#------------------------------------------------------------------------------
#$Date: 2016-03-26 13:40:09 +0100 (Sat 26 de Mar de 2016) $
#$Revision: 180272 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/58/7115848.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_7115848
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_absolute_configuration syn
_chemical_formula_sum            'C4 H2.85 Li2 O4.43'
_chemical_formula_weight         135.60
_chemical_name_common            'Lithium malate : fumarate'
_chemical_name_systematic
;
 Dilithium (L-malate)0.43 (fumarate)0.57
;
_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                   11.8093(10)
_cell_length_b                   11.8093(10)
_cell_length_c                   10.9615(11)
_cell_measurement_reflns_used    427
_cell_measurement_temperature    119.95(10)
_cell_measurement_theta_max      28.6171
_cell_measurement_theta_min      3.4434
_cell_volume                     1323.9(2)
_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, Mercury'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      119.95(10)
_diffrn_detector_area_resol_mean 16.1183
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.862
_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  0.0274
_diffrn_reflns_av_sigmaI/netI    0.0479
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            1330
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.68
_diffrn_reflns_theta_min         3.45
_exptl_absorpt_coefficient_mu    0.133
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60576
_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    1.531
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       shard
_exptl_crystal_F_000             614
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.347
_refine_diff_density_min         -0.251
_refine_diff_density_rms         0.062
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   4(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     107
_refine_ls_number_reflns         936
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0736
_refine_ls_R_factor_gt           0.0513
_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)+(0.0720P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1208
_refine_ls_wR_factor_ref         0.1389
_reflns_number_gt                696
_reflns_number_total             936
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            c4cc06136e2.cif
_cod_data_source_block           exp_2866
_cod_original_sg_symbol_H-M      'R 3'
_cod_database_code               7115848
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
O4 O 0.7573(4) -0.0391(4) 0.1458(3) 0.0333(10) Uani 1 1 d . . .
C1 C 0.8248(6) 0.2558(7) -0.1387(6) 0.0366(16) Uani 1 1 d . . .
O1 O 0.9049(4) 0.3741(4) -0.1306(3) 0.0331(10) Uani 1 1 d . . .
O2 O 0.7679(4) 0.1983(4) -0.2342(4) 0.0356(11) Uani 1 1 d . A .
Li2 Li 0.7443(10) -0.1682(11) 0.2651(10) 0.034(3) Uani 1 1 d . . .
C3A C 0.8674(16) 0.1777(13) 0.0544(13) 0.0456(19) Uani 0.575(12) 1 d P A 1
H3A H 0.9357 0.2625 0.0671 0.055 Uiso 0.575(12) 1 calc PR A 1
C2A C 0.8050(14) 0.1560(13) -0.0441(12) 0.0456(19) Uani 0.575(12) 1 d P A 1
H2A H 0.7407 0.0701 -0.0595 0.055 Uiso 0.575(12) 1 calc PR A 1
C2B C 0.7844(17) 0.1936(17) -0.0049(16) 0.0340(19) Uani 0.425(12) 1 d P A 2
H2B H 0.6963 0.1176 -0.0125 0.041 Uiso 0.425(12) 1 calc PR A 2
C3B C 0.8756(17) 0.1392(19) 0.0218(18) 0.0340(19) Uani 0.425(12) 1 d P A 2
H3B1 H 0.9663 0.2083 0.0173 0.041 Uiso 0.425(12) 1 calc PR A 2
H3B2 H 0.8616 0.0719 -0.0369 0.041 Uiso 0.425(12) 1 calc PR A 2
O5 O 0.7770(12) 0.2696(10) 0.0827(8) 0.086(5) Uani 0.425(12) 1 d P A 2
H5 H 0.7263 0.2941 0.0612 0.128 Uiso 0.425(12) 1 calc PR A 2
O3 O 0.9043(4) 0.1345(4) 0.2493(3) 0.0316(9) Uani 1 1 d . . .
Li1 Li 0.8293(9) 0.0831(10) 0.4076(10) 0.031(2) Uani 1 1 d . . .
C4 C 0.8423(6) 0.0813(6) 0.1520(5) 0.0302(14) Uani 1 1 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 0.0000 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
C4 O4 Li2 123.2(5) . .
C4 O4 Li1 143.0(5) . 9_654
Li2 O4 Li1 92.0(5) . 9_654
O1 C1 O2 125.1(6) . .
O1 C1 C2A 124.7(7) . .
O2 C1 C2A 108.9(8) . .
O1 C1 C2B 109.6(9) . .
O2 C1 C2B 124.2(9) . .
C2A C1 C2B 27.3(7) . .
C1 O1 Li2 142.9(5) . 7_554
C1 O1 Li1 122.3(5) . 6_664
Li2 O1 Li1 90.5(4) 7_554 6_664
C1 O2 Li1 128.3(6) . 5_544
C1 O2 Li2 126.7(5) . 5_544
Li1 O2 Li2 102.9(6) 5_544 5_544
O3 Li2 O1 112.5(6) 2_645 4_445
O3 Li2 O4 117.1(6) 2_645 .
O1 Li2 O4 89.8(5) 4_445 .
O3 Li2 O2 106.3(5) 2_645 9_655
O1 Li2 O2 119.9(6) 4_445 9_655
O4 Li2 O2 111.3(6) . 9_655
O3 Li2 Li1 124.7(4) 2_645 9_654
O1 Li2 Li1 45.8(3) 4_445 9_654
O4 Li2 Li1 44.1(3) . 9_654
O2 Li2 Li1 129.0(4) 9_655 9_654
O3 Li2 Li1 118.3(5) 2_645 .
O1 Li2 Li1 128.7(6) 4_445 .
O4 Li2 Li1 74.0(5) . .
O2 Li2 Li1 38.2(2) 9_655 .
Li1 Li2 Li1 104.9(3) 9_654 .
O3 Li2 Li1 35.4(4) 2_645 2_645
O1 Li2 Li1 122.8(5) 4_445 2_645
O4 Li2 Li1 141.3(6) . 2_645
O2 Li2 Li1 72.5(3) 9_655 2_645
Li1 Li2 Li1 157.9(3) 9_654 2_645
Li1 Li2 Li1 96.3(4) . 2_645
C2A C3A C4 126.3(8) . .
C3A C2A C1 126.0(8) . .
O5 C2B C3B 115.9(12) . .
O5 C2B C1 116.8(12) . .
C3B C2B C1 104.9(10) . .
C2B C3B C4 106.5(10) . .
C4 O3 Li1 123.2(5) . .
C4 O3 Li2 127.2(5) . 3_765
Li1 O3 Li2 109.1(6) . 3_765
O3 Li1 O2 110.4(6) . 9_655
O3 Li1 O4 124.6(6) . 5_545
O2 Li1 O4 108.9(5) 9_655 5_545
O3 Li1 O1 110.2(5) . 8_645
O2 Li1 O1 113.4(6) 9_655 8_645
O4 Li1 O1 87.5(5) 5_545 8_645
O3 Li1 Li2 127.6(4) . 5_545
O2 Li1 Li2 121.6(4) 9_655 5_545
O4 Li1 Li2 43.9(3) 5_545 5_545
O1 Li1 Li2 43.7(3) 8_645 5_545
O3 Li1 Li2 73.6(3) . .
O2 Li1 Li2 39.0(4) 9_655 .
O4 Li1 Li2 123.3(5) 5_545 .
O1 Li1 Li2 141.1(6) 8_645 .
Li2 Li1 Li2 158.3(3) 5_545 .
O3 Li1 Li2 35.5(2) . 3_765
O2 Li1 Li2 121.2(5) 9_655 3_765
O4 Li1 Li2 129.8(5) 5_545 3_765
O1 Li1 Li2 75.2(4) 8_645 3_765
Li2 Li1 Li2 104.2(3) 5_545 3_765
Li2 Li1 Li2 96.8(5) . 3_765
O3 C4 O4 122.6(6) . .
O3 C4 C3A 112.5(7) . .
O4 C4 C3A 124.4(7) . .
O3 C4 C3B 127.0(10) . .
O4 C4 C3B 109.2(10) . .
C3A C4 C3B 23.7(7) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O4 C4 1.268(7) .
O4 Li2 1.957(11) .
O4 Li1 1.962(11) 9_654
C1 O1 1.238(8) .
C1 O2 1.246(8) .
C1 C2A 1.498(13) .
C1 C2B 1.603(17) .
O1 Li2 1.947(11) 7_554
O1 Li1 2.022(12) 6_664
O2 Li1 1.931(11) 5_544
O2 Li2 1.965(12) 5_544
Li2 O3 1.913(12) 2_645
Li2 O1 1.947(11) 4_445
Li2 O2 1.965(12) 9_655
Li2 Li1 2.819(7) 9_654
Li2 Li1 3.046(17) .
Li2 Li1 3.110(15) 2_645
C3A C2A 1.259(11) .
C3A C4 1.480(13) .
C2B O5 1.35(2) .
C2B C3B 1.533(16) .
C3B C4 1.546(19) .
O3 C4 1.268(7) .
O3 Li1 1.905(12) .
O3 Li2 1.913(12) 3_765
Li1 O2 1.931(11) 9_655
Li1 O4 1.962(11) 5_545
Li1 O1 2.022(12) 8_645
Li1 Li2 2.819(7) 5_545
Li1 Li2 3.110(15) 3_765
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
O2 C1 O1 Li2 -131.0(8) . 7_554
C2A C1 O1 Li2 34.1(17) . 7_554
C2B C1 O1 Li2 60.0(13) . 7_554
O2 C1 O1 Li1 17.6(11) . 6_664
C2A C1 O1 Li1 -177.3(11) . 6_664
C2B C1 O1 Li1 -151.4(8) . 6_664
O1 C1 O2 Li1 -131.0(6) . 5_544
C2A C1 O2 Li1 61.9(11) . 5_544
C2B C1 O2 Li1 36.4(13) . 5_544
O1 C1 O2 Li2 29.5(10) . 5_544
C2A C1 O2 Li2 -137.7(9) . 5_544
C2B C1 O2 Li2 -163.1(9) . 5_544
C4 O4 Li2 O3 -79.1(8) . 2_645
Li1 O4 Li2 O3 113.0(5) 9_654 2_645
C4 O4 Li2 O1 165.5(4) . 4_445
Li1 O4 Li2 O1 -2.4(7) 9_654 4_445
C4 O4 Li2 O2 43.3(8) . 9_655
Li1 O4 Li2 O2 -124.6(4) 9_654 9_655
C4 O4 Li2 Li1 167.9(8) . 9_654
C4 O4 Li2 Li1 34.9(6) . .
Li1 O4 Li2 Li1 -133.0(4) 9_654 .
C4 O4 Li2 Li1 -44.9(10) . 2_645
Li1 O4 Li2 Li1 147.2(6) 9_654 2_645
C4 C3A C2A C1 175.6(19) . .
O1 C1 C2A C3A -1(2) . .
O2 C1 C2A C3A 166.0(15) . .
C2B C1 C2A C3A -65(2) . .
O1 C1 C2B O5 35.2(15) . .
O2 C1 C2B O5 -133.9(12) . .
C2A C1 C2B O5 164(3) . .
O1 C1 C2B C3B -94.6(11) . .
O2 C1 C2B C3B 96.3(11) . .
C2A C1 C2B C3B 34.1(17) . .
O5 C2B C3B C4 48.2(15) . .
C1 C2B C3B C4 178.5(14) . .
C4 O3 Li1 O2 56.2(7) . 9_655
Li2 O3 Li1 O2 -115.6(7) 3_765 9_655
C4 O3 Li1 O4 -76.4(9) . 5_545
Li2 O3 Li1 O4 111.8(6) 3_765 5_545
C4 O3 Li1 O1 -177.8(5) . 8_645
Li2 O3 Li1 O1 10.4(6) 3_765 8_645
C4 O3 Li1 Li2 -131.4(5) . 5_545
Li2 O3 Li1 Li2 56.8(5) 3_765 5_545
C4 O3 Li1 Li2 43.1(6) . .
Li2 O3 Li1 Li2 -128.7(5) 3_765 .
C4 O3 Li1 Li2 171.8(7) . 3_765
O3 Li2 Li1 O3 80.1(4) 2_645 .
O1 Li2 Li1 O3 -108.9(7) 4_445 .
O4 Li2 Li1 O3 -32.4(4) . .
O2 Li2 Li1 O3 160.3(4) 9_655 .
Li1 Li2 Li1 O3 -64.2(3) 9_654 .
Li1 Li2 Li1 O3 109.3(3) 2_645 .
O3 Li2 Li1 O2 -80.2(6) 2_645 9_655
O1 Li2 Li1 O2 90.8(5) 4_445 9_655
O4 Li2 Li1 O2 167.3(5) . 9_655
Li1 Li2 Li1 O2 135.5(4) 9_654 9_655
Li1 Li2 Li1 O2 -50.9(4) 2_645 9_655
O3 Li2 Li1 O4 -158.9(8) 2_645 5_545
O1 Li2 Li1 O4 12.1(7) 4_445 5_545
O4 Li2 Li1 O4 88.5(4) . 5_545
O2 Li2 Li1 O4 -78.8(7) 9_655 5_545
Li1 Li2 Li1 O4 56.8(6) 9_654 5_545
Li1 Li2 Li1 O4 -129.7(7) 2_645 5_545
O3 Li2 Li1 O1 -21.8(9) 2_645 8_645
O1 Li2 Li1 O1 149.2(7) 4_445 8_645
O4 Li2 Li1 O1 -134.4(8) . 8_645
O2 Li2 Li1 O1 58.3(7) 9_655 8_645
Li1 Li2 Li1 O1 -166.1(6) 9_654 8_645
Li1 Li2 Li1 O1 7.4(8) 2_645 8_645
O3 Li2 Li1 Li2 -111.7(10) 2_645 5_545
O1 Li2 Li1 Li2 59.3(11) 4_445 5_545
O4 Li2 Li1 Li2 135.8(7) . 5_545
O2 Li2 Li1 Li2 -31.5(9) 9_655 5_545
Li1 Li2 Li1 Li2 104.0(9) 9_654 5_545
Li1 Li2 Li1 Li2 -82.5(10) 2_645 5_545
O3 Li2 Li1 Li2 52.9(4) 2_645 3_765
O1 Li2 Li1 Li2 -136.0(6) 4_445 3_765
O4 Li2 Li1 Li2 -59.6(5) . 3_765
O2 Li2 Li1 Li2 133.1(5) 9_655 3_765
Li1 Li2 Li1 Li2 -91.3(3) 9_654 3_765
Li1 Li2 Li1 Li2 82.2(3) 2_645 3_765
Li1 O3 C4 O4 -34.2(9) . .
Li2 O3 C4 O4 136.1(6) 3_765 .
Li1 O3 C4 C3A 138.1(10) . .
Li2 O3 C4 C3A -51.6(11) 3_765 .
Li1 O3 C4 C3B 159.9(10) . .
Li2 O3 C4 C3B -29.8(13) 3_765 .
Li2 O4 C4 O3 -18.1(10) . .
Li1 O4 C4 O3 141.6(7) 9_654 .
Li2 O4 C4 C3A 170.6(12) . .
Li1 O4 C4 C3A -29.8(16) 9_654 .
Li2 O4 C4 C3B 150.1(9) . .
Li1 O4 C4 C3B -50.3(12) 9_654 .
C2A C3A C4 O3 -168.4(15) . .
C2A C3A C4 O4 4(2) . .
C2A C3A C4 C3B 59(2) . .
C2B C3B C4 O3 -100.1(11) . .
C2B C3B C4 O4 92.4(11) . .
C2B C3B C4 C3A -42(2) . .
