#------------------------------------------------------------------------------
#$Date: 2016-02-20 02:53:41 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176768 $
#$URL: svn://www.crystallography.net/cod/cif/2/10/42/2104273.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_2104273
loop_
_publ_author_name
'Dittrich, B.'
'McKinnon, J. J.'
'Warren, J. E.'
_publ_section_title
;
 Improvement of anisotropic displacement parameters from invariom-model
 refinements for three <small>L</small>-hydroxylysine structures
;
_journal_coeditor_code           WS5058
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              750
_journal_page_last               759
_journal_paper_doi               10.1107/S0108768108032163
_journal_volume                  64
_journal_year                    2008
_chemical_formula_moiety         'C6 H16 N2 O3, H2 O, 2(Cl)'
_chemical_formula_sum            'C6 H18 Cl2 N2 O4'
_chemical_formula_weight         253.12
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_creation_method
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
and XD routine XDCIF
;
_cell_angle_alpha                79.382(4)
_cell_angle_beta                 73.191(5)
_cell_angle_gamma                69.544(5)
_cell_formula_units_Z            1
_cell_length_a                   5.4491(3)
_cell_length_b                   7.3962(4)
_cell_length_c                   8.1337(4)
_cell_measurement_reflns_used    34253
_cell_measurement_temperature    100
_cell_measurement_theta_max      51.42
_cell_measurement_theta_min      2.6214
_cell_volume                     292.75(3)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
;
_computing_molecular_graphics    'Koritsanszky et al, (2003)'
_computing_publication_material  'Koritsanszky et al, (2003)'
_computing_structure_refinement  'Koritsanszky et al, (2003)'
_diffrn_detector_area_resol_mean 16.0009
_diffrn_measured_fraction_theta_full 0.90
_diffrn_measured_fraction_theta_max 0.99
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur S'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0216
_diffrn_reflns_av_sigmaI/netI    0.0261
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            45855
_diffrn_reflns_theta_full        51.00
_diffrn_reflns_theta_max         51.42
_diffrn_reflns_theta_min         2.6214
_exptl_absorpt_coefficient_mu    0.547
_exptl_absorpt_correction_T_max  0.924
_exptl_absorpt_correction_T_min  0.845
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.4364
_exptl_crystal_description       rectangle
_exptl_crystal_F_000             134.00
_exptl_crystal_size_max          0.4406
_exptl_crystal_size_mid          0.4015
_exptl_crystal_size_min          0.1833
_refine_diff_density_max         0.703
_refine_diff_density_min         -0.231
_refine_ls_abs_structure_details '(Dittrich et al., 2006c)'
_refine_ls_abs_structure_Flack   -0.030(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.7268
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         10693
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0241
_refine_ls_R_factor_gt           0.0204
_refine_ls_shift/su_max          0
_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         0.0194
_reflns_number_gt                10693
_reflns_number_total             12708
_reflns_threshold_expression     F>3u(F)
_cod_data_source_file            ws5058.cif
_cod_data_source_block           III
_cod_database_code               2104273
_cod_database_fobs_code          2104273
loop_
_symmetry_equiv_pos_as_xyz
+X,+Y,+Z
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
CL(1) 0.80699 0.2266 0.15254 0.017 1
CL(2) 0.73962(3) 0.55375(2) 0.62145(2) 0.016 1
O(1) 1.30652(8) -0.53581(7) 1.04021(5) 0.02 1
O(2) 1.24225(8) -0.35346(7) 1.25037(5) 0.021 1
O(3) 0.78915(8) -0.03575(6) 0.60225(5) 0.016 1
O(1W) 0.21638(8) 0.07649(7) 0.38356(5) 0.019 1
N(1) 0.71901(8) -0.18568(7) 1.26703(5) 0.014 1
N(2) 0.37616(8) 0.32178(7) 0.55969(5) 0.014 1
C(1) 1.16180(9) -0.40042(7) 1.14575(6) 0.013 1
C(2) 0.87696(9) -0.30458(7) 1.11993(5) 0.012 1
C(3) 0.88502(9) -0.18022(7) 0.94660(5) 0.013 1
C(4) 0.60511(9) -0.06778(8) 0.91499(5) 0.013 1
C(5) 0.62716(9) 0.06783(7) 0.74930(5) 0.012 1
C(6) 0.34985(9) 0.18560(8) 0.71956(6) 0.015 1
H(1) 1.47328 -0.60217 1.07327 0.034(3) 1
H(3) 0.76776 -0.16195 0.62169 0.024(3) 1
H(1A) 0.7381 -0.26547 1.38211 0.022(2) 1
H(1B) 0.51589 -0.13231 1.27628 0.035(3) 1
H(1C) 0.77532 -0.06493 1.25552 0.030(3) 1
H(2A) 0.4727 0.41362 0.57052 0.037(3) 1
H(2B) 0.19222 0.41384 0.54513 0.025(3) 1
H(2C) 0.46362 0.24433 0.45431 0.019(2) 1
H(2) 0.78332 -0.41633 1.12631 0.025(2) 1
H(3A) 0.99143 -0.07779 0.94161 0.029(3) 1
H(3B) 0.99922 -0.28077 0.84779 0.025(2) 1
H(4A) 0.50096 -0.16796 0.90951 0.028(2) 1
H(4B) 0.47796 0.02397 1.01852 0.018(2) 1
H(5) 0.73194 0.1696 0.75142 0.029(3) 1
H(6A) 0.25431 0.08704 0.69692 0.028(3) 1
H(6B) 0.22726 0.26754 0.8311 0.036(3) 1
H(1W) 0.09377 0.02703 0.47576 0.042(3) 1
H(2W) 0.13095 0.15269 0.29419 0.038(3) 1
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 'Invariom modelling (Acta Cryst. A61, 314--320)'
H H 0.0000 0.0000 'Invariom modelling (Acta Cryst. A61, 314--320)'
N N 0.0061 0.0033 'Invariom modelling (Acta Cryst. A61, 314--320)'
O O 0.0106 0.0060 'Invariom modelling (Acta Cryst. A61, 314--320)'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C(1) O(1) H(1) 1_555 1_555 1_555 107.84 yes
H(1W) O(1W) H(2W) 1_555 1_555 1_555 112.00 yes
H(1A) N(1) H(1B) 1_555 1_555 1_555 105.21 yes
H(1A) N(1) H(1C) 1_555 1_555 1_555 110.66 yes
H(1B) N(1) H(1C) 1_555 1_555 1_555 104.13 yes
H(2A) N(2) H(2B) 1_555 1_555 1_555 103.03 yes
H(2A) N(2) H(2C) 1_555 1_555 1_555 115.03 yes
H(2B) N(2) H(2C) 1_555 1_555 1_555 107.50 yes
O(1) C(1) O(2) 1_555 1_555 1_555 125.06(4) yes
O(1) C(1) C(2) 1_555 1_555 1_555 111.94(4) yes
O(2) C(1) C(2) 1_555 1_555 1_555 122.94(5) yes
C(1) C(2) C(3) 1_555 1_555 1_555 110.09(4) yes
C(1) C(2) H(2) 1_555 1_555 1_555 109.65 yes
C(3) C(2) H(2) 1_555 1_555 1_555 110.82 yes
C(2) C(3) C(4) 1_555 1_555 1_555 113.65(4) yes
C(2) C(3) H(3A) 1_555 1_555 1_555 108.65 yes
C(2) C(3) H(3B) 1_555 1_555 1_555 105.83 yes
C(4) C(3) H(3A) 1_555 1_555 1_555 109.06 yes
C(4) C(3) H(3B) 1_555 1_555 1_555 109.62 yes
H(3A) C(3) H(3B) 1_555 1_555 1_555 109.86 yes
C(3) C(4) C(5) 1_555 1_555 1_555 110.78(4) yes
C(3) C(4) H(4A) 1_555 1_555 1_555 110.32 yes
C(3) C(4) H(4B) 1_555 1_555 1_555 111.64 yes
C(5) C(4) H(4A) 1_555 1_555 1_555 110.53 yes
C(5) C(4) H(4B) 1_555 1_555 1_555 106.16 yes
H(4A) C(4) H(4B) 1_555 1_555 1_555 107.20 yes
C(4) C(5) C(6) 1_555 1_555 1_555 111.33(4) yes
C(4) C(5) H(5) 1_555 1_555 1_555 111.93 yes
C(6) C(5) H(5) 1_555 1_555 1_555 107.91 yes
C(5) C(6) H(6A) 1_555 1_555 1_555 108.96 yes
C(5) C(6) H(6B) 1_555 1_555 1_555 109.65 yes
H(6A) C(6) H(6B) 1_555 1_555 1_555 111.67 yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
O(1) C(1) 1_555 1_555 1.3164(6) yes
O(1) H(1) 1_555 1_555 0.9595 yes
O(2) C(1) 1_555 1_555 1.2121(5) yes
O(3) H(3) 1_555 1_555 0.9596 yes
O(1W) H(1W) 1_555 1_555 0.9597 yes
O(1W) H(2W) 1_555 1_555 0.9618 yes
N(1) H(1A) 1_555 1_555 1.0224 yes
N(1) H(1B) 1_555 1_555 1.0216 yes
N(1) H(1C) 1_555 1_555 1.0221 yes
N(2) H(2A) 1_555 1_555 1.0221 yes
N(2) H(2B) 1_555 1_555 1.0220 yes
N(2) H(2C) 1_555 1_555 1.0211 yes
C(1) C(2) 1_555 1_555 1.5235(6) yes
C(2) C(3) 1_555 1_555 1.5329(6) yes
C(2) H(2) 1_555 1_555 1.0999 yes
C(3) C(4) 1_555 1_555 1.5319(6) yes
C(3) H(3A) 1_555 1_555 1.0926 yes
C(3) H(3B) 1_555 1_555 1.0919 yes
C(4) C(5) 1_555 1_555 1.5259(6) yes
C(4) H(4A) 1_555 1_555 1.0926 yes
C(4) H(4B) 1_555 1_555 1.0920 yes
C(5) C(6) 1_555 1_555 1.5217(6) yes
C(5) H(5) 1_555 1_555 1.0972 yes
C(6) H(6A) 1_555 1_555 1.0985 yes
C(6) H(6B) 1_555 1_555 1.0972 yes
