#------------------------------------------------------------------------------
#$Date: 2020-10-14 03:25:33 +0200 (Wed 14 de Oct de 2020) $
#$Revision: 258352 $
#$URL: svn://www.crystallography.net/cod/cif/7/24/13/7241392.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_7241392
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                   6.5224(11)
_cell_length_b                   6.0741(8)
_cell_length_c                   7.8268(12)
_cell_measurement_reflns_used    499
_cell_measurement_temperature    228(2)
_cell_measurement_theta_max      28.8747
_cell_measurement_theta_min      6.0737
_cell_volume                     310.08(8)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_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      228(2)
_diffrn_detector_area_resol_mean 15.9821
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.852
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0184795000
_diffrn_orient_matrix_UB_12      0.0692266000
_diffrn_orient_matrix_UB_13      0.0714918000
_diffrn_orient_matrix_UB_21      -0.0677230000
_diffrn_orient_matrix_UB_22      -0.0799642000
_diffrn_orient_matrix_UB_23      0.0344171000
_diffrn_orient_matrix_UB_31      0.0831395000
_diffrn_orient_matrix_UB_32      -0.0497746000
_diffrn_orient_matrix_UB_33      0.0440157000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0068
_diffrn_reflns_av_unetI/netI     0.0107
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.852
_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            823
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.852
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.914
_diffrn_reflns_theta_min         6.079
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.199
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84108
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
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    1.929
_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         0.492
_refine_diff_density_min         -0.176
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     32
_refine_ls_number_reflns         352
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0299
_refine_ls_R_factor_gt           0.0284
_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)+(0.0349P)²+0.1079P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0683
_refine_ls_wR_factor_ref         0.0692
_reflns_Friedel_coverage         0.000
_reflns_number_gt                339
_reflns_number_total             352
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0ce01080d2.cif
_cod_data_source_block           alpha_C2_228
_cod_database_code               7241392
_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   0.928
_shelx_estimated_absorpt_t_min   0.918
_shelx_res_file
;
TITL BKS-C2-ORTHO-228 in Pbca #61
CELL 0.71073 6.5224 6.07412 7.82681 90 90 90
ZERR 4 0.00112 0.0008 0.00124 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 -45(3)
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-228/C2-I-228.hkl</H
REM KL>

WGHT    0.034900    0.107900
FVAR      17.35754
O2    3    0.470716    0.042860    0.782522    11.00000    0.02637    0.01887 =
         0.01228    0.00118   -0.00084    0.00437
C1    1    0.442830    0.084396    0.944536    11.00000    0.01220    0.01237 =
         0.01429    0.00079   -0.00092   -0.00200
O1    3    0.342764    0.232661    1.005198    11.00000    0.01966    0.01657 =
         0.01832   -0.00128   -0.00114    0.00526
H2    2    0.413120    0.146218    0.718692    11.00000    0.04427
HKLF 4

REM  BKS-C2-ORTHO-228 in Pbca #61
REM R1 =  0.0284 for     339 Fo > 4sig(Fo)  and  0.0299 for all     352 data
REM     32 parameters refined using      0 restraints

END

WGHT      0.0349      0.1079

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

REM Highest difference peak  0.492,  deepest hole -0.176,  1-sigma level  0.057
Q1    1   0.5000  0.0000  1.0000  10.50000  0.05    0.49
Q2    1   0.3609  0.2141  1.1331  11.00000  0.05    0.17
Q3    1   0.4502  0.0670  0.8716  11.00000  0.05    0.16
Q4    1   0.2308  0.0041  1.0009  11.00000  0.05    0.15
Q5    1   0.4827  0.2666  0.7631  11.00000  0.05    0.13
Q6    1   0.2584  0.0333  1.0926  11.00000  0.05    0.11
Q7    1   0.3527  0.0971  0.9809  11.00000  0.05    0.10
Q8    1   0.4835  0.2607  0.6274  11.00000  0.05    0.10
Q9    1   0.6554  0.2297  0.7868  11.00000  0.05    0.08
Q10   1   0.4517  0.1756  0.9671  11.00000  0.05    0.07
Q11   1   0.3618  0.4688  0.8947  11.00000  0.05    0.07
Q12   1   0.4522 -0.0499  0.5610  11.00000  0.05    0.07
Q13   1   0.5687  0.0764  0.5418  11.00000  0.05    0.06
Q14   1   0.3331 -0.2008  0.8135  11.00000  0.05    0.05
Q15   1   0.3692 -0.0378  0.8342  11.00000  0.05    0.03
Q16   1   0.3439  0.1424  0.7244  11.00000  0.05    0.02
Q17   1   0.5929  0.2548  0.9951  11.00000  0.05    0.02
Q18   1   0.2466  0.1140  0.7971  11.00000  0.05    0.01
Q19   1   0.3966 -0.1285  0.9184  11.00000  0.05    0.01
;
_shelx_res_checksum              45152
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 0.47072(13) 0.04286(13) 0.78252(10) 0.0192(3) Uani 1 1 d . . . . .
C1 C 0.44283(14) 0.08440(15) 0.94454(12) 0.0130(3) Uani 1 1 d . . . . .
O1 O 0.34276(12) 0.23266(12) 1.00520(9) 0.0182(3) Uani 1 1 d . . . . .
H2 H 0.413(3) 0.146(3) 0.719(2) 0.044(5) 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 0.0264(5) 0.0189(4) 0.0123(4) 0.0012(3) -0.0008(3) 0.0044(3)
C1 0.0122(4) 0.0124(5) 0.0143(5) 0.0008(4) -0.0009(4) -0.0020(3)
O1 0.0197(4) 0.0166(4) 0.0183(4) -0.0013(3) -0.0011(3) 0.0053(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 110.6(11) . . ?
O2 C1 C1 110.62(10) . 5_657 ?
O1 C1 O2 126.90(9) . . ?
O1 C1 C1 122.48(11) . 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 0.886(17) . ?
C1 C1 1.5366(19) 5_657 ?
C1 O1 1.2093(12) . ?
