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#$Date: 2016-03-25 09:08:17 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179715 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/17/7001738.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_7001738
loop_
_publ_author_name
'Cheng, Xiao-Ning'
'Xue, Wei'
'Huang, Jun-Hou'
'Chen, Xiao-Ming'
_publ_section_title
;
 Spin canting and/or metamagnetic behaviours of four isostructural
 grid-type coordination networks
;
_journal_issue                   29
_journal_name_full               'Dalton Transactions'
_journal_page_first              5701
_journal_paper_doi               10.1039/b901524h
_journal_year                    2009
_chemical_formula_sum            'C13 H11 Mn N O5'
_chemical_formula_weight         316.17
_chemical_name_systematic
;
?
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.9740(16)
_cell_length_b                   10.0241(10)
_cell_length_c                   7.6552(8)
_cell_measurement_temperature    293(2)
_cell_volume                     1225.8(2)
_computing_cell_refinement       SAINT
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       '/w 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  0.0170
_diffrn_reflns_av_sigmaI/netI    0.0354
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            4676
_diffrn_reflns_theta_full        26.99
_diffrn_reflns_theta_max         26.99
_diffrn_reflns_theta_min         2.03
_exptl_absorpt_coefficient_mu    1.096
_exptl_absorpt_correction_T_max  0.8983
_exptl_absorpt_correction_T_min  0.8106
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellowish
_exptl_crystal_density_diffrn    1.713
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             644
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.270
_refine_diff_density_min         -0.347
_refine_diff_density_rms         0.081
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.026(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         2242
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0283
_refine_ls_R_factor_gt           0.0267
_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)+(0.0386P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0687
_refine_ls_wR_factor_ref         0.0696
_reflns_number_gt                2122
_reflns_number_total             2242
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b901524h.txt
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      Pca2(1)
_cod_database_code               7001738
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x+1/2, y, z+1/2'
'x+1/2, -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
Mn1 Mn -0.363323(18) -0.43625(3) 0.65716(5) 0.02817(11) Uani 1 1 d . . .
O1 O -0.40077(10) -0.32138(15) 0.4099(2) 0.0320(4) Uani 1 1 d . . .
O2 O -0.41741(11) -0.57298(15) 0.4730(2) 0.0361(4) Uani 1 1 d . . .
O3 O -0.50908(10) -0.60753(16) 0.2590(3) 0.0422(4) Uani 1 1 d . . .
O4 O -0.24086(12) -0.45849(16) 0.5406(3) 0.0420(4) Uani 1 1 d . . .
N1 N -0.34465(12) -0.21664(19) 0.7025(2) 0.0302(4) Uani 1 1 d . . .
C1 C -0.31856(15) -0.1655(2) 0.8522(3) 0.0369(5) Uani 1 1 d . . .
H1A H -0.2989 -0.2229 0.9384 0.044 Uiso 1 1 calc R . .
C2 C -0.31947(17) -0.0280(3) 0.8861(3) 0.0423(6) Uani 1 1 d . . .
H2A H -0.3009 0.0041 0.9932 0.051 Uiso 1 1 calc R . .
C3 C -0.34718(17) 0.0575(2) 0.7639(4) 0.0387(6) Uani 1 1 d . . .
H3A H -0.3479 0.1486 0.7867 0.046 Uiso 1 1 calc R . .
C4 C -0.37512(13) 0.0092(2) 0.6013(4) 0.0309(5) Uani 1 1 d . . .
C5 C -0.40514(16) 0.0915(2) 0.4638(4) 0.0398(6) Uani 1 1 d . . .
H5A H -0.4060 0.1837 0.4771 0.048 Uiso 1 1 calc R . .
C6 C -0.43255(16) 0.0354(2) 0.3131(4) 0.0410(6) Uani 1 1 d . . .
H6A H -0.4517 0.0904 0.2238 0.049 Uiso 1 1 calc R . .
C7 C -0.43284(15) -0.1038(2) 0.2879(4) 0.0374(5) Uani 1 1 d . . .
H7A H -0.4525 -0.1400 0.1838 0.045 Uiso 1 1 calc R . .
C8 C -0.40402(13) -0.1850(2) 0.4180(3) 0.0291(5) Uani 1 1 d . . .
C9 C -0.37322(12) -0.1316(2) 0.5766(3) 0.0271(5) Uani 1 1 d . . .
C10 C -0.45416(14) -0.3897(2) 0.2891(3) 0.0336(5) Uani 1 1 d . . .
H10A H -0.4310 -0.3844 0.1721 0.040 Uiso 1 1 calc R . .
H10B H -0.5092 -0.3488 0.2881 0.040 Uiso 1 1 calc R . .
C11 C -0.46070(14) -0.5347(2) 0.3462(3) 0.0298(5) Uani 1 1 d . . .
C12 C -0.19809(14) -0.5578(2) 0.5007(3) 0.0312(5) Uani 1 1 d . . .
C13 C -0.20237(19) -0.6825(2) 0.6090(4) 0.0468(7) Uani 1 1 d . . .
H13A H -0.2068 -0.6591 0.7302 0.070 Uiso 1 1 calc R . .
H13B H -0.1526 -0.7344 0.5908 0.070 Uiso 1 1 calc R . .
H13C H -0.2505 -0.7338 0.5751 0.070 Uiso 1 1 calc R . .
O5 O -0.15055(12) -0.56312(19) 0.3697(3) 0.0437(5) Uani 1 1 d . . .
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'
Mn Mn 0.3368 0.7283 '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'
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
O5 Mn1 O2 99.58(7) 3_455 . ?
O5 Mn1 O4 99.41(7) 3_455 . ?
O2 Mn1 O4 91.56(7) . . ?
O5 Mn1 O3 86.80(7) 3_455 2_445 ?
O2 Mn1 O3 89.27(7) . 2_445 ?
O4 Mn1 O3 173.49(7) . 2_445 ?
O5 Mn1 N1 117.68(8) 3_455 . ?
O2 Mn1 N1 141.21(7) . . ?
O4 Mn1 N1 92.56(6) . . ?
O3 Mn1 N1 82.78(6) 2_445 . ?
O5 Mn1 O1 168.86(7) 3_455 . ?
O2 Mn1 O1 70.97(6) . . ?
O4 Mn1 O1 86.97(7) . . ?
O3 Mn1 O1 87.20(7) 2_445 . ?
N1 Mn1 O1 70.77(6) . . ?
C8 O1 C10 118.95(17) . . ?
C8 O1 Mn1 118.24(13) . . ?
C10 O1 Mn1 116.61(12) . . ?
C11 O2 Mn1 122.37(14) . . ?
C11 O3 Mn1 129.43(16) . 2_444 ?
C12 O4 Mn1 132.87(15) . . ?
C1 N1 C9 118.3(2) . . ?
C1 N1 Mn1 123.71(16) . . ?
C9 N1 Mn1 117.27(15) . . ?
N1 C1 C2 122.5(2) . . ?
N1 C1 H1A 118.7 . . ?
C2 C1 H1A 118.7 . . ?
C3 C2 C1 120.1(2) . . ?
C3 C2 H2A 119.9 . . ?
C1 C2 H2A 119.9 . . ?
C2 C3 C4 120.0(2) . . ?
C2 C3 H3A 120.0 . . ?
C4 C3 H3A 120.0 . . ?
C3 C4 C5 124.2(2) . . ?
C3 C4 C9 116.8(2) . . ?
C5 C4 C9 119.0(2) . . ?
C6 C5 C4 119.9(2) . . ?
C6 C5 H5A 120.1 . . ?
C4 C5 H5A 120.1 . . ?
C5 C6 C7 121.9(2) . . ?
C5 C6 H6A 119.1 . . ?
C7 C6 H6A 119.1 . . ?
C8 C7 C6 119.3(2) . . ?
C8 C7 H7A 120.3 . . ?
C6 C7 H7A 120.3 . . ?
C7 C8 O1 125.1(2) . . ?
C7 C8 C9 121.1(2) . . ?
O1 C8 C9 113.8(2) . . ?
N1 C9 C8 119.0(2) . . ?
N1 C9 C4 122.2(2) . . ?
C8 C9 C4 118.8(2) . . ?
O1 C10 C11 108.18(18) . . ?
O1 C10 H10A 110.1 . . ?
C11 C10 H10A 110.1 . . ?
O1 C10 H10B 110.1 . . ?
C11 C10 H10B 110.1 . . ?
H10A C10 H10B 108.4 . . ?
O2 C11 O3 125.0(2) . . ?
O2 C11 C10 118.5(2) . . ?
O3 C11 C10 116.4(2) . . ?
O4 C12 O5 124.1(2) . . ?
O4 C12 C13 120.3(2) . . ?
O5 C12 C13 115.6(2) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 O5 Mn1 131.47(16) . 3_454 ?
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
Mn1 O5 2.0767(19) 3_455 ?
Mn1 O2 2.1477(17) . ?
Mn1 O4 2.1615(19) . ?
Mn1 O3 2.2258(16) 2_445 ?
Mn1 N1 2.2485(19) . ?
Mn1 O1 2.2951(16) . ?
O1 C8 1.369(3) . ?
O1 C10 1.432(3) . ?
O2 C11 1.252(3) . ?
O3 C11 1.256(3) . ?
O3 Mn1 2.2258(16) 2_444 ?
O4 C12 1.245(3) . ?
N1 C1 1.323(3) . ?
N1 C9 1.365(3) . ?
C1 C2 1.403(3) . ?
C1 H1A 0.9300 . ?
C2 C3 1.343(4) . ?
C2 H2A 0.9300 . ?
C3 C4 1.409(4) . ?
C3 H3A 0.9300 . ?
C4 C5 1.421(4) . ?
C4 C9 1.424(3) . ?
C5 C6 1.356(4) . ?
C5 H5A 0.9300 . ?
C6 C7 1.409(3) . ?
C6 H6A 0.9300 . ?
C7 C8 1.366(3) . ?
C7 H7A 0.9300 . ?
C8 C9 1.415(3) . ?
C10 C11 1.521(3) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C12 O5 1.259(3) . ?
C12 C13 1.501(3) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
O5 Mn1 2.0767(19) 3_454 ?
