#------------------------------------------------------------------------------
#$Date: 2016-02-18 16:37:37 +0100 (jue 18 de feb de 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/51/54/1515490.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_1515490
loop_
_publ_author_name
'Saines, Paul J.'
'Jain, Prashant'
'Cheetham, Anthony K.'
_publ_section_title
;
 Evolution of the structures and magnetic properties of the manganese
 dicarboxylates, Mn2(CO2(CH2)nCO2)(OH)2 and Mn4(CO2(CH2)nCO2)3(OH)2
;
_journal_issue                   10
_journal_name_full               'Chemical Science'
_journal_page_first              1929
_journal_paper_doi               10.1039/c1sc00253h
_journal_volume                  2
_journal_year                    2011
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C21 H32 Mn4 O14'
_chemical_formula_sum            'C21 H32 Mn4 O14'
_chemical_formula_weight         728.23
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_date             2010-11-19T09:54:54-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90.848(4)
_cell_angle_beta                 90.047(4)
_cell_angle_gamma                90.770(5)
_cell_formula_units_Z            2
_cell_length_a                   5.0585(3)
_cell_length_b                   12.4647(7)
_cell_length_c                   20.8241(9)
_cell_measurement_reflns_used    4958
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      71.8303
_cell_measurement_theta_min      3.5437
_cell_measurement_wavelength     0.71073
_cell_volume                     1312.75(12)
_computing_cell_refinement       'CrysAlisPro (Oxford Diffraction, 2010)'
_computing_data_collection       'CrysAlisPro (Oxford Diffraction 2010)'
_computing_data_reduction        'CrysAlisPro (Oxford Diffraction, 2010)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2007)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 16.1183
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Enhance Ultra (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0415
_diffrn_reflns_av_unetI/netI     0.0576
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            8448
_diffrn_reflns_theta_full        67.08
_diffrn_reflns_theta_max         72.36
_diffrn_reflns_theta_min         3.55
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    15.901
_exptl_absorpt_correction_T_max  0.798
_exptl_absorpt_correction_T_min  0.149
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug 2 2010,13:00:58)
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            colourless
_exptl_crystal_density_diffrn    1.848
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             740
_exptl_crystal_size_max          0.3837
_exptl_crystal_size_mid          0.0177
_exptl_crystal_size_min          0.0155
_refine_diff_density_max         1.187
_refine_diff_density_min         -1.395
_refine_diff_density_rms         0.216
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     358
_refine_ls_number_reflns         4906
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.0807
_refine_ls_R_factor_gt           0.0709
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0888P)²+10.4479P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1955
_refine_ls_wR_factor_ref         0.2035
_reflns_number_gt                4209
_reflns_number_total             4906
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1sc00253h.txt
_cod_data_source_block           6
_cod_database_code               1515490
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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Mn1 Mn -0.3286(2) 0.33762(9) 0.35246(5) 0.0197(3) Uani 1 1 d .
Mn2 Mn 0.1190(2) 0.17896(9) 0.31082(5) 0.0174(3) Uani 1 1 d .
Mn3 Mn 0.1606(2) 0.17161(9) 0.15472(5) 0.0196(3) Uani 1 1 d .
Mn4 Mn 0.6183(2) 0.33754(8) 0.19430(5) 0.0177(3) Uani 1 1 d .
O1 O -0.4226(11) 0.5003(4) 0.3444(3) 0.0280(11) Uani 1 1 d .
O1H O 0.4019(10) 0.2019(4) 0.2365(2) 0.0179(9) Uani 1 1 d D
O2 O -0.6071(11) 0.4592(4) 0.2511(3) 0.0285(12) Uani 1 1 d .
O2H O -0.0950(9) 0.3159(4) 0.2691(2) 0.0194(10) Uani 1 1 d D
O3 O -0.1264(11) 0.0730(5) 0.2503(3) 0.0291(12) Uani 1 1 d .
O4 O 0.0492(11) 0.0036(4) 0.1613(3) 0.0282(11) Uani 1 1 d .
O11 O -0.0752(10) 0.3729(4) 0.4297(2) 0.0228(10) Uani 1 1 d .
O12 O 0.2768(10) 0.3016(4) 0.3822(2) 0.0201(10) Uani 1 1 d .
O13 O 0.3764(10) 0.0729(4) 0.3603(2) 0.0202(10) Uani 1 1 d .
O14 O -0.2469(10) 0.1682(4) 0.3676(2) 0.0203(10) Uani 1 1 d .
O21 O 0.4146(10) 0.1313(4) 0.0789(2) 0.0244(11) Uani 1 1 d .
O22 O 0.7712(10) 0.2064(4) 0.1230(2) 0.0194(10) Uani 1 1 d .
O23 O -0.1206(10) 0.4369(4) 0.1404(2) 0.0199(10) Uani 1 1 d .
O24 O 0.2538(10) 0.3424(4) 0.1377(2) 0.0191(10) Uani 1 1 d .
C1 C -0.5755(15) 0.5208(6) 0.2989(3) 0.0230(15) Uani 1 1 d .
C2 C -0.7279(18) 0.6244(7) 0.3047(4) 0.0336(18) Uani 1 1 d .
H2B H -0.8471 0.6183 0.3410 0.040 Uiso 1 1 calc R
H2A H -0.6030 0.6820 0.3147 0.040 Uiso 1 1 calc R
C3 C -0.8863(17) 0.6565(6) 0.2476(4) 0.0294(17) Uani 1 1 d .
H3B H -1.0211 0.6022 0.2387 0.035 Uiso 1 1 calc R
H3A H -0.7714 0.6606 0.2104 0.035 Uiso 1 1 calc R
C4 C -0.0193(17) -0.2339(6) 0.2587(4) 0.0304(17) Uani 1 1 d .
H4B H -0.1308 -0.2376 0.2965 0.036 Uiso 1 1 calc R
H4A H 0.1160 -0.1794 0.2667 0.036 Uiso 1 1 calc R
C5 C -0.1868(17) -0.2014(6) 0.2011(4) 0.0300(17) Uani 1 1 d .
H5A H -0.0764 -0.2002 0.1630 0.036 Uiso 1 1 calc R
H5B H -0.3255 -0.2548 0.1940 0.036 Uiso 1 1 calc R
C6 C -0.3100(17) -0.0931(6) 0.2105(4) 0.0303(17) Uani 1 1 d .
H6B H -0.3976 -0.0910 0.2519 0.036 Uiso 1 1 calc R
H6A H -0.4437 -0.0838 0.1777 0.036 Uiso 1 1 calc R
C7 C -0.1131(15) -0.0005(6) 0.2074(3) 0.0225(14) Uani 1 1 d .
C11 C 0.1608(14) 0.3492(5) 0.4300(3) 0.0190(14) Uani 1 1 d .
C12 C 0.3249(15) 0.3766(6) 0.4886(3) 0.0219(14) Uani 1 1 d .
H12B H 0.2117 0.4088 0.5209 0.026 Uiso 1 1 calc R
H12A H 0.4578 0.4297 0.4770 0.026 Uiso 1 1 calc R
C13 C 0.4640(15) 0.2795(6) 0.5180(3) 0.0229(15) Uani 1 1 d .
H13A H 0.5787 0.2478 0.4858 0.027 Uiso 1 1 calc R
H13B H 0.5744 0.3046 0.5534 0.027 Uiso 1 1 calc R
C14 C 0.7259(15) -0.1933(6) 0.4576(3) 0.0241(15) Uani 1 1 d .
H14A H 0.8465 -0.2250 0.4268 0.029 Uiso 1 1 calc R
H14B H 0.8296 -0.1644 0.4933 0.029 Uiso 1 1 calc R
C15 C 0.5758(15) -0.1027(6) 0.4260(3) 0.0230(15) Uani 1 1 d .
H15A H 0.4826 -0.1311 0.3886 0.028 Uiso 1 1 calc R
H15B H 0.4453 -0.0753 0.4559 0.028 Uiso 1 1 calc R
C16 C 0.7556(14) -0.0119(6) 0.4058(3) 0.0225(14) Uani 1 1 d .
H16A H 0.8839 -0.0397 0.3755 0.027 Uiso 1 1 calc R
H16B H 0.8518 0.0147 0.4432 0.027 Uiso 1 1 calc R
C17 C 0.6121(14) 0.0819(5) 0.3751(3) 0.0182(14) Uani 1 1 d .
C21 C 0.6514(14) 0.1544(5) 0.0772(3) 0.0200(14) Uani 1 1 d .
C22 C 0.8134(14) 0.1226(5) 0.0192(3) 0.0196(13) Uani 1 1 d .
H22A H 0.6987 0.0874 -0.0122 0.024 Uiso 1 1 calc R
H22B H 0.9453 0.0714 0.0321 0.024 Uiso 1 1 calc R
C23 C 0.9530(15) 0.2188(6) -0.0123(3) 0.0216(14) Uani 1 1 d .
H23B H 1.0701 0.2528 0.0190 0.026 Uiso 1 1 calc R
H23A H 1.0613 0.1924 -0.0474 0.026 Uiso 1 1 calc R
C24 C 0.7684(15) 0.3024(6) -0.0379(4) 0.0239(15) Uani 1 1 d .
H24B H 0.6606 0.3299 -0.0030 0.029 Uiso 1 1 calc R
H24A H 0.6512 0.2692 -0.0695 0.029 Uiso 1 1 calc R
C25 C 0.0817(14) 0.6051(6) 0.0685(3) 0.0209(14) Uani 1 1 d .
H25A H -0.0431 0.5752 0.0375 0.025 Uiso 1 1 calc R
H25B H -0.0186 0.6326 0.1047 0.025 Uiso 1 1 calc R
C26 C 0.2605(14) 0.5159(5) 0.0916(3) 0.0195(14) Uani 1 1 d .
H26A H 0.3523 0.4855 0.0549 0.023 Uiso 1 1 calc R
H26B H 0.3927 0.5469 0.1204 0.023 Uiso 1 1 calc R
C27 C 0.1158(14) 0.4266(5) 0.1259(3) 0.0175(13) Uani 1 1 d .
H2H H 0.046(11) 0.350(6) 0.261(4) 0.026 Uiso 1 1 d D
H1H H 0.509(14) 0.151(5) 0.238(4) 0.026 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 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn -0.5299 2.8052 '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
O11 Mn1 O1 90.9(2) . .
O11 Mn1 O2H 108.16(19) . .
O1 Mn1 O2H 100.4(2) . .
O11 Mn1 O12 112.78(19) . 1_455
O1 Mn1 O12 90.4(2) . 1_455
O2H Mn1 O12 137.40(19) . 1_455
O11 Mn1 O14 87.61(19) . .
O1 Mn1 O14 175.7(2) . .
O2H Mn1 O14 83.87(18) . .
O12 Mn1 O14 86.49(19) 1_455 .
O11 Mn1 Mn2 83.81(14) . .
O1 Mn1 Mn2 139.31(17) . .
O2H Mn1 Mn2 44.94(13) . .
O12 Mn1 Mn2 128.79(14) 1_455 .
O14 Mn1 Mn2 44.48(13) . .
O1H Mn2 O13 91.56(18) . .
O1H Mn2 O3 92.4(2) . .
O13 Mn2 O3 104.5(2) . .
O1H Mn2 O14 164.74(19) . .
O13 Mn2 O14 102.48(18) . .
O3 Mn2 O14 78.41(19) . .
O1H Mn2 O2H 86.38(18) . .
O13 Mn2 O2H 167.87(19) . .
O3 Mn2 O2H 87.6(2) . .
O14 Mn2 O2H 81.11(18) . .
O1H Mn2 O12 98.69(18) . .
O13 Mn2 O12 83.56(18) . .
O3 Mn2 O12 166.1(2) . .
O14 Mn2 O12 88.92(18) . .
O2H Mn2 O12 84.94(18) . .
O1H Mn2 Mn1 126.83(13) . .
O13 Mn2 Mn1 134.98(14) . .
O3 Mn2 Mn1 97.11(15) . .
O14 Mn2 Mn1 44.06(12) . .
O2H Mn2 Mn1 42.32(13) . .
O12 Mn2 Mn1 69.58(13) . .
O21 Mn3 O1H 106.85(19) . .
O21 Mn3 O22 112.73(19) . 1_455
O1H Mn3 O22 138.17(19) . 1_455
O21 Mn3 O4 88.8(2) . .
O1H Mn3 O4 104.5(2) . .
O22 Mn3 O4 89.5(2) 1_455 .
O21 Mn3 O24 88.66(19) . .
O1H Mn3 O24 81.56(18) . .
O22 Mn3 O24 86.27(18) 1_455 .
O4 Mn3 O24 173.8(2) . .
O21 Mn3 Mn4 84.25(14) . .
O1H Mn3 Mn4 43.42(13) . .
O22 Mn3 Mn4 127.73(14) 1_455 .
O4 Mn3 Mn4 141.77(16) . .
O24 Mn3 Mn4 43.39(13) . .
O23 Mn4 O2H 92.74(19) 1_655 1_655
O23 Mn4 O24 102.20(18) 1_655 .
O2H Mn4 O24 164.53(19) 1_655 .
O23 Mn4 O1H 165.24(18) 1_655 .
O2H Mn4 O1H 86.25(18) 1_655 .
O24 Mn4 O1H 80.32(18) . .
O23 Mn4 O2 101.6(2) 1_655 1_655
O2H Mn4 O2 93.4(2) 1_655 1_655
O24 Mn4 O2 79.8(2) . 1_655
O1H Mn4 O2 93.13(19) . 1_655
O23 Mn4 O22 82.12(18) 1_655 .
O2H Mn4 O22 97.82(18) 1_655 .
O24 Mn4 O22 88.28(18) . .
O1H Mn4 O22 83.43(17) . .
O2 Mn4 O22 168.0(2) 1_655 .
O23 Mn4 Mn3 133.19(14) 1_655 .
O2H Mn4 Mn3 125.80(14) 1_655 .
O24 Mn4 Mn3 43.86(12) . .
O1H Mn4 Mn3 41.58(13) . .
O2 Mn4 Mn3 101.36(15) 1_655 .
O22 Mn4 Mn3 68.54(13) . .
C1 O1 Mn1 114.6(5) . .
Mn3 O1H Mn2 100.1(2) . .
Mn3 O1H Mn4 95.01(18) . .
Mn2 O1H Mn4 137.0(2) . .
C1 O2 Mn4 139.4(5) . 1_455
Mn1 O2H Mn4 101.5(2) . 1_455
Mn1 O2H Mn2 92.73(18) . .
Mn4 O2H Mn2 136.5(2) 1_455 .
C7 O3 Mn2 142.4(5) . .
C7 O4 Mn3 105.0(5) . .
C11 O11 Mn1 123.2(4) . .
C11 O12 Mn1 123.8(4) . 1_655
C11 O12 Mn2 130.2(4) . .
Mn1 O12 Mn2 105.8(2) 1_655 .
C17 O13 Mn2 131.3(4) . .
C17 O14 Mn1 135.6(4) 1_455 .
C17 O14 Mn2 125.2(4) 1_455 .
Mn1 O14 Mn2 91.46(18) . .
C21 O21 Mn3 124.6(5) . .
C21 O22 Mn3 123.7(4) . 1_655
C21 O22 Mn4 130.7(4) . .
Mn3 O22 Mn4 105.3(2) 1_655 .
C27 O23 Mn4 131.3(4) . 1_455
C27 O24 Mn4 126.5(4) . .
C27 O24 Mn3 134.9(4) . .
Mn4 O24 Mn3 92.75(18) . .
O1 C1 O2 122.9(7) . .
O1 C1 C2 116.3(7) . .
O2 C1 C2 120.8(7) . .
C3 C2 C1 117.0(7) . .
C2 C3 C4 111.6(7) . 1_465
C5 C4 C3 112.0(7) . 1_645
C6 C5 C4 112.5(7) . .
C5 C6 C7 113.6(7) . .
O4 C7 O3 122.4(7) . .
O4 C7 C6 119.4(7) . .
O3 C7 C6 118.1(7) . .
O11 C11 O12 123.3(6) . .
O11 C11 C12 118.9(6) . .
O12 C11 C12 117.8(6) . .
C11 C12 C13 114.0(6) . .
C14 C13 C12 113.8(6) 2_656 .
C13 C14 C15 111.0(6) 2_656 .
C16 C15 C14 112.5(6) . .
C15 C16 C17 114.2(6) . .
O13 C17 O14 124.3(6) . 1_655
O13 C17 C16 120.2(6) . .
O14 C17 C16 115.5(6) 1_655 .
O21 C21 O22 122.8(6) . .
O21 C21 C22 119.8(7) . .
O22 C21 C22 117.4(6) . .
C21 C22 C23 112.9(6) . .
C24 C23 C22 114.5(6) . .
C23 C24 C25 111.9(6) . 2_665
C24 C25 C26 113.5(6) 2_665 .
C27 C26 C25 114.1(6) . .
O23 C27 O24 124.5(6) . .
O23 C27 C26 119.9(6) . .
O24 C27 C26 115.6(6) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 O11 2.094(5) .
Mn1 O1 2.099(5) .
Mn1 O2H 2.117(5) .
Mn1 O12 2.135(5) 1_455
Mn1 O14 2.184(5) .
Mn1 Mn2 3.1401(15) .
Mn2 O1H 2.129(5) .
Mn2 O13 2.143(5) .
Mn2 O3 2.186(5) .
Mn2 O14 2.201(5) .
Mn2 O2H 2.221(5) .
Mn2 O12 2.255(5) .
Mn3 O21 2.095(5) .
Mn3 O1H 2.121(5) .
Mn3 O22 2.129(5) 1_455
Mn3 O4 2.168(5) .
Mn3 O24 2.208(5) .
Mn3 Mn4 3.1833(16) .
Mn4 O23 2.130(5) 1_655
Mn4 O2H 2.150(5) 1_655
Mn4 O24 2.189(5) .
Mn4 O1H 2.196(5) .
Mn4 O2 2.235(5) 1_655
Mn4 O22 2.332(5) .
O1 C1 1.255(9) .
O2 C1 1.256(9) .
O2 Mn4 2.235(5) 1_455
O2H Mn4 2.150(5) 1_455
O3 C7 1.272(9) .
O4 C7 1.264(9) .
O11 C11 1.234(9) .
O12 C11 1.295(8) .
O12 Mn1 2.135(5) 1_655
O13 C17 1.234(9) .
O14 C17 1.295(8) 1_455
O21 C21 1.229(9) .
O22 C21 1.293(9) .
O22 Mn3 2.129(5) 1_655
O23 C27 1.242(9) .
O23 Mn4 2.130(5) 1_455
O24 C27 1.295(8) .
C1 C2 1.516(10) .
C2 C3 1.496(11) .
C3 C4 1.546(10) 1_465
C4 C5 1.530(11) .
C4 C3 1.546(10) 1_645
C5 C6 1.504(11) .
C6 C7 1.517(10) .
C11 C12 1.507(10) .
C12 C13 1.542(9) .
C13 C14 1.525(10) 2_656
C14 C13 1.525(10) 2_656
C14 C15 1.526(9) .
C15 C16 1.507(10) .
C16 C17 1.532(9) .
C17 O14 1.295(8) 1_655
C21 C22 1.511(9) .
C22 C23 1.538(9) .
C23 C24 1.511(9) .
C24 C25 1.520(10) 2_665
C25 C24 1.520(10) 2_665
C25 C26 1.526(9) .
C26 C27 1.513(9) .
