#------------------------------------------------------------------------------
#$Date: 2016-02-20 02:53:41 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176768 $
#$URL: svn://www.crystallography.net/cod/cif/2/10/47/2104774.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_2104774
loop_
_publ_author_name
'Biju, A. R.'
'Rajasekharan, M. V.'
_publ_section_title
;
 Polymorphism in the nitrate salt of the
 [Mn(acetylacetonate)₂(H₂O)₂]⁺ ion
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              373
_journal_page_last               379
_journal_paper_doi               10.1107/S0108768110009961
_journal_volume                  66
_journal_year                    2010
_chemical_formula_sum            'C10 H20 Mn N O10'
_chemical_formula_weight         369.21
_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                97.8890(10)
_cell_angle_beta                 91.533(2)
_cell_angle_gamma                118.3800(10)
_cell_formula_units_Z            2
_cell_length_a                   7.7085(7)
_cell_length_b                   7.7158(7)
_cell_length_c                   15.9918(14)
_cell_measurement_reflns_used    3333
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      24.97
_cell_measurement_theta_min      2.59
_cell_volume                     824.28(13)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0225
_diffrn_reflns_av_sigmaI/netI    0.0271
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            8507
_diffrn_reflns_theta_full        25.93
_diffrn_reflns_theta_max         25.93
_diffrn_reflns_theta_min         1.29
_exptl_absorpt_coefficient_mu    0.847
_exptl_absorpt_correction_T_max  0.8488
_exptl_absorpt_correction_T_min  0.8225
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.488
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             384
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.484
_refine_diff_density_min         -0.367
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         3194
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_gt           0.0421
_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)+(0.0573P)²+0.4936P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1091
_refine_ls_wR_factor_ref         0.1144
_reflns_number_gt                2677
_reflns_number_total             3194
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            zb5009.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               2104774
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn Mn1 0.0000 0.0000 0.0000 0.04353(18) Uani d S 1 . .
Mn Mn2 0.0000 0.0000 0.5000 0.03354(16) Uani d S 1 . .
O O1 -0.2556(3) -0.1732(3) 0.03123(13) 0.0507(5) Uani d . 1 . .
O O2 -0.0175(3) 0.2333(3) 0.04385(13) 0.0514(5) Uani d . 1 . .
O O3 0.1361(4) 0.0080(4) 0.12652(14) 0.0631(6) Uani d D 1 . .
H H31 0.056(5) -0.038(6) 0.161(3) 0.095 Uiso d D 1 . .
H H32 0.225(5) 0.112(5) 0.150(3) 0.095 Uiso d D 1 . .
O O4 -0.0797(3) 0.1412(3) 0.58285(12) 0.0544(5) Uani d . 1 . .
O O5 -0.1226(3) 0.0544(3) 0.40979(12) 0.0550(5) Uani d . 1 . .
O O6 0.2777(4) 0.2763(4) 0.49672(15) 0.0720(7) Uani d D 1 . .
H H61 0.321(7) 0.311(7) 0.456(2) 0.108 Uiso d D 1 . .
H H62 0.336(6) 0.347(6) 0.541(2) 0.108 Uiso d D 1 . .
N N1 0.4541(4) 0.4012(4) 0.29868(15) 0.0515(6) Uani d . 1 . .
O O7 0.5850(5) 0.5431(5) 0.3418(2) 0.1466(17) Uani d . 1 . .
O O8 0.4553(4) 0.3780(4) 0.22129(16) 0.0910(9) Uani d . 1 . .
O O9 0.3241(5) 0.2830(6) 0.3305(2) 0.1379(16) Uani d . 1 . .
C C1 -0.1236(5) 0.4467(5) 0.1138(2) 0.0651(9) Uani d . 1 . .
H H1A -0.0176 0.5113 0.1590 0.098 Uiso calc R 1 . .
H H1B -0.2424 0.4397 0.1343 0.098 Uiso calc R 1 . .
H H1C -0.0891 0.5218 0.0681 0.098 Uiso calc R 1 . .
C C2 -0.1577(4) 0.2401(4) 0.08276(16) 0.0474(6) Uani d . 1 . .
C C3 -0.3270(4) 0.0742(5) 0.09698(19) 0.0530(7) Uani d . 1 . .
H H3 -0.4201 0.0957 0.1258 0.064 Uiso calc R 1 . .
C C4 -0.3692(4) -0.1220(4) 0.07172(17) 0.0473(6) Uani d . 1 . .
C C5 -0.5564(4) -0.2907(5) 0.0921(2) 0.0652(9) Uani d . 1 . .
H H5A -0.6005 -0.4046 0.0478 0.098 Uiso calc R 1 . .
H H5B -0.6567 -0.2507 0.0966 0.098 Uiso calc R 1 . .
H H5C -0.5320 -0.3250 0.1450 0.098 Uiso calc R 1 . .
C C6 -0.3238(11) 0.1937(11) 0.6556(5) 0.075(2) Uani d P 0.50 . .
H H6A -0.3346 0.3133 0.6537 0.090 Uiso calc PR 0.50 . .
H H6B -0.2328 0.2179 0.7044 0.090 Uiso calc PR 0.50 . .
C C7 -0.2562(8) 0.1335(8) 0.5751(4) 0.0478(13) Uani d P 0.50 . .
C C8 -0.2995(8) 0.0582(8) 0.4205(4) 0.0501(13) Uani d P 0.50 . .
C C9 -0.3590(9) 0.0993(9) 0.4984(4) 0.0583(15) Uani d P 0.50 . .
H H9 -0.4774 0.1039 0.4983 0.070 Uiso calc PR 0.50 . .
C C10 -0.4157(11) 0.0365(11) 0.3396(5) 0.074(2) Uani d P 0.50 . .
H H10D -0.3543 0.0112 0.2907 0.089 Uiso calc PR 0.50 . .
H H10E -0.4268 0.1558 0.3370 0.089 Uiso calc PR 0.50 . .
C C6A -0.0916(11) 0.4397(11) 0.6433(4) 0.0674(17) Uiso d P 0.50 . .
H H6A1 -0.1149 0.5420 0.6262 0.101 Uiso calc PR 0.50 . .
H H6A2 0.0321 0.5006 0.6787 0.101 Uiso calc R 1 . .
H H6A3 -0.1972 0.3595 0.6745 0.101 Uiso calc PR 0.50 . .
C C7A -0.0833(8) 0.3109(8) 0.5667(3) 0.0455(12) Uiso d P 0.50 . .
C C8A -0.1170(8) 0.2319(8) 0.4118(3) 0.0441(12) Uiso d P 0.50 . .
C C9A -0.1032(8) 0.3517(9) 0.4865(4) 0.0525(13) Uiso d P 0.50 . .
H H9A -0.1075 0.4689 0.4828 0.063 Uiso calc PR 0.50 . .
C C10A -0.1577(10) 0.2775(11) 0.3293(4) 0.0648(16) Uiso d P 0.50 . .
H H10A -0.0551 0.2886 0.2941 0.097 Uiso calc PR 0.50 . .
H H10B -0.1610 0.4015 0.3381 0.097 Uiso calc PR 0.50 . .
H H10C -0.2833 0.1722 0.3019 0.097 Uiso calc R 1 . .
O O1W 0.8769(5) 0.8320(5) 0.23999(16) 0.0923(9) Uani d D 1 . .
H H1W 0.791(7) 0.732(6) 0.247(4) 0.138 Uiso d D 1 . .
H H2W 0.931(7) 0.907(7) 0.283(3) 0.138 Uiso d D 1 . .
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O2 Mn1 O2 . 2 180.00(15) ?
O2 Mn1 O1 . . 92.27(8) ?
O2 Mn1 O1 2 . 87.73(8) ?
O2 Mn1 O1 . 2 87.73(8) ?
O2 Mn1 O1 2 2 92.27(8) ?
O1 Mn1 O1 . 2 180.00(15) ?
O2 Mn1 O3 . 2 89.68(9) ?
O2 Mn1 O3 2 2 90.32(9) ?
O1 Mn1 O3 . 2 90.59(9) ?
O1 Mn1 O3 2 2 89.41(9) ?
O2 Mn1 O3 . . 90.32(9) ?
O2 Mn1 O3 2 . 89.68(9) ?
O1 Mn1 O3 . . 89.41(9) ?
O1 Mn1 O3 2 . 90.59(9) ?
O3 Mn1 O3 2 . 180.00(14) ?
O4 Mn2 O4 . 2_556 180.0000(10) ?
O4 Mn2 O5 . 2_556 88.21(8) ?
O4 Mn2 O5 2_556 2_556 91.79(8) ?
O4 Mn2 O5 . . 91.79(8) ?
O4 Mn2 O5 2_556 . 88.21(8) ?
O5 Mn2 O5 2_556 . 180.0000(10) ?
O4 Mn2 O6 . . 90.08(10) ?
O4 Mn2 O6 2_556 . 89.92(10) ?
O5 Mn2 O6 2_556 . 89.78(10) ?
O5 Mn2 O6 . . 90.22(10) ?
O4 Mn2 O6 . 2_556 89.92(10) ?
O4 Mn2 O6 2_556 2_556 90.08(10) ?
O5 Mn2 O6 2_556 2_556 90.22(10) ?
O5 Mn2 O6 . 2_556 89.78(10) ?
O6 Mn2 O6 . 2_556 180.00(13) ?
C4 O1 Mn1 . . 127.12(18) ?
C2 O2 Mn1 . . 126.97(18) ?
C7 O4 C7A . . 62.6(3) ?
C7 O4 Mn2 . . 122.8(3) ?
C7A O4 Mn2 . . 119.6(3) ?
C8A O5 C8 . . 63.3(3) ?
C8A O5 Mn2 . . 122.2(3) ?
C8 O5 Mn2 . . 119.0(3) ?
O9 N1 O7 . . 119.6(3) ?
O9 N1 O8 . . 120.5(3) ?
O7 N1 O8 . . 119.9(3) ?
O2 C2 C3 . . 124.3(3) ?
O2 C2 C1 . . 114.4(3) ?
C3 C2 C1 . . 121.2(3) ?
C2 C3 C4 . . 125.1(3) ?
O1 C4 C3 . . 124.1(2) ?
O1 C4 C5 . . 115.4(3) ?
C3 C4 C5 . . 120.5(3) ?
C7 C6 C10 . 2_456 103.8(5) ?
O4 C7 C9 . . 122.9(5) ?
O4 C7 C6 . . 115.8(5) ?
C9 C7 C6 . . 120.8(6) ?
C9 C8 O5 . . 124.6(5) ?
C9 C8 C10 . . 120.5(5) ?
O5 C8 C10 . . 114.5(5) ?
C7 C9 C8 . . 124.7(5) ?
C7 C9 C9 . 2_456 109.1(6) ?
C8 C9 C9 . 2_456 109.1(6) ?
C8 C10 C6 . 2_456 103.8(5) ?
O4 C7A C9A . . 124.7(5) ?
O4 C7A C6A . . 114.5(5) ?
C9A C7A C6A . . 120.4(5) ?
O5 C8A C9A . . 122.5(5) ?
O5 C8A C10A . . 116.0(5) ?
C9A C8A C10A . . 120.9(5) ?
C8A C9A C7A . . 124.8(6) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Mn1 O2 . 1.9076(19) ?
Mn1 O2 2 1.9076(19) ?
Mn1 O1 . 1.9104(18) ?
Mn1 O1 2 1.9104(18) ?
Mn1 O3 2 2.234(2) ?
Mn1 O3 . 2.234(2) ?
Mn2 O4 . 1.8983(18) ?
Mn2 O4 2_556 1.8983(18) ?
Mn2 O5 2_556 1.9026(18) ?
Mn2 O5 . 1.9026(18) ?
Mn2 O6 . 2.197(2) ?
Mn2 O6 2_556 2.197(2) ?
O1 C4 . 1.277(3) ?
O2 C2 . 1.280(3) ?
O4 C7 . 1.335(6) ?
O4 C7A . 1.382(6) ?
O5 C8A . 1.346(6) ?
O5 C8 . 1.392(6) ?
N1 O9 . 1.175(3) ?
N1 O7 . 1.182(4) ?
N1 O8 . 1.227(3) ?
C1 C2 . 1.495(4) ?
C2 C3 . 1.379(4) ?
C3 C4 . 1.385(4) ?
C4 C5 . 1.496(4) ?
C6 C7 . 1.499(8) ?
C7 C9 . 1.365(9) ?
C8 C9 . 1.386(9) ?
C8 C10 . 1.497(9) ?
C6A C7A . 1.492(9) ?
C7A C9A . 1.383(8) ?
C8A C9A . 1.374(8) ?
C8A C10A . 1.475(8) ?
