#------------------------------------------------------------------------------
#$Date: 2019-11-17 07:33:34 +0100 (dom 17 de nov de 2019) $
#$Revision: 228880 $
#$URL: svn://www.crystallography.net/cod/cif/7/23/08/7230808.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_7230808
loop_
_publ_author_name
'Lucaioli, Paolo'
'Nauha, Elisa'
'Gimondi, Ilaria'
'Price, Louise S.'
'Guo, Rui'
'Iuzzolino, Luca'
'Singh, Ishwar'
'Salvalaglio, Matteo'
'Price, Sarah L.'
'Blagden, Nicholas'
_publ_section_title
;
 Serendipitous isolation of a disappearing conformational polymorph of
 succinic acid challenges computational polymorph prediction
;
_journal_issue                   28
_journal_name_full               CrystEngComm
_journal_page_first              3971
_journal_paper_doi               10.1039/C8CE00625C
_journal_volume                  20
_journal_year                    2018
_chemical_formula_moiety         'C4 H6 O4'
_chemical_formula_sum            'C4 H6 O4'
_chemical_formula_weight         118.09
_chemical_name_common            'succinic acid'
_chemical_name_systematic        '1,4-Butanedioic acid'
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-04-11 deposited with the CCDC.
2018-05-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.374(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.7015(5)
_cell_length_b                   8.4154(8)
_cell_length_c                   10.3538(8)
_cell_measurement_reflns_used    2129
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.09
_cell_measurement_theta_min      4.32
_cell_volume                     496.77(7)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker D8 Venture Photon'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1089
_diffrn_reflns_av_unetI/netI     0.0379
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            11388
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.202
_diffrn_reflns_theta_min         3.936
_exptl_absorpt_coefficient_mu    0.145
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6938
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.579
_exptl_crystal_description       Needle
_exptl_crystal_F_000             248
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Methanol'
_exptl_crystal_size_max          0.143
_exptl_crystal_size_mid          0.077
_exptl_crystal_size_min          0.023
_refine_diff_density_max         0.317
_refine_diff_density_min         -0.220
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     40
_refine_ls_number_reflns         671
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0734
_refine_ls_R_factor_gt           0.0472
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0251P)²+0.6686P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0818
_refine_ls_wR_factor_ref         0.0887
_reflns_Friedel_coverage         0.000
_reflns_number_gt                509
_reflns_number_total             671
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8ce00625c2.cif
_cod_data_source_block           mo_PL_LLOH14_0m
_cod_depositor_comments
'Adding full bibliography for 7230808--7230809.cif.'
_cod_database_code               7230808
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.980
_shelx_estimated_absorpt_t_max   0.997
_shelx_res_file
;

    mo_PL_LLOH14_0m.res created by SHELXL-2014/7


TITL mo_PL_LLOH14_triclinic_0m_a.res in C2/c
REM Old TITL mo_PL_LLOH14_triclinic_0m in C2/c
REM SHELXT solution in C2/c
REM R1 0.110,  Rweak 0.015,  Alpha 0.034,  Orientation as input
REM Formula found by SHELXT:  C2 O2
TITL mo_PL_LLOH14_triclinic_0m in C2/c
CELL 0.71073   5.70150   8.41540  10.35380  90.0000  90.3737  90.0000
ZERR    4.00   0.00050   0.00080   0.00080   0.0000   0.0032   0.0000
LATT  7
SYMM -X, Y, 0.5-Z
SFAC C H O
UNIT 16 24 16
TEMP -100.150
SIZE 0.023 0.077 0.143
ACTA
CONF
HTAB
EQIV $1 -x+3/2, -y+1/2, -z+1
HTAB O1 O2_$1
EQIV $2 -x+2, y, -z+1/2
HTAB C2 O1_$2
L.S. 10
BOND $H
LIST 6
FMAP 2
PLAN 5
WGHT    0.025100    0.668600
FVAR       0.29482
O1    3    0.897867    0.394896    0.400514    11.00000    0.01636    0.02789 =
         0.02269    0.00742   -0.00379   -0.00207
H1    2    0.922103    0.322643    0.463368    11.00000   -1.20000
O2    3    0.522118    0.323096    0.418198    11.00000    0.01820    0.02377 =
         0.02554    0.00852   -0.00212   -0.00327
C1    1    0.673784    0.407253    0.370676    11.00000    0.01751    0.01503 =
         0.01182   -0.00489    0.00022   -0.00137
C2    1    0.625622    0.536588    0.274903    11.00000    0.01852    0.01497 =
         0.01596   -0.00093    0.00070   -0.00185
AFIX  23
H2A   2    0.733170    0.524245    0.200894    11.00000   -1.20000
H2B   2    0.659218    0.640511    0.315836    11.00000   -1.20000
AFIX   0
HKLF 4

REM  mo_PL_LLOH14_triclinic_0m in C2/c
REM R1 =  0.0472 for     509 Fo > 4sig(Fo)  and  0.0734 for all     671 data
REM     40 parameters refined using      0 restraints

END

WGHT      0.0251      0.6686

REM Instructions for potential hydrogen bonds
HTAB O1 O2_$1
HTAB C2 O1_$2

REM Highest difference peak  0.317,  deepest hole -0.220,  1-sigma level  0.058
Q1    1   0.5000  0.5314  0.2500  10.50000  0.05    0.32
Q2    1   0.6746  0.4525  0.3017  11.00000  0.05    0.21
Q3    1   0.5977  0.3186  0.5011  11.00000  0.05    0.20
Q4    1   0.6762  0.4958  0.3404  11.00000  0.05    0.19
Q5    1   0.9636  0.6786  0.2442  11.00000  0.05    0.17
;
_shelx_res_checksum              11145
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
O1 O 0.89787(19) 0.39490(15) 0.40051(11) 0.0223(3) Uani 1 1 d . .
H1 H 0.922(3) 0.323(2) 0.463(2) 0.027 Uiso 1 1 d . U
O2 O 0.52212(19) 0.32310(14) 0.41820(11) 0.0225(3) Uani 1 1 d . .
C1 C 0.6738(3) 0.40725(18) 0.37068(14) 0.0148(3) Uani 1 1 d . .
C2 C 0.6256(3) 0.53659(19) 0.27490(15) 0.0165(3) Uani 1 1 d . .
H2A H 0.7332 0.5242 0.2009 0.020 Uiso 1 1 calc R U
H2B H 0.6592 0.6405 0.3158 0.020 Uiso 1 1 calc R U
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O1 0.0164(6) 0.0279(7) 0.0227(6) 0.0074(5) -0.0038(5) -0.0021(5)
O2 0.0182(6) 0.0238(6) 0.0255(6) 0.0085(5) -0.0021(5) -0.0033(5)
C1 0.0175(7) 0.0150(7) 0.0118(7) -0.0049(6) 0.0002(5) -0.0014(6)
C2 0.0185(8) 0.0150(8) 0.0160(7) -0.0009(6) 0.0007(6) -0.0019(6)
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'
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 O1 H1 111.5(12) . .
O2 C1 O1 123.18(15) . .
O2 C1 C2 124.08(14) . .
O1 C1 C2 112.74(13) . .
C1 C2 C2 113.17(12) . 2_655
C1 C2 H2A 108.9 . .
C2 C2 H2A 108.9 2_655 .
C1 C2 H2B 108.9 . .
C2 C2 H2B 108.9 2_655 .
H2A C2 H2B 107.8 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O1 C1 1.3166(18) .
O1 H1 0.90(2) .
O2 C1 1.2235(19) .
C1 C2 1.497(2) .
C2 C2 1.519(3) 2_655
C2 H2A 0.9900 .
C2 H2B 0.9900 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1 O2 0.90(2) 1.76(2) 2.6619(16) 177.5(19) 7_656
C2 H2A O1 0.99 2.60 3.4880(19) 149.8 2_755
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_4
O2 C1 C2 C2 -9.4(2) 2_655
O1 C1 C2 C2 171.66(14) 2_655
