#------------------------------------------------------------------------------
#$Date: 2016-03-26 01:59:01 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180117 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/15/7101511.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_7101511
loop_
_publ_author_name
'Lionel Dubois'
'Lilian Jacquamet'
'Jacques Pecaut'
'Jean-Marc Latour'
_publ_section_title
;
X-ray photoreduction of a di(μ-oxo)MnIIIMnIV complex
occurs at temperatures as low as 20 K
;
_journal_issue                   43
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/b609072a
_journal_year                    2006
_chemical_formula_sum            'C20 H38 Mn2 N4 Na O19'
_chemical_formula_weight         771.41
_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                 94.816(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.9552(19)
_cell_length_b                   6.7285(7)
_cell_length_c                   24.535(3)
_cell_measurement_temperature    298(2)
_cell_volume                     3118.2(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.904
_diffrn_measured_fraction_theta_max 0.904
_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  0.0629
_diffrn_reflns_av_sigmaI/netI    0.0577
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            9671
_diffrn_reflns_theta_full        28.96
_diffrn_reflns_theta_max         28.96
_diffrn_reflns_theta_min         1.67
_exptl_absorpt_coefficient_mu    0.912
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.49
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.643
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needles
_exptl_crystal_F_000             1596
_exptl_crystal_preparation       'acetone - water'
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.893
_refine_diff_density_min         -1.305
_refine_diff_density_rms         0.215
_refine_ls_extinction_coef       0.0110(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.167
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         3730
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.165
_refine_ls_R_factor_all          0.0966
_refine_ls_R_factor_gt           0.0803
_refine_ls_shift/su_max          0.029
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1209P)²+13.5579P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2136
_refine_ls_wR_factor_ref         0.2242
_reflns_number_gt                2979
_reflns_number_total             3730
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b609072a.txt
_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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7101511
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
Mn Mn 0.29415(3) 0.69927(10) 0.54291(3) 0.0164(3) Uani 1 1 d .
O1 O 0.28228(16) 0.9076(5) 0.49541(13) 0.0213(7) Uani 1 1 d .
O2 O 0.23447(19) 0.7828(5) 0.60710(16) 0.0315(8) Uani 1 1 d .
O3 O 0.1556(2) 0.6465(7) 0.65757(19) 0.0472(12) Uani 1 1 d .
O4 O 0.37744(17) 0.8122(5) 0.58531(13) 0.0202(7) Uani 1 1 d .
O5 O 0.45134(19) 0.7708(5) 0.65970(14) 0.0278(8) Uani 1 1 d .
O6 O 0.5000 0.3836(11) 0.7500 0.072(3) Uani 1 2 d SD
H1O6 H 0.499(6) 0.327(13) 0.7190(19) 0.086 Uiso 1 1 d D
O7 O 0.3901(2) 0.8387(8) 0.7746(2) 0.0467(11) Uani 1 1 d D
H1O7 H 0.363(4) 0.745(9) 0.783(3) 0.056 Uiso 1 1 d D
H2O7 H 0.382(4) 0.848(13) 0.8080(10) 0.056 Uiso 1 1 d D
N1 N 0.30901(18) 0.4585(5) 0.59720(15) 0.0157(7) Uani 1 1 d .
N2 N 0.36571(19) 0.5194(6) 0.50210(16) 0.0198(8) Uani 1 1 d .
C1 C 0.3267(2) 0.2780(6) 0.56595(19) 0.0217(9) Uani 1 1 d .
H1A H 0.2834 0.2163 0.5502 0.026 Uiso 1 1 calc R
H1B H 0.3512 0.1830 0.5905 0.026 Uiso 1 1 calc R
C2 C 0.3728(2) 0.3313(6) 0.52114(19) 0.0198(9) Uani 1 1 d .
C3 C 0.4152(3) 0.1949(7) 0.4979(2) 0.0270(10) Uani 1 1 d .
H3 H 0.4200 0.0666 0.5118 0.032 Uiso 1 1 calc R
C4 C 0.4510(3) 0.2524(8) 0.4533(2) 0.0329(12) Uani 1 1 d .
H4 H 0.4790 0.1616 0.4364 0.040 Uiso 1 1 calc R
C5 C 0.4446(3) 0.4459(9) 0.4342(2) 0.0350(12) Uani 1 1 d .
H5 H 0.4684 0.4871 0.4046 0.042 Uiso 1 1 calc R
C6 C 0.4023(3) 0.5755(8) 0.4599(2) 0.0277(10) Uani 1 1 d .
H6 H 0.3988 0.7064 0.4478 0.033 Uiso 1 1 calc R
C7 C 0.2402(2) 0.4348(7) 0.6218(2) 0.0239(10) Uani 1 1 d .
H7A H 0.2478 0.3672 0.6567 0.029 Uiso 1 1 calc R
H7B H 0.2083 0.3546 0.5978 0.029 Uiso 1 1 calc R
C8 C 0.2073(2) 0.6371(8) 0.6299(2) 0.0251(10) Uani 1 1 d .
C9 C 0.3675(2) 0.5138(7) 0.63917(19) 0.0229(9) Uani 1 1 d .
H9A H 0.4036 0.4113 0.6404 0.028 Uiso 1 1 calc R
H9B H 0.3489 0.5187 0.6748 0.028 Uiso 1 1 calc R
C10 C 0.4013(2) 0.7120(7) 0.62802(19) 0.0203(9) Uani 1 1 d .
Na Na 0.5000 0.7239(4) 0.7500 0.0275(6) Uani 1 2 d S
O8 O 0.3187(5) 0.0806(15) 0.6945(4) 0.123(4) Uani 1 1 d D
H1O8 H 0.349(5) 0.009(18) 0.713(5) 0.148 Uiso 1 1 d D
H2O8 H 0.307(8) 0.160(19) 0.719(5) 0.148 Uiso 1 1 d D
O9 O 0.3114(3) 0.5011(10) 0.7734(3) 0.0785(18) Uani 1 1 d D
H1O9 H 0.270(2) 0.517(16) 0.784(4) 0.094 Uiso 1 1 d D
H2O9 H 0.3559(10) 0.484(17) 0.778(4) 0.094 Uiso 1 1 d D
O10 O 0.0018(2) 0.6656(6) 0.6499(2) 0.0408(10) Uani 1 1 d D
H1O1 H 0.0463(7) 0.648(12) 0.653(3) 0.049 Uiso 1 1 d D
H2O1 H -0.010(4) 0.665(12) 0.6157(6) 0.049 Uiso 1 1 d 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'
Na Na 0.0362 0.0249 '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
O1 Mn O1 85.59(15) 7_566 .
O1 Mn O4 179.17(15) 7_566 .
O1 Mn O4 95.24(14) . .
O1 Mn O2 92.17(14) 7_566 .
O1 Mn O2 103.25(14) . .
O4 Mn O2 87.64(14) . .
O1 Mn N1 94.69(14) 7_566 .
O1 Mn N1 179.29(14) . .
O4 Mn N1 84.48(13) . .
O2 Mn N1 77.40(14) . .
O1 Mn N2 92.51(14) 7_566 .
O1 Mn N2 100.69(14) . .
O4 Mn N2 87.34(14) . .
O2 Mn N2 155.89(15) . .
N1 Mn N2 78.65(14) . .
O1 Mn Mn 43.03(11) 7_566 7_566
O1 Mn Mn 42.56(10) . 7_566
O4 Mn Mn 137.80(10) . 7_566
O2 Mn Mn 100.51(11) . 7_566
N1 Mn Mn 137.72(10) . 7_566
N2 Mn Mn 99.01(11) . 7_566
Mn O1 Mn 94.41(14) 7_566 .
C8 O2 Mn 113.1(3) . .
C10 O4 Mn 115.9(3) . .
C10 O5 Na 140.2(3) . .
C1 N1 C7 111.3(3) . .
C1 N1 C9 111.8(3) . .
C7 N1 C9 111.8(4) . .
C1 N1 Mn 109.0(3) . .
C7 N1 Mn 105.3(3) . .
C9 N1 Mn 107.3(3) . .
C6 N2 C2 119.1(4) . .
C6 N2 Mn 126.2(3) . .
C2 N2 Mn 114.7(3) . .
N1 C1 C2 110.6(3) . .
N2 C2 C3 121.7(4) . .
N2 C2 C1 115.5(4) . .
C3 C2 C1 122.6(4) . .
C2 C3 C4 118.8(5) . .
C5 C4 C3 119.6(5) . .
C6 C5 C4 118.6(5) . .
N2 C6 C5 122.2(5) . .
N1 C7 C8 109.9(4) . .
O3 C8 O2 125.1(5) . .
O3 C8 C7 118.0(5) . .
O2 C8 C7 116.9(4) . .
N1 C9 C10 113.3(4) . .
O5 C10 O4 122.5(4) . .
O5 C10 C9 118.7(4) . .
O4 C10 C9 118.7(4) . .
O6 Na O7 109.20(15) . .
O6 Na O7 109.20(15) . 6_657
O7 Na O7 141.6(3) . 6_657
O6 Na O5 97.71(11) . 6_657
O7 Na O5 90.00(15) . 6_657
O7 Na O5 84.94(16) 6_657 6_657
O6 Na O5 97.71(12) . .
O7 Na O5 84.94(16) . .
O7 Na O5 90.00(15) 6_657 .
O5 Na O5 164.6(2) 6_657 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn O1 1.809(3) 7_566
Mn O1 1.825(3) .
Mn O4 1.969(3) .
Mn O2 2.092(4) .
Mn N1 2.102(4) .
Mn N2 2.129(4) .
Mn Mn 2.6662(13) 7_566
O1 Mn 1.809(3) 7_566
O2 C8 1.259(6) .
O3 C8 1.240(6) .
O4 C10 1.295(6) .
O5 C10 1.240(6) .
O5 Na 2.348(3) .
O6 Na 2.290(8) .
O7 Na 2.347(4) .
N1 C1 1.490(5) .
N1 C7 1.490(5) .
N1 C9 1.495(6) .
N2 C6 1.347(6) .
N2 C2 1.352(6) .
C1 C2 1.503(6) .
C2 C3 1.376(7) .
C3 C4 1.389(8) .
C4 C5 1.385(8) .
C5 C6 1.373(8) .
C7 C8 1.517(7) .
C9 C10 1.514(6) .
Na O7 2.347(4) 6_657
Na O5 2.348(3) 6_657
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O6 H1O6 O10 0.851(5) 2.016(13) 2.863(6) 173(10) 3_545
O7 H1O7 O9 0.851(5) 1.91(4) 2.716(8) 157(8) .
O7 H2O7 O3 0.850(5) 2.31(8) 2.838(6) 120(7) 8_557
O8 H1O8 O7 0.850(5) 2.01(5) 2.810(9) 158(13) 1_545
O9 H1O9 O8 0.851(5) 1.858(17) 2.705(10) 174(11) 8_557
O10 H1O1 O3 0.850(5) 2.066(14) 2.910(6) 172(8) .
