#------------------------------------------------------------------------------
#$Date: 2020-10-14 03:25:33 +0200 (Wed 14 de Oct de 2020) $
#$Revision: 258352 $
#$URL: svn://www.crystallography.net/cod/cif/7/24/13/7241395.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_7241395
loop_
_publ_author_name
'Bhattacharya, Suman'
_publ_section_title
;
 Thermal expansion and dimensionality of the hydrogen bond network: a case
 study on dimorphic Oxalic acid
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D0CE01080D
_journal_year                    2020
_chemical_formula_moiety         'C2 H2 O4'
_chemical_formula_sum            'C2 H2 O4'
_chemical_formula_weight         90.04
_chemical_name_systematic        'Oxalic acid alpha polymorph'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2014-02-10
_audit_creation_method
;
Olex2 1.2
(compiled 2013.11.15 svn.r2834 for OlexSys, GUI svn.r4715)
;
_audit_update_record
;
2020-07-19 deposited with the CCDC.	2020-10-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.5399(11)
_cell_length_b                   6.0841(7)
_cell_length_c                   7.8385(12)
_cell_measurement_reflns_used    484
_cell_measurement_temperature    264(2)
_cell_measurement_theta_max      28.8137
_cell_measurement_theta_min      6.0611
_cell_volume                     311.89(8)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS-2013 (Sheldrick, 2008)'
_diffrn_ambient_temperature      264(2)
_diffrn_detector_area_resol_mean 15.9821
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.857
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0183291000
_diffrn_orient_matrix_UB_12      0.0690967000
_diffrn_orient_matrix_UB_13      0.0713855000
_diffrn_orient_matrix_UB_21      -0.0677033000
_diffrn_orient_matrix_UB_22      -0.0796934000
_diffrn_orient_matrix_UB_23      0.0343378000
_diffrn_orient_matrix_UB_31      0.0827845000
_diffrn_orient_matrix_UB_32      -0.0499024000
_diffrn_orient_matrix_UB_33      0.0439356000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0072
_diffrn_reflns_av_unetI/netI     0.0108
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.857
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            834
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.857
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.856
_diffrn_reflns_theta_min         6.068
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.198
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86907
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.917
_exptl_crystal_description       block
_exptl_crystal_F_000             184
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.38
_refine_diff_density_max         0.422
_refine_diff_density_min         -0.149
_refine_diff_density_rms         0.043
_refine_ls_extinction_coef       0.140(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     33
_refine_ls_number_reflns         354
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.122
_refine_ls_R_factor_all          0.0277
_refine_ls_R_factor_gt           0.0263
_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)+(0.0338P)²+0.0746P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0644
_refine_ls_wR_factor_ref         0.0652
_reflns_Friedel_coverage         0.000
_reflns_number_gt                340
_reflns_number_total             354
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0ce01080d2.cif
_cod_data_source_block           alpha_C2_264
_cod_database_code               7241395
_shelxl_version_number           2013-4
_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_max   0.929
_shelx_estimated_absorpt_t_min   0.918
_shelx_res_file
;
TITL BKS-C2-ORTHO-264 in Pbca #61
CELL 0.71073 6.53995 6.08414 7.83847 90 90 90
ZERR 4 0.00106 0.00073 0.00116 0 0 0
LATT 1
SYMM 0.5-X,-Y,0.5+Z
SYMM 0.5+X,0.5-Y,-Z
SYMM -X,0.5+Y,0.5-Z

SFAC C H O
UNIT 8 8 16

L.S. 4
PLAN  20
SIZE 0.44 0.4 0.38
TEMP -9(2)
htab
bond $h
REM reset to Pbca #61
BOND
MORE -1
fmap 2
acta 50
CONF
REM <HKL>D:/desktop-27-06-2013/C2-ORTHO/olex2_BKS-C2-ORTHO-264/C2-I-264.hkl</H
REM KL>

WGHT    0.033800    0.074600
EXTI    0.139593
FVAR      17.94627
O2    3    0.470739    0.042995    0.782943    11.00000    0.03120    0.02289 =
         0.01470    0.00142   -0.00085    0.00534
C1    1    0.443035    0.084372    0.944739    11.00000    0.01539    0.01518 =
         0.01663    0.00063   -0.00115   -0.00198
O1    3    0.343550    0.232389    1.005215    11.00000    0.02411    0.02004 =
         0.02150   -0.00141   -0.00120    0.00631
H2    2    0.412856    0.144069    0.718434    11.00000    0.04451
HKLF 4

REM  BKS-C2-ORTHO-264 in Pbca #61
REM R1 =  0.0263 for     340 Fo > 4sig(Fo)  and  0.0277 for all     354 data
REM     33 parameters refined using      0 restraints

END

WGHT      0.0338      0.0746

REM Instructions for potential hydrogen bonds
EQIV $1 x, -y+1/2, z-1/2
HTAB O2 O1_$1

REM Highest difference peak  0.422,  deepest hole -0.149,  1-sigma level  0.043
Q1    1   0.5000  0.0000  1.0000  10.50000  0.05    0.42
Q2    1   0.3441  0.2229  1.1271  11.00000  0.05    0.18
Q3    1   0.4560  0.0662  0.8663  11.00000  0.05    0.17
Q4    1   0.2579  0.2656  0.9193  11.00000  0.05    0.10
Q5    1   0.4394  0.1861  0.9687  11.00000  0.05    0.09
Q6    1   0.5488  0.2650  0.6349  11.00000  0.05    0.08
Q7    1   0.6588  0.1015  0.8234  11.00000  0.05    0.07
Q8    1   0.3814  0.1418  0.9764  11.00000  0.05    0.07
Q9    1   0.3830 -0.0746  0.8051  11.00000  0.05    0.07
Q10   1   0.5648  0.2801  0.8607  11.00000  0.05    0.07
Q11   1   0.4057 -0.1002  0.7527  11.00000  0.05    0.06
Q12   1   0.6133  0.0003  0.6365  11.00000  0.05    0.06
Q13   1   0.3201 -0.0064  0.6454  11.00000  0.05    0.05
Q14   1   0.5295  0.0373  0.6378  11.00000  0.05    0.05
Q15   1   0.4662  0.3428  0.8966  11.00000  0.05    0.05
Q16   1   0.3131  0.3605  1.0944  11.00000  0.05    0.05
Q17   1   0.2025  0.2368  0.8254  11.00000  0.05    0.05
Q18   1   0.2374  0.0986  0.7989  11.00000  0.05    0.04
Q19   1   0.4092  0.0751  0.7356  11.00000  0.05    0.04
Q20   1   0.4536 -0.0573  0.5748  11.00000  0.05    0.04
;
_shelx_res_checksum              22247
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -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
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O2 O 0.47074(12) 0.04300(12) 0.78294(9) 0.0229(3) Uani 1 1 d . . . . .
C1 C 0.44304(14) 0.08437(14) 0.94474(12) 0.0157(3) Uani 1 1 d . . . . .
O1 O 0.34355(11) 0.23239(12) 1.00522(8) 0.0219(3) Uani 1 1 d . . . . .
H2 H 0.413(3) 0.144(2) 0.7184(19) 0.045(4) Uiso 1 1 d . . . . .
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
O2 0.0312(5) 0.0229(4) 0.0147(4) 0.0014(3) -0.0008(3) 0.0053(3)
C1 0.0154(5) 0.0152(4) 0.0166(5) 0.0006(3) -0.0012(4) -0.0020(3)
O1 0.0241(4) 0.0200(4) 0.0215(4) -0.0014(2) -0.0012(3) 0.0063(3)
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
_geom_angle_publ_flag
C1 O2 H2 111.3(10) . . ?
O2 C1 C1 110.59(10) . 5_657 ?
O1 C1 O2 126.85(9) . . ?
O1 C1 C1 122.56(10) . 5_657 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O2 C1 1.3056(12) . ?
O2 H2 0.882(16) . ?
C1 C1 1.5362(17) 5_657 ?
C1 O1 1.2079(11) . ?
