#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:17:58 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179962 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/56/7025640.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_7025640
loop_
_publ_author_name
'Pardo, Emilio'
'Train, Cyrille'
'Lescouëzec, Rodrigue'
'Boubekeur, Kamal'
'Ruiz, Eliseo'
'Lloret, Francesc'
'Verdaguer, Michel'
_publ_section_title
;
 Synthesis, crystal structure and magnetic properties of two
 oxalato-bridged dimetallic trinuclear complexes combined with a polar
 cation.
;
_journal_issue                   20
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4951
_journal_page_last               4958
_journal_paper_doi               10.1039/c002468f
_journal_volume                  39
_journal_year                    2010
_chemical_formula_moiety         'C12 H4 Cr2 Mn O26, 4(C5 H7 N2), 2.99(H2 O)'
_chemical_formula_sum            'C32 H37.98 Cr2 Mn N8 O29'
_chemical_formula_weight         1157.46
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 100.447(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.5113(15)
_cell_length_b                   20.250(3)
_cell_length_c                   21.810(4)
_cell_measurement_reflns_used    195
_cell_measurement_temperature    250(2)
_cell_measurement_theta_max      23.06
_cell_measurement_theta_min      4.17
_cell_volume                     4999.7(14)
_computing_cell_refinement
'DIRAX/LSQ (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'COLLECT (Nonius BV, 1997-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      250(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0260
_diffrn_reflns_av_sigmaI/netI    0.0237
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            29683
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.13
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.774
_exptl_absorpt_correction_T_max  0.8976
_exptl_absorpt_correction_T_min  0.7770
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.538
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'hexagonal plate'
_exptl_crystal_F_000             2363.9
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.798
_refine_diff_density_min         -0.760
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         7281
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0519
_refine_ls_R_factor_gt           0.0429
_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)+(0.0887P)²+2.9307P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1266
_refine_ls_wR_factor_ref         0.1366
_reflns_number_gt                5577
_reflns_number_total             7281
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c002468f.txt
_cod_data_source_block           emil16
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        4999.9(13)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7025640
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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 -0.2500 0.2500 0.0000 0.02580(13) Uani 1 2 d S
Cr1 Cr 0.18439(3) 0.210457(19) 0.149438(17) 0.02320(11) Uani 1 1 d .
O1 O -0.10561(14) 0.17492(9) 0.02133(8) 0.0286(3) Uani 1 1 d .
O2 O -0.11887(15) 0.29874(9) 0.07297(8) 0.0301(4) Uani 1 1 d .
O3 O 0.05885(15) 0.28005(9) 0.13280(8) 0.0289(4) Uani 1 1 d .
O4 O 0.06922(14) 0.16022(8) 0.08560(8) 0.0260(3) Uani 1 1 d .
O5 O 0.30652(15) 0.14046(9) 0.15405(9) 0.0326(4) Uani 1 1 d .
O6 O 0.26913(15) 0.24714(9) 0.08559(8) 0.0286(4) Uani 1 1 d .
O7 O 0.43267(18) 0.23185(12) 0.04493(10) 0.0424(5) Uani 1 1 d .
O8 O 0.4712(2) 0.11538(12) 0.11759(12) 0.0545(6) Uani 1 1 d .
O9 O 0.12379(15) 0.17070(9) 0.22045(8) 0.0299(4) Uani 1 1 d .
O10 O 0.28184(16) 0.26321(10) 0.21582(9) 0.0331(4) Uani 1 1 d .
O11 O 0.3257(3) 0.26951(14) 0.32029(11) 0.0617(7) Uani 1 1 d .
O12 O 0.1575(2) 0.17241(11) 0.32540(9) 0.0437(5) Uani 1 1 d .
O13 O -0.33475(16) 0.19677(11) 0.06494(9) 0.0360(4) Uani 1 1 d .
H13A H -0.399(2) 0.20109(18) 0.06363(9) 0.043 Uiso 1 1 d R
H13B H -0.3069(9) 0.2022(2) 0.0986(11) 0.043 Uiso 1 1 d R
C1 C -0.02394(19) 0.19357(11) 0.06325(10) 0.0230(4) Uani 1 1 d .
C2 C -0.03025(19) 0.26353(11) 0.09194(11) 0.0236(4) Uani 1 1 d .
C3 C 0.3852(2) 0.15094(14) 0.11955(12) 0.0321(5) Uani 1 1 d .
C4 C 0.3639(2) 0.21503(13) 0.07910(11) 0.0284(5) Uani 1 1 d .
C5 C 0.1752(2) 0.19188(13) 0.27442(12) 0.0298(5) Uani 1 1 d .
C6 C 0.2698(2) 0.24674(14) 0.27184(13) 0.0349(5) Uani 1 1 d .
N1 N 0.1292(3) 0.54401(18) 0.05610(18) 0.0669(9) Uani 1 1 d .
H1 H 0.0965 0.5804 0.0656 0.096(18) Uiso 1 1 calc R
N2 N 0.2922(3) 0.37260(14) 0.01779(13) 0.0479(6) Uani 1 1 d .
H2A H 0.2708 0.3352 0.0319 0.057 Uiso 1 1 calc R
H2B H 0.3497 0.3738 -0.0032 0.057 Uiso 1 1 calc R
C7 C 0.2165(5) 0.5463(2) 0.0226(2) 0.0749(12) Uani 1 1 d .
H7 H 0.2394 0.5874 0.0087 0.090 Uiso 1 1 calc R
C8 C 0.2728(4) 0.49038(18) 0.0084(2) 0.0588(9) Uani 1 1 d .
H8 H 0.3345 0.4933 -0.0144 0.071 Uiso 1 1 calc R
C9 C 0.2374(3) 0.42764(15) 0.02821(14) 0.0391(6) Uani 1 1 d .
C10 C 0.1431(3) 0.42795(18) 0.06221(16) 0.0482(7) Uani 1 1 d .
H10 H 0.1157 0.3878 0.0760 0.058 Uiso 1 1 calc R
C11 C 0.0922(3) 0.4855(2) 0.07501(19) 0.0585(9) Uani 1 1 d .
H11 H 0.0299 0.4846 0.0975 0.070 Uiso 1 1 calc R
N3 N 0.4663(4) 0.5472(2) 0.17047(19) 0.0747(10) Uani 1 1 d .
H3 H 0.4668 0.5901 0.1710 0.090 Uiso 1 1 calc R
N4 N 0.4665(3) 0.34792(19) 0.17359(18) 0.0686(9) Uani 1 1 d .
H4A H 0.4082 0.3268 0.1851 0.082 Uiso 1 1 calc R
H4B H 0.5260 0.3261 0.1642 0.082 Uiso 1 1 calc R
C12 C 0.5589(5) 0.5140(2) 0.1546(2) 0.0724(12) Uani 1 1 d .
H12 H 0.6231 0.5378 0.1446 0.087 Uiso 1 1 calc R
C13 C 0.5600(4) 0.4484(3) 0.1531(2) 0.0710(12) Uani 1 1 d .
H13 H 0.6236 0.4264 0.1405 0.100(18) Uiso 1 1 calc R
C14 C 0.4649(3) 0.4102(2) 0.17056(17) 0.0542(8) Uani 1 1 d .
C15 C 0.3689(3) 0.4470(3) 0.18562(18) 0.0652(11) Uani 1 1 d .
H15 H 0.3030 0.4249 0.1957 0.078 Uiso 1 1 calc R
C16 C 0.3722(4) 0.5139(2) 0.18553(19) 0.0656(10) Uani 1 1 d .
H16 H 0.3086 0.5378 0.1960 0.038(8) Uiso 1 1 calc R
O14 O 0.3703(6) 0.0652(3) 0.2701(2) 0.148(2) Uani 1 1 d D
H14A H 0.3639(6) 0.1002(6) 0.2446(4) 0.178 Uiso 1 1 d RD
H14B H 0.4116(8) 0.0709(3) 0.3085(6) 0.178 Uiso 1 1 d RD
O15 O 0.0000 0.394(2) 0.2500 0.247(18) Uiso 0.33 2 d SPD
H15A H 0.0650(13) 0.372(2) 0.24435(11) 0.296 Uiso 0.33 1 d PRD
O16 O 0.3537(14) -0.0822(8) 0.1420(7) 0.123(5) Uiso 0.33 1 d PD
H16A H 0.3538(14) -0.0385(10) 0.1326(7) 0.147 Uiso 0.33 1 d PRD
H16B H 0.2896(17) -0.0989(8) 0.1160(8) 0.147 Uiso 0.33 1 d PRD
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'
Cr Cr 0.3209 0.6236 '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
O13 Mn1 O13 180.00(12) 7_455 .
O13 Mn1 O2 94.68(7) 7_455 7_455
O13 Mn1 O2 85.32(7) . 7_455
O13 Mn1 O2 85.32(7) 7_455 .
O13 Mn1 O2 94.68(7) . .
O2 Mn1 O2 180.00(11) 7_455 .
O13 Mn1 O1 86.05(7) 7_455 7_455
O13 Mn1 O1 93.95(7) . 7_455
O2 Mn1 O1 76.70(6) 7_455 7_455
O2 Mn1 O1 103.30(6) . 7_455
O13 Mn1 O1 93.95(7) 7_455 .
O13 Mn1 O1 86.05(7) . .
O2 Mn1 O1 103.30(6) 7_455 .
O2 Mn1 O1 76.70(6) . .
O1 Mn1 O1 180.00(12) 7_455 .
O13 Mn1 Cr1 89.48(5) 7_455 .
O13 Mn1 Cr1 90.52(5) . .
O2 Mn1 Cr1 141.88(4) 7_455 .
O2 Mn1 Cr1 38.12(4) . .
O1 Mn1 Cr1 141.42(4) 7_455 .
O1 Mn1 Cr1 38.58(4) . .
O10 Cr1 O9 83.14(7) . .
O10 Cr1 O6 91.48(8) . .
O9 Cr1 O6 171.33(7) . .
O10 Cr1 O5 92.64(8) . .
O9 Cr1 O5 90.96(8) . .
O6 Cr1 O5 82.48(7) . .
O10 Cr1 O3 92.72(8) . .
O9 Cr1 O3 94.75(8) . .
O6 Cr1 O3 92.28(7) . .
O5 Cr1 O3 172.60(8) . .
O10 Cr1 O4 173.59(7) . .
O9 Cr1 O4 93.11(7) . .
O6 Cr1 O4 92.84(7) . .
O5 Cr1 O4 92.62(7) . .
O3 Cr1 O4 82.38(7) . .
O10 Cr1 Mn1 133.51(6) . .
O9 Cr1 Mn1 96.38(5) . .
O6 Cr1 Mn1 92.26(5) . .
O5 Cr1 Mn1 133.78(6) . .
O3 Cr1 Mn1 40.83(5) . .
O4 Cr1 Mn1 41.57(5) . .
C1 O1 Mn1 112.34(15) . .
C2 O2 Mn1 113.05(15) . .
C2 O3 Cr1 113.85(15) . .
C1 O4 Cr1 113.31(14) . .
C3 O5 Cr1 114.62(16) . .
C4 O6 Cr1 114.74(15) . .
C5 O9 Cr1 114.19(15) . .
C6 O10 Cr1 114.04(16) . .
Mn1 O13 H13A 119.0 . .
Mn1 O13 H13B 113.9 . .
H13A O13 H13B 105.4 . .
O1 C1 O4 125.9(2) . .
O1 C1 C2 119.2(2) . .
O4 C1 C2 114.98(19) . .
O2 C2 O3 125.8(2) . .
O2 C2 C1 118.7(2) . .
O3 C2 C1 115.44(19) . .
O8 C3 O5 125.1(3) . .
O8 C3 C4 120.7(2) . .
O5 C3 C4 114.2(2) . .
O7 C4 O6 124.9(2) . .
O7 C4 C3 121.3(2) . .
O6 C4 C3 113.7(2) . .
O12 C5 O9 126.4(2) . .
O12 C5 C6 119.3(2) . .
O9 C5 C6 114.2(2) . .
O11 C6 O10 125.9(3) . .
O11 C6 C5 119.8(2) . .
O10 C6 C5 114.2(2) . .
C7 N1 C11 120.3(3) . .
C7 N1 H1 119.8 . .
C11 N1 H1 119.8 . .
C9 N2 H2A 120.0 . .
C9 N2 H2B 120.0 . .
H2A N2 H2B 120.0 . .
N1 C7 C8 121.6(4) . .
N1 C7 H7 119.2 . .
C8 C7 H7 119.2 . .
C7 C8 C9 119.7(3) . .
C7 C8 H8 120.1 . .
C9 C8 H8 120.1 . .
N2 C9 C10 121.8(3) . .
N2 C9 C8 121.9(3) . .
C10 C9 C8 116.2(3) . .
C11 C10 C9 120.7(3) . .
C11 C10 H10 119.7 . .
C9 C10 H10 119.7 . .
N1 C11 C10 121.3(3) . .
N1 C11 H11 119.3 . .
C10 C11 H11 119.3 . .
C16 N3 C12 120.8(4) . .
C16 N3 H3 119.6 . .
C12 N3 H3 119.6 . .
C14 N4 H4A 120.0 . .
C14 N4 H4B 120.0 . .
H4A N4 H4B 120.0 . .
C13 C12 N3 120.8(4) . .
C13 C12 H12 119.6 . .
N3 C12 H12 119.6 . .
C12 C13 C14 121.1(4) . .
C12 C13 H13 119.4 . .
C14 C13 H13 119.4 . .
N4 C14 C15 121.1(4) . .
N4 C14 C13 122.9(4) . .
C15 C14 C13 116.0(4) . .
C16 C15 C14 120.1(4) . .
C16 C15 H15 120.0 . .
C14 C15 H15 120.0 . .
C15 C16 N3 121.1(4) . .
C15 C16 H16 119.4 . .
N3 C16 H16 119.4 . .
H14A O14 H14B 116.7 . .
H16A O16 H16B 104.8 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 O13 2.1496(19) 7_455
Mn1 O13 2.1496(19) .
Mn1 O2 2.2168(18) 7_455
Mn1 O2 2.2168(18) .
Mn1 O1 2.2383(17) 7_455
Mn1 O1 2.2383(17) .
Cr1 O10 1.9765(19) .
Cr1 O9 1.9813(17) .
Cr1 O6 1.9837(17) .
Cr1 O5 1.9861(18) .
Cr1 O3 2.0039(17) .
Cr1 O4 2.0154(17) .
O1 C1 1.245(3) .
O2 C2 1.252(3) .
O3 C2 1.275(3) .
O4 C1 1.286(3) .
O5 C3 1.296(3) .
O6 C4 1.300(3) .
O7 C4 1.229(3) .
O8 C3 1.232(3) .
O9 C5 1.291(3) .
O10 C6 1.298(3) .
O11 C6 1.223(3) .
O12 C5 1.231(3) .
O13 H13A 0.7363 .
O13 H13B 0.7549 .
C1 C2 1.556(3) .
C3 C4 1.564(4) .
C5 C6 1.564(4) .
N1 C7 1.346(6) .
N1 C11 1.349(6) .
N1 H1 0.8700 .
N2 C9 1.321(4) .
N2 H2A 0.8700 .
N2 H2B 0.8700 .
C7 C8 1.369(6) .
C7 H7 0.9400 .
C8 C9 1.425(5) .
C8 H8 0.9400 .
C9 C10 1.421(4) .
C10 C11 1.356(5) .
C10 H10 0.9400 .
C11 H11 0.9400 .
N3 C16 1.365(6) .
N3 C12 1.357(6) .
N3 H3 0.8700 .
N4 C14 1.263(5) .
N4 H4A 0.8700 .
N4 H4B 0.8700 .
C12 C13 1.330(7) .
C12 H12 0.9400 .
C13 C14 1.447(6) .
C13 H13 0.9400 .
C14 C15 1.419(6) .
C15 C16 1.357(7) .
C15 H15 0.9400 .
C16 H16 0.9400 .
O14 H14A 0.8939 .
O14 H14B 0.8936 .
O15 H15A 0.8943 .
O16 H16A 0.9089 .
O16 H16B 0.9103 .
