#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:10:25 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179955 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/50/7025070.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_7025070
loop_
_publ_author_name
'Escuer, Albert'
'Cordero, Beatriz'
'Font-Bardia, Mercé'
'Calvet, Teresa'
'Roubeau, Olivier'
'Teat, Simon J.'
'Fedi, Serena'
'Fabrizi de Biani, Fabrizia'
_publ_section_title
;
 Manganese clusters derived from a 2,6-diacetylpyridine dioximato ligand:
 structure and magnetic study
;
_journal_issue                   20
_journal_name_full               'Dalton Transactions'
_journal_page_first              4817
_journal_paper_doi               10.1039/b924977j
_journal_volume                  39
_journal_year                    2010
_chemical_formula_moiety         'C54 H56 Mn8 N20 O20, H2O'
_chemical_formula_sum            'C54 H56 Mn8 N20 O21'
_chemical_formula_weight         1760.71
_chemical_name_systematic
;
?
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_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                 95.27(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   18.169(11)
_cell_length_b                   14.096(7)
_cell_length_c                   13.809(6)
_cell_measurement_reflns_used    726
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      31
_cell_measurement_theta_min      3
_cell_volume                     3522(3)
_computing_cell_refinement       AUTOMAR
_computing_data_collection       MARXDS
_computing_data_reduction        MARSCALE
_computing_molecular_graphics    'ORTEP (Brueggermann and Smith, 1990)'
_computing_publication_material  'PLATON (Spek, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'MAR345 with image plate detector'
_diffrn_measurement_method       'phi 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  0.0604
_diffrn_reflns_av_sigmaI/netI    0.0842
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            21967
_diffrn_reflns_theta_full        32.43
_diffrn_reflns_theta_max         32.43
_diffrn_reflns_theta_min         2.58
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    1.470
_exptl_absorpt_correction_T_max  0.86
_exptl_absorpt_correction_T_min  0.83
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.660
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.916
_refine_diff_density_min         -0.828
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     270
_refine_ls_number_reflns         6517
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.1301
_refine_ls_R_factor_gt           0.0758
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1119P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1996
_refine_ls_wR_factor_ref         0.2284
_reflns_number_gt                3922
_reflns_number_total             6517
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b924977j.txt
_cod_data_source_block           aemm49a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      C2/m
_cod_database_code               7025070
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -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
Mn1 Mn 0.55539(3) 0.38058(4) 0.14196(4) 0.03554(17) Uani 1 1 d U
Mn2 Mn 0.71394(4) 0.5000 0.23421(6) 0.0343(2) Uani 1 2 d SU
Mn3 Mn 0.65371(4) 0.5000 -0.00935(6) 0.0348(2) Uani 1 2 d SU
O1 O 0.63384(19) 0.5000 0.1468(3) 0.0333(5) Uani 1 2 d SU
O2 O 0.40187(15) 0.36784(19) -0.0061(2) 0.0376(6) Uani 1 1 d .
O3 O 0.8030(2) 0.5000 0.3381(3) 0.0336(7) Uani 1 2 d SU
O4 O 0.7196(3) 0.5000 0.4410(4) 0.0639(13) Uani 1 2 d S
O5 O 0.8365(3) 0.5000 0.4932(4) 0.0581(12) Uani 1 2 d S
O6 O 0.71200(16) 0.3664(2) 0.2638(3) 0.0483(7) Uani 1 1 d .
O7 O 0.2024(2) 0.5000 -0.1441(3) 0.0455(9) Uani 1 2 d S
O8 O 0.4919(2) 0.5000 0.1793(3) 0.0384(7) Uani 1 2 d SU
N1 N 0.7871(3) 0.5000 0.4258(4) 0.0456(11) Uani 1 2 d S
N2 N 0.5110(2) 0.2609(3) 0.2291(3) 0.0452(8) Uani 1 1 d .
N3 N 0.64330(19) 0.3282(2) 0.2545(3) 0.0423(7) Uani 1 1 d U
N4 N 0.44047(17) 0.3245(2) 0.0734(3) 0.0387(7) Uani 1 1 d U
N5 N 0.2726(3) 0.5000 0.1352(4) 0.0422(11) Uani 1 2 d S
N6 N 0.2237(3) 0.5000 -0.0484(4) 0.0399(10) Uani 1 2 d S
N7 N 0.4149(3) 0.5000 0.1678(4) 0.0393(10) Uani 1 2 d S
C1 C 0.5556(2) 0.2246(3) 0.3063(4) 0.0487(10) Uani 1 1 d .
C2 C 0.5284(3) 0.1577(4) 0.3677(5) 0.0703(15) Uani 1 1 d .
H2 H 0.5582 0.1322 0.4195 0.084 Uiso 1 1 calc R
C3 C 0.4537(4) 0.1298(5) 0.3487(5) 0.0779(19) Uani 1 1 d .
H3 H 0.4337 0.0873 0.3906 0.093 Uiso 1 1 calc R
C4 C 0.4104(3) 0.1637(4) 0.2703(4) 0.0631(13) Uani 1 1 d .
H4 H 0.3617 0.1438 0.2565 0.076 Uiso 1 1 calc R
C5 C 0.4426(2) 0.2294(3) 0.2123(3) 0.0434(9) Uani 1 1 d .
C6 C 0.6299(3) 0.2651(3) 0.3194(4) 0.0504(10) Uani 1 1 d .
C7 C 0.6880(4) 0.2353(5) 0.3976(5) 0.0804(19) Uani 1 1 d .
H7A H 0.7333 0.2681 0.3893 0.121 Uiso 1 1 calc R
H7B H 0.6959 0.1681 0.3934 0.121 Uiso 1 1 calc R
H7C H 0.6720 0.2505 0.4601 0.121 Uiso 1 1 calc R
C8 C 0.4002(2) 0.2708(3) 0.1254(3) 0.0382(8) Uani 1 1 d .
C9 C 0.3205(3) 0.2518(4) 0.0990(5) 0.0629(14) Uani 1 1 d .
H9A H 0.3063 0.2764 0.0352 0.094 Uiso 1 1 calc R
H9B H 0.2918 0.2821 0.1453 0.094 Uiso 1 1 calc R
H9C H 0.3117 0.1847 0.0996 0.094 Uiso 1 1 calc R
C10 C 0.1995(3) 0.5000 0.1148(5) 0.0461(13) Uani 1 2 d S
C11 C 0.1509(4) 0.5000 0.1858(5) 0.0583(17) Uani 1 2 d S
H11 H 0.1001 0.5000 0.1698 0.070 Uiso 1 2 calc SR
C12 C 0.1805(5) 0.5000 0.2819(7) 0.076(2) Uani 1 2 d S
H12 H 0.1491 0.5000 0.3315 0.091 Uiso 1 2 calc SR
C13 C 0.2542(4) 0.5000 0.3040(5) 0.0523(15) Uani 1 2 d S
H13 H 0.2742 0.5000 0.3685 0.063 Uiso 1 2 calc SR
C14 C 0.3002(3) 0.5000 0.2282(4) 0.0403(12) Uani 1 2 d S
C15 C 0.1743(3) 0.5000 0.0108(5) 0.0499(14) Uani 1 2 d S
C16 C 0.0926(4) 0.5000 -0.0275(7) 0.073(2) Uani 1 2 d S
H16A H 0.0883 0.5000 -0.0973 0.110 Uiso 1 2 calc SR
H16B H 0.0691 0.5556 -0.0046 0.110 Uiso 0.50 1 calc PR
H16C H 0.0691 0.4444 -0.0046 0.110 Uiso 0.50 1 calc PR
C17 C 0.3816(4) 0.5000 0.2430(5) 0.0469(13) Uani 1 2 d S
C18 C 0.4219(5) 0.5000 0.3447(8) 0.085(3) Uani 1 2 d S
H18A H 0.4743 0.5000 0.3400 0.128 Uiso 1 2 calc SR
H18B H 0.4084 0.4444 0.3791 0.128 Uiso 0.50 1 calc PR
H18C H 0.4084 0.5556 0.3791 0.128 Uiso 0.50 1 calc PR
O1W O 0.5055(12) 0.0000 0.3843(14) 0.125(6) Uani 0.50 2 d SP
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
O2 Mn1 O8 122.38(13) 2_655 .
O2 Mn1 O1 78.53(12) 2_655 .
O8 Mn1 O1 75.64(12) . .
O2 Mn1 N3 106.94(13) 2_655 .
O8 Mn1 N3 117.30(15) . .
O1 Mn1 N3 79.27(12) . .
O2 Mn1 N2 126.11(13) 2_655 .
O8 Mn1 N2 103.48(14) . .
O1 Mn1 N2 144.58(14) . .
N3 Mn1 N2 69.70(13) . .
O2 Mn1 N4 89.94(12) 2_655 .
O8 Mn1 N4 83.25(13) . .
O1 Mn1 N4 144.88(12) . .
N3 Mn1 N4 135.78(13) . .
N2 Mn1 N4 67.43(12) . .
O1 Mn2 O6 96.45(10) . 6_565
O1 Mn2 O6 96.45(10) . .
O6 Mn2 O6 155.3(2) 6_565 .
O1 Mn2 O7 101.02(18) . 5_665
O6 Mn2 O7 99.06(10) 6_565 5_665
O6 Mn2 O7 99.06(10) . 5_665
O1 Mn2 O3 177.95(16) . .
O6 Mn2 O3 83.17(10) 6_565 .
O6 Mn2 O3 83.17(10) . .
O7 Mn2 O3 81.03(16) 5_665 .
O2 Mn3 O2 121.14(15) 5_665 2_655
O2 Mn3 O1 77.45(9) 5_665 .
O2 Mn3 O1 77.45(9) 2_655 .
O2 Mn3 N5 112.95(9) 5_665 5_665
O2 Mn3 N5 112.95(9) 2_655 5_665
O1 Mn3 N5 153.72(16) . 5_665
O2 Mn3 N6 114.67(9) 5_665 5_665
O2 Mn3 N6 114.67(9) 2_655 5_665
O1 Mn3 N6 84.37(16) . 5_665
N5 Mn3 N6 69.35(18) 5_665 5_665
O2 Mn3 N7 83.18(10) 5_665 5_665
O2 Mn3 N7 83.18(10) 2_655 5_665
O1 Mn3 N7 139.77(15) . 5_665
N5 Mn3 N7 66.51(17) 5_665 5_665
N6 Mn3 N7 135.86(17) 5_665 5_665
Mn2 O1 Mn1 120.01(12) . .
Mn2 O1 Mn1 120.01(12) . 6_565
Mn1 O1 Mn1 99.67(15) . 6_565
Mn2 O1 Mn3 117.21(19) . .
Mn1 O1 Mn3 97.67(12) . .
Mn1 O1 Mn3 97.67(12) 6_565 .
N4 O2 Mn1 122.8(2) . 2_655
N4 O2 Mn3 120.9(2) . 5_665
Mn1 O2 Mn3 103.34(12) 2_655 5_665
N1 O3 Mn2 115.5(3) . .
N3 O6 Mn2 113.8(2) . .
N6 O7 Mn2 115.8(3) . 5_665
N7 O8 Mn1 122.18(14) . 6_565
N7 O8 Mn1 122.18(14) . .
Mn1 O8 Mn1 104.42(17) 6_565 .
O5 N1 O4 121.7(6) . .
O5 N1 O3 120.4(5) . .
O4 N1 O3 117.9(5) . .
C5 N2 C1 119.2(4) . .
C5 N2 Mn1 122.3(3) . .
C1 N2 Mn1 118.4(3) . .
C6 N3 O6 115.8(4) . .
C6 N3 Mn1 122.3(3) . .
O6 N3 Mn1 121.6(3) . .
C8 N4 O2 114.8(3) . .
C8 N4 Mn1 119.6(3) . .
O2 N4 Mn1 122.4(2) . .
C10 N5 C14 118.8(5) . .
C10 N5 Mn3 118.8(4) . 5_665
C14 N5 Mn3 122.4(4) . 5_665
C15 N6 O7 118.6(5) . .
C15 N6 Mn3 119.8(4) . 5_665
O7 N6 Mn3 121.6(3) . 5_665
C17 N7 O8 117.6(5) . .
C17 N7 Mn3 120.3(4) . 5_665
O8 N7 Mn3 122.1(3) . 5_665
N2 C1 C2 120.5(4) . .
N2 C1 C6 115.0(4) . .
C2 C1 C6 124.5(5) . .
C1 C2 C3 117.7(5) . .
C1 C2 H2 121.1 . .
C3 C2 H2 121.1 . .
C4 C3 C2 121.6(6) . .
C4 C3 H3 119.2 . .
C2 C3 H3 119.2 . .
C3 C4 C5 116.5(5) . .
C3 C4 H4 121.7 . .
C5 C4 H4 121.7 . .
N2 C5 C4 124.3(4) . .
N2 C5 C8 114.8(4) . .
C4 C5 C8 120.9(4) . .
N3 C6 C1 114.2(4) . .
N3 C6 C7 121.6(4) . .
C1 C6 C7 124.1(5) . .
C6 C7 H7A 109.5 . .
C6 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
C6 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
N4 C8 C5 113.3(3) . .
N4 C8 C9 123.4(4) . .
C5 C8 C9 123.3(4) . .
C8 C9 H9A 109.5 . .
C8 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
C8 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
N5 C10 C11 122.8(6) . .
N5 C10 C15 114.9(6) . .
C11 C10 C15 122.3(6) . .
C10 C11 C12 117.7(7) . .
C10 C11 H11 121.2 . .
C12 C11 H11 121.2 . .
C13 C12 C11 120.5(8) . .
C13 C12 H12 119.7 . .
C11 C12 H12 119.7 . .
C12 C13 C14 118.7(7) . .
C12 C13 H13 120.7 . .
C14 C13 H13 120.7 . .
N5 C14 C13 121.5(5) . .
N5 C14 C17 114.6(5) . .
C13 C14 C17 123.8(6) . .
N6 C15 C10 117.1(6) . .
N6 C15 C16 119.9(7) . .
C10 C15 C16 122.9(6) . .
C15 C16 H16A 109.5 . .
C15 C16 H16B 109.5 . .
H16A C16 H16B 109.5 . .
C15 C16 H16C 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
N7 C17 C14 116.2(6) . .
N7 C17 C18 122.6(6) . .
C14 C17 C18 121.3(6) . .
C17 C18 H18A 109.5 . .
C17 C18 H18B 109.5 . .
H18A C18 H18B 109.5 . .
C17 C18 H18C 109.5 . .
H18A C18 H18C 109.5 . .
H18B C18 H18C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 O2 2.103(3) 2_655
Mn1 O8 2.130(2) .
Mn1 O1 2.203(2) .
Mn1 N3 2.248(3) .
Mn1 N2 2.263(4) .
Mn1 N4 2.349(3) .
Mn2 O1 1.804(4) .
Mn2 O6 1.927(3) 6_565
Mn2 O6 1.927(3) .
Mn2 O7 2.051(4) 5_665
Mn2 O3 2.062(4) .
Mn3 O2 2.139(3) 5_665
Mn3 O2 2.139(3) 2_655
Mn3 O1 2.218(4) .
Mn3 N5 2.289(5) 5_665
Mn3 N6 2.296(5) 5_665
Mn3 N7 2.416(5) 5_665
O1 Mn1 2.203(2) 6_565
O2 N4 1.388(4) .
O2 Mn1 2.103(3) 2_655
O2 Mn3 2.139(3) 5_665
O3 N1 1.271(6) .
O4 N1 1.263(7) .
O5 N1 1.233(7) .
O6 N3 1.355(4) .
O7 N6 1.342(6) .
O7 Mn2 2.051(4) 5_665
O8 N7 1.395(6) .
O8 Mn1 2.130(2) 6_565
N2 C5 1.319(5) .
N2 C1 1.378(6) .
N3 C6 1.301(6) .
N4 C8 1.311(5) .
N5 C10 1.333(8) .
N5 C14 1.335(8) .
N5 Mn3 2.289(5) 5_665
N6 C15 1.268(8) .
N6 Mn3 2.296(5) 5_665
N7 C17 1.249(8) .
N7 Mn3 2.416(5) 5_665
C1 C2 1.389(7) .
C1 C6 1.462(6) .
C2 C3 1.413(8) .
C2 H2 0.9300 .
C3 C4 1.365(8) .
C3 H3 0.9300 .
C4 C5 1.389(7) .
C4 H4 0.9300 .
C5 C8 1.485(6) .
C6 C7 1.499(7) .
C7 H7A 0.9600 .
C7 H7B 0.9600 .
C7 H7C 0.9600 .
C8 C9 1.486(6) .
C9 H9A 0.9600 .
C9 H9B 0.9600 .
C9 H9C 0.9600 .
C10 C11 1.377(10) .
C10 C15 1.467(9) .
C11 C12 1.384(11) .
C11 H11 0.9300 .
C12 C13 1.347(10) .
C12 H12 0.9300 .
C13 C14 1.399(9) .
C13 H13 0.9300 .
C14 C17 1.474(9) .
C15 C16 1.530(9) .
C16 H16A 0.9600 .
C16 H16B 0.9600 .
C16 H16C 0.9600 .
C17 C18 1.523(11) .
C18 H18A 0.9600 .
C18 H18B 0.9600 .
C18 H18C 0.9600 .
