# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_alpha_C2_298
_database_code_depnum_ccdc_archive 'CCDC 1854356'
loop_
_audit_author_name
_audit_author_address
'Suman Bhattacharya'
;Department of Chemistry, Pondicherry University
India
;
_audit_update_record             
;
2020-07-19 deposited with the CCDC.	2020-10-13 downloaded from the CCDC.
;
_audit_creation_date             2014-02-10
_audit_creation_method           
;
Olex2 1.2
(compiled 2013.11.15 svn.r2834 for OlexSys, GUI svn.r4715)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        'Oxalic acid alpha polymorph'
_chemical_formula_moiety         'C2 H2 O4'
_chemical_formula_sum            'C2 H2 O4'
_chemical_formula_weight         90.04
_chemical_melting_point          ?

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'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'
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'

_cell_length_a                   6.5678(8)
_cell_length_b                   6.0983(7)
_cell_length_c                   7.8715(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     315.27(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    499
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.6886
_cell_measurement_theta_min      4.2181
_shelx_estimated_absorpt_T_max   0.929
_shelx_estimated_absorpt_T_min   0.919
_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_density_meas      ?
_exptl_crystal_density_method    ?
_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
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_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_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_source                   'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                351
_reflns_number_total             367
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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)'
_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_R_factor_all          0.0281
_refine_ls_R_factor_gt           0.0254
_refine_ls_restrained_S_all      1.105
_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
_refine_special_details          
;
Hydrogen atoms of the carboxylic acid 
group have been refined isostropically.
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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) . ?

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 ?

_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
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_alpha_C2_228
_database_code_depnum_ccdc_archive 'CCDC 1854358'
loop_
_audit_author_name
_audit_author_address
'Suman Bhattacharya'
;Department of Chemistry, Pondicherry University
India
;
_audit_update_record             
;
2020-07-19 deposited with the CCDC.	2020-10-13 downloaded from the CCDC.
;
_audit_creation_date             2014-02-10
_audit_creation_method           
;
Olex2 1.2
(compiled 2013.11.15 svn.r2834 for OlexSys, GUI svn.r4715)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        'Oxalic acid alpha polymorph'
_chemical_formula_moiety         'C2 H2 O4'
_chemical_formula_sum            'C2 H2 O4'
_chemical_formula_weight         90.04
_chemical_melting_point          ?

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'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'
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'

_cell_length_a                   6.5224(11)
_cell_length_b                   6.0741(8)
_cell_length_c                   7.8268(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     310.08(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    499
_cell_measurement_temperature    228(2)
_cell_measurement_theta_max      28.8747
_cell_measurement_theta_min      6.0737
_shelx_estimated_absorpt_T_max   0.928
_shelx_estimated_absorpt_T_min   0.918
_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_density_meas      ?
_exptl_crystal_density_method    ?
_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
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_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_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_source                   'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                339
_reflns_number_total             352
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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)'
_refine_diff_density_max         0.492
_refine_diff_density_min         -0.176
_refine_diff_density_rms         0.057
_refine_ls_extinction_coef       .
_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_R_factor_all          0.0299
_refine_ls_R_factor_gt           0.0284
_refine_ls_restrained_S_all      1.126
_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
_refine_special_details          
;
Hydrogen atoms of the carboxylic acid 
group have been refined isostropically.
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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) . ?

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 ?

_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
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_alpha_C2_156
_database_code_depnum_ccdc_archive 'CCDC 1854360'
loop_
_audit_author_name
_audit_author_address
'Suman Bhattacharya'
;Department of Chemistry, Pondicherry University
India
;
_audit_update_record             
;
2020-07-19 deposited with the CCDC.	2020-10-13 downloaded from the CCDC.
;
_audit_creation_date             2014-02-10
_audit_creation_method           
;
Olex2 1.2
(compiled 2013.11.15 svn.r2834 for OlexSys, GUI svn.r4715)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        'Oxalic acid alpha polymorph'
_chemical_formula_moiety         'C2 H2 O4'
_chemical_formula_sum            'C2 H2 O4'
_chemical_formula_weight         90.04
_chemical_melting_point          ?

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'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'
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'

_cell_length_a                   6.4914(5)
_cell_length_b                   6.0556(5)
_cell_length_c                   7.8020(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     306.69(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    604
_cell_measurement_temperature    156(2)
_cell_measurement_theta_max      28.9979
_cell_measurement_theta_min      4.5953
_shelx_estimated_absorpt_T_max   0.927
_shelx_estimated_absorpt_T_min   0.917
_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_density_meas      ?
_exptl_crystal_density_method    ?
_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
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_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_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_source                   'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                341
_reflns_number_total             355
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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)'
_refine_diff_density_max         0.466
_refine_diff_density_min         -0.208
_refine_diff_density_rms         0.052
_refine_ls_extinction_coef       .
_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_R_factor_all          0.0273
_refine_ls_R_factor_gt           0.0259
_refine_ls_restrained_S_all      1.109
_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
_refine_special_details          
;
Hydrogen atoms bonded to the carboxylic acid
 group have been refined isotropically.
;

_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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) . ?

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 ?

_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
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_alpha_C2_192
_database_code_depnum_ccdc_archive 'CCDC 1854359'
loop_
_audit_author_name
_audit_author_address
'Suman Bhattacharya'
;Department of Chemistry, Pondicherry University
India
;
_audit_update_record             
;
2020-07-19 deposited with the CCDC.	2020-10-13 downloaded from the CCDC.
;
_audit_creation_date             2014-02-10
_audit_creation_method           
;
Olex2 1.2
(compiled 2013.11.15 svn.r2834 for OlexSys, GUI svn.r4715)
;
_shelxl_version_number           2013-4
_chemical_name_systematic        'Oxalic acid alpha polymorph'
_chemical_name_common            ?
_chemical_formula_moiety         'C2 H2 O4'
_chemical_formula_sum            'C2 H2 O4'
_chemical_formula_weight         90.04
_chemical_melting_point          ?
_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_diffrn_ambient_temperature      192(2)

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'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'
_chemical_absolute_configuration ?
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'

_cell_length_a                   6.5045(6)
_cell_length_b                   6.0640(6)
_cell_length_c                   7.8072(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     307.94(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    501
_cell_measurement_temperature    192(2)
_cell_measurement_theta_max      28.9059
_cell_measurement_theta_min      4.0688
_shelx_estimated_absorpt_T_max   0.928
_shelx_estimated_absorpt_T_min   0.917
_exptl_absorpt_coefficient_mu    0.200
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82798
_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_primary    colourless
_exptl_crystal_density_diffrn    1.942
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             184
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.38
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0064
_diffrn_reflns_av_unetI/netI     0.0087
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.857
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            814
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.857
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.976
_diffrn_reflns_theta_min         6.095
_diffrn_detector_area_resol_mean 15.9821
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.857
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0185042000
_diffrn_orient_matrix_UB_12      -0.0692103000
_diffrn_orient_matrix_UB_13      0.0715687000
_diffrn_orient_matrix_UB_21      0.0676790000
_diffrn_orient_matrix_UB_22      0.0802025000
_diffrn_orient_matrix_UB_23      0.0345046000
_diffrn_orient_matrix_UB_31      -0.0834159000
_diffrn_orient_matrix_UB_32      0.0496664000
_diffrn_orient_matrix_UB_33      0.0439832000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                336
_reflns_number_total             353
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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)'
_refine_diff_density_max         0.450
_refine_diff_density_min         -0.181
_refine_diff_density_rms         0.053
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.173
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     32
_refine_ls_number_reflns         353
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0287
_refine_ls_R_factor_gt           0.0266
_refine_ls_restrained_S_all      1.173
_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)+(0.0340P)²+0.1039P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0668
_refine_ls_wR_factor_ref         0.0684
_refine_special_details          
;
Hydrogen atoms of the carboxylic acid 
group have been refined isotropically.
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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(12) 0.04267(12) 0.78208(9) 0.0165(3) Uani 1 1 d . . . . .
C1 C 0.44245(14) 0.08441(15) 0.94439(12) 0.0115(3) Uani 1 1 d . . . . .
O1 O 0.34205(11) 0.23291(12) 1.00511(9) 0.0156(3) Uani 1 1 d . . . . .
H2 H 0.412(3) 0.145(3) 0.717(2) 0.042(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 0.0232(4) 0.0156(4) 0.0107(4) 0.0011(3) -0.0006(3) 0.0038(3)
C1 0.0112(4) 0.0103(4) 0.0129(5) 0.0007(3) -0.0007(3) -0.0020(3)
O1 0.0173(4) 0.0137(4) 0.0157(4) -0.0012(2) -0.0010(3) 0.0040(3)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 1.3053(12) . ?
O2 H2 0.887(18) . ?
C1 C1 1.5370(18) 5_657 ?
C1 O1 1.2092(12) . ?

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 111.2(11) . . ?
O2 C1 C1 110.53(10) . 5_657 ?
O1 C1 O2 126.95(9) . . ?
O1 C1 C1 122.52(11) . 5_657 ?

_shelx_res_file                  
;
TITL BKS-C2-ORTHO-192 in Pbca #61
CELL 0.71073 6.504464 6.063978 7.807227 90 90 90
ZERR 4 0.000589 0.000629 0.000881 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. 100
PLAN  20
SIZE 0.44 0.4 0.38
TEMP -81(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-192/C2-I-192.hkl</H
REM KL>

WGHT    0.034000    0.103900
FVAR      17.06954
O2    3    0.470721    0.042668    0.782076    11.00000    0.02319    0.01565 =
         0.01067    0.00113   -0.00060    0.00385
C1    1    0.442454    0.084407    0.944393    11.00000    0.01119    0.01026 =
         0.01295    0.00069   -0.00072   -0.00199
O1    3    0.342050    0.232905    1.005109    11.00000    0.01727    0.01370 =
         0.01572   -0.00124   -0.00097    0.00402
H2    2    0.412263    0.144772    0.716951    11.00000    0.04217
HKLF 4

REM  BKS-C2-ORTHO-192 in Pbca #61
REM R1 =  0.0266 for     336 Fo > 4sig(Fo)  and  0.0287 for all     353 data
REM     32 parameters refined using      0 restraints

END

WGHT      0.0343      0.1037

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

REM Highest difference peak  0.450,  deepest hole -0.181,  1-sigma level  0.053
Q1    1   0.5000  0.0000  1.0000  10.50000  0.05    0.45
Q2    1   0.4047  0.2831  0.6317  11.00000  0.05    0.15
Q3    1   0.4563  0.1890  0.9763  11.00000  0.05    0.15
Q4    1   0.4453  0.0671  0.8732  11.00000  0.05    0.12
Q5    1   0.5373  0.2847  0.8992  11.00000  0.05    0.12
Q6    1   0.5580  0.2593  1.0008  11.00000  0.05    0.12
Q7    1   0.2815  0.0030  0.6399  11.00000  0.05    0.11
Q8    1   0.2664  0.0285  1.1022  11.00000  0.05    0.10
Q9    1   0.6495 -0.0245  0.6717  11.00000  0.05    0.10
Q10   1   0.6554 -0.1113  0.8120  11.00000  0.05    0.09
Q11   1   0.2474 -0.0232  0.8995  11.00000  0.05    0.09
Q12   1   0.6906 -0.0225  0.7465  11.00000  0.05    0.09
Q13   1   0.2341  0.0142  1.0052  11.00000  0.05    0.08
Q14   1   0.4687  0.2837  0.7750  11.00000  0.05    0.08
Q15   1   0.2861  0.0332  0.8384  11.00000  0.05    0.08
Q16   1   0.2734  0.0222  0.7673  11.00000  0.05    0.07
Q17   1   0.3593  0.1203  0.9735  11.00000  0.05    0.07
Q18   1   0.4182  0.3526  0.8238  11.00000  0.05    0.07
Q19   1   0.3216 -0.0905  0.8039  11.00000  0.05    0.06
Q20   1   0.5488  0.3830  1.0133  11.00000  0.05    0.06
;
_shelx_res_checksum              38766
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_alpha_C2_264
_database_code_depnum_ccdc_archive 'CCDC 1854357'
loop_
_audit_author_name
_audit_author_address
'Suman Bhattacharya'
;Department of Chemistry, Pondicherry University
India
;
_audit_update_record             
;
2020-07-19 deposited with the CCDC.	2020-10-13 downloaded from the CCDC.
;
_audit_creation_date             2014-02-10
_audit_creation_method           
;
Olex2 1.2
(compiled 2013.11.15 svn.r2834 for OlexSys, GUI svn.r4715)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        'Oxalic acid alpha polymorph'
_chemical_formula_moiety         'C2 H2 O4'
_chemical_formula_sum            'C2 H2 O4'
_chemical_formula_weight         90.04
_chemical_melting_point          ?

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'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'
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'

_cell_length_a                   6.5399(11)
_cell_length_b                   6.0841(7)
_cell_length_c                   7.8385(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     311.89(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    484
_cell_measurement_temperature    264(2)
_cell_measurement_theta_max      28.8137
_cell_measurement_theta_min      6.0611
_shelx_estimated_absorpt_T_max   0.929
_shelx_estimated_absorpt_T_min   0.918
_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_density_meas      ?
_exptl_crystal_density_method    ?
_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
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_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_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_source                   'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                340
_reflns_number_total             354
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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)'
_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_R_factor_all          0.0277
_refine_ls_R_factor_gt           0.0263
_refine_ls_restrained_S_all      1.122
_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
_refine_special_details          
;
Hydrogen atoms of the carboxylic acid group 
have been refined isostropically.
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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) . ?

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 ?

_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
