#------------------------------------------------------------------------------
#$Date: 2016-03-23 20:24:42 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179410 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/07/4330763.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_4330763
loop_
_publ_author_name
'Paul J. Saines'
'Mark Steinmann'
'Jin-Chong Tan'
'Hamish H.-M. Yeung'
'Wei Li'
'Phillip T. Barton'
'Anthony K. Cheetham'
_publ_contact_author_address
;Department of Materials Science and Metallurgy
The University of Cambridge
Cambridge
Cambs, UK
;
_publ_contact_author_email       akc30@cam.ac.uk
_publ_contact_author_fax         441223334567
_publ_contact_author_name        'Cheetham, Anthony K.'
_publ_contact_author_phone       441223767061
_publ_section_title
;
 Isomer-Directed Structural Diversity and Its Effect on the Nanosheet
 Exfoliation and Magnetic Properties of 2,3-Dimethylsuccinate Hybrid
 Frameworks
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11198
_journal_page_last               11209
_journal_paper_doi               10.1021/ic302011x
_journal_volume                  51
_journal_year                    2012
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C6 H8 Mn1 O4'
_chemical_formula_sum            'C6 H8 Mn O4'
_chemical_formula_weight         199.06
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      148
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-01-16T12:29:05-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   11.2083(7)
_cell_length_b                   11.2083(7)
_cell_length_c                   30.269(3)
_cell_measurement_reflns_used    3458
_cell_measurement_temperature    125(2)
_cell_measurement_theta_max      32.5972
_cell_measurement_theta_min      3.4068
_cell_measurement_wavelength     0.71073
_cell_volume                     3293.1(4)
_computing_cell_refinement
'CrysAlisPro V1.171.35.11 (Agilent Technologies)'
_computing_data_collection
'CrysAlisPro V1.171.35.11 (Agilent Technologies)'
_computing_data_reduction
'CrysAlisPro V1.171.35.11 (Agilent Technologies)'
_computing_molecular_graphics    'Diamond (Brandenburg 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'DIRDIF-2008 (Beurskens, 2008)'
_diffrn_ambient_temperature      125(2)
_diffrn_detector_area_resol_mean 16.1183
_diffrn_measured_fraction_theta_full 0.9942
_diffrn_measured_fraction_theta_max 0.916
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_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  0.0493
_diffrn_reflns_av_unetI/netI     0.0418
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            7397
_diffrn_reflns_theta_full        30.44
_diffrn_reflns_theta_max         32.67
_diffrn_reflns_theta_min         3.41
_exptl_absorpt_coefficient_mu    1.768
_exptl_absorpt_correction_T_max  0.819
_exptl_absorpt_correction_T_min  0.667
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
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    1.807
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             1818
_exptl_crystal_size_max          0.3684
_exptl_crystal_size_mid          0.2908
_exptl_crystal_size_min          0.1456
_refine_diff_density_max         1.106
_refine_diff_density_min         -1.042
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     107
_refine_ls_number_reflns         2472
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0561
_refine_ls_R_factor_gt           0.0509
_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)+(0.0772P)²+21.1605P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1319
_refine_ls_wR_factor_ref         0.1377
_reflns_number_gt                2219
_reflns_number_total             2472
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302011x_si_002_3.cif
_cod_data_source_block           Compound2
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4330763
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.8333 -0.3333 0.6667 0.01405(14) Uani 1 2 d S . .
Mn2 Mn 1.0000 0.0000 0.635820(19) 0.01370(15) Uani 1 3 d S . .
Mn3 Mn 1.0000 0.0000 0.5000 0.01281(17) Uani 1 6 d S . .
O1 O 0.85716(19) -0.20177(18) 0.60983(6) 0.0193(3) Uani 1 1 d . . .
O2 O 0.83384(19) -0.1524(2) 0.54024(6) 0.0233(4) Uani 1 1 d . . .
O3 O 0.64314(18) -0.52139(17) 0.65152(6) 0.0192(3) Uani 1 1 d . . .
O4 O 0.42227(18) -0.63976(19) 0.63136(6) 0.0220(4) Uani 1 1 d . . .
C1 C 0.8023(3) -0.2340(3) 0.57131(8) 0.0231(5) Uani 0.586(4) 1 d P A 1
C2 C 0.7085(6) -0.3894(5) 0.56563(17) 0.0307(7) Uani 0.586(4) 1 d P A 1
H2 H 0.7529 -0.4368 0.5791 0.037 Uiso 0.586(4) 1 calc PR A 1
C3 C 0.6815(8) -0.4289(7) 0.5166(3) 0.0560(11) Uani 0.586(4) 1 d P A 1
H3A H 0.6303 -0.3899 0.5039 0.084 Uiso 0.586(4) 1 calc PR A 1
H3B H 0.6296 -0.5274 0.5139 0.084 Uiso 0.586(4) 1 calc PR A 1
H3C H 0.7678 -0.3942 0.5014 0.084 Uiso 0.586(4) 1 calc PR A 1
C4 C 0.5631(6) -0.4416(6) 0.58854(19) 0.0307(7) Uani 0.586(4) 1 d P A 1
H4 H 0.4935 -0.4974 0.5664 0.037 Uiso 0.586(4) 1 calc PR A 1
C5 C 0.5314(8) -0.3336(7) 0.6027(3) 0.0560(11) Uani 0.586(4) 1 d P A 1
H5A H 0.5912 -0.2816 0.6266 0.084 Uiso 0.586(4) 1 calc PR A 1
H5B H 0.4373 -0.3762 0.6123 0.084 Uiso 0.586(4) 1 calc PR A 1
H5C H 0.5452 -0.2732 0.5783 0.084 Uiso 0.586(4) 1 calc PR A 1
C6 C 0.5407(3) -0.5391(2) 0.62800(8) 0.0208(4) Uani 0.586(4) 1 d P A 1
C1A C 0.8023(3) -0.2340(3) 0.57131(8) 0.0231(5) Uani 0.414(4) 1 d P A 2
C2A C 0.6584(8) -0.3687(7) 0.5628(2) 0.0307(7) Uani 0.414(4) 1 d P A 2
H2A H 0.6118 -0.3501 0.5386 0.037 Uiso 0.414(4) 1 calc PR A 2
C3A C 0.6955(12) -0.4734(11) 0.5472(4) 0.0560(11) Uani 0.414(4) 1 d P A 2
H3AA H 0.7564 -0.4372 0.5223 0.084 Uiso 0.414(4) 1 calc PR A 2
H3AB H 0.6134 -0.5562 0.5386 0.084 Uiso 0.414(4) 1 calc PR A 2
H3AC H 0.7405 -0.4935 0.5706 0.084 Uiso 0.414(4) 1 calc PR A 2
C4A C 0.5667(9) -0.4101(8) 0.6031(3) 0.0307(7) Uani 0.414(4) 1 d P A 2
H4A H 0.5962 -0.3321 0.6234 0.037 Uiso 0.414(4) 1 calc PR A 2
C5A C 0.4362(12) -0.4405(10) 0.5792(4) 0.0560(11) Uani 0.414(4) 1 d P A 2
H5AA H 0.4538 -0.3632 0.5610 0.084 Uiso 0.414(4) 1 calc PR A 2
H5AB H 0.3659 -0.4569 0.6003 0.084 Uiso 0.414(4) 1 calc PR A 2
H5AC H 0.4062 -0.5207 0.5610 0.084 Uiso 0.414(4) 1 calc PR A 2
C6A C 0.5407(3) -0.5391(2) 0.62800(8) 0.0208(4) Uani 0.414(4) 1 d P A 2
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'
O O 0.0106 0.006 '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
O4 Mn1 O4 180.00(7) 15_446 3_755
O4 Mn1 O3 86.77(7) 15_446 13_646
O4 Mn1 O3 93.23(7) 3_755 13_646
O4 Mn1 O3 93.23(7) 15_446 .
O4 Mn1 O3 86.77(7) 3_755 .
O3 Mn1 O3 180.00(9) 13_646 .
O4 Mn1 O1 90.60(7) 15_446 13_646
O4 Mn1 O1 89.40(7) 3_755 13_646
O3 Mn1 O1 102.57(7) 13_646 13_646
O3 Mn1 O1 77.43(7) . 13_646
O4 Mn1 O1 89.40(7) 15_446 .
O4 Mn1 O1 90.60(7) 3_755 .
O3 Mn1 O1 77.43(7) 13_646 .
O3 Mn1 O1 102.57(7) . .
O1 Mn1 O1 180.00(5) 13_646 .
O1 Mn2 O1 107.55(5) 3_765 2_645
O1 Mn2 O1 107.55(5) 3_765 .
O1 Mn2 O1 107.54(5) 2_645 .
O1 Mn2 O3 87.89(7) 3_765 14_666
O1 Mn2 O3 76.24(6) 2_645 14_666
O1 Mn2 O3 161.48(7) . 14_666
O1 Mn2 O3 161.48(7) 3_765 13_646
O1 Mn2 O3 87.89(7) 2_645 13_646
O1 Mn2 O3 76.25(6) . 13_646
O3 Mn2 O3 85.91(7) 14_666 13_646
O1 Mn2 O3 76.24(6) 3_765 15_446
O1 Mn2 O3 161.48(7) 2_645 15_446
O1 Mn2 O3 87.89(7) . 15_446
O3 Mn2 O3 85.91(7) 14_666 15_446
O3 Mn2 O3 85.91(7) 13_646 15_446
O2 Mn3 O2 91.46(7) 11_666 12_546
O2 Mn3 O2 91.46(7) 11_666 10_756
O2 Mn3 O2 91.46(7) 12_546 10_756
O2 Mn3 O2 88.54(7) 11_666 3_765
O2 Mn3 O2 179.999(1) 12_546 3_765
O2 Mn3 O2 88.54(7) 10_756 3_765
O2 Mn3 O2 180.00(11) 11_666 2_645
O2 Mn3 O2 88.54(7) 12_546 2_645
O2 Mn3 O2 88.54(7) 10_756 2_645
O2 Mn3 O2 91.46(7) 3_765 2_645
O2 Mn3 O2 88.54(7) 11_666 .
O2 Mn3 O2 88.54(7) 12_546 .
O2 Mn3 O2 180.0 10_756 .
O2 Mn3 O2 91.46(7) 3_765 .
O2 Mn3 O2 91.46(7) 2_645 .
C1 O1 Mn2 128.70(16) . .
C1 O1 Mn1 130.04(16) . .
Mn2 O1 Mn1 101.26(7) . .
C1 O2 Mn3 145.92(19) . .
C6 O3 Mn1 129.64(15) . .
C6 O3 Mn2 130.65(15) . 13_646
Mn1 O3 Mn2 99.11(7) . 13_646
C6 O4 Mn1 134.25(16) . 2_535
O2 C1 O1 124.4(2) . .
O2 C1 C2 122.5(3) . .
O1 C1 C2 112.5(3) . .
C1 C2 C3 111.2(4) . .
C1 C2 C4 111.4(5) . .
C3 C2 C4 107.3(5) . .
C5 C4 C6 109.3(5) . .
C5 C4 C2 116.4(5) . .
C6 C4 C2 111.7(4) . .
O4 C6 O3 124.2(2) . .
O4 C6 C4 115.2(3) . .
O3 C6 C4 120.2(3) . .
C3A C2A C4A 115.2(7) . .
C5A C4A C2A 96.6(7) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 O4 2.1634(18) 15_446
Mn1 O4 2.1633(18) 3_755
Mn1 O3 2.1689(17) 13_646
Mn1 O3 2.1688(17) .
Mn1 O1 2.1936(17) 13_646
Mn1 O1 2.1936(17) .
Mn2 O1 2.1624(17) 3_765
Mn2 O1 2.1624(17) 2_645
Mn2 O1 2.1624(17) .
Mn2 O3 2.2557(18) 14_666
Mn2 O3 2.2557(18) 13_646
Mn2 O3 2.2558(18) 15_446
Mn3 O2 2.1653(18) 11_666
Mn3 O2 2.1653(18) 12_546
Mn3 O2 2.1653(18) 10_756
Mn3 O2 2.1653(18) 3_765
Mn3 O2 2.1653(18) 2_645
Mn3 O2 2.1653(18) .
O1 C1 1.283(3) .
O2 C1 1.234(3) .
O3 C6 1.280(3) .
O3 Mn2 2.2557(17) 13_646
O4 C6 1.244(3) .
O4 Mn1 2.1634(18) 2_535
C1 C2 1.529(5) .
C2 C3 1.534(9) .
C2 C4 1.589(9) .
C4 C5 1.485(11) .
C4 C6 1.552(6) .
C2A C3A 1.504(15) .
C2A C4A 1.512(12) .
C4A C5A 1.511(13) .
