#------------------------------------------------------------------------------
#$Date: 2024-04-05 01:26:35 +0300 (Fri, 05 Apr 2024) $
#$Revision: 290804 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/13/28/7132842.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7132842
loop_
_publ_author_name
'Koyama, Ryosei'
'Anada, Masahiro'
'Sueki, Shunsuke'
'Makino, Kosho'
'Kojima, Tatsuhiro'
'Kawasaki-Takasuka, Tomoko'
'Mori, Keiji'
_publ_section_title
;
 Divergent synthesis of multi-substituted phenanthrenes via an
 internal redox reaction/ring expansion sequence.
;
_journal_issue                   28
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              3822
_journal_page_last               3825
_journal_paper_doi               10.1039/d4cc00797b
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C18 H24 O2'
_chemical_formula_sum            'C18 H24 O2'
_chemical_formula_weight         272.37
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-03-08
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-03-08 deposited with the CCDC.	2024-03-11 downloaded from the CCDC.
;
_cell_angle_alpha                105.1650(10)
_cell_angle_beta                 97.0650(10)
_cell_angle_gamma                105.2950(10)
_cell_formula_units_Z            4
_cell_length_a                   9.86400(10)
_cell_length_b                   9.86560(10)
_cell_length_c                   16.5931(2)
_cell_measurement_reflns_used    18573
_cell_measurement_temperature    101(1)
_cell_measurement_theta_max      68.0500
_cell_measurement_theta_min      2.8180
_cell_volume                     1471.00(3)
_computing_cell_refinement       'CrysAlisPro 1.171.42.88a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.88a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.88a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      101(1)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -66.00 -40.00   0.50    0.20    --  -42.87 110.00  82.00   52
  2  ω     23.00  48.00   0.50    0.20    --   42.87-110.00 -12.00   50
  3  ω   -124.00 -98.00   0.50    0.52    --  -80.25-110.00 -12.00   52
  4  ω    -82.00 -48.00   0.50    0.52    --  -80.25 110.00  82.00   68
  5  ω     59.00  94.00   0.50    0.52    --   94.32-110.00 -12.00   70
  6  ω    113.00 140.00   0.50    0.52    --   94.32 110.00  82.00   54
  7  ω    -52.00 -12.00   0.50    0.20    --   -8.00 124.00 117.69   80
  8  ω    -47.00  -9.00   0.50    0.20    --   -8.00 119.00  42.34   76
  9  ω    -30.00  -5.00   0.50    0.20    --    8.00 113.00 -35.83   50
 10  ω    -72.00 -24.00   0.50    0.20    --  -12.00 143.00-161.58   96
 11  ω    -13.00  13.00   0.50    0.20    --   20.00 102.00 130.23   52
 12  ω     -5.00  21.00   0.50    0.20    --   24.00  98.00-129.26   52
 13  ω     -4.00  21.00   0.50    0.20    --   28.00  98.00 -75.64   50
 14  ω     -4.00  21.00   0.50    0.20    --   28.00  99.00   9.48   50
 15  ω      0.00  25.00   0.50    0.20    --   32.00  98.00-163.05   50
 16  ω      0.00  25.00   0.50    0.20    --   32.00  98.00 -78.42   50
 17  ω      5.00  30.00   0.50    0.20    --   36.00  94.00  78.50   50
 18  ω      4.00  29.00   0.50    0.20    --   36.00  95.00 -35.96   50
 19  ω      9.00  34.00   0.50    0.20    --   40.00  94.00 111.52   50
 20  ω      9.00  34.00   0.50    0.20    --   40.00  94.00-154.28   50
 21  ω     11.00  38.00   0.50    0.20    --   40.00  88.00   1.46   54
 22  ω     54.00  90.00   0.50    0.20    --   42.87-138.00-180.00   72
 23  ω     15.00  40.00   0.50    0.20    --   44.00  88.00  98.41   50
 24  ω     14.00  39.00   0.50    0.20    --   44.00  91.00 -44.37   50
 25  ω     14.00  39.00   0.50    0.20    --   44.00  92.00  30.33   50
 26  ω     14.00  39.00   0.50    0.20    --   44.00  90.00 154.10   50
 27  ω     14.00  39.00   0.50    0.20    --   44.00  92.00 -97.02   50
 28  ω     14.00  39.00   0.50    0.20    --   44.00  92.00-140.59   50
 29  ω    -72.00 -27.00   0.50    0.20    --  -52.00 -77.00  59.77   90
 30  ω    -54.00 -29.00   0.50    0.20    --  -52.00 -71.00 -17.28   50
 31  ω    -56.00 -29.00   0.50    0.20    --  -52.00 -69.00 140.86   54
 32  ω    -54.00 -28.00   0.50    0.20    --  -52.00 -72.00-117.16   52
 33  ω   -108.00 -82.00   0.50    0.20    --  -52.00 -77.00  59.77   52
 34  ω     27.00  52.00   0.50    0.20    --   52.00  77.00 -82.77   50
 35  ω    -63.00 -37.00   0.50    0.20    --  -56.00 -63.00-166.38   52
 36  ω    -62.00 -33.00   0.50    0.20    --  -56.00 -71.00-130.17   58
 37  ω   -107.00 -81.00   0.50    0.20    --  -56.00 -71.00-130.17   52
 38  ω    -60.00 -34.00   0.50    0.20    --  -56.00 -73.00 104.90   52
 39  ω   -122.00 -91.00   0.50    0.20    --  -56.00 -73.00 130.56   62
 40  ω   -116.00 -91.00   0.50    0.20    --  -56.00 -72.00  25.67   50
 41  ω    -57.00 -32.00   0.50    0.20    --  -56.00 -72.00  25.67   50
 42  ω    -60.00 -32.00   0.50    0.20    --  -56.00 -73.00 130.56   56
 43  ω     31.00  57.00   0.50    0.20    --   56.00  77.00-126.55   52
 44  ω    -67.00 -37.00   0.50    0.20    --  -60.00 -72.00 -64.15   60
 45  ω   -112.00 -87.00   0.50    0.20    --  -60.00 -72.00 -64.15   50
 46  ω   -125.00-100.00   0.50    0.20    --  -60.00 -74.00 -70.73   50
 47  ω    -70.00 -36.00   0.50    0.20    --  -60.00 -74.00 -70.73   68
 48  ω   -106.00 -36.00   0.50    0.20    --  -60.00 -74.00 -15.25  140
 49  ω     40.00  70.00   0.50    0.20    --   64.00  76.00 128.87   60
 50  ω    -71.00 -41.00   0.50    0.20    --  -64.00 -76.00  21.52   60
 51  ω     94.00 128.00   0.50    0.20    --   64.00  76.00 128.87   68
 52  ω    -75.00 -43.00   0.50    0.20    --  -64.00 -69.00 -97.43   64
 53  ω    -65.00 -40.00   0.50    0.20    --  -64.00 -72.00 -41.12   50
 54  ω    -67.00 -40.00   0.50    0.20    --  -64.00 -76.00-153.53   54
 55  ω     47.00  73.00   0.50    0.20    --   68.00  77.00 -92.65   52
 56  ω    -74.00 -48.00   0.50    0.52    --  -72.00 -75.00-172.70   52
 57  ω    -74.00 -48.00   0.50    0.52    --  -72.00 -77.00  -5.53   52
 58  ω    -74.00 -47.00   0.50    0.52    --  -72.00 -77.00 -54.20   54
 59  ω   -119.00 -80.00   0.50    0.52    --  -72.00 -77.00 -54.20   78
 60  ω    -84.00 -47.00   0.50    0.52    --  -72.00 -76.00  13.06   74
 61  ω    -83.00 -51.00   0.50    0.52    --  -76.00 -76.00  39.14   64
 62  ω    -92.00 -51.00   0.50    0.52    --  -76.00 -76.00 126.71   82
 63  ω   -122.00 -96.00   0.50    0.52    --  -76.00 -76.00 126.71   52
 64  ω    -91.00 -51.00   0.50    0.52    --  -76.00 -76.00 148.94   80
 65  ω    -87.00 -52.00   0.50    0.52    --  -76.00 -74.00  51.41   70
 66  ω   -113.00 -55.00   0.50    0.52    --  -80.25 -77.00 120.00  116
 67  ω   -146.00 -56.00   0.50    0.52    --  -80.25 -77.00-180.00  180
 68  ω    -94.00 -55.00   0.50    0.52    --  -80.25 -77.00 -30.00   78
 69  ω    -91.00 -55.00   0.50    0.52    --  -80.25 -76.00 -72.07   72
 70  ω    -92.00 -57.00   0.50    0.52    --  -80.25 -77.00   0.00   70
 71  ω   -142.00-102.00   0.50    0.52    --  -80.25 -77.00   0.00   80
 72  ω    -86.00 -58.00   0.50    0.52    --  -80.25 -68.00  60.00   56
 73  ω    -90.00 -58.00   0.50    0.52    --  -80.25 -75.00  21.28   64
 74  ω    -84.00 -55.00   0.50    0.52    --  -80.25 -77.00 150.00   58
 75  ω   -141.00 -92.00   0.50    0.52    --  -80.25 -77.00-120.00   98
 76  ω    -81.00 -55.00   0.50    0.52    --  -80.25 -77.00-150.00   52
 77  ω   -142.00-116.00   0.50    0.52    --  -80.25 -77.00-150.00   52
 78  ω   -147.00 -55.00   0.50    0.52    --  -80.25 -77.00  90.00  184
 79  ω    -99.00 -55.00   0.50    0.52    --  -80.25 -77.00 -90.00   88
 80  ω    -85.00 -55.00   0.50    0.52    --  -80.25 -77.00-120.00   60
 81  ω   -128.00-102.00   0.50    0.52    --  -80.25 -77.00 -90.00   52
 82  ω     60.00  90.00   0.50    0.52    --   84.00  75.00   9.23   60
 83  ω     30.00  82.00   0.50    0.52    --   94.32 -68.00-120.00  104
 84  ω    108.00 159.00   0.50    0.52    --   94.32  68.00  55.95  102
 85  ω     72.00 104.00   0.50    0.52    --   94.32  68.00  55.95   64
 86  ω    114.00 158.00   0.50    0.52    --   94.32  42.00  90.00   88
 87  ω     35.00  60.00   0.50    0.52    --   94.32-117.00 -90.00   50
 88  ω     75.00 101.00   0.50    0.52    --   94.32  68.00 150.00   52
 89  ω     99.00 142.00   0.50    0.52    --   94.32 117.00-120.00   86
 90  ω     52.00 103.00   0.50    0.52    --   94.32-145.00-180.00  102
 91  ω     70.00 107.00   0.50    0.52    --   94.32  77.00 -90.00   74
 92  ω     70.00  95.00   0.50    0.52    --   94.32  77.00-150.00   50
 93  ω     72.00 157.00   0.50    0.52    --   94.32  77.00 150.00  170
 94  ω     26.00 104.00   0.50    0.52    --   94.32 -77.00   0.00  156
 95  ω     58.00 105.00   0.50    0.52    --   94.32 -96.00 150.00   94
 96  ω     70.00 156.00   0.50    0.52    --   94.32  77.00 120.00  172
 97  ω     72.00 161.00   0.50    0.52    --   94.32  68.00-180.00  178
 98  ω     72.00 115.00   0.50    0.52    --   94.32  77.00  90.00   86
 99  ω     72.00 108.00   0.50    0.52    --   94.32  68.00  30.00   72
100  ω    112.00 155.00   0.50    0.52    --   94.32  42.00  30.00   86
101  ω     36.00  69.00   0.50    0.52    --   94.32-117.00  90.00   66
102  ω    128.00 161.00   0.50    0.52    --   94.32  77.00  30.00   66
103  ω     35.00  80.00   0.50    0.52    --   94.32 -68.00 150.00   90
104  ω     71.00 119.00   0.50    0.52    --   94.32  77.00  30.00   96
105  ω     70.00 101.00   0.50    0.52    --   94.32  77.00 -30.00   62
106  ω    136.00 161.00   0.50    0.52    --   94.32  77.00  60.00   50
107  ω     70.00 112.00   0.50    0.52    --   94.32  77.00  60.00   84
108  ω     82.00 108.00   0.50    0.52    --   94.32-117.00  90.00   52
109  ω     29.00  68.00   0.50    0.52    --   94.32 -59.00 -90.00   78
110  ω     75.00 128.00   0.50    0.52    --   94.32  59.00 120.00  106
111  ω    102.00 155.00   0.50    0.52    --   94.32  68.00 -30.00  106
112  ω     30.00  55.00   0.50    0.52    --   94.32 -50.00   0.00   50
113  ω     31.00  56.00   0.50    0.52    --   94.32 -50.00  60.00   50
114  ω     70.00 134.00   0.50    0.52    --   94.32  77.00-120.00  128
115  ω     85.00 110.00   0.50    0.52    --   94.32-117.00-180.00   50
116  ω     30.00  60.00   0.50    0.52    --   94.32 -59.00  60.00   60
117  ω     72.00  98.00   0.50    0.52    --   94.32  68.00 -30.00   52
118  ω    116.00 154.00   0.50    0.52    --   94.32  77.00-150.00   76
119  ω     33.00  66.00   0.50    0.52    --   94.32-117.00-180.00   66
120  ω     34.00  78.00   0.50    0.52    --   94.32 -68.00-150.00   88
121  ω    104.00 137.00   0.50    0.52    --   94.32 117.00 -30.00   66
122  ω     78.00 136.00   0.50    0.52    --   94.32  59.00-150.00  116
123  ω    122.00 148.00   0.50    0.52    --   94.32  77.00 -60.00   52
124  ω     70.00 120.00   0.50    0.52    --   94.32  77.00 -60.00  100
125  ω    113.00 138.00   0.50    0.52    --   94.32  68.00 150.00   50
126  ω     61.00 108.00   0.50    0.52    --   94.32-117.00  30.00   94
127  ω     82.00 153.00   0.50    0.52    --   94.32  42.00 -60.00  142
128  ω    120.00 153.00   0.50    0.52    --   94.32  59.00-120.00   66
129  ω     79.00 108.00   0.50    0.52    --   94.32  59.00-120.00   58
130  ω     28.00  56.00   0.50    0.52    --   94.32 -50.00 -60.00   56
131  ω     93.00 119.00   0.50    0.52    --   94.32 -87.00-150.00   52
132  ω     30.00  79.00   0.50    0.52    --   94.32 -87.00-150.00   98
133  ω     75.00 154.00   0.50    0.52    --   94.32  68.00   0.00  158
134  ω     77.00 110.00   0.50    0.52    --   94.32-117.00 -90.00   66
135  ω    109.00 155.00   0.50    0.52    --   94.32  96.00 -60.00   92
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix3000'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0206422000
_diffrn_orient_matrix_UB_12      -0.0522667000
_diffrn_orient_matrix_UB_13      0.0790902000
_diffrn_orient_matrix_UB_21      -0.0300927000
_diffrn_orient_matrix_UB_22      0.1370695000
_diffrn_orient_matrix_UB_23      0.0545406000
_diffrn_orient_matrix_UB_31      -0.1614000000
_diffrn_orient_matrix_UB_32      -0.0861329000
_diffrn_orient_matrix_UB_33      -0.0208411000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_av_unetI/netI     0.0188
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            30651
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.314
_diffrn_reflns_theta_min         2.820
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.610
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.640
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.88a (Rigaku Oxford Diffraction, 2023)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.230
_exptl_crystal_description       block
_exptl_crystal_F_000             592
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.231
_refine_diff_density_min         -0.182
_refine_diff_density_rms         0.037
_refine_ls_extinction_coef       0.0008(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     408
_refine_ls_number_reflns         5350
_refine_ls_number_restraints     52
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0378
_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)+(0.0524P)²+0.4879P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0993
_refine_ls_wR_factor_ref         0.1024
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4831
_reflns_number_total             5350
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4cc00797b2.cif
_cod_data_source_block           koyamadiol_auto
_cod_depositor_comments
'Adding full bibliography for 7132841--7132842.cif.'
_cod_original_cell_volume        1470.99(3)
_cod_database_code               7132842
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         C18H24O2
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.959
_shelx_estimated_absorpt_t_min   0.888
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 H2A-O1
 2 with sigma of 0.02
 O2-C16 \\sim O2A-C16A
 with sigma of 0.02
 O4-C34 \\sim O4A-C34A
 with sigma of 0.02
 C19-C34 \\sim C19-C34A
 with sigma of 0.02
 O2-C1 \\sim O2A-C1
 with sigma of 0.04
 O4-C19 \\sim O4A-C19
 with sigma of 0.04
 C1-C16 \\sim C1-C16A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C19 \\sim C34A \\sim O4A: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
C1 \\sim C16A \\sim O2A: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
Uanis(C34A) \\sim Ueq, Uanis(O4A) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.04
4. Rigid body (RIGU) restrains
 C1, C16A, O2A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C16A)=Sof(H16C)=Sof(H16D)=Sof(O2A)=Sof(H2A)=1-FVAR(1)
 Sof(O2)=Sof(H2)=Sof(C16)=Sof(H16A)=Sof(H16B)=FVAR(1)
 Sof(C34A)=Sof(H34C)=Sof(H34D)=Sof(O4A)=Sof(H4AA)=1-FVAR(2)
 Sof(O4)=Sof(H4)=Sof(C34)=Sof(H34A)=Sof(H34B)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C6(H6), C24(H24)
6.b Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C15(H15A,H15B), C32(H32A,H32B), C16(H16A,H16B), C33(H33A,
 H33B), C5(H5A,H5B), C4(H4A,H4B), C3(H3A,H3B), C34(H34A,H34B), C35(H35A,H35B),
 C21(H21A,H21B), C17(H17A,H17B), C23(H23A,H23B), C22(H22A,H22B), C16A(H16C,
 H16D), C34A(H34C,H34D)
6.c Aromatic/amide H refined with riding coordinates:
 C27(H27), C30(H30), C28(H28), C29(H29), C12(H12), C10(H10), C11(H11), C9(H9)
6.d Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C36(H36A,H36B,H36C)
6.e Idealised tetrahedral OH refined as rotating group:
 O1(H1), O2(H2), O3(H3), O4(H4), O2A(H2A), O4A(H4AA)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.213
_oxdiff_exptl_absorpt_empirical_full_min 0.870
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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
O1 O 0.39888(9) 0.58197(10) 0.52612(5) 0.0279(2) Uani 1 1 d D . . . .
H1 H 0.321415 0.602237 0.520387 0.042 Uiso 1 1 calc R U . . .
O2 O 0.74257(9) 0.67926(10) 0.59814(6) 0.0246(3) Uani 0.937(3) 1 d D . P A 1
H2 H 0.684773 0.605816 0.559868 0.037 Uiso 0.937(3) 1 calc R U P A 1
O3 O 0.12986(10) 0.59171(11) 0.48666(6) 0.0317(2) Uani 1 1 d . . . . .
H3 H 0.090900 0.638741 0.521501 0.048 Uiso 1 1 calc R U . . .
O4 O -0.01589(10) 0.78558(12) 0.53429(6) 0.0283(3) Uani 0.894(3) 1 d D . P B 1
H4 H -0.087624 0.757479 0.555223 0.042 Uiso 0.894(3) 1 calc R U P B 1
C31 C 0.30555(13) 0.81957(13) 0.38019(8) 0.0228(3) Uani 1 1 d . . . . .
C2 C 0.58136(13) 0.71028(13) 0.75720(7) 0.0224(3) Uani 1 1 d . . . . .
C7 C 0.49611(13) 0.72834(13) 0.81477(7) 0.0231(3) Uani 1 1 d . . . . .
C27 C 0.36448(13) 0.74756(13) 0.24201(8) 0.0246(3) Uani 1 1 d . . . . .
H27 H 0.337518 0.716503 0.181515 0.029 Uiso 1 1 calc R U . . .
C25 C 0.10704(13) 0.73259(13) 0.25245(8) 0.0234(3) Uani 1 1 d . . . . .
C26 C 0.26113(13) 0.76818(13) 0.29078(7) 0.0221(3) Uani 1 1 d . . . . .
C8 C 0.36774(13) 0.77580(13) 0.79591(7) 0.0235(3) Uani 1 1 d . . . . .
C13 C 0.35081(13) 0.83091(13) 0.72651(7) 0.0231(3) Uani 1 1 d . . . . .
C30 C 0.44532(14) 0.83810(13) 0.41760(8) 0.0258(3) Uani 1 1 d . . . . .
H30 H 0.473043 0.867882 0.478024 0.031 Uiso 1 1 calc R U . . .
C14 C 0.46868(14) 0.85015(13) 0.67776(8) 0.0239(3) Uani 1 1 d . . . . .
H14A H 0.541452 0.947647 0.706647 0.029 Uiso 1 1 calc R U . . .
H14B H 0.428546 0.849391 0.619889 0.029 Uiso 1 1 calc R U . . .
C19 C 0.05169(13) 0.72999(14) 0.39551(8) 0.0247(3) Uani 1 1 d D U . . .
C15 C 0.43873(13) 0.58016(13) 0.61141(7) 0.0229(3) Uani 1 1 d . . . . .
H15A H 0.485202 0.502455 0.610717 0.028 Uiso 1 1 calc R U . . .
H15B H 0.351169 0.555042 0.634921 0.028 Uiso 1 1 calc R U . . .
C32 C 0.19626(14) 0.85152(14) 0.43193(8) 0.0255(3) Uani 1 1 d . . . . .
H32A H 0.184198 0.947781 0.431365 0.031 Uiso 1 1 calc R U . . .
H32B H 0.230576 0.857911 0.491846 0.031 Uiso 1 1 calc R U . . .
C20 C 0.00666(13) 0.71459(14) 0.30080(8) 0.0250(3) Uani 1 1 d . . . . .
C28 C 0.50531(14) 0.77162(14) 0.28032(8) 0.0274(3) Uani 1 1 d . . . . .
H28 H 0.574234 0.759057 0.246102 0.033 Uiso 1 1 calc R U . . .
C1 C 0.54223(13) 0.72969(13) 0.66979(7) 0.0217(3) Uani 1 1 d D U . . .
C16 C 0.67033(19) 0.7843(2) 0.62896(12) 0.0236(4) Uani 0.937(3) 1 d D . P A 1
H16A H 0.635189 0.816283 0.580793 0.028 Uiso 0.937(3) 1 calc R U P A 1
H16B H 0.741138 0.872160 0.671764 0.028 Uiso 0.937(3) 1 calc R U P A 1
C29 C 0.54575(14) 0.81387(14) 0.36826(8) 0.0273(3) Uani 1 1 d . . . . .
H29 H 0.641155 0.826200 0.394642 0.033 Uiso 1 1 calc R U . . .
C6 C 0.52125(14) 0.69502(14) 0.89900(8) 0.0251(3) Uani 1 1 d . . . . .
H6 H 0.426077 0.635373 0.905027 0.030 Uiso 1 1 calc R U . . .
C12 C 0.22852(14) 0.86965(14) 0.70528(8) 0.0279(3) Uani 1 1 d . . . . .
H12 H 0.217891 0.905267 0.657681 0.033 Uiso 1 1 calc R U . . .
C33 C 0.06832(14) 0.58167(14) 0.40168(8) 0.0270(3) Uani 1 1 d . . . . .
H33A H -0.027123 0.505507 0.383012 0.032 Uiso 1 1 calc R U . . .
H33B H 0.130188 0.550243 0.362643 0.032 Uiso 1 1 calc R U . . .
C5 C 0.62130(15) 0.59999(14) 0.89897(8) 0.0287(3) Uani 1 1 d . . . . .
H5A H 0.652406 0.599548 0.957917 0.034 Uiso 1 1 calc R U . . .
H5B H 0.568802 0.497058 0.863572 0.034 Uiso 1 1 calc R U . . .
C4 C 0.75241(14) 0.65883(15) 0.86403(8) 0.0290(3) Uani 1 1 d . . . . .
H4A H 0.805311 0.761544 0.899625 0.035 Uiso 1 1 calc R U . . .
H4B H 0.817328 0.598110 0.866688 0.035 Uiso 1 1 calc R U . . .
C3 C 0.70851(14) 0.65528(15) 0.77229(8) 0.0269(3) Uani 1 1 d . . . . .
H3A H 0.791188 0.716613 0.756211 0.032 Uiso 1 1 calc R U . . .
H3B H 0.684813 0.552592 0.734566 0.032 Uiso 1 1 calc R U . . .
C34 C -0.0625(3) 0.7678(3) 0.44567(15) 0.0251(6) Uani 0.894(3) 1 d D . P B 1
H34A H -0.077447 0.860185 0.439352 0.030 Uiso 0.894(3) 1 calc R U P B 1
H34B H -0.155039 0.687629 0.422407 0.030 Uiso 0.894(3) 1 calc R U P B 1
C10 C 0.13868(15) 0.80690(16) 0.82224(9) 0.0343(3) Uani 1 1 d . . . . .
H10 H 0.066940 0.799679 0.855589 0.041 Uiso 1 1 calc R U . . .
C35 C 0.10840(15) 0.86149(15) 0.14042(8) 0.0315(3) Uani 1 1 d . . . . .
H35A H 0.046189 0.918086 0.165201 0.038 Uiso 1 1 calc R U . . .
H35B H 0.208905 0.917665 0.170139 0.038 Uiso 1 1 calc R U . . .
C21 C -0.15243(14) 0.66734(16) 0.26334(8) 0.0319(3) Uani 1 1 d . . . . .
H21A H -0.197068 0.730668 0.300818 0.038 Uiso 1 1 calc R U . . .
H21B H -0.196164 0.564456 0.262848 0.038 Uiso 1 1 calc R U . . .
C11 C 0.12196(15) 0.85705(16) 0.75255(9) 0.0331(3) Uani 1 1 d . . . . .
H11 H 0.038281 0.882665 0.737149 0.040 Uiso 1 1 calc R U . . .
C17 C 0.57304(15) 0.83629(14) 0.97621(8) 0.0302(3) Uani 1 1 d . . . . .
H17A H 0.679119 0.875297 0.987240 0.036 Uiso 1 1 calc R U . . .
H17B H 0.533951 0.911943 0.962211 0.036 Uiso 1 1 calc R U . . .
C9 C 0.25992(14) 0.76687(15) 0.84391(8) 0.0297(3) Uani 1 1 d . . . . .
H9 H 0.269954 0.732818 0.892166 0.036 Uiso 1 1 calc R U . . .
C23 C -0.08863(14) 0.61773(15) 0.11988(8) 0.0318(3) Uani 1 1 d . . . . .
H23A H -0.115496 0.619674 0.060808 0.038 Uiso 1 1 calc R U . . .
H23B H -0.100111 0.514039 0.117833 0.038 Uiso 1 1 calc R U . . .
C24 C 0.06821(14) 0.71135(14) 0.15745(8) 0.0268(3) Uani 1 1 d . . . . .
H24 H 0.128852 0.654662 0.129104 0.032 Uiso 1 1 calc R U . . .
C22 C -0.18708(14) 0.67588(16) 0.17333(9) 0.0328(3) Uani 1 1 d . . . . .
H22A H -0.288230 0.616948 0.146652 0.039 Uiso 1 1 calc R U . . .
H22B H -0.175409 0.779678 0.175555 0.039 Uiso 1 1 calc R U . . .
C18 C 0.52755(18) 0.81052(17) 1.05689(8) 0.0374(3) Uani 1 1 d . . . . .
H18A H 0.423010 0.787198 1.049579 0.056 Uiso 1 1 calc R U . . .
H18B H 0.574012 0.899847 1.105449 0.056 Uiso 1 1 calc R U . . .
H18C H 0.556378 0.727960 1.067513 0.056 Uiso 1 1 calc R U . . .
C36 C 0.09394(19) 0.8502(2) 0.04674(10) 0.0501(4) Uani 1 1 d . . . . .
H36A H -0.007016 0.803240 0.017683 0.075 Uiso 1 1 calc R U . . .
H36B H 0.151969 0.790840 0.020933 0.075 Uiso 1 1 calc R U . . .
H36C H 0.127506 0.949354 0.041009 0.075 Uiso 1 1 calc R U . . .
C16A C 0.685(2) 0.748(4) 0.6351(16) 0.023(4) Uani 0.063(3) 1 d D U P A 2
H16C H 0.761544 0.833612 0.675565 0.028 Uiso 0.063(3) 1 calc R U P A 2
H16D H 0.714653 0.658705 0.630617 0.028 Uiso 0.063(3) 1 calc R U P A 2
O2A O 0.6647(18) 0.7698(19) 0.5542(9) 0.039(4) Uani 0.063(3) 1 d D U P A 2
H2A H 0.576468 0.743495 0.533154 0.058 Uiso 0.063(3) 1 calc DR U P A 2
C34A C -0.028(2) 0.806(3) 0.4605(18) 0.048(8) Uani 0.106(3) 1 d D U P B 2
H34C H 0.030565 0.842289 0.519321 0.057 Uiso 0.106(3) 1 calc R U P B 2
H34D H -0.050045 0.889519 0.445533 0.057 Uiso 0.106(3) 1 calc R U P B 2
O4A O -0.1556(13) 0.6893(15) 0.4520(8) 0.070(5) Uani 0.106(3) 1 d D U P B 2
H4AA H -0.185855 0.704822 0.497673 0.105 Uiso 0.106(3) 1 calc R U P B 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-4 -2 -1 0.0946
-1 4 6 0.0673
-6 2 5 0.0784
-5 -1 -3 0.0968
4 1 5 0.0930
-1 -1 11 0.0374
-1 6 1 0.0822
-1 -5 7 0.0799
0 -5 8 0.0684
6 -2 4 0.0882
1 -6 -1 0.0814
5 -5 -1 0.0905
1 0 -10 0.0357
3 0 -10 0.0371
-5 5 -2 0.0959
-1 6 -2 0.0774
1 -3 -8 0.0470
5 -1 -7 0.0476
0 2 -11 0.0289
1 2 -11 0.0274
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
C26 C31 C32 117.67(11) . . ?
C30 C31 C26 120.00(11) . . ?
C30 C31 C32 122.32(11) . . ?
C7 C2 C1 120.47(11) . . ?
C7 C2 C3 122.11(11) . . ?
C3 C2 C1 117.12(10) . . ?
C2 C7 C8 120.60(11) . . ?
C2 C7 C6 122.69(11) . . ?
C8 C7 C6 116.65(10) . . ?
C28 C27 C26 121.25(11) . . ?
C26 C25 C24 117.29(10) . . ?
C20 C25 C26 120.21(11) . . ?
C20 C25 C24 122.45(11) . . ?
C31 C26 C25 118.98(10) . . ?
C27 C26 C31 118.03(11) . . ?
C27 C26 C25 122.94(11) . . ?
C13 C8 C7 119.45(11) . . ?
C9 C8 C7 122.99(11) . . ?
C9 C8 C13 117.56(11) . . ?
C8 C13 C14 118.46(11) . . ?
C12 C13 C8 120.47(11) . . ?
C12 C13 C14 121.05(11) . . ?
C31 C30 C29 121.12(11) . . ?
C13 C14 C1 113.08(10) . . ?
C32 C19 C20 108.40(10) . . ?
C32 C19 C33 109.57(10) . . ?
C32 C19 C34 110.33(14) . . ?
C32 C19 C34A 94.5(7) . . ?
C20 C19 C33 108.12(10) . . ?
C20 C19 C34 111.01(13) . . ?
C20 C19 C34A 118.6(13) . . ?
C33 C19 C34 109.35(13) . . ?
C33 C19 C34A 116.4(12) . . ?
O1 C15 C1 112.23(10) . . ?
C31 C32 C19 110.53(10) . . ?
C25 C20 C19 120.12(11) . . ?
C25 C20 C21 122.18(11) . . ?
C21 C20 C19 117.52(10) . . ?
C29 C28 C27 120.15(11) . . ?
C2 C1 C14 109.82(9) . . ?
C2 C1 C15 106.76(9) . . ?
C2 C1 C16 115.60(11) . . ?
C2 C1 C16A 104.4(8) . . ?
C14 C1 C15 110.32(10) . . ?
C14 C1 C16 103.37(11) . . ?
C14 C1 C16A 119.6(11) . . ?
C15 C1 C16 110.95(11) . . ?
C15 C1 C16A 105.1(13) . . ?
O2 C16 C1 115.74(13) . . ?
C28 C29 C30 119.28(12) . . ?
C7 C6 C5 111.97(10) . . ?
C7 C6 C17 112.17(10) . . ?
C5 C6 C17 111.94(11) . . ?
C11 C12 C13 120.96(12) . . ?
O3 C33 C19 112.07(10) . . ?
C4 C5 C6 110.90(10) . . ?
C3 C4 C5 110.74(11) . . ?
C2 C3 C4 113.66(10) . . ?
O4 C34 C19 109.82(16) . . ?
C11 C10 C9 120.38(12) . . ?
C36 C35 C24 114.06(12) . . ?
C20 C21 C22 114.00(11) . . ?
C10 C11 C12 119.31(12) . . ?
C18 C17 C6 112.91(11) . . ?
C10 C9 C8 121.29(12) . . ?
C22 C23 C24 110.67(11) . . ?
C25 C24 C35 110.36(10) . . ?
C25 C24 C23 111.30(10) . . ?
C23 C24 C35 113.90(11) . . ?
C23 C22 C21 110.51(11) . . ?
O2A C16A C1 110.7(15) . . ?
O4A C34A C19 102.7(12) . . ?
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
O1 C15 1.4275(14) . ?
O2 C16 1.4301(18) . ?
O3 C33 1.4322(15) . ?
O4 C34 1.436(3) . ?
C31 C26 1.4069(17) . ?
C31 C30 1.3845(18) . ?
C31 C32 1.5047(16) . ?
C2 C7 1.3561(16) . ?
C2 C1 1.5284(16) . ?
C2 C3 1.5109(17) . ?
C7 C8 1.4875(17) . ?
C7 C6 1.5235(16) . ?
C27 C26 1.4007(16) . ?
C27 C28 1.3856(18) . ?
C25 C26 1.4839(17) . ?
C25 C20 1.3537(17) . ?
C25 C24 1.5205(16) . ?
C8 C13 1.4063(17) . ?
C8 C9 1.4033(17) . ?
C13 C14 1.4957(16) . ?
C13 C12 1.3908(18) . ?
C30 C29 1.3895(18) . ?
C14 C1 1.5338(16) . ?
C19 C32 1.5308(18) . ?
C19 C20 1.5355(16) . ?
C19 C33 1.5425(17) . ?
C19 C34 1.546(2) . ?
C19 C34A 1.559(17) . ?
C15 C1 1.5400(17) . ?
C20 C21 1.5129(18) . ?
C28 C29 1.3832(18) . ?
C1 C16 1.5454(19) . ?
C1 C16A 1.566(18) . ?
C6 C5 1.5300(17) . ?
C6 C17 1.5408(17) . ?
C12 C11 1.3858(18) . ?
C5 C4 1.5199(18) . ?
C4 C3 1.5191(17) . ?
C10 C11 1.380(2) . ?
C10 C9 1.3903(19) . ?
C35 C24 1.5388(19) . ?
C35 C36 1.5151(19) . ?
C21 C22 1.5201(18) . ?
C17 C18 1.5244(18) . ?
C23 C24 1.5306(18) . ?
C23 C22 1.5160(19) . ?
C16A O2A 1.413(18) . ?
C34A O4A 1.430(16) . ?
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-4.3993 -2.4995 -1.4213 -0.0726 -0.2877 0.9550
-0.7234 4.1828 5.7049 0.2177 0.9062 -0.3624
-5.7848 2.1245 5.1265 0.1750 0.7449 0.6438
-4.9855 -1.0242 -2.8136 -0.2719 -0.1438 0.9515
4.3298 0.7146 4.9584 0.4442 0.2381 -0.8637
-1.0705 -1.0067 10.7085 0.8775 0.4783 0.0363
-0.7444 5.9130 0.7834 -0.2625 0.8756 -0.4055
-1.1178 -5.2547 7.2800 0.8274 -0.2896 0.4813
0.3821 -5.4101 7.9066 0.9160 -0.3218 0.2395
5.5719 -1.7183 3.9736 0.5191 -0.1865 -0.8341
0.5683 -5.8811 -0.7569 0.2592 -0.8645 0.4306
5.3511 -4.6175 -1.2290 0.2546 -0.8610 -0.4403
1.2934 -0.4022 -10.1972 -0.7588 -0.6502 0.0384
3.0023 0.0739 -9.9523 -0.7290 -0.6230 -0.2835
-5.4023 4.6771 -1.6770 -0.4886 0.7122 0.5040
-1.1088 6.3623 -2.3171 -0.5387 0.7791 -0.3207
1.1322 -2.5064 -8.3892 -0.5091 -0.8352 0.2080
5.0795 -1.0120 -7.3947 -0.4271 -0.6949 -0.5786
0.2639 1.5240 -10.7206 -0.9221 -0.3838 0.0496
1.2638 1.7738 -10.7305 -0.9153 -0.3801 -0.1331
