#------------------------------------------------------------------------------
#$Date: 2020-10-14 04:25:33 +0300 (Wed, 14 Oct 2020) $
#$Revision: 258352 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/13/7241393.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_7241393
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                   6.4914(5)
_cell_length_b                   6.0556(5)
_cell_length_c                   7.8020(5)
_cell_measurement_reflns_used    604
_cell_measurement_temperature    156(2)
_cell_measurement_theta_max      28.9979
_cell_measurement_theta_min      4.5953
_cell_volume                     306.69(4)
_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 (Sheldrick, 2008)'
_diffrn_ambient_temperature      156(2)
_diffrn_detector_area_resol_mean 15.9821
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.853
_diffrn_measurement_details
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -25.00   18.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.4960  -99.0000    0.0000 43

#__ type_ start__ end____ width___ exp.time_
  2 omega  -82.00  -43.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.4960  -57.0000  -90.0000 39

#__ type_ start__ end____ width___ exp.time_
  3 omega  -35.00   15.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.4960  -89.0000   72.0000 50

#__ type_ start__ end____ width___ exp.time_
  4 omega  -48.00   31.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.4960   77.0000   30.0000 79
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0186087000
_diffrn_orient_matrix_UB_12      -0.0692874000
_diffrn_orient_matrix_UB_13      -0.0716650000
_diffrn_orient_matrix_UB_21      -0.0677724000
_diffrn_orient_matrix_UB_22      0.0803306000
_diffrn_orient_matrix_UB_23      -0.0345966000
_diffrn_orient_matrix_UB_31      0.0837316000
_diffrn_orient_matrix_UB_32      0.0496731000
_diffrn_orient_matrix_UB_33      -0.0440264000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0076
_diffrn_reflns_av_unetI/netI     0.0107
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.853
_diffrn_reflns_limit_h_max       5
_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       -9
_diffrn_reflns_number            1063
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.853
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         29.053
_diffrn_reflns_theta_min         5.227
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.201
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87395
_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    1.950
_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         0.466
_refine_diff_density_min         -0.208
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     32
_refine_ls_number_reflns         355
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0273
_refine_ls_R_factor_gt           0.0259
_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)+(0.0353P)²+0.1197P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0661
_refine_ls_wR_factor_ref         0.0672
_reflns_Friedel_coverage         0.000
_reflns_number_gt                341
_reflns_number_total             355
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0ce01080d2.cif
_cod_data_source_block           alpha_C2_156
_cod_database_code               7241393
_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   0.927
_shelx_estimated_absorpt_t_min   0.917
_shelx_res_file
;
TITL BKS-C2-ORTHO-156 in Pbca #61
CELL 0.71073 6.4914 6.05558 7.80201 90 90 90
ZERR 4 0.00052 0.00049 0.00049 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 -117(2)
REM reset to Pbca #61
BOND
htab
bond $h
MORE -1
fmap 2
acta 50
CONF
REM <HKL>D:/desktop-27-06-2013/C2-ORTHO/olex2_BKS-C2-ORTHO-156/C2-I-156.hkl</H
REM KL>

WGHT    0.035300    0.119700
FVAR      25.60383
O2    3    0.470665    0.042523    0.781647    11.00000    0.01808    0.01433 =
         0.00808    0.00090   -0.00059    0.00323
C1    1    0.442207    0.084447    0.944275    11.00000    0.00843    0.00975 =
         0.01007    0.00066   -0.00063   -0.00201
O1    3    0.341315    0.233086    1.005075    11.00000    0.01351    0.01263 =
         0.01255   -0.00100   -0.00076    0.00312
H2    2    0.413297    0.144851    0.717923    11.00000    0.03270
HKLF 4

REM  BKS-C2-ORTHO-156 in Pbca #61
REM R1 =  0.0259 for     341 Fo > 4sig(Fo)  and  0.0273 for all     355 data
REM     32 parameters refined using      0 restraints

END

WGHT      0.0353      0.1197

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

REM Highest difference peak  0.466,  deepest hole -0.208,  1-sigma level  0.052
Q1    1   0.5000  0.0000  1.0000  10.50000  0.05    0.47
Q2    1   0.4539  0.2025  0.9821  11.00000  0.05    0.14
Q3    1   0.4672  0.0676  0.8633  11.00000  0.05    0.13
Q4    1   0.4244 -0.0732  0.5462  11.00000  0.05    0.11
Q5    1   0.3651  0.2442  1.1135  11.00000  0.05    0.11
Q6    1   0.5624  0.0800  0.5326  11.00000  0.05    0.10
Q7    1   0.3000 -0.0116  0.6416  11.00000  0.05    0.10
Q8    1   0.3944  0.4677  0.9121  11.00000  0.05    0.10
Q9    1   0.5003  0.3588  0.9180  11.00000  0.05    0.10
Q10   1   0.3374  0.1125  1.1512  11.00000  0.05    0.09
Q11   1   0.6578 -0.0716  0.6945  11.00000  0.05    0.09
Q12   1   0.3549  0.3851  0.9252  11.00000  0.05    0.09
Q13   1   0.2090  0.2537  0.7398  11.00000  0.05    0.08
Q14   1   0.1635  0.1370  1.0942  11.00000  0.05    0.07
Q15   1   0.4405 -0.1342  0.6833  11.00000  0.05    0.07
Q16   1   0.5069  0.2553  1.0688  11.00000  0.05    0.07
Q17   1   0.4514  0.3156  0.7774  11.00000  0.05    0.07
Q18   1   0.3201 -0.1533  0.8228  11.00000  0.05    0.06
Q19   1   0.2126  0.2932  0.8427  11.00000  0.05    0.06
Q20   1   0.4012 -0.0666  0.7865  11.00000  0.05    0.06
;
_shelx_res_checksum              70875
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 0.47066(11) 0.04252(12) 0.78165(9) 0.0135(2) Uani 1 1 d . . . . .
C1 C 0.44221(14) 0.08445(14) 0.94428(11) 0.0094(3) Uani 1 1 d . . . . .
O1 O 0.34131(11) 0.23309(12) 1.00507(8) 0.0129(2) Uani 1 1 d . . . . .
H2 H 0.413(3) 0.145(3) 0.718(2) 0.033(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 0.0181(4) 0.0143(4) 0.0081(4) 0.0009(2) -0.0006(3) 0.0032(3)
C1 0.0084(4) 0.0097(4) 0.0101(5) 0.0007(3) -0.0006(3) -0.0020(3)
O1 0.0135(4) 0.0126(4) 0.0126(4) -0.0010(2) -0.0008(3) 0.0031(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 110.7(10) . . ?
O2 C1 C1 110.53(10) . 5_657 ?
O1 C1 O2 126.98(9) . . ?
O1 C1 C1 122.49(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 1.3071(11) . ?
O2 H2 0.877(16) . ?
C1 C1 1.5379(18) 5_657 ?
C1 O1 1.2100(11) . ?
