#------------------------------------------------------------------------------
#$Date: 2016-02-21 11:56:54 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176809 $
#$URL: svn://www.crystallography.net/cod/cif/2/31/00/2310008.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2310008
loop_
_publ_author_name
'Deutsch, Maxime'
'Claiser, Nicolas'
'Pillet, Sébastien'
'Chumakov, Yurii'
'Becker, Pierre'
'Gillet, Jean-Michel'
'Gillon, Béatrice'
'Lecomte, Claude'
'Souhassou, Mohamed'
_publ_section_title
;
 Experimental determination of spin-dependent electron density by joint
 refinement of X-ray and polarized neutron diffraction data
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section A'
_journal_page_first              675
_journal_page_last               686
_journal_paper_doi               10.1107/S0108767312031996
_journal_volume                  68
_journal_year                    2012
_chemical_formula_sum            'C7 H16 Cu Mn N2 O11'
_chemical_formula_weight         422.69
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                   12.7158(3)
_cell_length_b                   21.3520(5)
_cell_length_c                   5.1745(2)
_cell_measurement_temperature    10(5)
_cell_volume                     1404.92(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      10(5)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0266
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8505
_diffrn_reflns_theta_full        53.34
_diffrn_reflns_theta_max         53.34
_diffrn_reflns_theta_min         3.20
_exptl_absorpt_coefficient_mu    2.483
_exptl_absorpt_correction_T_max  0.880
_exptl_absorpt_correction_T_min  0.615
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
Numerical absorption correction based on gaussian integration over
   a multifaceted crystal model
;
_exptl_crystal_density_diffrn    1.998
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.2673
_exptl_crystal_size_mid          0.1561
_exptl_crystal_size_min          0.0620
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.958
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     140
_refine_ls_number_reflns         8505
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.958
_refine_ls_R_factor_all          0.0366
_refine_ls_R_factor_gt           0.0290
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0177P)²+1.3214P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0599
_refine_ls_wR_factor_ref         0.0615
_reflns_number_gt                6880
_reflns_number_total             8505
_reflns_threshold_expression     >3σ(I)
_cod_data_source_file            wl5162.cif
_cod_data_source_block           I
_cod_database_code               2310008
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -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
Cu Cu 0.050679(8) 0.2500 0.150042(19) 0.00415(2) Uani 1 2 d S
Mn Mn 0.0000 0.5000 0.0000 0.00501(2) Uani 1 2 d S
O1 O -0.06303(3) 0.423844(19) 0.22854(9) 0.00660(5) Uani 1 1 d .
O2 O 0.09575(4) 0.42089(2) -0.12554(9) 0.00716(6) Uani 1 1 d .
O3 O 0.11523(3) 0.317983(19) -0.06201(9) 0.00643(5) Uani 1 1 d .
O4 O -0.11791(4) 0.47868(2) -0.29552(9) 0.00889(6) Uani 1 1 d .
O5 O 0.17489(6) 0.2500 0.46535(14) 0.00904(9) Uani 1 2 d S
O6 O 0.21400(4) 0.41212(3) 0.42287(10) 0.01069(7) Uani 1 1 d .
N N -0.03674(4) 0.31734(2) 0.28494(10) 0.00587(6) Uani 1 1 d .
C1 C 0.07282(4) 0.37043(2) -0.01580(10) 0.00557(6) Uani 1 1 d .
C2 C -0.01646(4) 0.37163(2) 0.18463(10) 0.00536(6) Uani 1 1 d .
C4 C -0.10898(6) 0.2500 0.62761(15) 0.00669(9) Uani 1 2 d S
C3 C -0.12204(5) 0.31020(3) 0.47259(12) 0.00734(7) Uani 1 1 d .
H1 H -0.1630(17) 0.2500 0.761(4) 0.015(5) Uiso 1 2 d S
H2 H -0.0382(16) 0.2500 0.706(4) 0.013(4) Uiso 1 2 d S
H3 H -0.1877(12) 0.3103(7) 0.388(3) 0.015(3) Uiso 1 1 d .
H4 H -0.1224(11) 0.3445(7) 0.585(3) 0.015(3) Uiso 1 1 d .
H5 H -0.1509(15) 0.5102(9) -0.342(4) 0.036(5) Uiso 1 1 d .
H6 H -0.1047(13) 0.4602(8) -0.426(3) 0.021(4) Uiso 1 1 d .
H7 H 0.1673(14) 0.2199(8) 0.559(3) 0.034(5) Uiso 1 1 d .
H8 H 0.1986(14) 0.4119(8) 0.574(4) 0.028(4) Uiso 1 1 d .
H9 H 0.2733(15) 0.4166(8) 0.413(4) 0.034(5) Uiso 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 0.0030 0.0020 '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 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3370 0.7280 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3200 1.2650 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-17 -3 -2 0.0353 -16.9785 -3.0998 -1.9903 -0.7750 -0.4276 -0.4464
6 28 1 0.1044 5.9749 27.9737 0.9989 -0.1907 0.5540 0.8067
-3 2 7 0.0783 -2.9807 1.8927 6.9896 0.1378 -0.6912 0.6742
-9 21 4 0.1191 -8.9921 20.8404 3.9990 -0.5905 -0.3178 0.7626
11 -15 -4 0.0905 10.9050 -15.0785 -4.0044 0.5720 0.4731 -0.6090
17 2 2 0.0413 16.9792 2.1020 1.9902 0.7927 0.4117 0.4233
5 -2 -7 0.0737 4.9779 -1.8775 -6.9904 -0.0506 0.7568 -0.6520
18 -3 1 0.0240 17.9782 -3.1820 0.9782 0.8864 0.4502 0.2161
-18 2 -1 0.0346 -17.9781 1.8703 -0.9910 -0.8637 -0.4700 -0.2476
-15 -9 -3 0.0558 -15.0418 -8.8259 -2.9768 -0.6313 -0.3678 -0.6511
14 -16 -2 0.0878 13.9105 -16.1143 -2.0107 0.8082 0.3769 -0.4109
18 0 0 0.0273 17.9843 -0.1827 -0.0209 0.7903 0.5875 0.1907
-7 -27 0 0.1191 -6.9718 -26.9949 -0.0001 0.1729 -0.6601 -0.7002
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
N Cu N 95.22(3) 8_565 .
N Cu O3 83.962(18) 8_565 8_565
N Cu O3 165.67(2) . 8_565
N Cu O3 165.67(2) 8_565 .
N Cu O3 83.962(18) . .
O3 Cu O3 93.30(2) 8_565 .
N Cu O5 98.021(19) 8_565 .
N Cu O5 98.021(19) . .
O3 Cu O5 96.252(18) 8_565 .
O3 Cu O5 96.252(18) . .
O1 Mn O1 180.000(14) . 5_565
O1 Mn O2 102.260(16) . 5_565
O1 Mn O2 77.740(16) 5_565 5_565
O1 Mn O2 77.740(16) . .
O1 Mn O2 102.260(16) 5_565 .
O2 Mn O2 180.0 5_565 .
O1 Mn O4 88.387(18) . .
O1 Mn O4 91.613(18) 5_565 .
O2 Mn O4 89.242(18) 5_565 .
O2 Mn O4 90.758(18) . .
O1 Mn O4 91.613(18) . 5_565
O1 Mn O4 88.387(18) 5_565 5_565
O2 Mn O4 90.758(18) 5_565 5_565
O2 Mn O4 89.242(18) . 5_565
O4 Mn O4 180.0 . 5_565
C2 O1 Mn 112.66(3) . .
C1 O2 Mn 113.66(4) . .
C1 O3 Cu 111.36(4) . .
C2 N C3 120.42(5) . .
C2 N Cu 113.79(4) . .
C3 N Cu 125.73(3) . .
O2 C1 O3 125.19(5) . .
O2 C1 C2 117.60(5) . .
O3 C1 C2 117.17(5) . .
O1 C2 N 127.92(5) . .
O1 C2 C1 118.35(5) . .
N C2 C1 113.71(4) . .
C3 C4 C3 114.98(7) 8_565 .
N C3 C4 110.87(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu N 1.9469(5) 8_565
Cu N 1.9469(5) .
Cu O3 1.9962(4) 8_565
Cu O3 1.9962(4) .
Cu O5 2.2709(7) .
Mn O1 2.1645(4) .
Mn O1 2.1645(4) 5_565
Mn O2 2.1811(4) 5_565
Mn O2 2.1811(4) .
Mn O4 2.1894(5) .
Mn O4 2.1894(5) 5_565
O1 C2 1.2827(6) .
O2 C1 1.2524(7) .
O3 C1 1.2657(7) .
N C2 1.2960(7) .
N C3 1.4637(7) .
C1 C2 1.5378(7) .
C4 C3 1.5243(7) 8_565
C4 C3 1.5243(7) .
