatics
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3656
_journal_page_last               3657
_journal_paper_doi               10.1021/ja910818a
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         'C15 H13 Mn N O5'
_chemical_formula_sum            'C15 H13 Mn N O5'
_chemical_formula_weight         342.20
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                114.436(4)
_cell_angle_beta                 104.890(4)
_cell_angle_gamma                96.042(3)
_cell_formula_units_Z            2
_cell_length_a                   7.4362(12)
_cell_length_b                   10.2754(16)
_cell_length_c                   10.923(3)
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.9
_cell_measurement_theta_min      2.2
_cell_volume                     712.8(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT software (Bruker, 1999)'
_computing_molecular_graphics    'SHELXTL-PLUS (Sheldrick, 1990)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97(Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       'ω scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0259
_diffrn_reflns_av_sigmaI/netI    0.0639
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3896
_diffrn_reflns_theta_full        25.93
_diffrn_reflns_theta_max         25.93
_diffrn_reflns_theta_min         2.17
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    0.949
_exptl_absorpt_correction_T_max  0.755
_exptl_absorpt_correction_T_min  0.426
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.594
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             350
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.664
_refine_diff_density_min         -0.436
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     202
_refine_ls_number_reflns         2730
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0729
_refine_ls_R_factor_gt           0.0480
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0597P)²+0.4134P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1094
_refine_ls_wR_factor_ref         0.1222
_reflns_number_gt                2025
_reflns_number_total             2730
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja910818a_si_002_03.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        712.8(2)
_cod_database_code               4102138
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
C1 C -0.2655(6) 0.8136(4) 0.4726(5) 0.0269(9) Uani 1 1 d . . .
H1 H -0.3401 0.7435 0.3807 0.032 Uiso 1 1 calc R . .
C2 C -0.2375(6) 0.9611(5) 0.5078(5) 0.0270(10) Uani 1 1 d . . .
C3 C -0.1253(6) 1.0611(4) 0.6447(5) 0.0284(10) Uani 1 1 d . . .
H3 H -0.1037 1.1611 0.6704 0.034 Uiso 1 1 calc R . .
C4 C -0.0442(6) 1.0161(4) 0.7446(5) 0.0292(10) Uani 1 1 d . . .
C5 C -0.0794(6) 0.8661(4) 0.7033(4) 0.0243(9) Uani 1 1 d . . .
H5 H -0.0286 0.8323 0.7685 0.029 Uiso 1 1 calc R . .
C6 C -0.3296(7) 1.0084(5) 0.3986(6) 0.0416(12) Uani 1 1 d . . .
H6A H -0.2958 1.1139 0.4401 0.062 Uiso 1 1 calc R . .
H6B H -0.4663 0.9741 0.3674 0.062 Uiso 1 1 calc R . .
H6C H -0.2853 0.9675 0.3186 0.062 Uiso 1 1 calc R . .
C7 C 0.0783(7) 1.1237(5) 0.8953(5) 0.0428(13) Uani 1 1 d . . .
H7A H 0.0888 1.2224 0.9068 0.064 Uiso 1 1 calc R . .
H7B H 0.2036 1.1049 0.9145 0.064 Uiso 1 1 calc R . .
H7C H 0.0204 1.1125 0.9605 0.064 Uiso 1 1 calc R . .
C8 C 0.1856(6) 0.5606(4) 0.2944(4) 0.0184(8) Uani 1 1 d . . .
C9 C 0.0903(5) 0.5305(4) 0.1418(4) 0.0181(8) Uani 1 1 d . . .
C10 C -0.1086(5) 0.4992(4) 0.0858(4) 0.0201(8) Uani 1 1 d . . .
H10 H -0.1822 0.4981 0.1426 0.024 Uiso 1 1 calc R . .
C11 C 0.1979(6) 0.5303(4) 0.0542(4) 0.0221(9) Uani 1 1 d . . .
H11 H 0.3309 0.5501 0.0901 0.027 Uiso 1 1 calc R . .
C12 C 0.3704(5) 0.7339(4) 0.7298(4) 0.0169(8) Uani 1 1 d . . .
C13 C 0.4394(5) 0.8716(4) 0.8714(4) 0.0182(8) Uani 1 1 d . . .
C14 C 0.5840(5) 0.9859(4) 0.8976(4) 0.0218(9) Uani 1 1 d . . .
H14 H 0.6411 0.9763 0.8289 0.026 Uiso 1 1 calc R . .
C15 C 0.3555(6) 0.8852(4) 0.9744(4) 0.0225(9) Uani 1 1 d . . .
H15 H 0.2592 0.8084 0.9579 0.027 Uiso 1 1 calc R . .
N1 N -0.1864(4) 0.7705(3) 0.5695(3) 0.0190(7) Uani 1 1 d . . .
O1 O -0.2188(4) 0.6264(3) 0.5307(3) 0.0209(6) Uani 1 1 d . . .
O2 O 0.0879(4) 0.5963(3) 0.3759(3) 0.0198(6) Uani 1 1 d . . .
O3 O 0.3555(4) 0.5481(3) 0.3277(3) 0.0225(6) Uani 1 1 d . . .
O4 O 0.2026(4) 0.6616(3) 0.6951(3) 0.0219(6) Uani 1 1 d . . .
O5 O 0.4835(4) 0.7039(3) 0.6609(3) 0.0207(6) Uani 1 1 d . . .
Mn1 Mn -0.5000 0.5000 0.5000 0.0135(2) Uani 1 2 d S . .
Mn2 Mn 0.0000 0.5000 0.5000 0.0138(2) Uani 1 2 d S . .
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
_geom_angle_publ_flag
N1 C1 C2 120.5(4) . . ?
N1 C1 H1 119.8 . . ?
C2 C1 H1 119.8 . . ?
C3 C2 C1 117.9(4) . . ?
C3 C2 C6 122.1(4) . . ?
C1 C2 C6 120.0(4) . . ?
C2 C3 C4 121.4(4) . . ?
C2 C3 H3 119.3 . . ?
C4 C3 H3 119.3 . . ?
C3 C4 C5 118.0(4) . . ?
C3 C4 C7 122.3(4) . . ?
C5 C4 C7 119.7(4) . . ?
N1 C5 C4 119.8(4) . . ?
N1 C5 H5 120.1 . . ?
C4 C5 H5 120.1 . . ?
C2 C6 H6A 109.5 . . ?
C2 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C2 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C4 C7 H7A 109.5 . . ?
C4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
O2 C8 O3 126.1(4) . . ?
O2 C8 C9 116.9(3) . . ?
O3 C8 C9 117.0(3) . . ?
C10 C9 C11 118.8(4) . . ?
C10 C9 C8 119.9(3) . . ?
C11 C9 C8 121.3(3) . . ?
C11 C10 C9 120.5(4) 2_565 . ?
C11 C10 H10 119.7 2_565 . ?
C9 C10 H10 119.7 . . ?
C10 C11 C9 120.7(4) 2_565 . ?
C10 C11 H11 119.7 2_565 . ?
C9 C11 H11 119.7 . . ?
O5 C12 O4 127.2(3) . . ?
O5 C12 C13 117.6(3) . . ?
O4 C12 C13 115.1(3) . . ?
C14 C13 C15 119.7(3) . . ?
C14 C13 C12 120.1(3) . . ?
C15 C13 C12 120.2(3) . . ?
C13 C14 C15 120.6(4) . 2_677 ?
C13 C14 H14 119.7 . . ?
C15 C14 H14 119.7 2_677 . ?
C13 C15 C14 119.7(4) . 2_677 ?
C13 C15 H15 120.2 . . ?
C14 C15 H15 120.2 2_677 . ?
O1 N1 C1 118.3(3) . . ?
O1 N1 C5 119.3(3) . . ?
C1 N1 C5 122.4(3) . . ?
N1 O1 Mn2 123.5(2) . . ?
N1 O1 Mn1 121.2(2) . . ?
Mn2 O1 Mn1 115.25(10) . . ?
C8 O2 Mn2 132.5(2) . . ?
C8 O3 Mn1 126.8(2) . 1_655 ?
C12 O4 Mn2 133.8(2) . . ?
C12 O5 Mn1 131.9(2) . 1_655 ?
O5 Mn1 O5 180.0 1_455 2_566 ?
O5 Mn1 O3 87.56(10) 1_455 2_566 ?
O5 Mn1 O3 92.44(10) 2_566 2_566 ?
O5 Mn1 O3 92.44(10) 1_455 1_455 ?
O5 Mn1 O3 87.56(10) 2_566 1_455 ?
O3 Mn1 O3 180.000(1) 2_566 1_455 ?
O5 Mn1 O1 84.69(9) 1_455 . ?
O5 Mn1 O1 95.31(9) 2_566 . ?
O3 Mn1 O1 88.20(10) 2_566 . ?
O3 Mn1 O1 91.80(10) 1_455 . ?
O5 Mn1 O1 95.31(9) 1_455 2_466 ?
O5 Mn1 O1 84.69(9) 2_566 2_466 ?
O3 Mn1 O1 91.80(10) 2_566 2_466 ?
O3 Mn1 O1 88.20(10) 1_455 2_466 ?
O1 Mn1 O1 180.0 . 2_466 ?
O4 Mn2 O4 180.0 2_566 . ?
O4 Mn2 O2 93.86(10) 2_566 2_566 ?
O4 Mn2 O2 86.14(10) . 2_566 ?
O4 Mn2 O2 86.14(10) 2_566 . ?
O4 Mn2 O2 93.86(10) . . ?
O2 Mn2 O2 180.000(1) 2_566 . ?
O4 Mn2 O1 88.58(10) 2_566 . ?
O4 Mn2 O1 91.42(10) . . ?
O2 Mn2 O1 87.76(10) 2_566 . ?
O2 Mn2 O1 92.24(10) . . ?
O4 Mn2 O1 91.42(10) 2_566 2_566 ?
O4 Mn2 O1 88.58(10) . 2_566 ?
O2 Mn2 O1 92.24(10) 2_566 2_566 ?
O2 Mn2 O1 87.76(10) . 2_566 ?
O1 Mn2 O1 180.000(1) . 2_566 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.336(5) . ?
C1 C2 1.378(6) . ?
C1 H1 0.9300 . ?
C2 C3 1.377(6) . ?
C2 C6 1.503(6) . ?
C3 C4 1.381(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.388(6) . ?
C4 C7 1.508(6) . ?
C5 N1 1.336(5) . ?
C5 H5 0.9300 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 O2 1.254(4) . ?
C8 O3 1.257(5) . ?
C8 C9 1.515(5) . ?
C9 C10 1.392(5) . ?
C9 C11 1.396(5) . ?
C10 C11 1.387(5) 2_565 ?
C10 H10 0.9300 . ?
C11 C10 1.387(5) 2_565 ?
C11 H11 0.9300 . ?
C12 O5 1.247(4) . ?
C12 O4 1.258(4) . ?
C12 C13 1.512(5) . ?
C13 C14 1.384(5) . ?
C13 C15 1.387(5) . ?
C14 C15 1.389(5) 2_677 ?
C14 H14 0.9300 . ?
C15 C14 1.389(5) 2_677 ?
C15 H15 0.9300 . ?
N1 O1 1.335(4) . ?
O1 Mn2 2.193(2) . ?
O1 Mn1 2.209(2) . ?
O2 Mn2 2.161(3) . ?
O3 Mn1 2.188(3) 1_655 ?
O4 Mn2 2.113(2) . ?
O5 Mn1 2.148(2) 1_655 ?
Mn1 O5 2.148(2) 1_455 ?
Mn1 O5 2.148(2) 2_566 ?
Mn1 O3 2.188(3) 2_566 ?
Mn1 O3 2.188(3) 1_455 ?
Mn1 O1 2.209(3) 2_466 ?
Mn2 O4 2.113(2) 2_566 ?
Mn2 O2 2.161(3) 2_566 ?
Mn2 O1 2.193(2) 2_566 ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 C3 0.4(6) . . . . ?
N1 C1 C2 C6 -179.1(4) . . . . ?
C1 C2 C3 C4 -0.5(6) . . . . ?
C6 C2 C3 C4 178.9(4) . . . . ?
C2 C3 C4 C5 -0.2(6) . . . . ?
C2 C3 C4 C7 -179.7(4) . . . . ?
C3 C4 C5 N1 1.1(6) . . . . ?
C7 C4 C5 N1 -179.4(4) . . . . ?
O2 C8 C9 C10 -19.3(5) . . . . ?
O3 C8 C9 C10 161.0(3) . . . . ?
O2 C8 C9 C11 162.1(3) . . . . ?
O3 C8 C9 C11 -17.6(5) . . . . ?
C11 C9 C10 C11 -0.6(6) . . . 2_565 ?
C8 C9 C10 C11 -179.2(3) . . . 2_565 ?
C10 C9 C11 C10 0.6(6) . . . 2_565 ?
C8 C9 C11 C10 179.2(3) . . . 2_565 ?
O5 C12 C13 C14 24.3(5) . . . . ?
O4 C12 C13 C14 -156.0(4) . . . . ?
O5 C12 C13 C15 -157.1(4) . . . . ?
O4 C12 C13 C15 22.7(5) . . . . ?
C15 C13 C14 C15 -0.7(7) . . . 2_677 ?
C12 C13 C14 C15 178.0(4) . . . 2_677 ?
C14 C13 C15 C14 0.6(7) . . . 2_677 ?
C12 C13 C15 C14 -178.0(4) . . . 2_677 ?
C2 C1 N1 O1 179.5(3) . . . . ?
C2 C1 N1 C5 0.6(6) . . . . ?
C4 C5 N1 O1 179.8(3) . . . . ?
C4 C5 N1 C1 -1.3(6) . . . . ?
C1 N1 O1 Mn2 108.5(3) . . . . ?
C5 N1 O1 Mn2 -72.6(4) . . . . ?
C1 N1 O1 Mn1 -73.6(4) . . . . ?
C5 N1 O1 Mn1 105.3(3) . . . . ?
O3 C8 O2 Mn2 -58.8(5) . . . . ?
C9 C8 O2 Mn2 121.5(3) . . . . ?
O2 C8 O3 Mn1 25.3(5) . . . 1_655 ?
C9 C8 O3 Mn1 -155.0(2) . . . 1_655 ?
O5 C12 O4 Mn2 -19.1(6) . . . . ?
C13 C12 O4 Mn2 161.2(2) . . . . ?
O4 C12 O5 Mn1 -23.0(6) . . . 1_655 ?
C13 C12 O5 Mn1 156.7(3) . . . 1_655 ?
N1 O1 Mn1 O5 -30.4(3) . . . 1_455 ?
Mn2 O1 Mn1 O5 147.62(14) . . . 1_455 ?
N1 O1 Mn1 O5 149.6(3) . . . 2_566 ?
Mn2 O1 Mn1 O5 -32.38(14) . . . 2_566 ?
N1 O1 Mn1 O3 -118.2(3) . . . 2_566 ?
Mn2 O1 Mn1 O3 59.90(13) . . . 2_566 ?
N1 O1 Mn1 O3 61.8(3) . . . 1_455 ?
Mn2 O1 Mn1 O3 -120.10(13) . . . 1_455 ?
N1 O1 Mn1 O1 -164(100) . . . 2_466 ?
Mn2 O1 Mn1 O1 14(100) . . . 2_466 ?
C12 O4 Mn2 O4 -153(100) . . . 2_566 ?
C12 O4 Mn2 O2 145.6(3) . . . 2_566 ?
C12 O4 Mn2 O2 -34.4(3) . . . . ?
C12 O4 Mn2 O1 -126.7(3) . . . . ?
C12 O4 Mn2 O1 53.3(3) . . . 2_566 ?
C8 O2 Mn2 O4 -75.8(3) . . . 2_566 ?
C8 O2 Mn2 O4 104.2(3) . . . . ?
C8 O2 Mn2 O2 -89(100) . . . 2_566 ?
C8 O2 Mn2 O1 -164.2(3) . . . . ?
C8 O2 Mn2 O1 15.8(3) . . . 2_566 ?
N1 O1 Mn2 O4 -132.7(3) . . . 2_566 ?
Mn1 O1 Mn2 O4 49.33(13) . . . 2_566 ?
N1 O1 Mn2 O4 47.3(3) . . . . ?
Mn1 O1 Mn2 O4 -130.67(13) . . . . ?
N1 O1 Mn2 O2 133.4(3) . . . 2_566 ?
Mn1 O1 Mn2 O2 -44.59(13) . . . 2_566 ?
N1 O1 Mn2 O2 -46.6(3) . . . . ?
Mn1 O1 Mn2 O2 135.41(13) . . . . ?
N1 O1 Mn2 O1 159(100) . . . 2_566 ?
Mn1 O1 Mn2 O1 -19(100) . . . 2_566 ?
