#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:06:27 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179313 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/10/4321048.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_4321048
loop_
_publ_author_name
'Vasilis Tangoulis'
'Dora A. Malamatari'
'Georgios A. Spyroulias'
'Catherine P. Raptopoulou'
'Aris Terzis'
'Dimitris P. Kessissoglou'
_publ_section_title
;
 An EPR and1H NMR Active Mixed-Valence Manganese (III/II/III) Trinuclear
 Compound
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2621
_journal_page_last               2630
_journal_paper_doi               10.1021/ic991430x
_journal_volume                  39
_journal_year                    2000
_chemical_formula_analytical     '[Mn3(C11 H13 N O3)2 (C7 H5 O3)4. 2CH3CN]'
_chemical_formula_structural     '[Mn3(SALADHP)2(HSAL)4.2CH3CN]'
_chemical_formula_sum            'C54 H52 Mn3 N4 O18'
_chemical_formula_weight         1209.82
_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
_cell_angle_alpha                112.56(1)
_cell_angle_beta                 93.42(2)
_cell_angle_gamma                115.43(1)
_cell_formula_units_Z            1
_cell_length_a                   10.367(6)
_cell_length_b                   11.369(6)
_cell_length_c                   13.967(8)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298
_cell_measurement_theta_max      11.7
_cell_measurement_theta_min      5.4
_cell_volume                     1322.3(13)
_computing_cell_refinement
'Program LEAST (UCLA Crystallographic Package)'
_computing_data_collection
'Program COLLECT (UCLA Crystallographic Package)'
_computing_data_reduction
'Program REDUCE (UCLA Crystallographic Package)'
_computing_molecular_graphics    ORTEP
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298
_diffrn_measurement_device
'Crystal Logic Dual Goniometer Diffractometer'
_diffrn_measurement_method       'profile data from ω 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  0.0106
_diffrn_reflns_av_sigmaI/netI    0.0445
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            4953
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.08
_diffrn_standards_decay_%        -4.3
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.785
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.519
_exptl_crystal_density_meas      1.50
_exptl_crystal_density_method    'floating method'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             623
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.211
_refine_diff_density_min         -0.319
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.072
_refine_ls_goodness_of_fit_obs   1.096
_refine_ls_matrix_type           full
_refine_ls_number_parameters     464
_refine_ls_number_reflns         4666
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_restrained_S_obs      1.096
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_obs          0.0302
_refine_ls_shift/esd_max         -0.130
_refine_ls_shift/esd_mean        0.013
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0231P)²+0.6824P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0879
_refine_ls_wR_factor_obs         0.0829
_reflns_number_observed          4093
_reflns_number_total             4668
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic991430x.cif
_cod_data_source_block           shel93
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0231P)^2^+0.6824P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0231P)^2^+0.6824P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1322.3(1)
_cod_database_code               4321048
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Mn1 Mn 0.0000 0.0000 0.0000 0.02980(12) Uani 1 d S .
Mn2 Mn 0.30971(3) 0.01141(3) 0.12602(2) 0.03055(10) Uani 1 d . .
O1 O 0.5101(2) 0.0896(2) 0.18826(13) 0.0397(4) Uani 1 d . .
O2 O 0.10602(15) -0.0967(2) 0.05699(12) 0.0329(3) Uani 1 d . .
N1 N 0.2528(2) -0.0970(2) 0.21252(14) 0.0330(4) Uani 1 d . .
O4 O 0.3750(2) 0.0745(2) 0.01763(12) 0.0384(3) Uani 1 d . .
O5 O 0.1987(2) 0.1069(2) -0.04878(13) 0.0430(4) Uani 1 d . .
O7 O 0.3144(2) 0.2138(2) 0.21945(13) 0.0431(4) Uani 1 d . .
O8 O 0.1000(2) 0.1916(2) 0.15249(13) 0.0453(4) Uani 1 d . .
C1 C 0.5769(2) 0.0592(2) 0.2515(2) 0.0351(5) Uani 1 d . .
C2 C 0.7316(3) 0.1235(3) 0.2755(2) 0.0440(6) Uani 1 d . .
C3 C 0.8070(3) 0.0992(3) 0.3435(2) 0.0533(7) Uani 1 d . .
C4 C 0.7330(3) 0.0095(3) 0.3889(2) 0.0596(7) Uani 1 d . .
C5 C 0.5816(3) -0.0567(3) 0.3651(2) 0.0508(6) Uani 1 d . .
C6 C 0.5003(2) -0.0329(2) 0.2966(2) 0.0366(5) Uani 1 d . .
C7 C 0.3420(3) -0.1038(3) 0.2757(2) 0.0380(5) Uani 1 d . .
C8 C 0.0890(2) -0.1721(2) 0.1971(2) 0.0376(5) Uani 1 d . .
C9 C 0.0265(2) -0.2165(2) 0.0795(2) 0.0368(5) Uani 1 d . .
C10 C 0.0513(3) -0.0597(3) 0.2728(2) 0.0472(6) Uani 1 d . .
C11 C 0.0299(3) -0.3057(3) 0.2184(3) 0.0533(7) Uani 1 d . .
O3 O 0.1302(4) -0.0063(4) 0.3798(2) 0.0677(10) Uani 0.709(5) d P .
HO3 H 0.1254 0.0800 0.4268 0.080 Uiso 0.71 d P .
O3A O 0.0515(7) -0.4105(7) 0.1573(6) 0.057(2) Uani 0.291(5) d P .
C12 C 0.3283(2) 0.1327(2) -0.0297(2) 0.0322(4) Uani 1 d . .
C13 C 0.4434(2) 0.2380(2) -0.0581(2) 0.0336(4) Uani 1 d . .
C14 C 0.4010(3) 0.2987(3) -0.1147(2) 0.0447(5) Uani 1 d . .
C15 C 0.5033(3) 0.4011(3) -0.1398(2) 0.0542(7) Uani 1 d . .
C16 C 0.6522(3) 0.4464(3) -0.1068(2) 0.0524(6) Uani 1 d . .
C17 C 0.6968(3) 0.3883(3) -0.0509(2) 0.0460(6) Uani 1 d . .
C18 C 0.5943(2) 0.2816(2) -0.0280(2) 0.0374(5) Uani 1 d . .
O6 O 0.6493(2) 0.2237(2) 0.0212(2) 0.0540(5) Uani 1 d . .
C19 C 0.2250(2) 0.2607(2) 0.2207(2) 0.0343(5) Uani 1 d . .
C20 C 0.2652(2) 0.4078(2) 0.3071(2) 0.0341(5) Uani 1 d . .
C21 C 0.4032(3) 0.4937(3) 0.3824(2) 0.0473(6) Uani 1 d . .
C22 C 0.4432(4) 0.6295(3) 0.4628(2) 0.0597(7) Uani 1 d . .
C23 C 0.3424(4) 0.6798(3) 0.4717(2) 0.0580(7) Uani 1 d . .
C24 C 0.2053(3) 0.5976(3) 0.3993(2) 0.0527(6) Uani 1 d . .
C25 C 0.1662(3) 0.4625(2) 0.3158(2) 0.0396(5) Uani 1 d . .
O9 O 0.0318(2) 0.3893(2) 0.2429(2) 0.0565(5) Uani 1 d . .
N2 N 0.1672(4) 0.2797(5) 0.5395(4) 0.1272(15) Uani 1 d . .
C26 C 0.2054(4) 0.3938(5) 0.6033(4) 0.0844(10) Uani 1 d . .
C27 C 0.2573(7) 0.5388(5) 0.6853(6) 0.111(2) Uani 1 d . .
HO6 H 0.5877(37) 0.1757(36) 0.0360(27) 0.067(11) Uiso 1 d . .
HO9 H 0.0168(37) 0.3010(38) 0.1919(28) 0.081(11) Uiso 1 d . .
H2 H 0.7823(29) 0.1829(29) 0.2465(21) 0.046(7) Uiso 1 d . .
H3 H 0.9084(33) 0.1434(30) 0.3590(22) 0.055(8) Uiso 1 d . .
H4 H 0.7863(34) -0.0075(31) 0.4359(24) 0.062(8) Uiso 1 d . .
H5 H 0.5267(33) -0.1218(33) 0.3925(24) 0.066(9) Uiso 1 d . .
H7 H 0.3031(28) -0.1564(28) 0.3171(21) 0.047(7) Uiso 1 d . .
H9A H 0.0410(23) -0.2954(24) 0.0332(17) 0.027(5) Uiso 1 d . .
H9B H -0.0794(25) -0.2418(23) 0.0659(17) 0.028(5) Uiso 1 d . .
H10A H -0.0570(33) -0.1046(31) 0.2608(22) 0.058(8) Uiso 1 d . .
H10B H 0.0776(33) 0.0213(33) 0.2544(24) 0.064(8) Uiso 1 d . .
H11A H -0.0697(33) -0.3510(30) 0.1999(22) 0.051(8) Uiso 1 d . .
H11B H 0.0547(36) -0.2818(35) 0.2931(28) 0.072(10) Uiso 1 d . .
H14 H 0.3022(33) 0.2665(31) -0.1367(23) 0.057(8) Uiso 1 d . .
H15 H 0.4717(31) 0.4352(30) -0.1839(23) 0.057(8) Uiso 1 d . .
H16 H 0.7248(33) 0.5167(31) -0.1209(23) 0.060(8) Uiso 1 d . .
H17 H 0.7899(35) 0.4176(33) -0.0277(24) 0.061(9) Uiso 1 d . .
H21 H 0.4728(29) 0.4557(28) 0.3749(20) 0.047(7) Uiso 1 d . .
H22 H 0.5320(37) 0.6770(36) 0.5058(27) 0.074(10) Uiso 1 d . .
H23 H 0.3615(34) 0.7652(35) 0.5245(26) 0.070(9) Uiso 1 d . .
H24 H 0.1294(34) 0.6253(33) 0.4053(25) 0.069(9) Uiso 1 d . .
H27A H 0.1859(64) 0.5469(59) 0.7264(46) 0.154(20) Uiso 1 d . .
H27B H 0.3454(63) 0.6054(59) 0.6900(43) 0.143(20) Uiso 1 d . .
H27C H 0.2106(84) 0.5608(84) 0.6439(62) 0.203(39) Uiso 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'
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O8 Mn1 O8 180.0 2 . ?
O8 Mn1 O2 90.68(7) 2 2 ?
O8 Mn1 O2 89.32(7) . 2 ?
O8 Mn1 O2 89.31(7) 2 . ?
O8 Mn1 O2 90.69(7) . . ?
O2 Mn1 O2 180.0 2 . ?
O8 Mn1 O5 87.32(7) 2 2 ?
O8 Mn1 O5 92.68(7) . 2 ?
O2 Mn1 O5 89.13(7) 2 2 ?
O2 Mn1 O5 90.87(7) . 2 ?
O8 Mn1 O5 92.68(7) 2 . ?
O8 Mn1 O5 87.32(7) . . ?
O2 Mn1 O5 90.87(7) 2 . ?
O2 Mn1 O5 89.13(7) . . ?
O5 Mn1 O5 180.0 2 . ?
O1 Mn2 O2 170.76(7) . . ?
O1 Mn2 O4 85.91(7) . . ?
O2 Mn2 O4 96.97(7) . . ?
O1 Mn2 N1 91.04(7) . . ?
O2 Mn2 N1 83.83(7) . . ?
O4 Mn2 N1 164.38(7) . . ?
O1 Mn2 O7 92.40(7) . . ?
O2 Mn2 O7 96.33(7) . . ?
O4 Mn2 O7 90.65(7) . . ?
N1 Mn2 O7 104.80(8) . . ?
C1 O1 Mn2 130.92(14) . . ?
C9 O2 Mn2 113.82(12) . . ?
C9 O2 Mn1 122.73(12) . . ?
Mn2 O2 Mn1 119.98(8) . . ?
C7 N1 C8 122.3(2) . . ?
C7 N1 Mn2 126.1(2) . . ?
C8 N1 Mn2 111.58(13) . . ?
C12 O4 Mn2 130.86(13) . . ?
C12 O5 Mn1 136.15(14) . . ?
C19 O7 Mn2 135.13(15) . . ?
C19 O8 Mn1 133.16(14) . . ?
O1 C1 C2 118.1(2) . . ?
O1 C1 C6 123.2(2) . . ?
C2 C1 C6 118.7(2) . . ?
C3 C2 C1 120.5(3) . . ?
C2 C3 C4 121.3(3) . . ?
C5 C4 C3 119.2(3) . . ?
C4 C5 C6 121.1(3) . . ?
C1 C6 C5 119.2(2) . . ?
C1 C6 C7 122.3(2) . . ?
C5 C6 C7 118.6(2) . . ?
N1 C7 C6 125.9(2) . . ?
N1 C8 C9 103.3(2) . . ?
N1 C8 C11 114.2(2) . . ?
C9 C8 C11 110.8(2) . . ?
N1 C8 C10 107.5(2) . . ?
C9 C8 C10 111.2(2) . . ?
C11 C8 C10 109.7(2) . . ?
O2 C9 C8 109.3(2) . . ?
O3 C10 C8 108.7(2) . . ?
O3A C11 C8 115.7(3) . . ?
O5 C12 O4 123.6(2) . . ?
O5 C12 C13 120.9(2) . . ?
O4 C12 C13 115.4(2) . . ?
C14 C13 C18 118.3(2) . . ?
C14 C13 C12 119.0(2) . . ?
C18 C13 C12 122.7(2) . . ?
C15 C14 C13 121.7(2) . . ?
C14 C15 C16 119.4(2) . . ?
C17 C16 C15 120.1(2) . . ?
C16 C17 C18 121.1(2) . . ?
O6 C18 C17 116.4(2) . . ?
O6 C18 C13 124.2(2) . . ?
C17 C18 C13 119.4(2) . . ?
O7 C19 O8 124.6(2) . . ?
O7 C19 C20 119.1(2) . . ?
O8 C19 C20 116.4(2) . . ?
C21 C20 C25 118.4(2) . . ?
C21 C20 C19 120.1(2) . . ?
C25 C20 C19 121.5(2) . . ?
C22 C21 C20 121.4(2) . . ?
C21 C22 C23 119.3(3) . . ?
C24 C23 C22 120.8(3) . . ?
C23 C24 C25 120.1(3) . . ?
O9 C25 C24 117.5(2) . . ?
O9 C25 C20 122.5(2) . . ?
C24 C25 C20 120.0(2) . . ?
N2 C26 C27 178.6(5) . . ?
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 O8 2.143(2) 2 ?
Mn1 O8 2.143(2) . ?
Mn1 O2 2.157(2) 2 ?
Mn1 O2 2.157(2) . ?
Mn1 O5 2.199(2) 2 ?
Mn1 O5 2.199(2) . ?
Mn2 O1 1.862(2) . ?
Mn2 O2 1.876(2) . ?
Mn2 O4 1.950(2) . ?
Mn2 N1 1.982(2) . ?
Mn2 O7 2.142(2) . ?
O1 C1 1.321(3) . ?
O2 C9 1.424(3) . ?
N1 C7 1.287(3) . ?
N1 C8 1.493(3) . ?
O4 C12 1.297(3) . ?
O5 C12 1.234(3) . ?
O7 C19 1.251(3) . ?
O8 C19 1.268(3) . ?
C1 C2 1.400(3) . ?
C1 C6 1.405(3) . ?
C2 C3 1.375(4) . ?
C3 C4 1.383(4) . ?
C4 C5 1.369(4) . ?
C5 C6 1.413(3) . ?
C6 C7 1.434(3) . ?
C8 C9 1.526(3) . ?
C8 C11 1.529(3) . ?
C8 C10 1.532(3) . ?
C10 O3 1.415(4) . ?
C11 O3A 1.292(7) . ?
C12 C13 1.487(3) . ?
C13 C14 1.390(3) . ?
C13 C18 1.401(3) . ?
C14 C15 1.378(4) . ?
C15 C16 1.382(4) . ?
C16 C17 1.368(4) . ?
C17 C18 1.390(3) . ?
C18 O6 1.361(3) . ?
C19 C20 1.490(3) . ?
C20 C21 1.392(3) . ?
C20 C25 1.399(3) . ?
C21 C22 1.371(4) . ?
C22 C23 1.381(4) . ?
C23 C24 1.371(4) . ?
C24 C25 1.385(3) . ?
C25 O9 1.363(3) . ?
N2 C26 1.124(5) . ?
C26 C27 1.426(7) . ?
