#------------------------------------------------------------------------------
#$Date: 2020-10-06 10:25:03 +0300 (Tue, 06 Oct 2020) $
#$Revision: 257364 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/74/1557451.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_1557451
loop_
_publ_author_name
'Sharma, Mahendra K.'
'Blomeyer, Sebastian'
'Glodde, Timo'
'Neumann, Beate'
'Stammler, Hans-Georg'
'Hinz, Alexander'
'van Gastel, Maurice'
'Ghadwal, Rajendra S.'
_publ_section_title
;
 Isolation of singlet carbene derived 2-phospha-1,3-butadienes and their
 sequential one-electron oxidation to radical cations and dications
;
_journal_issue                   7
_journal_name_full               'Chemical Science'
_journal_page_first              1975
_journal_page_last               1984
_journal_paper_doi               10.1039/C9SC05598C
_journal_volume                  11
_journal_year                    2020
_chemical_formula_moiety         'C57 H76 N3 P'
_chemical_formula_sum            'C57 H76 N3 P'
_chemical_formula_weight         834.17
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2019-08-02
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2019-08-28 deposited with the CCDC.	2020-01-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.6144(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.56527(11)
_cell_length_b                   11.96597(7)
_cell_length_c                   22.85445(16)
_cell_measurement_reflns_used    64190
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      76.3380
_cell_measurement_theta_min      3.6430
_cell_volume                     4973.19(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.58a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.58a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.58a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -64.00  30.00   1.00    2.50    --  -38.50  57.00 120.00   94
  2  ω   -124.00  47.00   1.00    2.50    --  -38.50   0.00  60.00  171
  3  ω    -87.00  -6.00   1.00    2.50    --  -38.50 125.00 150.00   81
  4  ω     18.00 111.00   1.00    2.50    --   42.89  57.00-120.00   93
  5  ω     18.00 111.00   1.00    2.50    --   42.89  57.00 120.00   93
  6  ω     22.00 114.00   1.00    2.50    --   42.89  38.00  30.00   92
  7  ω     14.00 113.00   1.00    2.50    --   42.89  73.00-101.60   99
  8  ω     27.00  97.00   1.00    2.50    --   42.89-125.00  30.00   70
  9  ω     14.00 113.00   1.00    2.50    --   42.89  72.00 140.00   99
 10  ω     12.00  42.00   1.00    2.50    --   42.89  81.00 178.39   30
 11  ω     12.00  42.00   1.00    2.50    --   42.89  81.00 101.76   30
 12  ω     12.00  42.00   1.00    2.50    --   42.89  80.00 -52.82   30
 13  ω     12.00  42.00   1.00    2.50    --   42.89  81.00  34.54   30
 14  ω     15.00 112.00   1.00    2.50    --   42.89  68.00 -21.87   97
 15  ω     14.00 113.00   1.00    2.50    --   42.89  72.00  29.88   99
 16  ω     27.00  97.00   1.00    2.50    --   42.89-125.00 -30.00   70
 17  ω     82.00 178.00   1.00   10.00    --  111.00  72.00 163.64   96
 18  ω     85.00 178.00   1.00   10.00    --  111.00  61.00-175.96   93
 19  ω     84.00 178.00   1.00   10.00    --  111.00  63.00 136.57   94
 20  ω     82.00 178.00   1.00   10.00    --  111.00  74.00 107.27   96
 21  ω     86.00 178.00   1.00   10.00    --  111.00  55.00 174.59   92
 22  ω     85.00 178.00   1.00   10.00    --  111.00  60.00  45.28   93
 23  ω     85.00 178.00   1.00   10.00    --  111.00  61.00  47.09   93
 24  ω     86.00 178.00   1.00   10.00    --  111.00  58.00 -76.64   92
 25  ω     85.00 178.00   1.00   10.00    --  111.00  61.00-126.03   93
 26  ω     82.00 178.00   1.00   10.00    --  111.00  72.00 -82.85   96
 27  ω     85.00 178.00   1.00   10.00    --  111.00  62.00-168.96   93
 28  ω     85.00 178.00   1.00   10.00    --  111.00  61.00-150.00   93
 29  ω     83.00 178.00   1.00   10.00    --  111.00  70.00   4.84   95
 30  ω     84.00 178.00   1.00   10.00    --  111.00  65.00-161.95   94
 31  ω     86.00 178.00   1.00   10.00    --  111.00  58.00  -0.31   92
 32  ω     83.00 178.00   1.00   10.00    --  111.00  68.00-111.86   95
 33  ω     31.00 107.00   1.00   10.00    --  111.00 -94.00 150.00   76
 34  ω     83.00 178.00   1.00   10.00    --  111.00  67.00  61.43   95
 35  ω     83.00 178.00   1.00   10.00    --  111.00  69.00 -26.70   95
 36  ω     86.00 178.00   1.00   10.00    --  111.00  58.00 100.14   92
 37  ω     40.00 141.00   1.00   10.00    --  111.00 -77.00 -60.00  101
 38  ω     31.00 107.00   1.00   10.00    --  111.00 -94.00 -90.00   76
 39  ω     31.00 107.00   1.00   10.00    --  111.00 -94.00  90.00   76
 40  ω     85.00 178.00   1.00   10.00    --  111.00  62.00-140.37   93
 41  ω     34.00 107.00   1.00   10.00    --  111.00-101.00-139.95   73
 42  ω     84.00 178.00   1.00   10.00    --  111.00  64.00 -39.03   94
 43  ω     41.00 133.00   1.00   10.00    --  111.00 -45.00 120.00   92
 44  ω     85.00 165.00   1.00   10.00    --  111.00  61.00  30.00   80
 45  ω     33.00 107.00   1.00   10.00    --  111.00 -94.00  60.00   74
 46  ω     85.00 111.00   1.00   10.00    --  111.00  61.00  90.00   26
 47  ω     85.00 112.00   1.00   10.00    --  111.00  61.00   0.00   27
 48  ω     85.00 112.00   1.00   10.00    --  111.00  61.00 -30.00   27
 49  ω     87.00 112.00   1.00   10.00    --  111.00  56.00  82.08   25
 50  ω     89.00 116.00   1.00   10.00    --  111.00  45.00-180.00   27
 51  ω     86.00 122.00   1.00   10.00    --  111.00  55.00 117.00   36
 52  ω     85.00 165.00   1.00   10.00    --  111.00  61.00-120.00   80
 53  ω     53.00  80.00   1.00   10.00    --  111.00 -94.00 120.00   27
 54  ω     82.00 107.00   1.00   10.00    --  111.00 -94.00 120.00   25
 55  ω     49.00 108.00   1.00   10.00    --  111.00-105.00  18.55   59
 56  ω     86.00 112.00   1.00   10.00    --  111.00  55.00  67.05   26
 57  ω     84.00 110.00   1.00   10.00    --  111.00  63.00 -51.59   26
 58  ω    119.00 177.00   1.00   10.00    --  111.00  70.00 142.33   58
 59  ω     85.00 176.00   1.00   10.00    --  111.00  61.00 -60.00   91
 60  ω     86.00 111.00   1.00   10.00    --  111.00  61.00 -90.00   25
 61  ω     83.00 109.00   1.00   10.00    --  111.00  70.00 142.33   26
 62  ω     85.00 111.00   1.00   10.00    --  111.00  59.00 -91.60   26
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0793358000
_diffrn_orient_matrix_UB_12      0.0281599000
_diffrn_orient_matrix_UB_13      0.0314052000
_diffrn_orient_matrix_UB_21      0.0056074000
_diffrn_orient_matrix_UB_22      -0.1129886000
_diffrn_orient_matrix_UB_23      0.0329524000
_diffrn_orient_matrix_UB_31      0.0291181000
_diffrn_orient_matrix_UB_32      -0.0550007000
_diffrn_orient_matrix_UB_33      -0.0516063000
_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  0.0828
_diffrn_reflns_av_unetI/netI     0.0277
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            142708
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.911
_diffrn_reflns_theta_min         2.430
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.770
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.471
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.58a (Rigaku Oxford Diffraction, 2019)
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 brownish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.114
_exptl_crystal_description       block
_exptl_crystal_F_000             1816
_exptl_crystal_size_max          0.428
_exptl_crystal_size_mid          0.332
_exptl_crystal_size_min          0.245
_refine_diff_density_max         0.669
_refine_diff_density_min         -0.454
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     564
_refine_ls_number_reflns         10414
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0459
_refine_ls_R_factor_gt           0.0419
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0766P)²+1.1302P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1173
_refine_ls_wR_factor_ref         0.1215
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9389
_reflns_number_total             10414
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9sc05598c2.cif
_cod_data_source_block           compound5
_cod_depositor_comments
'Adding full bibliography for 1557449--1557455.cif.'
_cod_original_cell_volume        4973.19(5)
_cod_database_code               1557451
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C57H76N3P
_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.
;
_diffrn_oxdiff_digest_frames
;
012caedbe09c26fa864cd64709c4de2f4304536cee8
;
_diffrn_oxdiff_digest_hkl
;
0155ef85aaaa70260cfd703a959ba82dba7b28
;
_reflns_odcompleteness_completeness 99.99
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_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
2.a Ternary CH refined with riding coordinates:
 C20(H20), C23(H23), C32(H32), C35(H35), C50(H50), C53(H53)
2.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B),
 C13(H13A,H13B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C16(H16), C17(H17), C18(H18), C28(H28), C29(H29), C30(H30),
 C38(H38), C39(H39), C40(H40), C41(H41), C42(H42), C46(H46), C47(H47), C48(H48)
2.d Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C25(H25A,H25B,
 H25C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C36(H36A,H36B,H36C), C37(H37A,
 H37B,H37C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C54(H54A,H54B,H54C),
 C55(H55A,H55B,H55C), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C)
;
_olex2_date_sample_data_collection 2019-08-01
_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 5.777
_oxdiff_exptl_absorpt_empirical_full_min 0.249
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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
P1 P 0.27082(2) 0.53303(2) 0.14106(2) 0.01600(8) Uani 1 1 d . . . . .
N1 N 0.13070(5) 0.62785(8) 0.18616(4) 0.01654(19) Uani 1 1 d . . . . .
N2 N 0.11881(5) 0.48645(8) 0.24544(4) 0.01628(19) Uani 1 1 d . . . . .
N3 N 0.39790(5) 0.53036(8) 0.10419(4) 0.01702(19) Uani 1 1 d . . . . .
C1 C 0.16883(6) 0.53435(8) 0.21360(5) 0.0151(2) Uani 1 1 d . . . . .
C2 C 0.06105(6) 0.63422(9) 0.20059(5) 0.0199(2) Uani 1 1 d . . . . .
H2 H 0.024904 0.689559 0.186866 0.024 Uiso 1 1 calc R . . . .
C3 C 0.05408(6) 0.54962(10) 0.23677(5) 0.0199(2) Uani 1 1 d . . . . .
H3 H 0.012417 0.534673 0.253786 0.024 Uiso 1 1 calc R . . . .
C4 C 0.23705(6) 0.49459(9) 0.20776(5) 0.0154(2) Uani 1 1 d . . . . .
C5 C 0.36613(6) 0.52744(8) 0.15421(5) 0.0153(2) Uani 1 1 d . . . . .
C6 C 0.47990(6) 0.52651(9) 0.11766(5) 0.0194(2) Uani 1 1 d . . . . .
C7 C 0.49534(6) 0.56674(10) 0.18238(5) 0.0201(2) Uani 1 1 d . . . . .
H7A H 0.500552 0.649081 0.183949 0.024 Uiso 1 1 calc R . . . .
H7B H 0.541424 0.533077 0.204777 0.024 Uiso 1 1 calc R . . . .
C8 C 0.42939(6) 0.53009(9) 0.20985(5) 0.0166(2) Uani 1 1 d . . . . .
C9 C 0.41197(6) 0.61716(9) 0.25452(5) 0.0208(2) Uani 1 1 d . . . . .
H9A H 0.404895 0.690978 0.234631 0.025 Uiso 1 1 calc R . . . .
H9B H 0.365285 0.596543 0.266383 0.025 Uiso 1 1 calc R . . . .
C10 C 0.47263(7) 0.62665(11) 0.31066(6) 0.0271(3) Uani 1 1 d . . . . .
H10A H 0.518085 0.655151 0.299504 0.033 Uiso 1 1 calc R . . . .
H10B H 0.457410 0.680900 0.338552 0.033 Uiso 1 1 calc R . . . .
C11 C 0.48848(8) 0.51395(11) 0.34193(5) 0.0290(3) Uani 1 1 d . . . . .
H11A H 0.529863 0.521908 0.376532 0.035 Uiso 1 1 calc R . . . .
H11B H 0.444714 0.489033 0.356986 0.035 Uiso 1 1 calc R . . . .
C12 C 0.50786(7) 0.42678(10) 0.29898(5) 0.0243(2) Uani 1 1 d . . . . .
H12A H 0.515155 0.353381 0.319294 0.029 Uiso 1 1 calc R . . . .
H12B H 0.554511 0.447931 0.287215 0.029 Uiso 1 1 calc R . . . .
C13 C 0.44668(6) 0.41708(9) 0.24286(5) 0.0180(2) Uani 1 1 d . . . . .
H13A H 0.401464 0.388673 0.254465 0.022 Uiso 1 1 calc R . . . .
H13B H 0.461714 0.362121 0.215233 0.022 Uiso 1 1 calc R . . . .
C14 C 0.15373(6) 0.72256(9) 0.15568(5) 0.0174(2) Uani 1 1 d . . . . .
C15 C 0.12318(6) 0.73545(10) 0.09465(5) 0.0204(2) Uani 1 1 d . . . . .
C16 C 0.13037(7) 0.83945(10) 0.06878(5) 0.0261(3) Uani 1 1 d . . . . .
H16 H 0.108871 0.851036 0.027868 0.031 Uiso 1 1 calc R . . . .
C17 C 0.16807(8) 0.92574(10) 0.10142(6) 0.0291(3) Uani 1 1 d . . . . .
H17 H 0.171322 0.996465 0.083243 0.035 Uiso 1 1 calc R . . . .
C18 C 0.20131(8) 0.90914(10) 0.16095(6) 0.0268(3) Uani 1 1 d . . . . .
H18 H 0.229204 0.967814 0.182585 0.032 Uiso 1 1 calc R . . . .
C19 C 0.19439(6) 0.80775(9) 0.18941(5) 0.0204(2) Uani 1 1 d . . . . .
C20 C 0.08437(7) 0.64136(11) 0.05632(5) 0.0241(2) Uani 1 1 d . . . . .
H20 H 0.087497 0.572761 0.081706 0.029 Uiso 1 1 calc R . . . .
C21 C 0.12282(7) 0.61648(11) 0.00420(5) 0.0274(3) Uani 1 1 d . . . . .
H21A H 0.120437 0.682686 -0.021354 0.041 Uiso 1 1 calc GR . . . .
H21B H 0.098171 0.553768 -0.019222 0.041 Uiso 1 1 calc GR . . . .
H21C H 0.174367 0.597107 0.019932 0.041 Uiso 1 1 calc GR . . . .
C22 C 0.00274(8) 0.66844(14) 0.03344(6) 0.0354(3) Uani 1 1 d . . . . .
H22A H -0.021810 0.675656 0.067405 0.053 Uiso 1 1 calc GR . . . .
H22B H -0.020358 0.608135 0.007210 0.053 Uiso 1 1 calc GR . . . .
H22C H -0.001730 0.738836 0.011076 0.053 Uiso 1 1 calc GR . . . .
C23 C 0.22691(7) 0.79134(10) 0.25535(5) 0.0231(2) Uani 1 1 d . . . . .
H23 H 0.239673 0.710453 0.261644 0.028 Uiso 1 1 calc R . . . .
C24 C 0.29720(7) 0.85886(11) 0.27668(6) 0.0288(3) Uani 1 1 d . . . . .
H24A H 0.331035 0.846564 0.249467 0.043 Uiso 1 1 calc GR . . . .
H24B H 0.320614 0.834803 0.317019 0.043 Uiso 1 1 calc GR . . . .
H24C H 0.285004 0.938483 0.277231 0.043 Uiso 1 1 calc GR . . . .
C25 C 0.17009(8) 0.81976(14) 0.29333(6) 0.0348(3) Uani 1 1 d . . . . .
H25A H 0.156843 0.898955 0.288321 0.052 Uiso 1 1 calc GR . . . .
H25B H 0.191054 0.804701 0.335472 0.052 Uiso 1 1 calc GR . . . .
H25C H 0.126064 0.773776 0.280493 0.052 Uiso 1 1 calc GR . . . .
C26 C 0.12159(6) 0.37918(9) 0.27422(5) 0.0166(2) Uani 1 1 d . . . . .
C27 C 0.11446(6) 0.28190(9) 0.23905(5) 0.0186(2) Uani 1 1 d . . . . .
C28 C 0.11987(6) 0.17920(10) 0.26857(6) 0.0231(2) Uani 1 1 d . . . . .
H28 H 0.117683 0.112083 0.246077 0.028 Uiso 1 1 calc R . . . .
C29 C 0.12839(6) 0.17348(10) 0.33017(6) 0.0247(2) Uani 1 1 d . . . . .
H29 H 0.132696 0.102863 0.349551 0.030 Uiso 1 1 calc R . . . .
C30 C 0.13063(6) 0.27043(10) 0.36346(5) 0.0228(2) Uani 1 1 d . . . . .
H30 H 0.134259 0.265497 0.405436 0.027 Uiso 1 1 calc R . . . .
C31 C 0.12765(6) 0.37539(10) 0.33640(5) 0.0195(2) Uani 1 1 d . . . . .
C32 C 0.09687(6) 0.28958(10) 0.17118(5) 0.0219(2) Uani 1 1 d . . . . .
H32 H 0.125617 0.353254 0.159152 0.026 Uiso 1 1 calc R . . . .
C33 C 0.11658(7) 0.18423(11) 0.14001(6) 0.0267(3) Uani 1 1 d . . . . .
H33A H 0.084307 0.122819 0.146794 0.040 Uiso 1 1 calc GR . . . .
H33B H 0.167867 0.163982 0.156219 0.040 Uiso 1 1 calc GR . . . .
H33C H 0.110216 0.198317 0.097034 0.040 Uiso 1 1 calc GR . . . .
C34 C 0.01467(7) 0.31509(12) 0.14932(6) 0.0316(3) Uani 1 1 d . . . . .
H34A H 0.003986 0.322808 0.105742 0.047 Uiso 1 1 calc GR . . . .
H34B H 0.002299 0.384864 0.167481 0.047 Uiso 1 1 calc GR . . . .
H34C H -0.014674 0.253844 0.160820 0.047 Uiso 1 1 calc GR . . . .
C35 C 0.12907(7) 0.47999(11) 0.37422(5) 0.0264(3) Uani 1 1 d . . . . .
H35 H 0.134245 0.546087 0.348611 0.032 Uiso 1 1 calc R . . . .
C36 C 0.19298(8) 0.48173(14) 0.42830(6) 0.0361(3) Uani 1 1 d . . . . .
H36A H 0.186658 0.421251 0.455743 0.054 Uiso 1 1 calc GR . . . .
H36B H 0.193721 0.553682 0.448901 0.054 Uiso 1 1 calc GR . . . .
H36C H 0.239444 0.471375 0.414875 0.054 Uiso 1 1 calc GR . . . .
C37 C 0.05605(9) 0.49123(14) 0.39554(7) 0.0395(3) Uani 1 1 d . . . . .
H37A H 0.015040 0.486929 0.361108 0.059 Uiso 1 1 calc GR . . . .
H37B H 0.054695 0.563323 0.415632 0.059 Uiso 1 1 calc GR . . . .
H37C H 0.051837 0.430601 0.423483 0.059 Uiso 1 1 calc GR . . . .
C38 C 0.28698(6) 0.39836(10) 0.30526(5) 0.0203(2) Uani 1 1 d . . . . .
H38 H 0.279223 0.464828 0.325868 0.024 Uiso 1 1 calc R . . . .
C39 C 0.31658(7) 0.30475(11) 0.33767(5) 0.0256(3) Uani 1 1 d . . . . .
H39 H 0.328449 0.307881 0.380055 0.031 Uiso 1 1 calc R . . . .
C40 C 0.32884(7) 0.20706(11) 0.30854(6) 0.0261(3) Uani 1 1 d . . . . .
H40 H 0.348337 0.143018 0.330769 0.031 Uiso 1 1 calc R . . . .
C41 C 0.31234(6) 0.20378(10) 0.24657(6) 0.0228(2) Uani 1 1 d . . . . .
H41 H 0.321420 0.137699 0.226175 0.027 Uiso 1 1 calc R . . . .
C42 C 0.28262(6) 0.29689(9) 0.21443(5) 0.0183(2) Uani 1 1 d . . . . .
H42 H 0.271517 0.293532 0.172031 0.022 Uiso 1 1 calc R . . . .
C43 C 0.26856(6) 0.39594(9) 0.24301(5) 0.0162(2) Uani 1 1 d . . . . .
C44 C 0.35619(6) 0.52673(10) 0.04400(5) 0.0183(2) Uani 1 1 d . . . . .
C45 C 0.34495(6) 0.62776(10) 0.01136(5) 0.0223(2) Uani 1 1 d . . . . .
C46 C 0.30821(7) 0.62317(11) -0.04830(6) 0.0273(3) Uani 1 1 d . . . . .
H46 H 0.300812 0.690056 -0.071112 0.033 Uiso 1 1 calc R . . . .
C47 C 0.28241(7) 0.52310(12) -0.07475(6) 0.0286(3) Uani 1 1 d . . . . .
H47 H 0.258403 0.521433 -0.115589 0.034 Uiso 1 1 calc R . . . .
C48 C 0.29158(7) 0.42542(11) -0.04171(5) 0.0251(2) Uani 1 1 d . . . . .
H48 H 0.272793 0.357363 -0.060107 0.030 Uiso 1 1 calc R . . . .
C49 C 0.32784(6) 0.42462(10) 0.01809(5) 0.0201(2) Uani 1 1 d . . . . .
C50 C 0.36762(7) 0.74096(10) 0.03952(6) 0.0265(3) Uani 1 1 d . . . . .
H50 H 0.402369 0.727325 0.078357 0.032 Uiso 1 1 calc R . . . .
C51 C 0.40728(8) 0.81486(12) 0.00106(7) 0.0343(3) Uani 1 1 d . . . . .
H51A H 0.448469 0.773316 -0.009279 0.051 Uiso 1 1 calc GR . . . .
H51B H 0.425886 0.882214 0.023490 0.051 Uiso 1 1 calc GR . . . .
H51C H 0.372802 0.836210 -0.035580 0.051 Uiso 1 1 calc GR . . . .
C52 C 0.30093(8) 0.80237(12) 0.05304(7) 0.0348(3) Uani 1 1 d . . . . .
H52A H 0.265019 0.814404 0.015817 0.052 Uiso 1 1 calc GR . . . .
H52B H 0.316398 0.874673 0.071508 0.052 Uiso 1 1 calc GR . . . .
H52C H 0.278472 0.757522 0.080480 0.052 Uiso 1 1 calc GR . . . .
C53 C 0.33094(7) 0.31514(10) 0.05219(5) 0.0232(2) Uani 1 1 d . . . . .
H53 H 0.355738 0.329160 0.094600 0.028 Uiso 1 1 calc R . . . .
C54 C 0.37409(9) 0.22414(11) 0.02654(6) 0.0326(3) Uani 1 1 d . . . . .
H54A H 0.348201 0.204728 -0.013899 0.049 Uiso 1 1 calc GR . . . .
H54B H 0.378258 0.157653 0.052039 0.049 Uiso 1 1 calc GR . . . .
H54C H 0.423354 0.251997 0.025127 0.049 Uiso 1 1 calc GR . . . .
C55 C 0.51561(7) 0.60139(12) 0.07722(6) 0.0262(3) Uani 1 1 d . . . . .
H55A H 0.491608 0.589110 0.035441 0.039 Uiso 1 1 calc GR . . . .
H55B H 0.567983 0.583102 0.082575 0.039 Uiso 1 1 calc GR . . . .
H55C H 0.510094 0.679876 0.087743 0.039 Uiso 1 1 calc GR . . . .
C56 C 0.50662(7) 0.40722(11) 0.10966(6) 0.0254(3) Uani 1 1 d . . . . .
H56A H 0.481076 0.354841 0.131436 0.038 Uiso 1 1 calc GR . . . .
H56B H 0.559710 0.402706 0.125315 0.038 Uiso 1 1 calc GR . . . .
H56C H 0.496145 0.387903 0.067119 0.038 Uiso 1 1 calc GR . . . .
C57 C 0.25252(8) 0.27301(12) 0.05151(6) 0.0304(3) Uani 1 1 d . . . . .
H57A H 0.224721 0.330995 0.067645 0.046 Uiso 1 1 calc GR . . . .
H57B H 0.254775 0.205474 0.076063 0.046 Uiso 1 1 calc GR . . . .
H57C H 0.228087 0.255722 0.010379 0.046 Uiso 1 1 calc GR . . . .
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'
P P 0.2955 0.4335 '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
-1 1 -2 0.0657
2 -1 0 0.1346
0 0 -1 0.1276
2 1 -1 0.1653
-1 -2 -1 0.1628
-2 -1 1 0.1726
0 1 1 0.1321
1 0 -2 0.1431
-1 1 2 0.1980
-1 -1 2 0.1679
0 -1 0 0.1614
0 1 0 0.1203
0 -1 2 0.1484
-1 2 -1 0.0995
1 0 1 0.1824
-1 0 0 0.1558
1 0 0 0.1735
-2 -1 -2 0.1571
-1 -1 -2 0.1364
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
C5 P1 C4 110.87(5) . . ?
C1 N1 C14 132.23(9) . . ?
C2 N1 C1 110.19(9) . . ?
C2 N1 C14 116.72(9) . . ?
C1 N2 C26 129.15(9) . . ?
C3 N2 C1 110.06(9) . . ?
C3 N2 C26 119.82(9) . . ?
C5 N3 C6 114.48(9) . . ?
C5 N3 C44 123.44(9) . . ?
C44 N3 C6 121.84(9) . . ?
N1 C1 N2 103.26(9) . . ?
C4 C1 N1 128.33(10) . . ?
C4 C1 N2 128.29(10) . . ?
N1 C2 H2 125.8 . . ?
C3 C2 N1 108.38(10) . . ?
C3 C2 H2 125.8 . . ?
N2 C3 H3 125.9 . . ?
C2 C3 N2 108.10(10) . . ?
C2 C3 H3 125.9 . . ?
C1 C4 P1 118.02(8) . . ?
C1 C4 C43 119.36(9) . . ?
C43 C4 P1 119.46(8) . . ?
N3 C5 P1 116.35(8) . . ?
N3 C5 C8 107.33(9) . . ?
C8 C5 P1 136.06(8) . . ?
N3 C6 C7 100.08(9) . . ?
N3 C6 C55 113.91(9) . . ?
N3 C6 C56 110.19(9) . . ?
C7 C6 C55 112.38(10) . . ?
C7 C6 C56 114.00(9) . . ?
C55 C6 C56 106.43(10) . . ?
C6 C7 H7A 110.3 . . ?
C6 C7 H7B 110.3 . . ?
C6 C7 C8 107.11(9) . . ?
H7A C7 H7B 108.5 . . ?
C8 C7 H7A 110.3 . . ?
C8 C7 H7B 110.3 . . ?
C5 C8 C13 115.49(8) . . ?
C7 C8 C5 101.77(9) . . ?
C7 C8 C13 109.97(9) . . ?
C9 C8 C5 109.45(9) . . ?
C9 C8 C7 111.51(9) . . ?
C9 C8 C13 108.56(9) . . ?
C8 C9 H9A 109.0 . . ?
C8 C9 H9B 109.0 . . ?
H9A C9 H9B 107.8 . . ?
C10 C9 C8 112.88(10) . . ?
C10 C9 H9A 109.0 . . ?
C10 C9 H9B 109.0 . . ?
C9 C10 H10A 109.3 . . ?
C9 C10 H10B 109.3 . . ?
H10A C10 H10B 108.0 . . ?
C11 C10 C9 111.50(10) . . ?
C11 C10 H10A 109.3 . . ?
C11 C10 H10B 109.3 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 108.1 . . ?
C12 C11 C10 110.56(10) . . ?
C12 C11 H11A 109.5 . . ?
C12 C11 H11B 109.5 . . ?
C11 C12 H12A 109.4 . . ?
C11 C12 H12B 109.4 . . ?
C11 C12 C13 111.01(10) . . ?
H12A C12 H12B 108.0 . . ?
C13 C12 H12A 109.4 . . ?
C13 C12 H12B 109.4 . . ?
C8 C13 H13A 109.1 . . ?
C8 C13 H13B 109.1 . . ?
C12 C13 C8 112.71(9) . . ?
C12 C13 H13A 109.1 . . ?
C12 C13 H13B 109.1 . . ?
H13A C13 H13B 107.8 . . ?
C15 C14 N1 117.85(10) . . ?
C19 C14 N1 119.04(10) . . ?
C19 C14 C15 122.06(10) . . ?
C14 C15 C20 122.82(10) . . ?
C16 C15 C14 117.70(11) . . ?
C16 C15 C20 119.48(10) . . ?
C15 C16 H16 119.3 . . ?
C17 C16 C15 121.32(11) . . ?
C17 C16 H16 119.3 . . ?
C16 C17 H17 120.0 . . ?
C16 C17 C18 119.95(11) . . ?
C18 C17 H17 120.0 . . ?
C17 C18 H18 119.5 . . ?
C17 C18 C19 121.08(12) . . ?
C19 C18 H18 119.5 . . ?
C14 C19 C23 120.90(10) . . ?
C18 C19 C14 117.74(11) . . ?
C18 C19 C23 121.31(10) . . ?
C15 C20 H20 108.0 . . ?
C15 C20 C21 110.54(10) . . ?
C15 C20 C22 111.20(10) . . ?
C21 C20 H20 108.0 . . ?
C22 C20 H20 108.0 . . ?
C22 C20 C21 110.96(10) . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C19 C23 H23 107.7 . . ?
C19 C23 C24 113.04(10) . . ?
C19 C23 C25 110.59(10) . . ?
C24 C23 H23 107.7 . . ?
C24 C23 C25 110.03(10) . . ?
C25 C23 H23 107.7 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C27 C26 N2 119.13(10) . . ?
C31 C26 N2 118.69(10) . . ?
C31 C26 C27 122.10(10) . . ?
C26 C27 C32 120.60(10) . . ?
C28 C27 C26 117.60(10) . . ?
C28 C27 C32 121.70(10) . . ?
C27 C28 H28 119.4 . . ?
C29 C28 C27 121.11(11) . . ?
C29 C28 H28 119.4 . . ?
C28 C29 H29 119.9 . . ?
C30 C29 C28 120.12(11) . . ?
C30 C29 H29 119.9 . . ?
C29 C30 H30 119.4 . . ?
C29 C30 C31 121.11(11) . . ?
C31 C30 H30 119.4 . . ?
C26 C31 C35 122.58(10) . . ?
C30 C31 C26 117.74(11) . . ?
C30 C31 C35 119.66(10) . . ?
C27 C32 H32 108.0 . . ?
C27 C32 C33 113.75(10) . . ?
C27 C32 C34 109.77(10) . . ?
C33 C32 H32 108.0 . . ?
C33 C32 C34 109.11(10) . . ?
C34 C32 H32 108.0 . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C32 C34 H34A 109.5 . . ?
C32 C34 H34B 109.5 . . ?
C32 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C31 C35 H35 108.1 . . ?
C31 C35 C36 113.11(11) . . ?
C31 C35 C37 109.73(11) . . ?
C36 C35 H35 108.1 . . ?
C36 C35 C37 109.43(11) . . ?
C37 C35 H35 108.1 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C35 C37 H37A 109.5 . . ?
C35 C37 H37B 109.5 . . ?
C35 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C39 C38 H38 119.5 . . ?
C39 C38 C43 120.99(11) . . ?
C43 C38 H38 119.5 . . ?
C38 C39 H39 119.7 . . ?
C40 C39 C38 120.52(11) . . ?
C40 C39 H39 119.7 . . ?
C39 C40 H40 120.3 . . ?
C39 C40 C41 119.34(11) . . ?
C41 C40 H40 120.3 . . ?
C40 C41 H41 120.0 . . ?
C42 C41 C40 120.03(11) . . ?
C42 C41 H41 120.0 . . ?
C41 C42 H42 119.2 . . ?
C41 C42 C43 121.58(11) . . ?
C43 C42 H42 119.2 . . ?
C38 C43 C4 121.80(10) . . ?
C38 C43 C42 117.51(10) . . ?
C42 C43 C4 120.68(10) . . ?
C45 C44 N3 118.23(10) . . ?
C49 C44 N3 120.73(10) . . ?
C49 C44 C45 121.04(10) . . ?
C44 C45 C50 122.62(10) . . ?
C46 C45 C44 118.18(11) . . ?
C46 C45 C50 119.12(11) . . ?
C45 C46 H46 119.4 . . ?
C47 C46 C45 121.25(12) . . ?
C47 C46 H46 119.4 . . ?
C46 C47 H47 120.0 . . ?
C46 C47 C48 119.95(11) . . ?
C48 C47 H47 120.0 . . ?
C47 C48 H48 119.3 . . ?
C47 C48 C49 121.47(12) . . ?
C49 C48 H48 119.3 . . ?
C44 C49 C53 123.95(10) . . ?
C48 C49 C44 118.02(11) . . ?
C48 C49 C53 117.95(11) . . ?
C45 C50 H50 107.7 . . ?
C45 C50 C51 113.21(11) . . ?
C45 C50 C52 110.37(11) . . ?
C51 C50 H50 107.7 . . ?
C52 C50 H50 107.7 . . ?
C52 C50 C51 109.95(11) . . ?
C50 C51 H51A 109.5 . . ?
C50 C51 H51B 109.5 . . ?
C50 C51 H51C 109.5 . . ?
H51A C51 H51B 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
C50 C52 H52A 109.5 . . ?
C50 C52 H52B 109.5 . . ?
C50 C52 H52C 109.5 . . ?
H52A C52 H52B 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C49 C53 H53 108.4 . . ?
C49 C53 C54 112.59(10) . . ?
C49 C53 C57 109.85(10) . . ?
C54 C53 H53 108.4 . . ?
C54 C53 C57 109.22(11) . . ?
C57 C53 H53 108.4 . . ?
C53 C54 H54A 109.5 . . ?
C53 C54 H54B 109.5 . . ?
C53 C54 H54C 109.5 . . ?
H54A C54 H54B 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C6 C55 H55A 109.5 . . ?
C6 C55 H55B 109.5 . . ?
C6 C55 H55C 109.5 . . ?
H55A C55 H55B 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
C6 C56 H56A 109.5 . . ?
C6 C56 H56B 109.5 . . ?
C6 C56 H56C 109.5 . . ?
H56A C56 H56B 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C53 C57 H57A 109.5 . . ?
C53 C57 H57B 109.5 . . ?
C53 C57 H57C 109.5 . . ?
H57A C57 H57B 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
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
P1 C4 1.8203(11) . ?
P1 C5 1.7354(11) . ?
N1 C1 1.4025(13) . ?
N1 C2 1.3994(14) . ?
N1 C14 1.4396(14) . ?
N2 C1 1.4115(14) . ?
N2 C3 1.3996(14) . ?
N2 C26 1.4386(14) . ?
N3 C5 1.3884(14) . ?
N3 C6 1.4918(14) . ?
N3 C44 1.4370(14) . ?
C1 C4 1.3844(15) . ?
C2 H2 0.9500 . ?
C2 C3 1.3299(17) . ?
C3 H3 0.9500 . ?
C4 C43 1.4814(14) . ?
C5 C8 1.5480(14) . ?
C6 C7 1.5266(16) . ?
C6 C55 1.5308(16) . ?
C6 C56 1.5342(16) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C7 C8 1.5475(15) . ?
C8 C9 1.5381(15) . ?
C8 C13 1.5503(15) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C9 C10 1.5315(16) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 C11 1.5268(18) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.5243(18) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C12 C13 1.5369(15) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.4044(15) . ?
C14 C19 1.4032(16) . ?
C15 C16 1.3957(17) . ?
C15 C20 1.5166(16) . ?
C16 H16 0.9500 . ?
C16 C17 1.3792(19) . ?
C17 H17 0.9500 . ?
C17 C18 1.3904(18) . ?
C18 H18 0.9500 . ?
C18 C19 1.3948(16) . ?
C19 C23 1.5190(16) . ?
C20 H20 1.0000 . ?
C20 C21 1.5360(17) . ?
C20 C22 1.5350(17) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23 1.0000 . ?
C23 C24 1.5288(16) . ?
C23 C25 1.5332(18) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 C27 1.4056(16) . ?
C26 C31 1.4034(16) . ?
C27 C28 1.3959(16) . ?
C27 C32 1.5222(16) . ?
C28 H28 0.9500 . ?
C28 C29 1.3863(18) . ?
C29 H29 0.9500 . ?
C29 C30 1.3833(18) . ?
C30 H30 0.9500 . ?
C30 C31 1.3962(16) . ?
C31 C35 1.5183(17) . ?
C32 H32 1.0000 . ?
C32 C33 1.5283(16) . ?
C32 C34 1.5378(17) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35 1.0000 . ?
C35 C36 1.5315(18) . ?
C35 C37 1.5358(19) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38 0.9500 . ?
C38 C39 1.3933(16) . ?
C38 C43 1.3950(15) . ?
C39 H39 0.9500 . ?
C39 C40 1.3865(19) . ?
C40 H40 0.9500 . ?
C40 C41 1.3879(19) . ?
C41 H41 0.9500 . ?
C41 C42 1.3865(16) . ?
C42 H42 0.9500 . ?
C42 C43 1.4030(16) . ?
C44 C45 1.4137(16) . ?
C44 C49 1.4124(16) . ?
C45 C46 1.3976(17) . ?
C45 C50 1.5221(18) . ?
C46 H46 0.9500 . ?
C46 C47 1.383(2) . ?
C47 H47 0.9500 . ?
C47 C48 1.3833(19) . ?
C48 H48 0.9500 . ?
C48 C49 1.3967(16) . ?
C49 C53 1.5195(16) . ?
C50 H50 1.0000 . ?
C50 C51 1.5354(18) . ?
C50 C52 1.5240(18) . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C53 H53 1.0000 . ?
C53 C54 1.5363(18) . ?
C53 C57 1.5378(17) . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
C55 H55A 0.9800 . ?
C55 H55B 0.9800 . ?
C55 H55C 0.9800 . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?
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
P1 C4 C43 C38 136.27(9) . . . . ?
P1 C4 C43 C42 -42.16(13) . . . . ?
P1 C5 C8 C7 -159.01(9) . . . . ?
P1 C5 C8 C9 -40.93(14) . . . . ?
P1 C5 C8 C13 81.92(13) . . . . ?
N1 C1 C4 P1 -22.54(15) . . . . ?
N1 C1 C4 C43 177.63(10) . . . . ?
N1 C2 C3 N2 -0.91(13) . . . . ?
N1 C14 C15 C16 164.10(10) . . . . ?
N1 C14 C15 C20 -16.89(16) . . . . ?
N1 C14 C19 C18 -165.40(10) . . . . ?
N1 C14 C19 C23 12.08(16) . . . . ?
N2 C1 C4 P1 152.84(9) . . . . ?
N2 C1 C4 C43 -6.99(17) . . . . ?
N2 C26 C27 C28 177.90(10) . . . . ?
N2 C26 C27 C32 -5.70(15) . . . . ?
N2 C26 C31 C30 -179.68(10) . . . . ?
N2 C26 C31 C35 1.90(16) . . . . ?
N3 C5 C8 C7 14.69(10) . . . . ?
N3 C5 C8 C9 132.78(9) . . . . ?
N3 C5 C8 C13 -104.37(10) . . . . ?
N3 C6 C7 C8 29.78(11) . . . . ?
N3 C44 C45 C46 176.23(10) . . . . ?
N3 C44 C45 C50 -7.07(16) . . . . ?
N3 C44 C49 C48 -176.21(10) . . . . ?
N3 C44 C49 C53 7.08(17) . . . . ?
C1 N1 C2 C3 0.98(13) . . . . ?
C1 N1 C14 C15 115.73(13) . . . . ?
C1 N1 C14 C19 -75.73(15) . . . . ?
C1 N2 C3 C2 0.54(13) . . . . ?
C1 N2 C26 C27 -66.52(15) . . . . ?
C1 N2 C26 C31 116.64(12) . . . . ?
C1 C4 C43 C38 -64.19(14) . . . . ?
C1 C4 C43 C42 117.38(12) . . . . ?
C2 N1 C1 N2 -0.62(11) . . . . ?
C2 N1 C1 C4 175.66(11) . . . . ?
C2 N1 C14 C15 -76.11(13) . . . . ?
C2 N1 C14 C19 92.43(13) . . . . ?
C3 N2 C1 N1 0.06(11) . . . . ?
C3 N2 C1 C4 -176.21(11) . . . . ?
C3 N2 C26 C27 101.03(12) . . . . ?
C3 N2 C26 C31 -75.81(13) . . . . ?
C4 P1 C5 N3 166.13(8) . . . . ?
C4 P1 C5 C8 -20.58(12) . . . . ?
C5 P1 C4 C1 155.40(8) . . . . ?
C5 P1 C4 C43 -44.79(10) . . . . ?
C5 N3 C6 C7 -21.41(11) . . . . ?
C5 N3 C6 C55 -141.54(10) . . . . ?
C5 N3 C6 C56 98.95(11) . . . . ?
C5 N3 C44 C45 102.03(12) . . . . ?
C5 N3 C44 C49 -78.55(14) . . . . ?
C5 C8 C9 C10 -179.02(9) . . . . ?
C5 C8 C13 C12 -177.71(10) . . . . ?
C6 N3 C5 P1 179.42(7) . . . . ?
C6 N3 C5 C8 4.29(12) . . . . ?
C6 N3 C44 C45 -84.01(13) . . . . ?
C6 N3 C44 C49 95.41(13) . . . . ?
C6 C7 C8 C5 -28.06(11) . . . . ?
C6 C7 C8 C9 -144.66(9) . . . . ?
C6 C7 C8 C13 94.86(10) . . . . ?
C7 C8 C9 C10 -67.20(12) . . . . ?
C7 C8 C13 C12 67.85(12) . . . . ?
C8 C9 C10 C11 -56.22(14) . . . . ?
C9 C8 C13 C12 -54.40(12) . . . . ?
C9 C10 C11 C12 55.78(14) . . . . ?
C10 C11 C12 C13 -55.89(13) . . . . ?
C11 C12 C13 C8 56.57(13) . . . . ?
C13 C8 C9 C10 54.10(12) . . . . ?
C14 N1 C1 N2 168.12(10) . . . . ?
C14 N1 C1 C4 -15.61(19) . . . . ?
C14 N1 C2 C3 -169.70(10) . . . . ?
C14 C15 C16 C17 1.93(18) . . . . ?
C14 C15 C20 C21 -120.63(12) . . . . ?
C14 C15 C20 C22 115.66(13) . . . . ?
C14 C19 C23 C24 150.67(11) . . . . ?
C14 C19 C23 C25 -85.45(14) . . . . ?
C15 C14 C19 C18 2.64(17) . . . . ?
C15 C14 C19 C23 -179.89(11) . . . . ?
C15 C16 C17 C18 1.5(2) . . . . ?
C16 C15 C20 C21 58.37(14) . . . . ?
C16 C15 C20 C22 -65.35(15) . . . . ?
C16 C17 C18 C19 -3.1(2) . . . . ?
C17 C18 C19 C14 0.99(19) . . . . ?
C17 C18 C19 C23 -176.48(12) . . . . ?
C18 C19 C23 C24 -31.95(16) . . . . ?
C18 C19 C23 C25 91.94(14) . . . . ?
C19 C14 C15 C16 -4.07(17) . . . . ?
C19 C14 C15 C20 174.94(11) . . . . ?
C20 C15 C16 C17 -177.11(12) . . . . ?
C26 N2 C1 N1 168.57(10) . . . . ?
C26 N2 C1 C4 -7.70(18) . . . . ?
C26 N2 C3 C2 -169.21(10) . . . . ?
C26 C27 C28 C29 3.07(16) . . . . ?
C26 C27 C32 C33 160.10(10) . . . . ?
C26 C27 C32 C34 -77.33(13) . . . . ?
C26 C31 C35 C36 -129.84(12) . . . . ?
C26 C31 C35 C37 107.66(13) . . . . ?
C27 C26 C31 C30 3.58(16) . . . . ?
C27 C26 C31 C35 -174.84(11) . . . . ?
C27 C28 C29 C30 0.91(18) . . . . ?
C28 C27 C32 C33 -23.65(15) . . . . ?
C28 C27 C32 C34 98.92(13) . . . . ?
C28 C29 C30 C31 -2.82(17) . . . . ?
C29 C30 C31 C26 0.60(17) . . . . ?
C29 C30 C31 C35 179.07(11) . . . . ?
C30 C31 C35 C36 51.76(16) . . . . ?
C30 C31 C35 C37 -70.73(14) . . . . ?
C31 C26 C27 C28 -5.37(16) . . . . ?
C31 C26 C27 C32 171.03(10) . . . . ?
C32 C27 C28 C29 -173.29(11) . . . . ?
C38 C39 C40 C41 0.95(18) . . . . ?
C39 C38 C43 C4 -179.99(10) . . . . ?
C39 C38 C43 C42 -1.51(16) . . . . ?
C39 C40 C41 C42 -1.20(17) . . . . ?
C40 C41 C42 C43 0.08(17) . . . . ?
C41 C42 C43 C4 179.75(10) . . . . ?
C41 C42 C43 C38 1.26(16) . . . . ?
C43 C38 C39 C40 0.43(18) . . . . ?
C44 N3 C5 P1 -6.22(13) . . . . ?
C44 N3 C5 C8 178.65(9) . . . . ?
C44 N3 C6 C7 164.12(9) . . . . ?
C44 N3 C6 C55 44.00(14) . . . . ?
C44 N3 C6 C56 -75.51(12) . . . . ?
C44 C45 C46 C47 0.95(18) . . . . ?
C44 C45 C50 C51 134.78(12) . . . . ?
C44 C45 C50 C52 -101.50(13) . . . . ?
C44 C49 C53 C54 -119.71(13) . . . . ?
C44 C49 C53 C57 118.33(12) . . . . ?
C45 C44 C49 C48 3.19(17) . . . . ?
C45 C44 C49 C53 -173.52(11) . . . . ?
C45 C46 C47 C48 1.2(2) . . . . ?
C46 C45 C50 C51 -48.55(16) . . . . ?
C46 C45 C50 C52 75.18(14) . . . . ?
C46 C47 C48 C49 -1.23(19) . . . . ?
C47 C48 C49 C44 -0.96(18) . . . . ?
C47 C48 C49 C53 175.95(11) . . . . ?
C48 C49 C53 C54 63.58(15) . . . . ?
C48 C49 C53 C57 -58.38(14) . . . . ?
C49 C44 C45 C46 -3.19(17) . . . . ?
C49 C44 C45 C50 173.51(11) . . . . ?
C50 C45 C46 C47 -175.87(12) . . . . ?
C55 C6 C7 C8 151.01(9) . . . . ?
C56 C6 C7 C8 -87.79(11) . . . . ?
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
-0.9762 1.0312 -1.9687 -0.1102 -0.1869 0.0165
1.9405 -1.0531 -0.0501 0.1227 0.1282 0.1170
-0.0195 0.0026 -0.9948 -0.0327 -0.0332 0.0506
2.0530 0.9469 -1.0615 0.1562 -0.1305 0.0625
-1.1547 -1.9676 -0.9490 -0.1768 0.1846 0.1236
-2.0530 -0.9469 1.0615 -0.1562 0.1305 -0.0625
0.0854 0.9961 0.9865 0.0658 -0.0796 -0.1032
0.9644 -0.0219 -2.0188 0.0125 -0.0586 0.1335
-0.8984 1.0206 2.0105 0.0206 -0.0541 -0.1860
-1.0303 -0.9768 2.0271 -0.0456 0.1714 -0.0809
-0.0660 -0.9987 0.0083 -0.0331 0.1127 0.0526
0.0660 0.9987 -0.0083 0.0331 -0.1127 -0.0526
-0.0271 -1.0040 1.9979 0.0323 0.1791 -0.0487
-0.8907 2.0273 -0.9822 -0.0444 -0.2664 -0.0868
1.0227 -0.0299 0.9656 0.1106 0.0409 -0.0184
-1.0033 0.0272 0.0292 -0.0779 -0.0077 -0.0322
1.0033 -0.0272 -0.0292 0.0779 0.0077 0.0322
-2.1114 -0.9390 -1.9229 -0.2543 0.0309 0.0894
-1.1081 -0.9662 -1.9521 -0.1764 0.0386 0.1216
