#------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/51/54/1515485.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_1515485
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         'C3 H3 Mn3 O9'
_chemical_formula_sum            'C3 H3 Mn3 O9'
_chemical_formula_weight         347.87
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2010-11-17T11:59:26-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 108.259(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.9072(5)
_cell_length_b                   5.7181(2)
_cell_length_c                   12.6330(5)
_cell_measurement_reflns_used    1401
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      29.0855
_cell_measurement_theta_min      2.9677
_cell_measurement_wavelength     0.71073
_cell_volume                     748.23(6)
_computing_cell_refinement       'CrysAlisPro, Oxford Diffraction, 2010'
_computing_data_collection       'CrysAlisPro, Oxford Diffraction, 2010'
_computing_data_reduction        'CrysAlisPro, Oxford Diffraction, 2010'
_computing_molecular_graphics    'Diamond (Brandenburg 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.876
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0374
_diffrn_reflns_av_unetI/netI     0.0455
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            5302
_diffrn_reflns_theta_full        26.32
_diffrn_reflns_theta_max         29.15
_diffrn_reflns_theta_min         2.97
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.015
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85761
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.088
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.1706
_exptl_crystal_size_mid          0.0889
_exptl_crystal_size_min          0.0398
_refine_diff_density_max         0.643
_refine_diff_density_min         -0.585
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     145
_refine_ls_number_reflns         1764
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0674
_refine_ls_R_factor_gt           0.0348
_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)+(0.0220P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0648
_refine_ls_wR_factor_ref         0.0797
_reflns_number_gt                1145
_reflns_number_total             1764
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1sc00253h.txt
_cod_data_source_block           1
_cod_original_cell_volume        748.23(5)
_cod_database_code               1515485
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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
Mn3 Mn 0.83458(5) 0.22375(9) 0.20580(5) 0.00801(16) Uani 1 1 d .
Mn1 Mn 1.16424(6) 0.27453(9) 0.20252(5) 0.00856(16) Uani 1 1 d .
Mn2 Mn 1.01015(5) -0.24174(8) 0.29964(5) 0.00851(17) Uani 1 1 d .
O1 O 0.7586(2) 0.2175(4) 0.0197(2) 0.0104(6) Uani 1 1 d .
O2H O 0.8347(3) -0.0734(4) 0.3075(2) 0.0092(6) Uani 1 1 d D
H2H H 0.861(4) -0.024(6) 0.3733(19) 0.014 Uiso 1 1 d D
O6 O 0.9335(2) 0.4284(4) 0.3594(2) 0.0110(6) Uani 1 1 d .
O5 O 0.9242(2) 0.2337(4) 0.5109(2) 0.0105(6) Uani 1 1 d .
O4 O 0.9179(2) 0.7357(4) -0.0077(2) 0.0095(6) Uani 1 1 d .
O3 O 0.9151(3) 0.5451(4) 0.1471(2) 0.0115(6) Uani 1 1 d .
O1H O 1.0089(2) 0.0468(4) 0.1905(2) 0.0099(6) Uani 1 1 d D
H1H H 0.984(4) -0.025(6) 0.130(2) 0.015 Uiso 1 1 d D
O2 O 0.7497(3) 0.4288(4) -0.1315(2) 0.0135(6) Uani 1 1 d .
C1 C 0.7890(4) 0.3884(7) -0.0289(3) 0.0123(9) Uani 1 1 d .
C3 C 0.9588(3) 0.4011(6) 0.4639(3) 0.0081(8) Uani 1 1 d .
C2 C 0.8818(4) 0.5754(6) 0.0419(3) 0.0099(9) Uani 1 1 d .
O3H O 1.1812(3) 0.5635(4) 0.3142(2) 0.0100(6) Uani 1 1 d D
H3H H 1.209(4) 0.504(6) 0.377(2) 0.015 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 0 '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'
O O 0.0106 0.006 '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
O2H Mn3 O2H 108.48(6) . 2_655
O2H Mn3 O1H 81.39(10) . .
O2H Mn3 O1H 169.36(10) 2_655 .
O2H Mn3 O6 89.13(9) . .
O2H Mn3 O6 87.39(10) 2_655 .
O1H Mn3 O6 96.94(10) . .
O2H Mn3 O1 123.50(9) . .
O2H Mn3 O1 84.23(10) 2_655 .
O1H Mn3 O1 86.93(10) . .
O6 Mn3 O1 147.29(9) . .
O2H Mn3 O3 156.89(10) . .
O2H Mn3 O3 87.02(10) 2_655 .
O1H Mn3 O3 84.84(10) . .
O6 Mn3 O3 74.17(9) . .
O1 Mn3 O3 73.86(9) . .
O1H Mn1 O3H 106.60(10) . 2_745
O1H Mn1 O3H 115.23(11) . .
O3H Mn1 O3H 126.34(6) 2_745 .
O1H Mn1 O2 149.57(10) . 3_765
O3H Mn1 O2 86.90(10) 2_745 3_765
O3H Mn1 O2 73.81(10) . 3_765
O1H Mn1 O2 80.91(10) . 4_666
O3H Mn1 O2 72.58(10) 2_745 4_666
O3H Mn1 O2 82.18(9) . 4_666
O2 Mn1 O2 129.50(6) 3_765 4_666
O1H Mn1 O4 82.78(10) . 3_765
O3H Mn1 O4 86.31(10) 2_745 3_765
O3H Mn1 O4 129.59(9) . 3_765
O2 Mn1 O4 70.77(9) 3_765 3_765
O2 Mn1 O4 148.19(8) 4_666 3_765
O3H Mn2 O1H 106.63(11) 1_545 .
O3H Mn2 O2H 171.06(10) 1_545 .
O1H Mn2 O2H 81.99(10) . .
O3H Mn2 O3 86.94(10) 1_545 1_545
O1H Mn2 O3 87.57(10) . 1_545
O2H Mn2 O3 95.96(10) . 1_545
O3H Mn2 O5 86.62(10) 1_545 3_756
O1H Mn2 O5 126.64(9) . 3_756
O2H Mn2 O5 86.23(10) . 3_756
O3 Mn2 O5 145.54(9) 1_545 3_756
O3H Mn2 O6 86.62(10) 1_545 1_545
O1H Mn2 O6 156.49(10) . 1_545
O2H Mn2 O6 86.10(10) . 1_545
O3 Mn2 O6 73.55(9) 1_545 1_545
O5 Mn2 O6 72.31(8) 3_756 1_545
C1 O1 Mn3 115.8(2) . .
Mn3 O2H Mn3 123.16(12) . 2_645
Mn3 O2H Mn2 99.20(12) . .
Mn3 O2H Mn2 120.42(11) 2_645 .
C3 O6 Mn3 136.6(2) . .
C3 O6 Mn2 117.5(2) . 1_565
Mn3 O6 Mn2 105.82(11) . 1_565
C3 O5 Mn2 116.3(2) . 3_756
C2 O4 Mn1 115.8(2) . 3_765
C2 O3 Mn2 136.6(2) . 1_565
C2 O3 Mn3 116.0(2) . .
Mn2 O3 Mn3 106.43(11) 1_565 .
Mn1 O1H Mn2 125.89(12) . .
Mn1 O1H Mn3 113.88(10) . .
Mn2 O1H Mn3 97.33(12) . .
C1 O2 Mn1 120.0(2) . 3_765
C1 O2 Mn1 138.8(2) . 4_565
Mn1 O2 Mn1 96.70(11) 3_765 4_565
O2 C1 O1 126.4(4) . .
O2 C1 C2 114.8(3) . .
O1 C1 C2 118.7(3) . .
O5 C3 O6 126.2(3) . .
O5 C3 C3 119.2(4) . 3_766
O6 C3 C3 114.7(4) . 3_766
O4 C2 O3 126.5(3) . .
O4 C2 C1 118.1(3) . .
O3 C2 C1 115.4(3) . .
Mn2 O3H Mn1 113.13(11) 1_565 2_755
Mn2 O3H Mn1 116.96(12) 1_565 .
Mn1 O3H Mn1 106.16(13) 2_755 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn3 O2H 2.130(3) .
Mn3 O2H 2.142(3) 2_655
Mn3 O1H 2.215(3) .
Mn3 O6 2.233(2) .
Mn3 O1 2.235(3) .
Mn3 O3 2.260(3) .
Mn1 O1H 2.104(3) .
Mn1 O3H 2.137(3) 2_745
Mn1 O3H 2.143(3) .
Mn1 O2 2.256(3) 3_765
Mn1 O2 2.322(3) 4_666
Mn1 O4 2.342(3) 3_765
Mn2 O3H 2.131(3) 1_545
Mn2 O1H 2.148(3) .
Mn2 O2H 2.172(3) .
Mn2 O3 2.241(2) 1_545
Mn2 O5 2.273(3) 3_756
Mn2 O6 2.285(3) 1_545
O1 C1 1.253(5) .
O2H Mn3 2.142(3) 2_645
O6 C3 1.271(5) .
O6 Mn2 2.285(3) 1_565
O5 C3 1.245(4) .
O5 Mn2 2.273(3) 3_756
O4 C2 1.242(4) .
O4 Mn1 2.341(3) 3_765
O3 C2 1.275(5) .
O3 Mn2 2.241(2) 1_565
O2 C1 1.252(5) .
O2 Mn1 2.256(3) 3_765
O2 Mn1 2.322(3) 4_565
C1 C2 1.550(5) .
C3 C3 1.551(7) 3_766
O3H Mn2 2.131(3) 1_565
O3H Mn1 2.137(3) 2_755
