#------------------------------------------------------------------------------
#$Date: 2016-03-26 14:40:09 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180272 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/58/7115849.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_7115849
loop_
_publ_author_name
'Hamish H.-M. Yeung'
'Monica Kosa'
'John M. Griffin'
'Clare P. Grey'
'Dan T. Major'
'Anthony K. Cheetham'
_publ_section_title
;
 Topotactic elimination of water across a C-C ligand bond in a dense 3-D
 metal-organic framework
;
_journal_name_full               Chem.Commun.
_journal_page_first              13292
_journal_paper_doi               10.1039/C4cc06136E
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'C4 H2.44 Li2 O4.22'
_chemical_formula_sum            'C4 H2.44 Li2 O4.22'
_chemical_formula_weight         131.90
_chemical_name_common            'Lithium malate : fumarate'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           146
_symmetry_cell_setting           trigonal
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            9
_cell_length_a                   11.7600(6)
_cell_length_b                   11.7600(6)
_cell_length_c                   11.0689(7)
_cell_measurement_reflns_used    822
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      29.2281
_cell_measurement_theta_min      3.4579
_cell_volume                     1325.71(13)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_molecular_graphics    'Diamond and Mercury'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector_area_resol_mean 16.1183
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.873
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0184
_diffrn_reflns_av_sigmaI/netI    0.0361
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            2127
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.29
_diffrn_reflns_theta_min         3.46
_exptl_absorpt_coefficient_mu    0.128
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80749
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.487
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             596
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.221
_refine_diff_density_min         -0.221
_refine_diff_density_rms         0.048
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -2(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     113
_refine_ls_number_reflns         1273
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0588
_refine_ls_R_factor_gt           0.0425
_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)+(0.0677P)²+0.5189P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1084
_refine_ls_wR_factor_ref         0.1236
_reflns_number_gt                994
_reflns_number_total             1273
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            c4cc06136e2.cif
_cod_data_source_block           exp_2891
_cod_original_sg_symbol_H-M      'R 3'
_cod_database_code               7115849
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'
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
O2 O 0.4646(4) 0.0927(4) 0.9198(3) 0.0311(8) Uani 1 1 d . A .
O1 O 0.4339(5) 0.2343(4) 0.8138(3) 0.0325(9) Uani 1 1 d . . .
C1 C 0.4274(6) 0.1736(6) 0.9093(5) 0.0308(12) Uani 1 1 d D . .
Li1 Li 0.4226(10) -0.0773(10) 0.9843(8) 0.030(2) Uani 1 1 d . . .
C2A C 0.3552(10) 0.2015(8) 1.0108(8) 0.039(2) Uani 0.772(8) 1 d P A 1
H2A H 0.3395 0.2709 0.9996 0.046 Uiso 0.772(8) 1 calc PR A 1
Li2 Li 0.5814(11) 0.0792(10) 0.7955(10) 0.035(2) Uani 1 1 d . . .
C3A C 0.3153(11) 0.1368(10) 1.1088(8) 0.045(2) Uani 0.772(8) 1 d P A 1
H3A H 0.3345 0.0699 1.1209 0.055 Uiso 0.772(8) 1 calc PR A 1
C4 C 0.2424(6) 0.1583(6) 1.2039(5) 0.0306(12) Uani 1 1 d D . .
O3 O 0.2025(4) 0.2405(4) 1.1949(3) 0.0310(8) Uani 1 1 d . . .
O4 O 0.2335(5) 0.0976(4) 1.3001(3) 0.0327(9) Uani 1 1 d . . .
C3 C 0.269(3) 0.128(3) 1.0730(19) 0.036(3) Uani 0.228(8) 1 d PD A 2
H3A H 0.2409 0.0349 1.0668 0.044 Uiso 0.228(8) 1 calc PR A 2
H3B H 0.2182 0.1465 1.0160 0.044 Uiso 0.228(8) 1 calc PR A 2
C2 C 0.412(3) 0.207(3) 1.0402(18) 0.036(3) Uani 0.228(8) 1 d PD A 2
H2 H 0.4273 0.2965 1.0340 0.044 Uiso 0.228(8) 1 calc PR A 2
O5 O 0.4899(13) 0.2152(18) 1.1307(11) 0.090(6) Uani 0.228(8) 1 d P A 2
H5 H 0.4457 0.1640 1.1843 0.136 Uiso 0.228(8) 1 calc PR 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 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li -0.0003 0.0001 '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'
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
C1 O2 Li1 145.3(5) . .
C1 O2 Li2 121.1(5) . .
Li1 O2 Li2 90.1(4) . .
C1 O1 Li2 127.6(5) . 3_665
C1 O1 Li1 126.5(5) . 8_544
Li2 O1 Li1 105.2(6) 3_665 8_544
O2 C1 O1 124.9(5) . .
O2 C1 C2 103.8(13) . .
O1 C1 C2 129.1(13) . .
O2 C1 C2A 122.8(6) . .
O1 C1 C2A 112.1(6) . .
C2 C1 C2A 27.1(10) . .
O1 Li1 O4 106.1(5) 6 8_544
O1 Li1 O2 122.8(5) 6 .
O4 Li1 O2 109.0(5) 8_544 .
O1 Li1 O3 112.7(5) 6 7_544
O4 Li1 O3 115.8(5) 8_544 7_544
O2 Li1 O3 90.3(4) . 7_544
O1 Li1 Li2 130.6(4) 6 .
O4 Li1 Li2 123.1(3) 8_544 .
O2 Li1 Li2 45.9(3) . .
O3 Li1 Li2 44.5(3) 7_544 .
O1 Li1 Li2 37.2(2) 6 5_545
O4 Li1 Li2 119.1(6) 8_544 5_545
O2 Li1 Li2 131.3(5) . 5_545
O3 Li1 Li2 76.0(4) 7_544 5_545
Li2 Li1 Li2 106.6(3) . 5_545
O1 Li1 Li2 71.1(3) 6 6
O4 Li1 Li2 36.6(4) 8_544 6
O2 Li1 Li2 121.1(5) . 6
O3 Li1 Li2 141.2(6) 7_544 6
Li2 Li1 Li2 157.4(3) . 6
Li2 Li1 Li2 95.3(5) 5_545 6
C3A C2A C1 124.9(5) . .
O1 Li2 O4 108.0(5) 2_655 6_554
O1 Li2 O3 110.4(5) 2_655 7_544
O4 Li2 O3 122.1(6) 6_554 7_544
O1 Li2 O2 115.8(6) 2_655 .
O4 Li2 O2 111.0(6) 6_554 .
O3 Li2 O2 88.9(4) 7_544 .
O1 Li2 Li1 123.0(4) 2_655 .
O4 Li2 Li1 128.8(4) 6_554 .
O3 Li2 Li1 44.9(3) 7_544 .
O2 Li2 Li1 44.0(3) . .
O1 Li2 Li1 37.6(4) 2_655 9_654
O4 Li2 Li1 72.4(3) 6_554 9_654
O3 Li2 Li1 121.9(5) 7_544 9_654
O2 Li2 Li1 142.5(6) . 9_654
Li1 Li2 Li1 157.8(3) . 9_654
O1 Li2 Li1 119.2(5) 2_655 8_544
O4 Li2 Li1 36.5(2) 6_554 8_544
O3 Li2 Li1 130.1(5) 7_544 8_544
O2 Li2 Li1 75.3(4) . 8_544
Li1 Li2 Li1 105.8(3) . 8_544
Li1 Li2 Li1 95.9(5) 9_654 8_544
C2A C3A C4 125.7(5) . .
O4 C4 O3 122.7(5) . .
O4 C4 C3A 113.7(6) . .
O3 C4 C3A 123.3(6) . .
O4 C4 C3 128.5(13) . .
O3 C4 C3 107.3(12) . .
C3A C4 C3 24.0(10) . .
C4 O3 Li2 143.1(5) . 4_455
C4 O3 Li1 122.6(5) . 4_455
Li2 O3 Li1 90.6(5) 4_455 4_455
C4 O4 Li1 126.9(5) . 6
C4 O4 Li2 125.4(5) . 8_545
Li1 O4 Li2 106.8(5) 6 8_545
C2 C3 C4 111.9(16) . .
O5 C2 C3 112.3(19) . .
O5 C2 C1 125(2) . .
C3 C2 C1 107.8(15) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O2 C1 1.236(7) .
O2 Li1 1.939(10) .
O2 Li2 2.005(12) .
O1 C1 1.257(8) .
O1 Li2 1.917(12) 3_665
O1 Li1 1.934(10) 8_544
C1 C2 1.535(17) .
C1 C2A 1.540(8) .
Li1 O1 1.934(10) 6
Li1 O4 1.938(11) 8_544
Li1 O3 1.973(11) 7_544
Li1 Li2 2.793(5) .
Li1 Li2 3.059(16) 5_545
Li1 Li2 3.117(16) 6
C2A C3A 1.273(6) .
Li2 O1 1.917(12) 2_655
Li2 O4 1.943(11) 6_554
Li2 O3 1.957(10) 7_544
Li2 Li1 3.059(16) 9_654
Li2 Li1 3.117(16) 8_544
C3A C4 1.458(9) .
C4 O4 1.257(8) .
C4 O3 1.272(7) .
C4 C3 1.564(16) .
O3 Li2 1.957(10) 4_455
O3 Li1 1.973(11) 4_455
O4 Li1 1.938(11) 6
O4 Li2 1.943(11) 8_545
C3 C2 1.504(15) .
C2 O5 1.32(3) .
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
Li1 O2 C1 O1 -136.2(7) . .
Li2 O2 C1 O1 15.2(9) . .
Li1 O2 C1 C2 59.2(17) . .
Li2 O2 C1 C2 -149.4(13) . .
Li1 O2 C1 C2A 37.9(13) . .
Li2 O2 C1 C2A -170.7(7) . .
Li2 O1 C1 O2 -132.9(7) 3_665 .
Li1 O1 C1 O2 35.4(11) 8_544 .
Li2 O1 C1 C2 27.7(18) 3_665 .
Li1 O1 C1 C2 -164.0(16) 8_544 .
Li2 O1 C1 C2A 52.5(9) 3_665 .
Li1 O1 C1 C2A -139.3(6) 8_544 .
C1 O2 Li1 O1 -87.1(10) . 6
Li2 O2 Li1 O1 117.1(5) . 6
C1 O2 Li1 O4 37.7(11) . 8_544
Li2 O2 Li1 O4 -118.1(4) . 8_544
C1 O2 Li1 O3 155.3(8) . 7_544
Li2 O2 Li1 O3 -0.5(6) . 7_544
C1 O2 Li1 Li2 155.8(11) . .
C1 O2 Li1 Li2 -133.1(9) . 5_545
Li2 O2 Li1 Li2 71.1(5) . 5_545
C1 O2 Li1 Li2 -0.7(11) . 6
Li2 O2 Li1 Li2 -156.5(2) . 6
O2 C1 C2A C3A -7.4(12) . .
O1 C1 C2A C3A 167.4(7) . .
C2 C1 C2A C3A -58(3) . .
C1 O2 Li2 O1 84.1(7) . 2_655
Li1 O2 Li2 O1 -111.7(5) . 2_655
C1 O2 Li2 O4 -39.5(7) . 6_554
Li1 O2 Li2 O4 124.7(4) . 6_554
C1 O2 Li2 O3 -163.7(5) . 7_544
Li1 O2 Li2 O3 0.5(6) . 7_544
C1 O2 Li2 Li1 -164.2(7) . .
C1 O2 Li2 Li1 48.8(10) . 9_654
Li1 O2 Li2 Li1 -147.1(6) . 9_654
C1 O2 Li2 Li1 -31.5(6) . 8_544
Li1 O2 Li2 Li1 132.7(4) . 8_544
O1 Li1 Li2 O1 -5.0(5) 6 2_655
O4 Li1 Li2 O1 179.1(8) 8_544 2_655
O2 Li1 Li2 O1 94.3(7) . 2_655
O3 Li1 Li2 O1 -86.4(6) 7_544 2_655
Li2 Li1 Li2 O1 -37.9(3) 5_545 2_655
Li2 Li1 Li2 O1 157.1(10) 6 2_655
O1 Li1 Li2 O4 -179.4(8) 6 6_554
O4 Li1 Li2 O4 4.7(4) 8_544 6_554
O2 Li1 Li2 O4 -80.1(6) . 6_554
O3 Li1 Li2 O4 99.2(7) 7_544 6_554
Li2 Li1 Li2 O4 147.7(7) 5_545 6_554
Li2 Li1 Li2 O4 -17.3(8) 6 6_554
O1 Li1 Li2 O3 81.4(6) 6 7_544
O4 Li1 Li2 O3 -94.5(6) 8_544 7_544
O2 Li1 Li2 O3 -179.3(9) . 7_544
Li2 Li1 Li2 O3 48.5(6) 5_545 7_544
Li2 Li1 Li2 O3 -116.5(11) 6 7_544
O1 Li1 Li2 O2 -99.3(7) 6 .
O4 Li1 Li2 O2 84.8(6) 8_544 .
O3 Li1 Li2 O2 179.3(9) 7_544 .
Li2 Li1 Li2 O2 -132.2(5) 5_545 .
Li2 Li1 Li2 O2 62.8(7) 6 .
O1 Li1 Li2 Li1 19.7(8) 6 9_654
O4 Li1 Li2 Li1 -156.2(11) 8_544 9_654
O2 Li1 Li2 Li1 119.0(11) . 9_654
O3 Li1 Li2 Li1 -61.7(7) 7_544 9_654
Li2 Li1 Li2 Li1 -13.2(7) 5_545 9_654
Li2 Li1 Li2 Li1 -178.2(15) 6 9_654
O1 Li1 Li2 Li1 -147.0(7) 6 8_544
O4 Li1 Li2 Li1 37.1(3) 8_544 8_544
O2 Li1 Li2 Li1 -47.7(5) . 8_544
O3 Li1 Li2 Li1 131.6(5) 7_544 8_544
Li2 Li1 Li2 Li1 -179.8(5) 5_545 8_544
Li2 Li1 Li2 Li1 15.1(7) 6 8_544
C1 C2A C3A C4 -177.5(12) . .
C2A C3A C4 O4 -168.6(7) . .
C2A C3A C4 O3 4.9(12) . .
C2A C3A C4 C3 58(3) . .
O4 C4 O3 Li2 137.7(7) . 4_455
C3A C4 O3 Li2 -35.2(12) . 4_455
C3 C4 O3 Li2 -55.0(17) . 4_455
O4 C4 O3 Li1 -13.2(9) . 4_455
C3A C4 O3 Li1 173.9(8) . 4_455
C3 C4 O3 Li1 154.0(13) . 4_455
O3 C4 O4 Li1 132.0(6) . 6
C3A C4 O4 Li1 -54.4(9) . 6
C3 C4 O4 Li1 -32.3(18) . 6
O3 C4 O4 Li2 -35.9(10) . 8_545
C3A C4 O4 Li2 137.6(6) . 8_545
C3 C4 O4 Li2 159.8(16) . 8_545
O4 C4 C3 C2 -95.8(16) . .
O3 C4 C3 C2 97.9(14) . .
C3A C4 C3 C2 -38(3) . .
C4 C3 C2 O5 41.1(19) . .
C4 C3 C2 C1 -178(2) . .
O2 C1 C2 O5 36(3) . .
O1 C1 C2 O5 -128(2) . .
C2A C1 C2 O5 174(6) . .
O2 C1 C2 C3 -99.0(13) . .
O1 C1 C2 C3 97.3(16) . .
C2A C1 C2 C3 39(2) . .
