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#$Date: 2016-05-06 04:49:25 +0300 (Fri, 06 May 2016) $
#$Revision: 182735 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/87/7038721.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_7038721
loop_
_publ_author_name
'Sobocińska, M'
'Antkowiak, M.'
'Wojciechowski, M.'
'Kamieniarz, G.'
'Utko, J.'
'Lis, T.'
_publ_section_title
;
 New tetranuclear manganese clusters with [MnMn(III)] and [MnMn] metallic
 cores exhibiting low and high spin ground state.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7303
_journal_page_last               7311
_journal_paper_doi               10.1039/c5dt04869a
_journal_volume                  45
_journal_year                    2016
_chemical_formula_sum            'C18 H42 Cl4 Mn4 O12'
_chemical_formula_weight         812.07
_chemical_name_systematic        mars10a
_chemical_properties_physical    Air-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-11-16 deposited with the CCDC.
2016-03-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.16(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.252(3)
_cell_length_b                   13.134(4)
_cell_length_c                   11.161(3)
_cell_measurement_reflns_used    6946
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.05
_cell_measurement_theta_min      2.76
_cell_volume                     1592.0(8)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.923
_diffrn_measurement_device_type  'Xcalibur Ruby'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0353
_diffrn_reflns_av_unetI/netI     0.0373
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.923
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            17276
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.923
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         31.10
_diffrn_reflns_theta_min         2.76
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.937
_exptl_absorpt_correction_T_max  0.880
_exptl_absorpt_correction_T_min  0.742
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.694
_exptl_crystal_description       block
_exptl_crystal_F_000             828
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.663
_refine_diff_density_min         -0.512
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     175
_refine_ls_number_reflns         4717
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0437
_refine_ls_R_factor_gt           0.0295
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[σ²(Fo²)+(0.0211P)²+0.7442P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0564
_refine_ls_wR_factor_ref         0.0609
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3868
_reflns_number_total             4717
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5dt04869a2.cif
_cod_data_source_block           mars10a
_cod_depositor_comments
'Adding full bibliography for 7038720--7038721.cif.'
_cod_database_code               7038721
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.760
_shelx_estimated_absorpt_t_max   0.876
_shelxl_version_number           2013-2
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Mn1 Mn 0.42296(2) 0.52781(2) 0.59948(2) 0.00929(6) Uani 1 1 d . .
Mn2 Mn 0.72558(2) 0.48254(2) 0.69529(2) 0.01087(6) Uani 1 1 d . .
Cl1 Cl 0.40778(4) 0.63876(3) 0.75005(4) 0.01891(10) Uani 1 1 d . .
Cl2 Cl 0.90834(4) 0.58173(4) 0.73628(4) 0.02672(11) Uani 1 1 d . .
O1A O 0.54568(10) 0.45034(9) 0.71047(10) 0.0110(2) Uani 1 1 d . .
C1A C 0.53619(16) 0.41052(14) 0.82625(15) 0.0145(3) Uani 1 1 d . .
H1A1 H 0.5614 0.3381 0.8332 0.017 Uiso 1 1 calc R U
H1A2 H 0.4497 0.4145 0.8309 0.017 Uiso 1 1 calc R U
C2A C 0.61798(15) 0.47061(14) 0.93193(15) 0.0153(3) Uani 1 1 d . .
H2A1 H 0.5825 0.5389 0.9373 0.018 Uiso 1 1 calc R U
H2A2 H 0.6258 0.4349 1.0117 0.018 Uiso 1 1 calc R U
O2A O 0.73611(11) 0.47962(10) 0.90666(11) 0.0180(3) Uani 1 1 d . .
C3A C 0.82283(17) 0.53113(16) 1.00453(17) 0.0225(4) Uani 1 1 d . .
H3A1 H 0.7863 0.5945 1.0246 0.034 Uiso 1 1 calc R U
H3A2 H 0.8972 0.5467 0.9779 0.034 Uiso 1 1 calc R U
H3A3 H 0.8444 0.4874 1.0782 0.034 Uiso 1 1 calc R U
O1B O 0.30364(10) 0.59710(9) 0.47656(10) 0.0122(2) Uani 1 1 d . .
C1B C 0.27709(15) 0.70339(13) 0.46873(16) 0.0145(3) Uani 1 1 d . .
H1B1 H 0.3460 0.7414 0.4500 0.017 Uiso 1 1 calc R U
H1B2 H 0.2656 0.7284 0.5487 0.017 Uiso 1 1 calc R U
C2B C 0.16069(16) 0.71916(14) 0.36648(16) 0.0167(4) Uani 1 1 d . .
H2B1 H 0.0897 0.6882 0.3898 0.020 Uiso 1 1 calc R U
H2B2 H 0.1444 0.7928 0.3519 0.020 Uiso 1 1 calc R U
O2B O 0.17791(10) 0.67164(9) 0.25661(10) 0.0136(2) Uani 1 1 d . .
C3B C 0.07423(16) 0.68824(16) 0.15271(16) 0.0197(4) Uani 1 1 d . .
H3B1 H 0.0005 0.6586 0.1699 0.030 Uiso 1 1 calc R U
H3B2 H 0.0892 0.6560 0.0788 0.030 Uiso 1 1 calc R U
H3B3 H 0.0620 0.7615 0.1382 0.030 Uiso 1 1 calc R U
O1C O 0.58864(10) 0.57412(9) 0.53776(10) 0.0104(2) Uani 1 1 d . .
C1C C 0.60888(16) 0.67469(13) 0.49738(16) 0.0150(3) Uani 1 1 d . .
H1C1 H 0.6190 0.7230 0.5674 0.018 Uiso 1 1 calc R U
H1C2 H 0.5368 0.6965 0.4305 0.018 Uiso 1 1 calc R U
C2C C 0.72341(17) 0.67565(14) 0.44997(17) 0.0183(4) Uani 1 1 d . .
H2C1 H 0.7274 0.7394 0.4039 0.022 Uiso 1 1 calc R U
H2C2 H 0.7981 0.6711 0.5202 0.022 Uiso 1 1 calc R U
O2C O 0.71598(11) 0.58907(10) 0.36926(11) 0.0160(3) Uani 1 1 d . .
C3C C 0.83335(17) 0.55971(19) 0.3531(2) 0.0307(5) Uani 1 1 d . .
H3C1 H 0.8654 0.6142 0.3103 0.046 Uiso 1 1 calc R U
H3C2 H 0.8242 0.4973 0.3034 0.046 Uiso 1 1 calc R U
H3C3 H 0.8908 0.5475 0.4344 0.046 Uiso 1 1 calc R U
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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
O1B Mn1 O1A 174.45(5) . .
O1B Mn1 O1C 82.82(5) . 3_666
O1A Mn1 O1C 91.80(5) . 3_666
O1B Mn1 O1C 97.88(5) . .
O1A Mn1 O1C 79.83(5) . .
O1C Mn1 O1C 80.77(5) 3_666 .
O1B Mn1 Cl1 92.97(4) . .
O1A Mn1 Cl1 92.52(4) . .
O1C Mn1 Cl1 172.07(4) 3_666 .
O1C Mn1 Cl1 106.54(4) . .
O1B Mn1 O2C 92.87(5) . 3_666
O1A Mn1 O2C 87.13(5) . 3_666
O1C Mn1 O2C 76.01(5) 3_666 3_666
O1C Mn1 O2C 152.93(5) . 3_666
Cl1 Mn1 O2C 97.57(4) . 3_666
O1B Mn1 Mn1 90.97(4) . 3_666
O1A Mn1 Mn1 84.13(4) . 3_666
O1C Mn1 Mn1 42.93(3) 3_666 3_666
O1C Mn1 Mn1 37.85(3) . 3_666
Cl1 Mn1 Mn1 144.30(2) . 3_666
O2C Mn1 Mn1 117.65(4) 3_666 3_666
O1A Mn2 O1B 92.77(5) . 3_666
O1A Mn2 O2B 102.06(5) . 3_666
O1B Mn2 O2B 74.33(5) 3_666 3_666
O1A Mn2 O2A 73.29(5) . .
O1B Mn2 O2A 148.97(5) 3_666 .
O2B Mn2 O2A 81.55(5) 3_666 .
O1A Mn2 O1C 73.01(4) . .
O1B Mn2 O1C 70.17(5) 3_666 .
O2B Mn2 O1C 143.76(4) 3_666 .
O2A Mn2 O1C 128.09(4) . .
O1A Mn2 Cl2 153.06(4) . .
O1B Mn2 Cl2 111.36(4) 3_666 .
O2B Mn2 Cl2 96.09(4) 3_666 .
O2A Mn2 Cl2 90.10(4) . .
O1C Mn2 Cl2 103.25(4) . .
C1A O1A Mn1 125.21(10) . .
C1A O1A Mn2 116.49(10) . .
Mn1 O1A Mn2 112.91(6) . .
O1A C1A C2A 109.93(14) . .
O1A C1A H1A1 109.7 . .
C2A C1A H1A1 109.7 . .
O1A C1A H1A2 109.7 . .
C2A C1A H1A2 109.7 . .
H1A1 C1A H1A2 108.2 . .
O2A C2A C1A 107.19(13) . .
O2A C2A H2A1 110.3 . .
C1A C2A H2A1 110.3 . .
O2A C2A H2A2 110.3 . .
C1A C2A H2A2 110.3 . .
H2A1 C2A H2A2 108.5 . .
C3A O2A C2A 111.78(13) . .
C3A O2A Mn2 127.53(11) . .
C2A O2A Mn2 113.33(9) . .
O2A C3A H3A1 109.5 . .
O2A C3A H3A2 109.5 . .
H3A1 C3A H3A2 109.5 . .
O2A C3A H3A3 109.5 . .
H3A1 C3A H3A3 109.5 . .
H3A2 C3A H3A3 109.5 . .
C1B O1B Mn1 128.00(10) . .
C1B O1B Mn2 116.39(9) . 3_666
Mn1 O1B Mn2 109.32(6) . 3_666
O1B C1B C2B 107.89(14) . .
O1B C1B H1B1 110.1 . .
C2B C1B H1B1 110.1 . .
O1B C1B H1B2 110.1 . .
C2B C1B H1B2 110.1 . .
H1B1 C1B H1B2 108.4 . .
O2B C2B C1B 107.60(13) . .
O2B C2B H2B1 110.2 . .
C1B C2B H2B1 110.2 . .
O2B C2B H2B2 110.2 . .
C1B C2B H2B2 110.2 . .
H2B1 C2B H2B2 108.5 . .
C3B O2B C2B 111.29(13) . .
C3B O2B Mn2 124.06(11) . 3_666
C2B O2B Mn2 110.22(10) . 3_666
O2B C3B H3B1 109.5 . .
O2B C3B H3B2 109.5 . .
H3B1 C3B H3B2 109.5 . .
O2B C3B H3B3 109.5 . .
H3B1 C3B H3B3 109.5 . .
H3B2 C3B H3B3 109.5 . .
C1C O1C Mn1 110.96(10) . 3_666
C1C O1C Mn1 124.19(10) . .
Mn1 O1C Mn1 99.23(5) 3_666 .
C1C O1C Mn2 125.55(9) . .
Mn1 O1C Mn2 97.39(5) 3_666 .
Mn1 O1C Mn2 93.84(5) . .
O1C C1C C2C 109.70(14) . .
O1C C1C H1C1 109.7 . .
C2C C1C H1C1 109.7 . .
O1C C1C H1C2 109.7 . .
C2C C1C H1C2 109.7 . .
H1C1 C1C H1C2 108.2 . .
O2C C2C C1C 107.24(13) . .
O2C C2C H2C1 110.3 . .
C1C C2C H2C1 110.3 . .
O2C C2C H2C2 110.3 . .
C1C C2C H2C2 110.3 . .
H2C1 C2C H2C2 108.5 . .
C3C O2C C2C 112.78(14) . .
C3C O2C Mn1 121.97(13) . 3_666
C2C O2C Mn1 111.45(10) . 3_666
O2C C3C H3C1 109.5 . .
O2C C3C H3C2 109.5 . .
H3C1 C3C H3C2 109.5 . .
O2C C3C H3C3 109.5 . .
H3C1 C3C H3C3 109.5 . .
H3C2 C3C H3C3 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 O1B 1.8840(12) .
Mn1 O1A 1.8925(12) .
Mn1 O1C 2.0127(12) 3_666
Mn1 O1C 2.2341(12) .
Mn1 Cl1 2.2642(7) .
Mn1 O2C 2.2820(13) 3_666
Mn1 Mn1 3.2380(9) 3_666
Mn2 O1A 2.1177(13) .
Mn2 O1B 2.1332(12) 3_666
Mn2 O2B 2.2941(13) 3_666
Mn2 O2A 2.3313(14) .
Mn2 O1C 2.3442(12) .
Mn2 Cl2 2.3755(7) .
O1A C1A 1.424(2) .
C1A C2A 1.514(2) .
C1A H1A1 0.9900 .
C1A H1A2 0.9900 .
C2A O2A 1.434(2) .
C2A H2A1 0.9900 .
C2A H2A2 0.9900 .
O2A C3A 1.430(2) .
C3A H3A1 0.9800 .
C3A H3A2 0.9800 .
C3A H3A3 0.9800 .
O1B C1B 1.426(2) .
C1B C2B 1.510(2) .
C1B H1B1 0.9900 .
C1B H1B2 0.9900 .
C2B O2B 1.434(2) .
C2B H2B1 0.9900 .
C2B H2B2 0.9900 .
O2B C3B 1.430(2) .
C3B H3B1 0.9800 .
C3B H3B2 0.9800 .
C3B H3B3 0.9800 .
O1C C1C 1.433(2) .
C1C C2C 1.516(3) .
C1C H1C1 0.9900 .
C1C H1C2 0.9900 .
C2C O2C 1.440(2) .
C2C H2C1 0.9900 .
C2C H2C2 0.9900 .
O2C C3C 1.432(2) .
C3C H3C1 0.9800 .
C3C H3C2 0.9800 .
C3C H3C3 0.9800 .
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
C1A H1A1 Cl1 0.99 2.83 3.761(2) 157.0 2_646
C1A H1A2 O2C 0.99 2.51 3.094(2) 117.6 3_666
C2A H2A1 Cl1 0.99 2.79 3.4758(19) 126.6 .
C3A H3A2 Cl2 0.98 2.77 3.441(2) 126.1 .
C1B H1B2 Cl1 0.99 2.67 3.2134(19) 115.0 .
C1C H1C2 O1A 0.99 2.51 2.999(2) 110.3 3_666
C2C H2C2 Cl2 0.99 2.68 3.548(2) 146.8 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
O1C Mn1 O1A C1A -121.19(13) 3_666 .
O1C Mn1 O1A C1A 158.52(13) . .
Cl1 Mn1 O1A C1A 52.17(12) . .
O2C Mn1 O1A C1A -45.30(12) 3_666 .
Mn1 Mn1 O1A C1A -163.48(12) 3_666 .
O1C Mn1 O1A Mn2 85.81(6) 3_666 .
O1C Mn1 O1A Mn2 5.52(5) . .
Cl1 Mn1 O1A Mn2 -100.84(5) . .
O2C Mn1 O1A Mn2 161.70(6) 3_666 .
Mn1 Mn1 O1A Mn2 43.52(5) 3_666 .
Mn1 O1A C1A C2A -106.93(14) . .
Mn2 O1A C1A C2A 45.22(16) . .
O1A C1A C2A O2A -47.83(18) . .
C1A C2A O2A C3A -177.10(14) . .
C1A C2A O2A Mn2 30.44(16) . .
O1C Mn1 O1B C1B -155.39(13) 3_666 .
O1C Mn1 O1B C1B -75.80(13) . .
Cl1 Mn1 O1B C1B 31.36(13) . .
O2C Mn1 O1B C1B 129.10(13) 3_666 .
Mn1 Mn1 O1B C1B -113.15(13) 3_666 .
O1C Mn1 O1B Mn2 -4.75(5) 3_666 3_666
O1C Mn1 O1B Mn2 74.85(6) . 3_666
Cl1 Mn1 O1B Mn2 -177.99(5) . 3_666
O2C Mn1 O1B Mn2 -80.25(6) 3_666 3_666
Mn1 Mn1 O1B Mn2 37.50(5) 3_666 3_666
Mn1 O1B C1B C2B -170.59(11) . .
Mn2 O1B C1B C2B 40.50(16) 3_666 .
O1B C1B C2B O2B -53.48(18) . .
C1B C2B O2B C3B -176.53(15) . .
C1B C2B O2B Mn2 41.83(16) . 3_666
Mn1 O1C C1C C2C -56.22(15) 3_666 .
Mn1 O1C C1C C2C -174.11(10) . .
Mn2 O1C C1C C2C 60.08(17) . .
O1C C1C C2C O2C 46.48(18) . .
C1C C2C O2C C3C -159.26(15) . .
C1C C2C O2C Mn1 -17.81(16) . 3_666
