#------------------------------------------------------------------------------
#$Date: 2019-11-25 02:10:58 +0200 (Mon, 25 Nov 2019) $
#$Revision: 239940 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/35/05/4350554.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_4350554
loop_
_publ_author_name
'Moon, Hoi Ri'
'Kobayashi, Norihito'
'Suh, Myunghyun Paik'
_publ_section_title
;
 Porous metal-organic framework with coordinatively unsaturated Mn(II)
 sites:sorption properties for various gases.
;
_journal_issue                   21
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8672
_journal_page_last               8676
_journal_paper_doi               10.1021/ic0611948
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety         '(Mn 2+), (C12 H6 O4 2-), (C5 H11 N1 O1)'
_chemical_formula_sum            'C17 H17 Mn N O5'
_chemical_formula_weight         370.26
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yab'
_space_group_name_H-M_alt        'P 1 21/a 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2004-09-07T13:42:11-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 96.666(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.535(5)
_cell_length_b                   21.513(5)
_cell_length_c                   10.466(5)
_cell_measurement_temperature    153(2)
_cell_volume                     1685.1(14)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.956801E-1
_diffrn_orient_matrix_UB_12      0.20589E-2
_diffrn_orient_matrix_UB_13      -0.585661E-1
_diffrn_orient_matrix_UB_21      0.914859E-1
_diffrn_orient_matrix_UB_22      0.69593E-2
_diffrn_orient_matrix_UB_23      0.758024E-1
_diffrn_orient_matrix_UB_31      0.181579E-1
_diffrn_orient_matrix_UB_32      -0.459128E-1
_diffrn_orient_matrix_UB_33      0.88635E-2
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.052
_diffrn_reflns_av_unetI/netI     0.0734
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6691
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.3
_exptl_absorpt_coefficient_mu    0.809
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             764
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.49
_refine_diff_density_min         -0.333
_refine_diff_density_rms         0.075
_refine_ls_extinction_coef       0.0046(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     220
_refine_ls_number_reflns         3771
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.0834
_refine_ls_R_factor_gt           0.0457
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0533P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0996
_refine_ls_wR_factor_ref         0.1108
_reflns_number_gt                2575
_reflns_number_total             3771
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0611948si20060629_094922.cif
_cod_data_source_block           MnNDC-DEF
_cod_original_formula_sum        'C17 H17 N1 O5 Mn'
_cod_database_code               4350554
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x-1/2, -y-1/2, 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
Mn Mn 0.37440(4) 0.237610(17) 0.33259(3) 0.02198(14) Uani 1 1 d .
O1 O 0.4016(2) 0.32851(9) 0.44552(19) 0.0399(5) Uani 1 1 d .
O2 O 0.1352(2) 0.30368(8) 0.35258(17) 0.0288(4) Uani 1 1 d .
O3 O 0.2261(2) 0.16993(8) 0.22582(17) 0.0337(4) Uani 1 1 d .
O4 O -0.0516(2) 0.20607(9) 0.18095(17) 0.0341(4) Uani 1 1 d .
O5 O 0.3476(3) 0.19564(9) 0.52101(18) 0.0420(5) Uani 1 1 d .
N1 N 0.2363(3) 0.17704(15) 0.7092(3) 0.0561(8) Uani 1 1 d .
C1 C 0.0069(3) 0.42433(12) 0.4137(3) 0.0302(6) Uani 1 1 d .
C2 C 0.1743(3) 0.40306(12) 0.4576(3) 0.0294(6) Uani 1 1 d .
C3 C 0.2886(4) 0.44053(14) 0.5440(3) 0.0425(8) Uani 1 1 d .
C4 C 0.2312(3) 0.49591(14) 0.5860(3) 0.0419(8) Uani 1 1 d .
C5 C -0.0558(3) 0.48215(12) 0.4554(3) 0.0306(6) Uani 1 1 d .
C6 C 0.2409(3) 0.34209(12) 0.4169(2) 0.0277(6) Uani 1 1 d .
C7 C 0.1382(3) 0.06162(12) 0.0883(2) 0.0304(6) Uani 1 1 d .
C8 C 0.0140(3) 0.10589(12) 0.1062(2) 0.0272(6) Uani 1 1 d .
C9 C -0.1675(4) 0.09549(13) 0.0590(3) 0.0415(7) Uani 1 1 d .
C10 C -0.2170(4) 0.04138(14) -0.0048(3) 0.0445(8) Uani 1 1 d .
C11 C 0.0907(3) 0.00492(13) 0.0240(3) 0.0294(6) Uani 1 1 d .
C12 C 0.0657(3) 0.16541(12) 0.1771(2) 0.0261(6) Uani 1 1 d .
C13 C 0.2411(4) 0.20635(15) 0.5987(3) 0.0405(7) Uani 1 1 d .
C14 C 0.3659(6) 0.1274(2) 0.7508(4) 0.0836(13) Uani 1 1 d .
C15 C 0.2804(7) 0.0655(2) 0.7429(5) 0.1062(17) Uani 1 1 d .
C16 C 0.1048(5) 0.1963(2) 0.7956(3) 0.0726(12) Uani 1 1 d .
C17 C 0.1800(6) 0.2361(2) 0.9034(4) 0.0997(17) Uani 1 1 d .
H1 H -0.0668 0.4004 0.3556 0.036 Uiso 1 1 calc R
H3 H 0.4037 0.4269 0.5719 0.051 Uiso 1 1 calc R
H4 H 0.3075 0.5198 0.6424 0.05 Uiso 1 1 calc R
H7 H 0.2573 0.0688 0.1191 0.036 Uiso 1 1 calc R
H9 H -0.2531 0.1254 0.0714 0.05 Uiso 1 1 calc R
H10 H -0.3363 0.0352 -0.036 0.053 Uiso 1 1 calc R
H13 H 0.1572 0.2375 0.5781 0.049 Uiso 1 1 calc R
H14A H 0.417 0.1352 0.8387 0.1 Uiso 1 1 calc R
H14B H 0.4621 0.1281 0.6968 0.1 Uiso 1 1 calc R
H15A H 0.1905 0.0639 0.8008 0.159 Uiso 1 1 calc R
H15B H 0.3689 0.0342 0.7662 0.159 Uiso 1 1 calc R
H15C H 0.2261 0.0583 0.6566 0.159 Uiso 1 1 calc R
H16A H 0.054 0.1594 0.8302 0.087 Uiso 1 1 calc R
H16B H 0.0086 0.2186 0.7456 0.087 Uiso 1 1 calc R
H17A H 0.2756 0.2145 0.9534 0.15 Uiso 1 1 calc R
H17B H 0.0884 0.2458 0.9568 0.15 Uiso 1 1 calc R
H17C H 0.2249 0.2738 0.8702 0.15 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 0 '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 0.006 '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
O3 Mn O4 99.75(8) . 4_665 yes
O3 Mn O2 101.04(8) . 4_665 yes
O4 Mn O2 89.54(7) 4_665 4_665 yes
O3 Mn O5 95.44(8) . . yes
O4 Mn O5 164.67(7) 4_665 . yes
O2 Mn O5 85.47(7) 4_665 . yes
O3 Mn O1 152.68(7) . . yes
O4 Mn O1 83.25(8) 4_665 . yes
O2 Mn O1 106.15(7) 4_665 . yes
O5 Mn O1 84.24(8) . . yes
O3 Mn O2 95.89(7) . . yes
O4 Mn O2 89.54(7) 4_665 . yes
O2 Mn O2 162.95(7) 4_665 . yes
O5 Mn O2 91.00(7) . . yes
O1 Mn O2 56.85(6) . . yes
C6 O2 Mn 145.49(15) . 4_565 yes
C6 O2 Mn 90.03(13) . . yes
Mn O2 Mn 116.71(8) 4_565 . yes
C6 O1 Mn 92.85(15) . . yes
C13 O5 Mn 130.64(19) . . yes
C10 C9 C8 120.0(3) . . yes
N1 C16 C17 113.9(3) . . yes
N1 C14 C15 111.5(4) . . yes
C1 C2 C3 119.3(2) . . yes
C1 C2 C6 121.9(2) . . yes
C3 C2 C6 118.8(2) . . yes
O1 C6 O2 120.1(2) . . yes
O1 C6 C2 119.3(2) . . yes
O2 C6 C2 120.6(2) . . yes
C13 N1 C16 119.4(3) . . yes
C13 N1 C14 121.2(3) . . yes
C16 N1 C14 119.3(3) . . yes
C9 C10 C11 121.3(2) . 3 yes
C7 C8 C9 119.5(2) . . yes
C7 C8 C12 121.2(2) . . yes
C9 C8 C12 119.3(2) . . yes
C10 C11 C11 119.0(3) 3 3 yes
C10 C11 C7 122.6(2) 3 . yes
C11 C11 C7 118.5(3) 3 . yes
C4 C3 C2 120.7(2) . . yes
C2 C1 C5 121.1(2) . . yes
C3 C4 C5 120.8(2) . 3_566 yes
C5 C5 C1 119.2(3) 3_566 . yes
C5 C5 C4 118.9(3) 3_566 3_566 yes
C1 C5 C4 121.9(2) . 3_566 yes
O5 C13 N1 125.2(3) . . yes
C8 C7 C11 121.7(2) . . yes
C12 O4 Mn 132.34(17) . 4_565 yes
O4 C12 O3 125.6(2) . . yes
O4 C12 C8 117.9(2) . . yes
O3 C12 C8 116.5(2) . . yes
C12 O3 Mn 134.57(17) . . yes
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
Mn O3 2.0802(18) . yes
Mn O4 2.1221(19) 4_665 yes
Mn O2 2.1446(19) 4_665 yes
Mn O5 2.199(2) . yes
Mn O1 2.2819(19) . yes
Mn O2 2.3237(19) . yes
O2 C6 1.283(3) . yes
O2 Mn 2.1446(19) 4_565 yes
O1 C6 1.248(3) . yes
O5 C13 1.228(3) . yes
C9 C10 1.372(4) . yes
C9 C8 1.417(4) . yes
C16 N1 1.476(4) . yes
C16 C17 1.476(5) . yes
C14 N1 1.477(5) . yes
C14 C15 1.477(6) . yes
C2 C1 1.369(4) . yes
C2 C3 1.425(4) . yes
C2 C6 1.484(3) . yes
N1 C13 1.322(4) . yes
C10 C11 1.408(4) 3 yes
C8 C7 1.364(4) . yes
C8 C12 1.508(3) . yes
C11 C10 1.408(4) 3 yes
C11 C11 1.416(5) 3 yes
C11 C7 1.419(3) . yes
C3 C4 1.358(4) . yes
C1 C5 1.417(3) . yes
C4 C5 1.423(4) 3_566 yes
C5 C5 1.409(5) 3_566 yes
C5 C4 1.423(4) 3_566 yes
O4 C12 1.247(3) . yes
O4 Mn 2.1221(19) 4_565 yes
C12 O3 1.260(3) . yes
