#------------------------------------------------------------------------------
#$Date: 2020-10-14 03:25:33 +0200 (Wed 14 de Oct de 2020) $
#$Revision: 258352 $
#$URL: svn://www.crystallography.net/cod/cif/7/24/13/7241391.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_7241391
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                   6.5678(8)
_cell_length_b                   6.0983(7)
_cell_length_c                   7.8715(8)
_cell_measurement_reflns_used    499
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.6886
_cell_measurement_theta_min      4.2181
_cell_volume                     315.27(6)
_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      298(2)
_diffrn_detector_area_resol_mean 15.9821
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.886
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0183526000
_diffrn_orient_matrix_UB_12      -0.0690658000
_diffrn_orient_matrix_UB_13      0.0709286000
_diffrn_orient_matrix_UB_21      0.0678508000
_diffrn_orient_matrix_UB_22      0.0790850000
_diffrn_orient_matrix_UB_23      0.0340474000
_diffrn_orient_matrix_UB_31      -0.0820569000
_diffrn_orient_matrix_UB_32      0.0498960000
_diffrn_orient_matrix_UB_33      0.0440999000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0077
_diffrn_reflns_av_unetI/netI     0.0080
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.886
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            872
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.886
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.765
_diffrn_reflns_theta_min         5.180
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.196
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79823
_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    1.897
_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         0.432
_refine_diff_density_min         -0.131
_refine_diff_density_rms         0.042
_refine_ls_extinction_coef       0.162(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     33
_refine_ls_number_reflns         367
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0281
_refine_ls_R_factor_gt           0.0254
_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)+(0.0342P)²+0.0896P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0661
_refine_ls_wR_factor_ref         0.0671
_reflns_Friedel_coverage         0.000
_reflns_number_gt                351
_reflns_number_total             367
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0ce01080d2.cif
_cod_data_source_block           alpha_C2_298
_cod_database_code               7241391
_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   0.919
_shelx_res_file
;
TITL BKS-C2-ORTHO-298 in Pbca #61
CELL 0.71073 6.56781 6.09829 7.87145 90 90 90
ZERR 4 0.00083 0.00071 0.0008 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 25(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-298/C2-I-298.hkl</H
REM KL>

WGHT    0.034200    0.089600
EXTI    0.162308
FVAR      18.02687
O2    3    0.470898    0.043192    0.783473    11.00000    0.03622    0.02694 =
         0.01678    0.00165   -0.00093    0.00629
C1    1    0.443144    0.084418    0.944842    11.00000    0.01805    0.01795 =
         0.01871    0.00095   -0.00109   -0.00189
O1    3    0.344292    0.232113    1.005270    11.00000    0.02782    0.02407 =
         0.02401   -0.00154   -0.00156    0.00741
H2    2    0.418974    0.144732    0.721298    11.00000    0.04854
HKLF 4

REM  BKS-C2-ORTHO-298 in Pbca #61
REM R1 =  0.0254 for     351 Fo > 4sig(Fo)  and  0.0281 for all     367 data
REM     33 parameters refined using      0 restraints

END

WGHT      0.0342      0.0896

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

REM Highest difference peak  0.432,  deepest hole -0.131,  1-sigma level  0.042
Q1    1   0.5000  0.0000  1.0000  10.50000  0.05    0.43
Q2    1   0.3565  0.2176  1.1136  11.00000  0.05    0.13
Q3    1   0.3465  0.1181  0.9820  11.00000  0.05    0.13
Q4    1   0.4438  0.2037  0.9721  11.00000  0.05    0.12
Q5    1   0.4615  0.0701  0.8674  11.00000  0.05    0.12
Q6    1   0.4792 -0.0866  0.7641  11.00000  0.05    0.10
Q7    1   0.3292  0.3582  0.9498  11.00000  0.05    0.10
Q8    1   0.5297 -0.1524  0.8147  11.00000  0.05    0.08
Q9    1   0.1891  0.2532  0.7350  11.00000  0.05    0.08
Q10   1   0.3900  0.2809  1.0065  11.00000  0.05    0.07
Q11   1   0.2947  0.3803  1.0612  11.00000  0.05    0.07
Q12   1   0.3712  0.2459  0.8978  11.00000  0.05    0.07
Q13   1   0.2260  0.0315  1.1031  11.00000  0.05    0.07
Q14   1   0.2934  0.3172  0.7248  11.00000  0.05    0.06
Q15   1   0.2666  0.0379  1.0418  11.00000  0.05    0.05
Q16   1   0.2564  0.3165  0.8388  11.00000  0.05    0.05
Q17   1   0.5427  0.4415  0.9572  11.00000  0.05    0.05
Q18   1   0.6971 -0.0260  0.7396  11.00000  0.05    0.05
Q19   1   0.5665  0.2832  0.8746  11.00000  0.05    0.04
Q20   1   0.3291 -0.1371  0.8024  11.00000  0.05    0.04
;
_shelx_res_checksum              26345
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 0.47090(13) 0.04319(12) 0.78347(9) 0.0266(3) Uani 1 1 d . . . . .
C1 C 0.44314(14) 0.08442(14) 0.94484(11) 0.0182(3) Uani 1 1 d . . . . .
O1 O 0.34429(12) 0.23211(12) 1.00527(8) 0.0253(3) Uani 1 1 d . . . . .
H2 H 0.419(3) 0.145(3) 0.721(2) 0.049(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 0.0362(5) 0.0269(4) 0.0168(4) 0.0016(3) -0.0009(3) 0.0063(3)
C1 0.0181(5) 0.0179(5) 0.0187(5) 0.0010(3) -0.0011(3) -0.0019(3)
O1 0.0278(4) 0.0241(4) 0.0240(4) -0.0015(3) -0.0016(3) 0.0074(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 111.0(11) . . ?
O2 C1 C1 110.58(10) . 5_657 ?
O1 C1 O2 126.93(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 1.3076(12) . ?
O2 H2 0.860(16) . ?
C1 C1 1.5401(17) 5_657 ?
C1 O1 1.2079(11) . ?
