#------------------------------------------------------------------------------
#$Date: 2025-08-19 20:55:00 +0200 (Tue 19 de Aug de 2025) $
#$Revision: 301808 $
#$URL: svn://www.crystallography.net/cod/cif/2/30/03/2300362.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2300362
loop_
_publ_author_name
'Macchi, Piero'
'Bürgi, Hans-Beat'
'Chimpri, Abita S.'
'Hauser, Jürg'
'Gál, Zoltán'
_publ_section_title
;
 Low-energy contamination of Mo microsource X-ray radiation: analysis
 and solution of the problem
;
_journal_coeditor_code           HE5530
_journal_issue                   4
_journal_name_full               'Journal of Applied Crystallography'
_journal_page_first              763
_journal_page_last               771
_journal_paper_doi               10.1107/S0021889811016232
_journal_volume                  44
_journal_year                    2011
_chemical_formula_sum            'C8 H14 N2 O8'
_chemical_formula_weight         266.22
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             '25-May-05 T09:03:01-00:00'
_audit_creation_method           'XD routine XDCIF'
_cell_angle_alpha                90
_cell_angle_beta                 107.55(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.805(9)
_cell_length_b                   5.6535(18)
_cell_length_c                   12.126(9)
_cell_measurement_reflns_used    7916
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      52.6803
_cell_measurement_theta_min      3.5243
_cell_volume                     1033.1(10)
_computing_cell_refinement
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
        (compiled Aug  2 2010,13:00:58)
;
_computing_data_collection
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
        (compiled Aug  2 2010,13:00:58)
;
_computing_data_reduction
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
        (compiled Aug  2 2010,13:00:58)
;
_computing_molecular_graphics    'Volkov et al, (2006)'
_computing_publication_material  'Volkov et al, (2006)'
_computing_structure_refinement  'Volkov et al, (2006)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.0965
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.482
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       'ω and π scans'
_diffrn_orient_matrix_UB_11      -0.0167332
_diffrn_orient_matrix_UB_12      0.061209
_diffrn_orient_matrix_UB_13      0.0401365
_diffrn_orient_matrix_UB_21      -0.0009286
_diffrn_orient_matrix_UB_22      -0.106796
_diffrn_orient_matrix_UB_23      0.0300464
_diffrn_orient_matrix_UB_31      0.0439058
_diffrn_orient_matrix_UB_32      0.0210178
_diffrn_orient_matrix_UB_33      0.0355244
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0174
_diffrn_reflns_av_unetI/netI     0.0199
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            7082
_diffrn_reflns_theta_full        27.5
_diffrn_reflns_theta_max         53.01
_diffrn_reflns_theta_min         3.52
_exptl_absorpt_coefficient_mu    0.155
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.87712
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
        (compiled Aug  2 2010,13:00:58)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.712
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             560
_exptl_crystal_size_max          0.3604
_exptl_crystal_size_mid          0.3403
_exptl_crystal_size_min          0.1042
_refine_diff_density_max         0.356
_refine_diff_density_min         -0.442
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.964
_refine_ls_matrix_type           full
_refine_ls_number_parameters     89
_refine_ls_number_reflns         3673
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.038
_refine_ls_R_factor_gt           0.03
_refine_ls_shift/su_max          0.00006
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
        calc w1 = 1/[s²(Fo)]
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.036
_reflns_number_gt                2481
_reflns_number_total             2964
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            he5530.cif
_cod_data_source_block           IIA
_cod_database_code               2300362
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_local_axes_atom_label
_atom_local_axes_atom0
_atom_local_axes_ax1
_atom_local_axes_atom1
_atom_local_axes_atom2
_atom_local_axes_ax2
O(1) H(7) Z O(1) C(2) Y
O(2) C(1) Z O(2) O(3) Y
O(3) C(1) Z O(3) H(6) Y
O(4) C(2) Z O(4) O(1) Y
N(1) H(6) Z N(1) H(4) Y
C(1) O(2) Z C(1) O(3) Y
C(2) O(4) Z C(2) O(1) Y
C(3) H(1) Z C(3) H(5) Y
C(4) H(2) Z C(4) H(3) Y
H(7) O(1) Z H(7) C(2) Y
H(1) C(3) Z H(1) H(5) Y
H(2) C(4) Z H(2) H(3) Y
H(3) C(4) Z H(3) H(2) Y
H(4) N(1) Z H(4) H(6) Y
H(5) C(3) Z H(5) H(1) Y
H(6) N(1) Z H(6) H(4) Y
loop_
_atom_rho_multipole_atom_label
_atom_rho_multipole_coeff_Pv
_atom_rho_multipole_coeff_P00
_atom_rho_multipole_coeff_P11
_atom_rho_multipole_coeff_P1-1
_atom_rho_multipole_coeff_P10
_atom_rho_multipole_coeff_P20
_atom_rho_multipole_coeff_P21
_atom_rho_multipole_coeff_P2-1
_atom_rho_multipole_coeff_P22
_atom_rho_multipole_coeff_P2-2
_atom_rho_multipole_coeff_P30
_atom_rho_multipole_coeff_P31
_atom_rho_multipole_coeff_P3-1
_atom_rho_multipole_coeff_P32
_atom_rho_multipole_coeff_P3-2
_atom_rho_multipole_coeff_P33
_atom_rho_multipole_coeff_P3-3
_atom_rho_multipole_coeff_P40
_atom_rho_multipole_coeff_P41
_atom_rho_multipole_coeff_P4-1
_atom_rho_multipole_coeff_P42
_atom_rho_multipole_coeff_P4-2
_atom_rho_multipole_coeff_P43
_atom_rho_multipole_coeff_P4-3
_atom_rho_multipole_coeff_P44
_atom_rho_multipole_coeff_P4-4
_atom_rho_multipole_kappa
_atom_rho_multipole_kappa_prime0
_atom_rho_multipole_kappa_prime1
_atom_rho_multipole_kappa_prime2
_atom_rho_multipole_kappa_prime3
_atom_rho_multipole_kappa_prime4
O(1) 6.322 0 -0.0003 -0.0684 -0.0161 -0.0009 0.0038 0.061 0.0259 0.0027 0.0779
0.003 -0.0083 0.022 -0.0023 -0.0001 -0.014 0.0331 0.0013 0.0107 0.0019 0.0007
0.0004 0.0058 0.0044 -0.002 0.984981 1.070894 1.070894 1.070894 1.070894
1.070894
O(2) 6.3594 0 -0.0017 -0.0003 -0.0815 -0.0425 -0.0006 -0.0019 -0.0886 -0.0002
0.0373 0.0006 0.0035 0.0139 -0.0029 0.0031 0.0007 0.0126 0.0006 0.0023 0.0042
0.0001 -0.0011 -0.0006 0.0003 -0.001 0.978298 1.019145 1.019145 1.019145
1.019145 1.019145
O(3) 6.4137 0 0.0032 0.001 -0.0789 -0.053 -0.0009 0.0005 0.0627 -0.0232 0.0469
-0.0032 -0.002 -0.0207 0.0033 -0.0074 0.0044 0.011 -0.0048 -0.0006 -0.0035
0.0002 0.0017 -0.0017 0.0019 0.001 0.978298 1.019145 1.019145 1.019145 1.019145
1.019145
O(4) 6.2536 0 -0.0004 -0.0085 -0.0747 -0.0241 0.0007 -0.0046 -0.1009 0.0004
0.0296 -0.0004 0.0008 0.011 0 0.0015 -0.0022 0.0084 0.0011 -0.0007 0.0048
-0.0008 -0.0011 -0.0014 -0.0014 -0.0005 0.984504 1.100035 1.100035 1.100035
1.100035 1.100035
N(1) 5.5919 0 -0.003 0.0946 0.0616 0.0535 0.0023 -0.0414 -0.0699 0.0016 0.3193
0.0065 -0.0498 -0.0016 0.006 -0.0235 -0.2373 0.1209 -0.0037 0.0121 0.0221
-0.0074 0.0121 0.1014 0.0371 0 0.967858 0.787672 0.787672 0.787672 0.787672
0.787672
C(1) 3.9336 0 0.0098 0.0222 0.0315 0.1835 -0.0006 -0.0531 -0.1848 -0.0025 0.295
0.003 0.0434 0.2234 0.0012 -0.0038 0.0094 0.016 0.0008 -0.0126 -0.0182 0.0014
-0.0005 -0.007 0.0312 0.0025 1.006165 0.910331 0.910331 0.910331 0.910331
0.910331
C(2) 3.9598 0 0.0107 -0.0329 0.0812 0.2097 -0.0028 0.0163 -0.1732 -0.0009 0.2927
0.0041 0.0234 0.2331 -0.0012 -0.0029 -0.0037 -0.0096 0.0012 0.0302 -0.0545
0.0011 0.001 0.0127 0.0318 0 1.006165 0.910331 0.910331 0.910331 0.910331
0.910331
C(3) 4.1635 0 0.0725 0.1095 0.0709 0.0697 -0.0519 -0.0683 -0.11 -0.0778 0.307
0.0147 -0.01 0.0263 0.0227 -0.0298 -0.2335 0.1019 0.0116 0.0237 0.0016 -0.0102
0.013 0.1142 0.0271 0.0084 0.99475 0.885406 0.885406 0.885406 0.885406 0.885406
C(4) 4.1573 0 0.0693 0.1157 0.0728 0.0973 -0.0563 -0.0616 -0.1028 -0.079 0.3071
0.0189 -0.0144 0.0262 0.0147 -0.0217 -0.221 0.1007 0.0014 0.022 0.0073 -0.0028
0.0053 0.1044 0.0295 0.008 0.99475 0.885406 0.885406 0.885406 0.885406 0.885406
H(7) 0.6836 0 0.0037 0.008 0.1488 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
1.190362 1.190362 1.190362 1.190362 1.190362 1.190362
H(1) 0.7984 0 0.0024 -0.0037 0.1115 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
1.226428 1.226428 1.226428 1.226428 1.226428 1.226428
H(2) 0.769 0 0.002 -0.0077 0.1151 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
1.226428 1.226428 1.226428 1.226428 1.226428 1.226428
H(3) 0.7817 0 -0.0033 -0.0067 0.1089 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
1.226428 1.226428 1.226428 1.226428 1.226428 1.226428
H(4) 0.5266 0 -0.0016 0.004 0.0651 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
1.328905 1.328905 1.328905 1.328905 1.328905 1.328905
H(5) 0.7596 0 -0.0036 -0.0047 0.1099 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
1.226428 1.226428 1.226428 1.226428 1.226428 1.226428
H(6) 0.5261 0 0 0.0048 0.0795 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1.328905
1.328905 1.328905 1.328905 1.328905 1.328905
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_symmetry_multiplicity
O(1) O 0.24415(3) 0.89994(7) 0.38196(3) 0.01 Uani 1 8
O(2) O 0.31280(3) 1.32896(7) 0.42008(3) 0.009 Uani 1 8
O(3) O 0.18011(3) 1.48928(7) 0.33356(3) 0.009 Uani 1 8
O(4) O 0.11015(3) 1.05174(8) 0.28987(4) 0.014 Uani 1 8
N(1) N 0.07154(3) 1.48320(8) 0.10484(3) 0.009 Uani 1 8
C(1) C 0.23245(3) 1.31820(9) 0.36888(4) 0.007 Uani 1 8
C(2) C 0.18827(3) 1.07220(9) 0.34244(4) 0.008 Uani 1 8
C(3) C 0.04222(4) 1.27354(10) 0.02931(4) 0.01 Uani 1 8
C(4) C -0.00326(4) 1.64935(10) 0.09557(4) 0.009 Uani 1 8
H(7) H 0.214342 0.73048 0.365033 0.025(3) Uiso 1 8
H(1) H -0.006838 1.185105 0.061627 0.037(3) Uiso 1 8
H(2) H 0.022813 1.8014 0.150603 0.031(3) Uiso 1 8
H(3) H -0.053451 1.555922 0.12371 0.023(2) Uiso 1 8
H(4) H 0.120895 1.578402 0.083076 0.025(3) Uiso 1 8
H(5) H 0.099418 1.158186 0.040151 0.028(3) Uiso 1 8
H(6) H 0.09742 1.42835 0.190766 0.020(3) Uiso 1 8
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
5 8 0 0.0574
8 2 -16 0.1225
2 8 -4 0.0521
-2 -8 4 0.0521
2 8 -3 0.0617
6 3 -15 0.1151
1 -7 7 0.0654
-11 7 2 0.0396
11 -7 -3 0.1064
-17 3 -5 0.0638
12 -1 -16 0.1304
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
O2 C1 O3 127.01(3)
O2 C1 C2 118.69(3)
O3 C1 C2 114.25(2)
O4 C2 O1 126.24(3)
O4 C2 C1 121.31(2)
O1 C2 C1 112.45(3)
C4 N1 C3 111.36(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
O1 C2 1.3049(12)
O2 C1 1.2355(11)
O3 C1 1.2608(11)
C1 C2 1.5458(14)
C2 O4 1.2122(13)
N1 C4 1.4874(13)
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 30658414
2 PubChem 12147467
