#------------------------------------------------------------------------------
#$Date: 2024-07-05 20:24:20 +0300 (Fri, 05 Jul 2024) $
#$Revision: 293167 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/84/7248494.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_7248494
loop_
_publ_author_name
'MacLean, Ian'
'García, Montaña J.'
'Cabrera, Silvia'
'Marzo, Leyre'
'Alemán, José'
_publ_section_title
;
 Electrochemically driven green synthesis to unlock sustainable routes to
 β-keto spirolactones
;
_journal_issue                   11
_journal_name_full               'Green Chemistry'
_journal_page_first              6553
_journal_page_last               6558
_journal_paper_doi               10.1039/D4GC01127A
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'C28 H27 N O2, 3.6(O)'
_chemical_formula_sum            'C28 H27 N O5.6'
_chemical_formula_weight         467.10
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2023-09-20
_audit_creation_method
;
Olex2 1.5-ac5-024
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_audit_update_record
;
2024-03-04 deposited with the CCDC.	2024-04-18 downloaded from the CCDC.
;
_cell_angle_alpha                93.410(2)
_cell_angle_beta                 99.781(2)
_cell_angle_gamma                103.653(2)
_cell_formula_units_Z            2
_cell_length_a                   8.90130(10)
_cell_length_b                   10.1017(2)
_cell_length_c                   15.3407(3)
_cell_measurement_reflns_used    11050
_cell_measurement_temperature    250.00(10)
_cell_measurement_theta_max      68.0780
_cell_measurement_theta_min      2.9620
_cell_volume                     1313.79(4)
_computing_cell_refinement       'CrysAlisPro 1.171.42.101a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.101a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.101a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      250.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 100'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     30.00 112.00   0.50    0.20    --  106.21-125.00-150.00  164
  2  ω     30.00 112.00   0.50    0.20    --  106.21-125.00 -60.00  164
  3  ω     30.00 112.00   0.50    0.20    --  106.21-125.00 -30.00  164
  4  ω      5.00  94.00   0.50    0.10    --   45.89-107.00 101.00  178
  5  ω     31.00 107.00   0.50    0.20    --  106.21-107.00 101.00  152
  6  ω     33.00 105.00   0.50    0.20    --  106.21 -95.00-120.00  144
  7  ω     36.00 109.00   0.50    0.20    --  106.21 -77.00 -90.00  146
  8  ω     25.00  54.00   0.50    0.20    --  106.21 -45.00 -30.00   58
  9  ω     29.00  75.00   0.50    0.20    --  106.21 -61.00  30.00   92
 10  ω     29.00  75.00   0.50    0.20    --  106.21 -61.00  90.00   92
 11  ω     29.00  75.00   0.50    0.20    --  106.21 -61.00 120.00   92
 12  ω     25.00  54.00   0.50    0.20    --  106.21 -45.00  60.00   58
 13  ω    -37.00  30.00   0.50    0.10    --   45.89 -19.00 -30.00  134
 14  ω     81.00 178.00   0.50    0.20    --  106.21  61.00-150.00  194
 15  ω     32.00 133.00   0.50    0.10    --   62.00  76.00 114.40  202
 16  ω     13.00  42.00   0.50    0.10    --   45.89  80.00  -4.23   58
 17  ω     32.00 133.00   0.50    0.10    --   62.00  76.00 -40.39  202
 18  ω     32.00 133.00   0.50    0.10    --   62.00  76.00-179.04  202
 19  ω     16.00  42.00   0.50    0.10    --   50.00  83.00-126.20   52
 20  ω     12.00  42.00   0.50    0.10    --   50.00  89.00 -75.48   60
 21  ω     16.00  42.00   0.50    0.10    --   54.00  89.00 141.37   52
 22  ω     12.00  42.00   0.50    0.10    --   50.00  89.00  72.84   60
 23  ω     90.00 178.00   0.50    0.20    --  106.21 107.00-160.00  176
 24  ω    -95.00   1.00   0.50    0.10    --  -47.39 107.00-160.00  192
 25  ω   -107.00 -13.00   0.50    0.20    --  -88.28 107.00-160.00  188
 26  ω   -120.00 -19.00   0.50    0.20    --  -95.50 136.00 -56.46  202
 27  ω   -124.00 -22.00   0.50    0.20    --  -95.50 142.00 -37.30  204
 28  ω   -108.00 -20.00   0.50    0.20    --  -95.50 111.00 148.77  176
 29  ω   -102.00 -18.00   0.50    0.20    --  -88.28  77.00 120.00  168
 30  ω    -32.00  -6.00   0.50    0.20    --  -88.28  30.00 150.00   52
 31  ω    -32.00  -6.00   0.50    0.20    --  -88.28  30.00  90.00   52
 32  ω    -32.00  -6.00   0.50    0.20    --  -88.28  30.00  60.00   52
 33  ω    -32.00  -6.00   0.50    0.20    --  -88.28  30.00  30.00   52
 34  ω    -23.00  35.00   0.50    0.10    --  -47.39  19.00 -30.00  116
 35  ω    -32.00  -6.00   0.50    0.20    --  -88.28  30.00-180.00   52
 36  ω   -163.00 -83.00   0.50    0.20    --  -88.28-107.00 101.00  160
 37  ω   -164.00 -74.00   0.50    0.20    --  -88.28-125.00 150.00  180
 38  ω   -171.00 -70.00   0.50    0.20    --  -95.50 -64.00 165.85  202
 39  ω   -147.00 -45.00   0.50    0.10    --  -70.00 -60.00  40.58  204
 40  ω   -166.00 -64.00   0.50    0.20    --  -95.50 -77.00  -7.61  204
 41  ω   -168.00 -67.00   0.50    0.20    --  -95.50 -72.00 -36.08  202
 42  ω   -159.00-113.00   0.50    0.20    --  -88.28 -77.00 -90.00   92
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix-Arc 100'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0614784000
_diffrn_orient_matrix_UB_12      -0.0171976000
_diffrn_orient_matrix_UB_13      -0.0869300000
_diffrn_orient_matrix_UB_21      0.1231201000
_diffrn_orient_matrix_UB_22      -0.0686243000
_diffrn_orient_matrix_UB_23      0.0482360000
_diffrn_orient_matrix_UB_31      -0.1181767000
_diffrn_orient_matrix_UB_32      -0.1410480000
_diffrn_orient_matrix_UB_33      -0.0247901000
_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  0.0279
_diffrn_reflns_av_unetI/netI     0.0196
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            24018
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.437
_diffrn_reflns_theta_min         2.939
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.671
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.676
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.101a (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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.181
_exptl_crystal_description       plate
_exptl_crystal_F_000             494
_exptl_crystal_recrystallization_method 'obtained from dichloromethane'
_exptl_crystal_size_max          0.302
_exptl_crystal_size_mid          0.136
_exptl_crystal_size_min          0.021
_refine_diff_density_max         0.696
_refine_diff_density_min         -0.321
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     329
_refine_ls_number_reflns         4817
_refine_ls_number_restraints     278
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0827
_refine_ls_R_factor_gt           0.0766
_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)+(0.1486P)²+0.4142P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2364
_refine_ls_wR_factor_ref         0.2430
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4132
_reflns_number_total             4817
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4gc01127a2.cif
_cod_data_source_block           03904
_cod_depositor_comments          'Adding full bibliography for 7248494.cif.'
_cod_original_formula_sum        'C28 H27 N O5.60'
_cod_database_code               7248494
_shelx_shelxl_version_number     2019/1
_chemical_oxdiff_formula         C28H27NO2
_chemical_oxdiff_usercomment     IMG-150.F4
_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   0.986
_shelx_estimated_absorpt_t_min   0.823
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C26-C27A = C27A-C28A = C26-C27B = C27B-C28B
 1.5 with sigma of 0.02
 C25-C27A = C25-C27B = C26-C28A = C26-C28B
 2.5 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C27A) = Uanis(C27B)
Uanis(C28A) = Uanis(C28B)
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(H26C)=Sof(H26D)=Sof(C27B)=Sof(H27C)=Sof(H27D)=Sof(C28B)=Sof(H28D)=
 Sof(H28E)=Sof(H28F)=1-FVAR(1)
 Sof(H26A)=Sof(H26B)=Sof(C27A)=Sof(H27A)=Sof(H27B)=Sof(C28A)=Sof(H28A)=
 Sof(H28B)=Sof(H28C)=FVAR(1)
 Fixed Sof: O3W(0.25) O4W(0.5) O5W(0.75) O6W(0.3) O7W(0.25) O8W(0.3) O9W(0.5)
 O10W(0.25) O11W(0.25) O12W(0.25)
6.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C12(H12A,H12B), C25(H25A,H25B), C26(H26A,H26B), C26(H26C,H26D),
 C27A(H27A,H27B), C27B(H27C,H27D)
6.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C10(H10), C14(H14), C15(H15), C16(H16), C17(H17),
 C18(H18), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24)
6.c Idealised Me refined as rotating group:
 C28A(H28A,H28B,H28C), C28B(H28D,H28E,H28F)
;
_olex2_exptl_crystal_mounting_method 'placed on a MiTeGen micromount'
_olex2_submission_original_sample_id IMG-150.F4
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.650
_oxdiff_exptl_absorpt_empirical_full_min 0.767
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
C1 C 0.4217(2) 0.5493(2) 0.83833(15) 0.0470(5) Uani 1 1 d . . . . .
C2 C 0.3233(3) 0.4615(2) 0.89576(15) 0.0477(5) Uani 1 1 d . . . . .
H2A H 0.278389 0.517608 0.933400 0.057 Uiso 1 1 calc R U . . .
H2B H 0.386447 0.411998 0.933628 0.057 Uiso 1 1 calc R U . . .
C3 C 0.1930(2) 0.3617(2) 0.82736(15) 0.0461(5) Uani 1 1 d . . . . .
C4 C 0.2978(3) 0.5505(2) 0.75703(16) 0.0520(5) Uani 1 1 d . . . . .
C5 C 0.4965(3) 0.6969(2) 0.88133(15) 0.0499(5) Uani 1 1 d . . . . .
C6 C 0.6573(3) 0.7371(2) 0.86489(16) 0.0541(6) Uani 1 1 d . . . . .
C7 C 0.7647(4) 0.8657(3) 0.8845(2) 0.0712(7) Uani 1 1 d . . . . .
H7 H 0.737811 0.940331 0.911874 0.085 Uiso 1 1 calc R U . . .
C8 C 0.9099(4) 0.8795(4) 0.8626(2) 0.0861(9) Uani 1 1 d . . . . .
H8 H 0.983685 0.965033 0.873976 0.103 Uiso 1 1 calc R U . . .
C9 C 0.9490(4) 0.7670(4) 0.8233(2) 0.0854(9) Uani 1 1 d . . . . .
H9 H 1.049918 0.778153 0.809502 0.102 Uiso 1 1 calc R U . . .
C10 C 0.8445(3) 0.6406(4) 0.8044(2) 0.0720(7) Uani 1 1 d . . . . .
H10 H 0.872680 0.565911 0.778003 0.086 Uiso 1 1 calc R U . . .
C11 C 0.6954(3) 0.6259(3) 0.82532(17) 0.0558(6) Uani 1 1 d . . . . .
C12 C 0.5619(3) 0.4988(2) 0.81226(18) 0.0567(6) Uani 1 1 d . . . . .
H12A H 0.589017 0.430459 0.850658 0.068 Uiso 1 1 calc R U . . .
H12B H 0.536205 0.458411 0.750224 0.068 Uiso 1 1 calc R U . . .
C13 C 0.2447(2) 0.2358(2) 0.79632(16) 0.0506(5) Uani 1 1 d . . . . .
C14 C 0.2842(3) 0.1491(2) 0.8591(2) 0.0581(6) Uani 1 1 d . . . . .
H14 H 0.280702 0.170638 0.919041 0.070 Uiso 1 1 calc R U . . .
C15 C 0.3284(3) 0.0323(3) 0.8345(3) 0.0757(8) Uani 1 1 d . . . . .
H15 H 0.355368 -0.024482 0.877731 0.091 Uiso 1 1 calc R U . . .
C16 C 0.3331(4) -0.0010(3) 0.7476(3) 0.0869(10) Uani 1 1 d . . . . .
H16 H 0.362425 -0.080838 0.730681 0.104 Uiso 1 1 calc R U . . .
C17 C 0.2945(4) 0.0835(4) 0.6849(3) 0.0898(10) Uani 1 1 d . . . . .
H17 H 0.298066 0.060966 0.625095 0.108 Uiso 1 1 calc R U . . .
C18 C 0.2503(4) 0.2013(3) 0.7087(2) 0.0716(7) Uani 1 1 d . . . . .
H18 H 0.224120 0.257848 0.665083 0.086 Uiso 1 1 calc R U . . .
C19 C 0.0344(3) 0.3168(2) 0.85504(16) 0.0494(5) Uani 1 1 d . . . . .
C20 C -0.0985(3) 0.2588(3) 0.78992(19) 0.0617(6) Uani 1 1 d . . . . .
H20 H -0.088387 0.250101 0.729967 0.074 Uiso 1 1 calc R U . . .
C21 C -0.2444(3) 0.2139(3) 0.8121(2) 0.0704(7) Uani 1 1 d . . . . .
H21 H -0.332965 0.175429 0.767329 0.084 Uiso 1 1 calc R U . . .
C22 C -0.2608(3) 0.2253(3) 0.8994(2) 0.0664(7) Uani 1 1 d . . . . .
H22 H -0.360398 0.195246 0.914486 0.080 Uiso 1 1 calc R U . . .
C23 C -0.1309(3) 0.2808(3) 0.9645(2) 0.0648(7) Uani 1 1 d . . . . .
H23 H -0.141810 0.288089 1.024393 0.078 Uiso 1 1 calc R U . . .
C24 C 0.0163(3) 0.3263(3) 0.94265(18) 0.0586(6) Uani 1 1 d . . . . .
H24 H 0.104419 0.363971 0.987839 0.070 Uiso 1 1 calc R U . . .
C25 C 0.1761(4) 0.6249(4) 0.6283(2) 0.0921(10) Uani 1 1 d D . . . .
H25A H 0.107849 0.681102 0.645476 0.111 Uiso 1 1 calc R U . . .
H25B H 0.114195 0.529398 0.617079 0.111 Uiso 1 1 calc R U . . .
C26 C 0.2287(5) 0.6692(5) 0.5454(2) 0.1034(12) Uani 1 1 d D . . . .
H26A H 0.140330 0.685568 0.503574 0.124 Uiso 0.478(15) 1 calc R U P A 1
H26B H 0.311898 0.754556 0.558970 0.124 Uiso 0.478(15) 1 calc R U P A 1
H26C H 0.134982 0.647088 0.498049 0.124 Uiso 0.522(15) 1 calc R U P A 2
H26D H 0.265957 0.769268 0.554059 0.124 Uiso 0.522(15) 1 calc R U P A 2
C27A C 0.287(2) 0.5622(17) 0.5064(10) 0.119(3) Uani 0.478(15) 1 d D . P A 1
H27A H 0.207920 0.475118 0.501657 0.143 Uiso 0.478(15) 1 calc R U P A 1
H27B H 0.381844 0.553883 0.546896 0.143 Uiso 0.478(15) 1 calc R U P A 1
C27B C 0.3512(17) 0.6163(18) 0.5111(9) 0.119(3) Uani 0.522(15) 1 d D . P A 2
H27C H 0.318701 0.516096 0.507177 0.143 Uiso 0.522(15) 1 calc R U P A 2
H27D H 0.448124 0.645614 0.556056 0.143 Uiso 0.522(15) 1 calc R U P A 2
C28A C 0.327(3) 0.584(2) 0.4175(11) 0.143(5) Uani 0.478(15) 1 d D . P A 1
H28A H 0.417865 0.660994 0.422997 0.214 Uiso 0.478(15) 1 calc R U P A 1
H28B H 0.238217 0.602060 0.378483 0.214 Uiso 0.478(15) 1 calc R U P A 1
H28C H 0.351183 0.502144 0.392955 0.214 Uiso 0.478(15) 1 calc R U P A 1
C28B C 0.392(3) 0.653(2) 0.4246(10) 0.143(5) Uani 0.522(15) 1 d D . P A 2
H28D H 0.448195 0.749190 0.430489 0.214 Uiso 0.522(15) 1 calc R U P A 2
H28E H 0.296562 0.637848 0.380149 0.214 Uiso 0.522(15) 1 calc R U P A 2
H28F H 0.458449 0.597260 0.406557 0.214 Uiso 0.522(15) 1 calc R U P A 2
N1 N 0.3093(3) 0.6369(2) 0.70184(15) 0.0704(6) Uani 1 1 d . . . . .
O4 O 0.4305(2) 0.76386(17) 0.92279(13) 0.0653(5) Uani 1 1 d . . . . .
O5 O 0.16925(18) 0.44330(16) 0.75344(11) 0.0553(4) Uani 1 1 d . . . . .
O3W O 0.335(2) 1.1184(15) 0.3640(10) 0.120(4) Uiso 0.25 1 d . . P B 4
O4W O 0.3788(9) 1.0301(8) 0.4153(5) 0.101(2) Uiso 0.5 1 d . . P C 3
O5W O 0.3288(6) 0.9937(5) 0.4143(2) 0.0795(10) Uiso 0.75 1 d . . P D 1
O6W O 0.753(3) 0.8915(18) 0.6394(11) 0.154(5) Uiso 0.3 1 d . . P E 5
O7W O 0.866(2) 0.9334(19) 0.6252(11) 0.143(5) Uiso 0.25 1 d . . P F 2
O8W O 0.0907(9) 0.1459(8) 0.4544(5) 0.0696(17) Uiso 0.3 1 d . . P G 1
O9W O 0.1557(8) 0.2011(7) 0.4423(5) 0.0838(15) Uiso 0.5 1 d . . P H 3
O10W O 0.2085(10) 0.2295(8) 0.4182(5) 0.0584(18) Uiso 0.25 1 d . . P I 4
O11W O 0.1233(13) 0.1672(12) 0.4107(8) 0.076(3) Uiso 0.25 1 d . . P J 5
O12W O 0.2565(12) 0.9613(9) 0.4232(5) 0.066(2) Uiso 0.25 1 d . . P K 5
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'
N N 0.0311 0.0180 '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
2 0 1 0.1133
0 2 -1 0.0513
0 -2 1 0.0784
2 2 -1 0.0979
0 2 1 0.0519
-2 0 1 0.1407
-1 0 0 0.1363
-3 0 -1 0.1296
-1 0 -1 0.1128
0 0 -1 0.0089
0 0 1 0.0121
-1 -3 -2 0.0989
1 -2 1 0.1076
1 -2 3 0.0807
2 0 3 0.0872
-1 -2 1 0.1169
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
C2 C1 C5 113.18(18) . . ?
C2 C1 C12 117.05(19) . . ?
C4 C1 C2 101.41(17) . . ?
C4 C1 C5 109.44(18) . . ?
C4 C1 C12 111.51(19) . . ?
C5 C1 C12 104.30(18) . . ?
C1 C2 C3 103.55(18) . . ?
C13 C3 C2 112.26(18) . . ?
C19 C3 C2 115.81(19) . . ?
C19 C3 C13 109.57(17) . . ?
O5 C3 C2 102.92(16) . . ?
O5 C3 C13 109.69(18) . . ?
O5 C3 C19 106.08(17) . . ?
N1 C4 C1 125.6(2) . . ?
N1 C4 O5 124.5(2) . . ?
O5 C4 C1 109.85(18) . . ?
C6 C5 C1 108.08(19) . . ?
O4 C5 C1 124.2(2) . . ?
O4 C5 C6 127.7(2) . . ?
C7 C6 C5 128.3(2) . . ?
C11 C6 C5 110.0(2) . . ?
C11 C6 C7 121.8(2) . . ?
C8 C7 C6 118.0(3) . . ?
C7 C8 C9 120.3(3) . . ?
C10 C9 C8 121.9(3) . . ?
C9 C10 C11 118.3(3) . . ?
C6 C11 C10 119.8(2) . . ?
C6 C11 C12 111.9(2) . . ?
C10 C11 C12 128.3(3) . . ?
C11 C12 C1 104.52(19) . . ?
C14 C13 C3 118.5(2) . . ?
C18 C13 C3 123.2(2) . . ?
C18 C13 C14 118.2(2) . . ?
C15 C14 C13 121.0(3) . . ?
C16 C15 C14 120.3(3) . . ?
C15 C16 C17 119.4(3) . . ?
C16 C17 C18 121.0(3) . . ?
C13 C18 C17 120.1(3) . . ?
C20 C19 C3 118.9(2) . . ?
C24 C19 C3 122.9(2) . . ?
C24 C19 C20 118.1(2) . . ?
C21 C20 C19 121.0(3) . . ?
C22 C21 C20 120.1(3) . . ?
C21 C22 C23 119.7(2) . . ?
C22 C23 C24 120.5(3) . . ?
C19 C24 C23 120.6(2) . . ?
N1 C25 C26 112.0(3) . . ?
C27A C26 C25 108.4(8) . . ?
C27B C26 C25 121.1(7) . . ?
C26 C27A C28A 115.0(14) . . ?
C26 C27B C28B 119.9(13) . . ?
C4 N1 C25 118.5(2) . . ?
C4 O5 C3 110.93(17) . . ?
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
C1 C2 1.523(3) . ?
C1 C4 1.521(3) . ?
C1 C5 1.539(3) . ?
C1 C12 1.557(3) . ?
C2 C3 1.540(3) . ?
C3 C13 1.528(3) . ?
C3 C19 1.518(3) . ?
C3 O5 1.457(3) . ?
C4 N1 1.251(3) . ?
C4 O5 1.368(3) . ?
C5 C6 1.462(3) . ?
C5 O4 1.212(3) . ?
C6 C7 1.401(3) . ?
C6 C11 1.383(4) . ?
C7 C8 1.368(5) . ?
C8 C9 1.398(6) . ?
C9 C10 1.372(5) . ?
C10 C11 1.394(4) . ?
C11 C12 1.506(3) . ?
C13 C14 1.395(4) . ?
C13 C18 1.380(4) . ?
C14 C15 1.380(4) . ?
C15 C16 1.366(5) . ?
C16 C17 1.376(6) . ?
C17 C18 1.386(5) . ?
C19 C20 1.394(3) . ?
C19 C24 1.381(4) . ?
C20 C21 1.378(4) . ?
C21 C22 1.372(4) . ?
C22 C23 1.373(4) . ?
C23 C24 1.387(4) . ?
C25 C26 1.486(5) . ?
C25 N1 1.468(4) . ?
C26 C27A 1.448(12) . ?
C26 C27B 1.480(11) . ?
C27A C28A 1.481(13) . ?
C27B C28B 1.480(13) . ?
O6W O11W 1.65(2) 2_666 ?
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C13 85.5(2) . . . . ?
C1 C2 C3 C19 -147.66(18) . . . . ?
C1 C2 C3 O5 -32.4(2) . . . . ?
C1 C4 N1 C25 -178.3(3) . . . . ?
C1 C4 O5 C3 -0.9(2) . . . . ?
C1 C5 C6 C7 173.7(3) . . . . ?
C1 C5 C6 C11 -6.6(3) . . . . ?
C2 C1 C4 N1 159.4(3) . . . . ?
C2 C1 C4 O5 -19.7(2) . . . . ?
C2 C1 C5 C6 138.92(19) . . . . ?
C2 C1 C5 O4 -39.6(3) . . . . ?
C2 C1 C12 C11 -136.4(2) . . . . ?
C2 C3 C13 C14 61.8(3) . . . . ?
C2 C3 C13 C18 -119.9(2) . . . . ?
C2 C3 C19 C20 162.5(2) . . . . ?
C2 C3 C19 C24 -19.9(3) . . . . ?
C2 C3 O5 C4 21.0(2) . . . . ?
C3 C13 C14 C15 178.6(2) . . . . ?
C3 C13 C18 C17 -178.3(3) . . . . ?
C3 C19 C20 C21 178.7(2) . . . . ?
C3 C19 C24 C23 -178.5(2) . . . . ?
C4 C1 C2 C3 31.2(2) . . . . ?
C4 C1 C5 C6 -108.8(2) . . . . ?
C4 C1 C5 O4 72.6(3) . . . . ?
C4 C1 C12 C11 107.5(2) . . . . ?
C5 C1 C2 C3 148.32(18) . . . . ?
C5 C1 C4 N1 39.6(3) . . . . ?
C5 C1 C4 O5 -139.53(19) . . . . ?
C5 C1 C12 C11 -10.5(2) . . . . ?
C5 C6 C7 C8 -179.8(3) . . . . ?
C5 C6 C11 C10 -179.4(2) . . . . ?
C5 C6 C11 C12 -0.6(3) . . . . ?
C6 C7 C8 C9 -1.1(5) . . . . ?
C6 C11 C12 C1 7.3(3) . . . . ?
C7 C6 C11 C10 0.3(4) . . . . ?
C7 C6 C11 C12 179.1(2) . . . . ?
C7 C8 C9 C10 0.9(5) . . . . ?
C8 C9 C10 C11 0.0(5) . . . . ?
C9 C10 C11 C6 -0.6(4) . . . . ?
C9 C10 C11 C12 -179.2(3) . . . . ?
C10 C11 C12 C1 -174.0(3) . . . . ?
C11 C6 C7 C8 0.6(4) . . . . ?
C12 C1 C2 C3 -90.3(2) . . . . ?
C12 C1 C4 N1 -75.3(3) . . . . ?
C12 C1 C4 O5 105.6(2) . . . . ?
C12 C1 C5 C6 10.6(2) . . . . ?
C12 C1 C5 O4 -167.9(2) . . . . ?
C13 C3 C19 C20 -69.3(3) . . . . ?
C13 C3 C19 C24 108.4(2) . . . . ?
C13 C3 O5 C4 -98.7(2) . . . . ?
C13 C14 C15 C16 -0.5(4) . . . . ?
C14 C13 C18 C17 -0.1(4) . . . . ?
C14 C15 C16 C17 0.5(4) . . . . ?
C15 C16 C17 C18 -0.3(5) . . . . ?
C16 C17 C18 C13 0.1(5) . . . . ?
C18 C13 C14 C15 0.3(3) . . . . ?
C19 C3 C13 C14 -68.3(2) . . . . ?
C19 C3 C13 C18 109.9(2) . . . . ?
C19 C3 O5 C4 143.09(19) . . . . ?
C19 C20 C21 C22 -0.3(4) . . . . ?
C20 C19 C24 C23 -0.8(4) . . . . ?
C20 C21 C22 C23 -0.4(4) . . . . ?
C21 C22 C23 C24 0.5(4) . . . . ?
C22 C23 C24 C19 0.2(4) . . . . ?
C24 C19 C20 C21 0.9(4) . . . . ?
C25 C26 C27A C28A 173.1(11) . . . . ?
C25 C26 C27B C28B 175.0(9) . . . . ?
C26 C25 N1 C4 -145.9(3) . . . . ?
N1 C4 O5 C3 180.0(2) . . . . ?
N1 C25 C26 C27A 76.0(9) . . . . ?
N1 C25 C26 C27B 49.9(9) . . . . ?
O4 C5 C6 C7 -7.8(4) . . . . ?
O4 C5 C6 C11 171.9(2) . . . . ?
O5 C3 C13 C14 175.60(18) . . . . ?
O5 C3 C13 C18 -6.1(3) . . . . ?
O5 C3 C19 C20 49.1(3) . . . . ?
O5 C3 C19 C24 -133.3(2) . . . . ?
O5 C4 N1 C25 0.7(4) . . . . ?
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
1.9978 0.0055 1.0075 0.0351 0.2942 -0.2618
-0.0040 2.0004 -0.9970 0.0520 -0.1859 -0.2570
0.0040 -2.0004 0.9970 -0.0520 0.1859 0.2570
1.9949 2.0069 -0.9919 0.1744 0.0600 -0.4942
-0.0063 1.9983 1.0078 -0.1224 -0.0893 -0.3061
-2.0001 -0.0075 0.9973 -0.2095 -0.1976 0.2127
-0.9995 -0.0032 -0.0026 -0.0612 -0.1230 0.1186
-2.9972 -0.0087 -1.0100 -0.0963 -0.4171 0.3805
-0.9983 -0.0022 -1.0049 0.0260 -0.1712 0.1432
0.0012 0.0010 -1.0024 0.0872 -0.0483 0.0246
-0.0012 -0.0010 1.0024 -0.0872 0.0483 -0.0246
-0.9894 -3.0003 -2.0154 0.1660 -0.0131 0.5901
1.0035 -1.9972 0.9996 0.0091 0.3088 0.1383
1.0012 -1.9992 3.0043 -0.1652 0.4054 0.0892
1.9955 0.0034 3.0123 -0.1392 0.3907 -0.3110
-0.9955 -2.0037 0.9945 -0.1132 0.0629 0.3756
