#------------------------------------------------------------------------------
#$Date: 2018-12-01 06:40:03 +0200 (Sat, 01 Dec 2018) $
#$Revision: 212280 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/03/1550314.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_1550314
loop_
_publ_author_name
'Abdou, Moaz M.'
'Matziari, Magdalini'
'O'Neill, Paul M.'
'Amigues, Eric'
'Zhou, Ruixue'
'Wang, Ruiyao'
'Ali, Basem F.'
_publ_section_title
;
Methyl 3-(4-hydroxyphenyl)propionate
;
_journal_coeditor_code RZ4027
_journal_issue 11
_journal_name_full IUCrData
_journal_page_first x181662
_journal_paper_doi 10.1107/S2414314618016620
_journal_volume 3
_journal_year 2018
_chemical_formula_iupac 'C10 H12 O3'
_chemical_formula_moiety 'C10 H12 O3'
_chemical_formula_sum 'C10 H12 O3'
_chemical_formula_weight 180.20
_chemical_name_systematic
;
Methyl 3-(4-hydroxyphenyl)propionate
;
_space_group_crystal_system orthorhombic
_space_group_IT_number 19
_space_group_name_Hall 'P 2ac 2ab'
_space_group_name_H-M_alt 'P 21 21 21'
_symmetry_space_group_name_Hall 'P 2ac 2ab'
_symmetry_space_group_name_H-M 'P 21 21 21'
_atom_sites_solution_hydrogens mixed
_audit_creation_method SHELXL-2018/1
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 5.4774(6)
_cell_length_b 11.1557(12)
_cell_length_c 14.5610(17)
_cell_measurement_reflns_used 2736
_cell_measurement_temperature 180(2)
_cell_measurement_theta_max 27.59
_cell_measurement_theta_min 3.34
_cell_volume 889.74(17)
_computing_cell_refinement
;
SAINT (Bruker, 2016)
;
_computing_data_collection
;
APEX3 (Bruker, 2016)
;
_computing_data_reduction
;
SAINT (Bruker, 2016)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature 180(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type
;
Bruker D8 Venture diffractometer with PHOTON 100 CMOS detecter
;
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0563
_diffrn_reflns_av_unetI/netI 0.0414
_diffrn_reflns_limit_h_max 6
_diffrn_reflns_limit_h_min -6
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_l_max 17
_diffrn_reflns_limit_l_min -17
_diffrn_reflns_number 9443
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 25.998
_diffrn_reflns_theta_min 3.341
_exptl_absorpt_coefficient_mu 0.099
_exptl_absorpt_correction_T_max 0.7456
_exptl_absorpt_correction_T_min 0.6144
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2016)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.345
_exptl_crystal_description block
_exptl_crystal_F_000 384
_exptl_crystal_size_max 0.350
_exptl_crystal_size_mid 0.150
_exptl_crystal_size_min 0.100
_refine_diff_density_max 0.194
_refine_diff_density_min -0.150
_refine_ls_abs_structure_details
;
Flack x determined using 467 quotients
[(I^+^)-(I^-^)]/[(I^+^)+(I^-^)]
(Parsons et al., 2013)
;
_refine_ls_abs_structure_Flack -0.5(8)
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.042
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 122
_refine_ls_number_reflns 1756
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.042
_refine_ls_R_factor_all 0.0637
_refine_ls_R_factor_gt 0.0401
_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/[\s^2^(Fo^2^)+(0.0427P)^2^+0.1279P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0815
_refine_ls_wR_factor_ref 0.0905
_reflns_number_gt 1390
_reflns_number_total 1756
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file rz4027sup1.cif
_cod_data_source_block I
_cod_database_code 1550314
_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_min 0.966
_shelx_estimated_absorpt_t_max 0.990
_shelx_hkl_file
;
1 0 0 0.40 0.70
-1 0 0 -0.10 0.60
-1 0 0 0.70 0.80
-2 0 0 5.80 1.60
-2 0 0 4.90 1.60
2 0 0 6.60 1.60
2 0 0 7.00 1.50
-3 0 0 0.60 2.10
3 0 0 0.00 2.10
3 0 0 1.50 2.00
-3 0 0 -0.50 2.00
-4 0 0 124.49 7.00
-4 0 0 121.79 7.30
4 0 0 134.39 6.30
4 0 0 114.59 6.40
-5 0 0 8.70 4.90
-5 0 0 -2.50 4.80
5 0 0 1.90 4.40
-6 0 0 5.70 6.00
-6 0 0 -11.70 7.60
-7 0 0 11.20 9.10
-1 -1 0 72.09 2.30
1 -1 0 69.79 3.00
-1 1 0 72.29 3.00
-1 -1 0 70.79 2.40
1 1 0 71.29 2.20
1 -1 0 72.19 2.90
-1 1 0 69.39 2.90
1 1 0 69.79 2.20
2 1 0 5.00 1.20
-2 1 0 5.20 1.70
-2 -1 0 5.70 1.50
2 -1 0 3.90 1.60
2 1 0 4.50 1.00
-2 1 0 2.70 1.90
-2 -1 0 4.30 1.30
3 -1 0 109.49 5.60
-3 1 0 110.39 5.90
3 1 0 104.29 4.60
-3 -1 0 109.99 5.20
3 1 0 108.89 5.00
-3 1 0 121.49 5.90
-3 -1 0 106.49 5.20
-4 1 0 2.60 3.60
-4 -1 0 -1.10 2.70
4 1 0 -3.80 2.40
-4 1 0 -0.50 2.90
4 -1 0 -3.40 3.10
4 1 0 -1.10 2.10
-4 -1 0 -2.40 3.00
4 -1 0 -3.60 2.70
5 -1 0 208.78 10.30
-5 -1 0 210.08 10.40
-5 -1 0 192.48 10.60
-5 1 0 200.38 11.10
-5 1 0 213.08 11.10
5 1 0 209.18 9.10
-6 1 0 506.75 20.00
-6 1 0 484.05 21.10
-6 -1 0 467.55 19.80
-7 -1 0 -3.60 8.50
-7 1 0 -12.60 9.10
0 -2 0 2703.23 70.49
0 2 0 2797.82 70.99
-1 2 0 1073.19 28.70
-1 -2 0 1079.89 27.80
-1 2 0 1089.49 28.80
1 -2 0 1041.20 28.70
-1 -2 0 1083.49 27.80
1 -2 0 1101.89 28.80
-2 2 0 0.10 1.90
2 -2 0 3.60 1.70
2 2 0 1.60 0.60
2 -2 0 0.70 1.90
2 2 0 1.70 0.70
-2 -2 0 2.00 1.20
-2 2 0 -0.90 1.60
-2 -2 0 -0.10 1.00
-3 -2 0 467.75 13.80
-3 2 0 466.75 14.80
3 2 0 478.65 13.00
-3 -2 0 445.66 13.70
3 -2 0 452.55 14.50
3 2 0 461.95 12.80
-3 2 0 460.25 14.80
3 -2 0 478.65 14.70
4 2 0 2.40 2.00
-4 2 0 4.00 3.90
4 2 0 -0.40 1.80
-4 -2 0 0.40 2.90
-4 -2 0 3.00 2.60
-4 2 0 0.00 3.20
5 -2 0 16.20 5.40
-5 2 0 12.10 6.10
5 2 0 15.30 2.90
-5 -2 0 17.30 5.10
5 2 0 18.60 3.20
-5 -2 0 17.70 4.60
-5 2 0 25.60 5.50
-6 2 0 6.10 6.90
-6 2 0 6.60 9.10
-6 -2 0 -11.10 7.10
-6 -2 0 1.20 6.70
-7 2 0 -3.80 9.70
-7 -2 0 0.00 7.90
0 -3 0 0.80 1.40
0 3 0 1.00 0.90
0 -3 0 0.60 0.90
0 3 0 1.10 1.00
-1 -3 0 76.39 2.50
-1 3 0 70.59 3.70
1 -3 0 73.69 3.90
-1 -3 0 73.59 2.60
-1 3 0 73.39 3.80
1 -3 0 71.89 3.70
2 -3 0 145.49 6.40
-2 -3 0 149.09 4.80
2 -3 0 148.59 6.40
-2 -3 0 152.08 4.90
-2 3 0 144.69 6.40
-2 3 0 152.68 6.40
-3 -3 0 23.40 2.70
-3 3 0 25.00 4.00
3 -3 0 28.90 3.90
3 -3 0 24.90 3.90
-3 3 0 23.60 3.60
-3 -3 0 23.80 2.80
-4 3 0 17.90 4.60
4 -3 0 13.30 4.40
4 -3 0 6.80 4.20
-4 3 0 12.00 4.00
-4 -3 0 10.50 3.50
-4 -3 0 13.70 3.20
-5 3 0 69.19 8.70
5 -3 0 62.39 8.80
-5 -3 0 68.69 6.80
-5 -3 0 72.59 11.00
-5 3 0 64.19 8.40
-6 3 0 -5.90 9.50
-6 3 0 -6.90 7.10
-6 -3 0 12.00 10.00
6 -3 0 -3.00 8.10
-6 -3 0 2.00 5.60
-7 -3 0 14.10 8.50
-7 3 0 -4.00 10.10
0 4 0 118.89 4.40
0 -4 0 119.59 4.60
0 -4 0 116.49 4.60
0 4 0 123.19 4.40
-1 4 0 761.92 21.70
-1 4 0 774.82 21.80
-1 -4 0 777.72 20.70
-1 -4 0 795.02 20.70
1 -4 0 768.32 21.80
1 -4 0 790.32 21.90
2 -4 0 9.90 3.00
-2 -4 0 6.60 1.20
2 -4 0 9.00 2.80
-2 4 0 7.80 2.70
-2 4 0 3.10 2.90
-3 -4 0 10.60 1.80
-3 4 0 10.90 3.40
3 -4 0 13.00 3.60
-3 -4 0 13.20 2.20
-3 4 0 14.00 3.90
3 -4 0 13.00 7.10
-4 4 0 4.70 4.50
-4 -4 0 1.90 2.90
-4 4 0 -3.70 3.90
4 -4 0 -2.50 4.60
-4 -4 0 2.80 2.60
-5 -4 0 6.10 4.00
-5 -4 0 7.20 4.60
-5 4 0 -0.80 7.00
5 -4 0 3.00 6.00
-5 4 0 10.20 5.90
-6 -4 0 -1.30 6.90
-6 4 0 0.60 7.70
-6 4 0 7.50 11.30
-6 -4 0 -2.80 5.40
0 5 0 1.00 1.20
0 5 0 0.10 1.50
0 -5 0 -0.60 1.70
0 -5 0 0.20 1.50
-1 5 0 84.09 4.50
-1 -5 0 87.39 3.70
1 -5 0 86.79 4.90
1 -5 0 78.09 4.90
-1 5 0 81.49 4.70
-1 -5 0 85.59 3.50
1 5 0 80.09 2.50
-2 -5 0 0.60 1.20
2 -5 0 -2.70 2.70
-2 5 0 -1.70 2.90
-2 -5 0 1.30 1.00
2 -5 0 1.90 2.60
-3 -5 0 2.80 1.60
3 -5 0 1.80 4.00
3 -5 0 2.70 3.80
-3 5 0 4.10 3.90
-3 -5 0 0.50 1.90
-3 5 0 2.00 3.00
-4 5 0 73.99 7.90
-4 -5 0 65.49 5.30
-4 -5 0 58.39 4.80
-4 5 0 62.89 7.10
4 -5 0 71.29 7.80
4 -5 0 68.49 8.70
-5 5 0 79.69 10.50
-5 -5 0 84.29 7.10
-5 -5 0 94.59 7.90
5 -5 0 93.09 12.30
-6 5 0 6.20 8.30
-6 5 0 -12.50 12.50
-6 -5 0 -1.80 5.80
-6 -5 0 16.50 7.20
0 6 0 365.46 11.10
0 -6 0 347.67 11.40
0 -6 0 352.76 11.40
0 6 0 365.96 11.00
1 -6 0 31.80 4.10
1 -6 0 24.40 3.40
-1 -6 0 20.40 2.50
1 6 0 22.50 1.60
-1 6 0 27.30 3.50
-1 -6 0 19.20 2.30
2 -6 0 39.10 4.60
-2 6 0 30.00 5.30
2 -6 0 41.20 4.60
-2 -6 0 36.00 2.70
-2 6 0 37.80 4.70
-2 -6 0 37.80 3.00
-3 6 0 5.10 5.60
-3 -6 0 11.90 1.90
-3 -6 0 9.40 2.10
3 -6 0 9.80 4.30
-3 6 0 12.30 4.10
4 -6 0 53.69 7.30
-4 -6 0 43.40 4.60
-4 6 0 43.60 7.80
4 -6 0 45.00 7.10
-4 6 0 49.70 6.70
-5 -6 0 58.39 6.70
5 -6 0 46.60 9.70
-5 -6 0 49.99 5.90
5 -6 0 50.19 9.40
-5 6 0 54.59 8.40
-5 6 0 42.40 10.40
-6 6 0 36.60 15.80
-6 6 0 35.30 10.30
-6 -6 0 29.20 6.60
6 -6 0 29.90 17.40
-6 -6 0 30.60 8.00
0 -7 0 -0.30 2.20
0 7 0 2.70 1.70
0 7 0 3.60 2.30
0 -7 0 5.90 2.70
1 -7 0 67.89 5.40
-1 -7 0 49.99 3.80
1 -7 0 66.19 5.50
-1 -7 0 59.59 4.30
-2 7 0 123.79 9.60
-2 -7 0 118.59 5.00
-2 7 0 113.99 7.00
2 -7 0 119.99 8.00
-2 -7 0 117.39 5.30
2 -7 0 110.99 7.50
-3 -7 0 62.39 4.10
-3 7 0 70.09 7.30
3 -7 0 75.99 8.20
-3 -7 0 65.49 4.40
-3 7 0 56.89 7.00
-4 -7 0 50.79 4.40
-4 7 0 51.39 8.30
-4 7 0 55.09 7.30
4 -7 0 67.09 8.40
4 -7 0 60.89 8.20
-4 -7 0 59.29 5.10
5 -7 0 -2.70 8.50
-5 7 0 0.80 6.70
-6 7 0 26.30 10.60
6 -7 0 17.80 13.20
0 -8 0 252.27 10.00
0 8 0 266.27 9.50
0 8 0 253.77 9.00
0 -8 0 266.47 10.00
1 -8 0 5.90 3.80
-1 -8 0 5.70 2.90
1 -8 0 2.20 3.50
1 8 0 3.70 1.30
-1 -8 0 6.20 2.60
2 -8 0 889.11 28.10
-2 8 0 904.81 27.60
-2 -8 0 936.21 25.90
2 -8 0 941.61 28.30
-2 -8 0 949.40 25.90
-3 8 0 34.80 5.40
-3 -8 0 36.90 4.40
3 -8 0 43.80 7.00
-3 -8 0 30.30 3.90
4 -8 0 15.90 7.60
-4 8 0 -10.60 8.50
-4 8 0 7.30 6.20
-4 -8 0 9.60 3.50
-4 -8 0 11.40 2.90
4 -8 0 20.10 8.50
-5 8 0 13.50 8.10
5 -8 0 4.50 10.90
-5 -8 0 2.50 4.20
-5 -8 0 4.50 3.50
-6 8 0 11.00 10.90
-6 -8 0 3.90 6.20
0 -9 0 3.20 3.80
0 9 0 -0.30 3.30
0 9 0 -0.70 2.30
0 -9 0 -4.40 3.10
-1 -9 0 21.20 4.20
1 -9 0 25.80 5.00
-1 -9 0 21.30 3.70
1 -9 0 26.30 4.80
-1 9 0 21.50 3.90
-2 -9 0 20.60 3.40
2 -9 0 12.70 5.50
-2 9 0 18.80 4.80
2 -9 0 33.90 6.50
-2 -9 0 15.80 3.60
-3 9 0 120.49 12.10
-3 -9 0 113.29 6.60
3 -9 0 123.89 11.30
-3 -9 0 103.19 6.00
-3 9 0 107.69 9.20
-4 -9 0 23.40 3.80
4 -9 0 33.60 9.70
-4 -9 0 18.00 4.20
-4 9 0 25.40 7.50
4 -9 0 40.00 10.00
5 -9 0 12.00 11.90
-5 9 0 3.00 9.20
-5 -9 0 -2.90 4.60
-5 -9 0 6.80 4.20
0 -10 0 71.99 8.10
0 10 0 86.39 5.70
0 -10 0 81.59 7.60
1 -10 0 3.60 5.20
-1 10 0 -0.60 3.50
-1 -10 0 -1.10 3.40
1 -10 0 6.00 4.90
-1 -10 0 2.50 4.30
-2 -10 0 -3.00 3.10
2 -10 0 -1.90 6.20
-2 10 0 3.30 4.40
-2 -10 0 5.60 3.90
2 -10 0 -1.10 5.50
-3 -10 0 41.60 5.00
3 -10 0 46.30 9.10
-3 -10 0 46.80 5.60
-3 10 0 54.49 8.00
3 -10 0 40.50 8.90
4 -10 0 6.10 10.20
-4 -10 0 1.40 3.60
-4 10 0 19.70 7.80
-4 -10 0 0.90 4.20
5 -10 0 70.19 14.60
-5 10 0 77.29 12.40
-5 -10 0 52.39 5.90
0 -11 0 -1.40 4.70
0 -11 0 0.70 5.40
0 11 0 0.50 3.30
-1 -11 0 15.30 5.50
-1 -11 0 14.70 5.00
1 -11 0 14.10 6.10
1 -11 0 16.40 6.70
-1 11 0 28.30 6.10
-2 -11 0 7.40 4.70
2 -11 0 7.20 7.50
-2 -11 0 18.40 4.80
2 -11 0 3.90 7.80
-3 -11 0 2.50 4.60
-3 11 0 8.50 7.00
-3 -11 0 13.20 4.20
3 -11 0 -4.10 11.30
3 -11 0 9.20 9.20
4 -11 0 10.90 15.00
-4 -11 0 5.50 5.00
-4 11 0 22.80 8.80
4 -11 0 16.50 12.90
-4 -11 0 9.30 4.60
0 -12 0 12.10 7.20
0 -12 0 14.00 6.50
1 -12 0 15.40 7.70
-1 12 0 10.90 5.20
-1 -12 0 9.50 6.10
1 -12 0 11.80 7.40
-2 -12 0 1.70 6.10
2 -12 0 13.00 8.90
-2 -12 0 1.10 5.10
2 -12 0 -7.30 8.10
3 -12 0 16.20 10.50
-3 12 0 14.30 7.50
-3 -12 0 2.40 5.50
3 -12 0 13.30 12.50
-3 -12 0 4.00 5.00
4 -12 0 2.80 14.40
-4 -12 0 -3.00 6.00
-4 -12 0 5.80 6.30
0 -13 0 4.10 8.10
0 -13 0 6.80 7.70
-1 13 0 3.30 6.50
1 -13 0 -0.80 9.00
-1 -13 0 3.50 7.30
1 -13 0 2.70 9.20
2 -13 0 49.00 11.80
-2 -13 0 36.80 8.40
-2 -13 0 25.70 7.50
3 -13 0 4.90 12.80
-3 -13 0 2.60 7.00
0 -14 0 65.19 11.10
-1 -14 0 18.40 10.00
1 -14 0 17.40 11.90
2 -14 0 16.60 13.70
-2 -14 0 32.80 10.10
-1 0 -1 412.76 11.20
-1 0 1 427.16 11.40
-1 0 1 414.06 11.40
-1 0 -1 406.96 11.10
1 0 1 412.66 11.10
1 0 -1 426.36 11.30
1 0 1 382.46 11.10
-2 0 1 2.80 1.70
2 0 1 3.30 1.30
-2 0 1 3.00 1.50
2 0 -1 4.30 1.50
-2 0 -1 4.50 1.50
-2 0 -1 2.00 1.50
2 0 1 2.80 1.30
3 0 -1 96.09 4.90
3 0 -1 99.19 5.50
-3 0 1 94.59 5.10
3 0 1 102.49 4.70
-3 0 -1 96.79 5.10
-3 0 1 93.19 5.40
-3 0 -1 102.29 5.00
-4 0 1 51.49 6.00
-4 0 -1 59.49 5.80
4 0 1 57.19 5.00
-4 0 1 58.19 5.70
4 0 -1 68.59 5.60
-4 0 -1 58.19 5.30
4 0 1 69.59 4.80
-5 0 1 281.77 12.50
-5 0 -1 256.17 12.30
5 0 -1 276.57 11.60
5 0 1 281.67 11.20
-5 0 1 260.07 12.90
-5 0 -1 284.87 12.20
-6 0 1 -0.80 8.00
-6 0 1 -1.20 6.50
-6 0 -1 7.30 6.10
6 0 -1 2.20 6.60
-6 0 -1 -12.10 7.10
-7 0 1 10.10 8.70
-7 0 -1 9.10 9.10
1 1 -1 1382.56 37.20
1 1 -1 1472.25 37.10
1 -1 1 1480.35 37.50
-1 -1 -1 1363.26 36.80
-1 1 1 1447.26 37.50
-1 -1 -1 1419.06 37.00
-1 1 1 1448.06 37.50
-1 1 -1 1476.55 37.50
1 -1 -1 1487.75 37.50
1 -1 -1 1376.96 37.40
-1 -1 1 1379.76 37.10
-1 -1 1 1453.25 37.20
-1 1 -1 1449.35 37.50
2 1 -1 741.23 20.40
-2 1 1 771.12 21.20
-2 -1 -1 729.53 20.30
2 1 -1 767.72 20.40
-2 1 1 744.53 21.10
-2 -1 -1 763.72 20.30
2 -1 1 764.82 20.80
2 -1 -1 766.72 21.00
-2 -1 1 782.32 20.70
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;
TITL ruixue10 in P2(1)2(1)2(1)
ruixue10.res
created by SHELXL-2018/1 at 18:11:47 on 17-Sep-2018
CELL 0.71073 5.47740 11.15570 14.56100 90.0000 90.0000 90.0000
ZERR 4.00 0.00060 0.00120 0.00170 0.0000 0.0000 0.0000
LATT -1
SYMM 0.5-X, -Y, 0.5+Z
SYMM -X, 0.5+Y, 0.5-Z
SYMM 0.5+X, 0.5-Y, -Z
SFAC C H O
UNIT 40 48 12
omit -4 52
omit 3 2 0
omit -2 3 2
L.S. 16
EQIV $1 -x+1, y+1/2, -z+3/2
HTAB O1 O2_$1
conf
ACTA
BOND $H
FMAP 2
PLAN 20
SIZE 0.10 0.15 0.35
TEMP -93.0
WGHT 0.042700 0.127900
FVAR 0.75297
O1 3 0.546825 0.189771 0.771387 11.00000 0.02217 0.03215 =
0.03631 0.00369 0.00938 -0.00491
H1H 2 0.642465 0.234635 0.739809 11.00000 0.05138
O2 3 0.124877 -0.191948 0.845458 11.00000 0.02783 0.02716 =
0.03615 -0.00328 0.01017 0.00428
O3 3 -0.234802 -0.184207 0.917706 11.00000 0.02448 0.02037 =
0.03529 -0.00062 0.00837 -0.00200
C1 1 0.376180 0.257317 0.816963 11.00000 0.01926 0.02665 =
0.02007 0.00079 -0.00202 -0.00107
C2 1 0.386468 0.381461 0.820011 11.00000 0.02262 0.02887 =
0.02964 0.00503 -0.00285 -0.00851
AFIX 43
H2A 2 0.515418 0.422762 0.789969 11.00000 -1.20000
AFIX 0
C3 1 0.209141 0.445141 0.866751 11.00000 0.03286 0.01948 =
0.03549 0.00058 -0.00715 -0.00503
AFIX 43
H3A 2 0.215294 0.530216 0.868476 11.00000 -1.20000
AFIX 0
C4 1 0.023513 0.384880 0.910812 11.00000 0.02901 0.02591 =
0.03287 -0.00448 -0.00049 0.00212
AFIX 43
H4A 2 -0.097370 0.428212 0.943778 11.00000 -1.20000
AFIX 0
C5 1 0.013606 0.260683 0.906903 11.00000 0.02025 0.02651 =
0.02760 0.00089 0.00290 -0.00183
AFIX 43
H5A 2 -0.115233 0.219904 0.937426 11.00000 -1.20000
AFIX 0
C6 1 0.186581 0.194919 0.859696 11.00000 0.01901 0.02126 =
0.02057 0.00181 -0.00295 -0.00184
C7 1 0.180247 0.059577 0.850407 11.00000 0.02261 0.02482 =
0.02777 0.00151 0.00480 -0.00002
AFIX 23
H7A 2 0.191282 0.038987 0.784403 11.00000 -1.20000
H7B 2 0.326584 0.026163 0.881019 11.00000 -1.20000
AFIX 0
C8 1 -0.042441 -0.000591 0.889848 11.00000 0.02039 0.02225 =
0.02505 0.00134 0.00345 0.00154
AFIX 23
H8A 2 -0.055581 0.020109 0.955777 11.00000 -1.20000
H8B 2 -0.189442 0.030922 0.858512 11.00000 -1.20000
AFIX 0
C9 1 -0.037541 -0.134085 0.880183 11.00000 0.01998 0.02389 =
0.01880 0.00189 0.00157 0.00006
C10 1 -0.242085 -0.313691 0.917271 11.00000 0.03648 0.01946 =
0.03534 0.00011 0.00305 -0.00422
AFIX 33
H10A 2 -0.393610 -0.341096 0.946253 11.00000 -1.50000
H10B 2 -0.235700 -0.342708 0.853791 11.00000 -1.50000
H10C 2 -0.101883 -0.345081 0.951474 11.00000 -1.50000
AFIX 0
HKLF 4
REM ruixue10 in P2(1)2(1)2(1)
REM R1 = 0.0401 for 1390 Fo > 4sig(Fo) and 0.0637 for all 1756 data
REM 122 parameters refined using 0 restraints
END
WGHT 0.0427 0.1279
REM Highest difference peak 0.194, deepest hole -0.150, 1-sigma level 0.040
Q1 1 -0.4221 -0.3229 0.9127 11.00000 0.05 0.19
Q2 1 -0.1196 -0.3204 0.8450 11.00000 0.05 0.17
Q3 1 0.5823 0.0470 0.7615 11.00000 0.05 0.15
Q4 1 0.2655 0.2194 0.8285 11.00000 0.05 0.14
Q5 1 0.0764 0.4121 0.8588 11.00000 0.05 0.14
Q6 1 0.4044 0.3175 0.8409 11.00000 0.05 0.13
Q7 1 0.3733 0.0227 0.8182 11.00000 0.05 0.13
Q8 1 -0.1586 0.0495 0.9156 11.00000 0.05 0.13
Q9 1 0.2194 -0.1226 0.7791 11.00000 0.05 0.13
Q10 1 -0.2507 0.2156 0.9785 11.00000 0.05 0.13
Q11 1 -0.1292 -0.3443 0.9810 11.00000 0.05 0.13
Q12 1 -0.1252 0.2592 1.0370 11.00000 0.05 0.12
Q13 1 0.2210 0.1403 0.8755 11.00000 0.05 0.12
Q14 1 0.3300 0.4112 0.8649 11.00000 0.05 0.12
Q15 1 0.1405 0.1397 0.8338 11.00000 0.05 0.12
Q16 1 0.1294 0.1994 0.8444 11.00000 0.05 0.12
Q17 1 -0.0139 0.3961 0.9274 11.00000 0.05 0.12
Q18 1 0.3026 0.6644 0.8768 11.00000 0.05 0.12
Q19 1 0.5999 0.5063 0.8818 11.00000 0.05 0.12
Q20 1 0.4188 0.2481 0.8023 11.00000 0.05 0.12
;
_shelx_res_checksum 86398
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
loop_
_atom_site_type_symbol
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_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
O O1 0.5468(3) 0.18977(17) 0.77139(13) 0.0302(5) Uani d 1
H H1H 0.642(6) 0.235(3) 0.740(2) 0.051(11) Uiso d 1
O O2 0.1249(3) -0.19195(17) 0.84546(13) 0.0304(5) Uani d 1
O O3 -0.2348(3) -0.18421(16) 0.91771(11) 0.0267(5) Uani d 1
C C1 0.3762(5) 0.2573(2) 0.81696(17) 0.0220(6) Uani d 1
C C2 0.3865(5) 0.3815(2) 0.8200(2) 0.0270(7) Uani d 1
H H2A 0.515418 0.422762 0.789969 0.032 Uiso calc 1
C C3 0.2091(5) 0.4451(2) 0.86675(19) 0.0293(7) Uani d 1
H H3A 0.215294 0.530216 0.868476 0.035 Uiso calc 1
C C4 0.0235(6) 0.3849(2) 0.9108(2) 0.0293(7) Uani d 1
H H4A -0.097370 0.428212 0.943778 0.035 Uiso calc 1
C C5 0.0136(5) 0.2607(2) 0.90690(18) 0.0248(6) Uani d 1
H H5A -0.115233 0.219904 0.937426 0.030 Uiso calc 1
C C6 0.1866(4) 0.1949(2) 0.85970(16) 0.0203(6) Uani d 1
C C7 0.1802(5) 0.0596(2) 0.85041(19) 0.0251(6) Uani d 1
H H7A 0.191282 0.038987 0.784403 0.030 Uiso calc 1
H H7B 0.326584 0.026163 0.881019 0.030 Uiso calc 1
C C8 -0.0424(5) -0.0006(2) 0.88985(19) 0.0226(6) Uani d 1
H H8A -0.055581 0.020109 0.955777 0.027 Uiso calc 1
H H8B -0.189442 0.030922 0.858512 0.027 Uiso calc 1
C C9 -0.0375(5) -0.1341(2) 0.88018(19) 0.0209(6) Uani d 1
C C10 -0.2421(5) -0.3137(2) 0.91727(19) 0.0304(7) Uani d 1
H H10A -0.393610 -0.341096 0.946253 0.046 Uiso calc 1
H H10B -0.235700 -0.342708 0.853791 0.046 Uiso calc 1
H H10C -0.101883 -0.345081 0.951474 0.046 Uiso calc 1
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
O1 0.0222(10) 0.0322(11) 0.0363(12) -0.0049(10) 0.0094(9) 0.0037(10)
O2 0.0278(11) 0.0272(10) 0.0362(11) 0.0043(9) 0.0102(8) -0.0033(10)
O3 0.0245(10) 0.0204(9) 0.0353(11) -0.0020(9) 0.0084(8) -0.0006(9)
C1 0.0193(16) 0.0266(15) 0.0201(14) -0.0011(12) -0.0020(12) 0.0008(12)
C2 0.0226(17) 0.0289(16) 0.0296(18) -0.0085(12) -0.0028(14) 0.0050(12)
C3 0.0329(16) 0.0195(14) 0.0355(17) -0.0050(13) -0.0071(14) 0.0006(13)
C4 0.0290(18) 0.0259(16) 0.0329(18) 0.0021(13) -0.0005(15) -0.0045(12)
C5 0.0203(16) 0.0265(15) 0.0276(16) -0.0018(12) 0.0029(13) 0.0009(12)
C6 0.0190(13) 0.0213(13) 0.0206(14) -0.0018(12) -0.0030(11) 0.0018(12)
C7 0.0226(14) 0.0248(15) 0.0278(15) 0.0000(12) 0.0048(13) 0.0015(13)
C8 0.0204(14) 0.0223(13) 0.0251(14) 0.0015(11) 0.0034(12) 0.0013(12)
C9 0.0200(14) 0.0239(14) 0.0188(14) 0.0001(12) 0.0016(12) 0.0019(11)
C10 0.0365(16) 0.0195(14) 0.0353(16) -0.0042(14) 0.0031(13) 0.0001(13)
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_publ_flag
C1 O1 H1H 111(2) ?
C9 O3 C10 116.1(2) y
O1 C1 C2 122.4(3) y
O1 C1 C6 116.6(2) y
C2 C1 C6 120.9(3) y
C3 C2 C1 120.0(3) ?
C3 C2 H2A 120.0 ?
C1 C2 H2A 120.0 ?
C4 C3 C2 119.8(3) ?
C4 C3 H3A 120.1 ?
C2 C3 H3A 120.1 ?
C3 C4 C5 119.8(3) ?
C3 C4 H4A 120.1 ?
C5 C4 H4A 120.1 ?
C6 C5 C4 121.6(3) y
C6 C5 H5A 119.2 ?
C4 C5 H5A 119.2 ?
C5 C6 C1 117.8(2) ?
C5 C6 C7 123.9(2) ?
C1 C6 C7 118.3(2) ?
C8 C7 C6 115.4(2) ?
C8 C7 H7A 108.4 ?
C6 C7 H7A 108.4 ?
C8 C7 H7B 108.4 ?
C6 C7 H7B 108.4 ?
H7A C7 H7B 107.5 ?
C9 C8 C7 113.2(2) y
C9 C8 H8A 108.9 ?
C7 C8 H8A 108.9 ?
C9 C8 H8B 108.9 ?
C7 C8 H8B 108.9 ?
H8A C8 H8B 107.8 ?
O2 C9 O3 122.9(2) y
O2 C9 C8 125.7(2) y
O3 C9 C8 111.4(2) y
O3 C10 H10A 109.5 ?
O3 C10 H10B 109.5 ?
H10A C10 H10B 109.5 ?
O3 C10 H10C 109.5 ?
H10A C10 H10C 109.5 ?
H10B C10 H10C 109.5 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
O1 C1 1.372(3) y
O1 H1H 0.86(3) y
O2 C9 1.210(3) y
O3 C9 1.334(3) y
O3 C10 1.445(3) y
C1 C2 1.387(3) y
C1 C6 1.397(4) y
C2 C3 1.382(4) ?
C2 H2A 0.9500 ?
C3 C4 1.377(4) ?
C3 H3A 0.9500 ?
C4 C5 1.388(4) ?
C4 H4A 0.9500 ?
C5 C6 1.381(4) ?
C5 H5A 0.9500 ?
C6 C7 1.516(4) y
C7 C8 1.506(3) ?
C7 H7A 0.9900 ?
C7 H7B 0.9900 ?
C8 C9 1.496(3) y
C8 H8A 0.9900 ?
C8 H8B 0.9900 ?
C10 H10A 0.9800 ?
C10 H10B 0.9800 ?
C10 H10C 0.9800 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O1 H1H O2 3_656 0.86(3) 1.96(4) 2.805(3) 169(3) yes
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
O1 C1 C2 C3 179.8(2)
C6 C1 C2 C3 0.8(4)
C1 C2 C3 C4 0.5(4)
C2 C3 C4 C5 -0.9(4)
C3 C4 C5 C6 0.1(5)
C4 C5 C6 C1 1.2(4)
C4 C5 C6 C7 -177.9(3)
O1 C1 C6 C5 179.3(2)
C2 C1 C6 C5 -1.6(4)
O1 C1 C6 C7 -1.6(3)
C2 C1 C6 C7 177.5(2)
C5 C6 C7 C8 5.0(4)
C1 C6 C7 C8 -174.0(2)
C6 C7 C8 C9 -179.1(2)
C10 O3 C9 O2 1.8(4)
C10 O3 C9 C8 -176.4(2)
C7 C8 C9 O2 0.5(4)
C7 C8 C9 O3 178.6(2)
_cod_database_fobs_code 1550314