#------------------------------------------------------------------------------
#$Date: 2021-04-05 16:58:40 +0300 (Mon, 05 Apr 2021) $
#$Revision: 263635 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/79/7127933.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_7127933
loop_
_publ_author_name
'Hierlmeier, Gabriele'
'Uttendorfer, Maria K.'
'Wolf, Robert'
_publ_section_title
;
 Di-tert-butyldiphosphatetrahedrane as a building block for
 phosphaalkenes and phosphirenes.
;
_journal_issue                   19
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              2356
_journal_page_last               2359
_journal_paper_doi               10.1039/d0cc07103j
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C31 H42 N2 P2'
_chemical_formula_sum            'C31 H42 N2 P2'
_chemical_formula_weight         504.60
_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             2020-04-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-10-23 deposited with the CCDC.	2020-12-09 downloaded from the CCDC.
;
_cell_angle_alpha                93.857(2)
_cell_angle_beta                 95.926(2)
_cell_angle_gamma                110.711(2)
_cell_formula_units_Z            4
_cell_length_a                   8.5803(2)
_cell_length_b                   10.6253(2)
_cell_length_c                   35.5315(8)
_cell_measurement_reflns_used    9226
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      73.3780
_cell_measurement_theta_min      3.7630
_cell_volume                     2995.01(12)
_computing_cell_refinement       'CrysAlisPro 1.171.41.21a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.41.21a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.41.21a (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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3546
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -74.00  26.00   1.00   10.00    --  -41.60  77.00 -90.00  100
  2  ω     18.00 113.00   1.00   10.00    --   41.60  57.00 150.00   95
  3  ω    -26.00  68.00   1.00   10.00    --   41.60 -57.00   0.00   94
  4  ω     38.00  77.00   1.00   41.00    --  106.46 -45.00-120.00   39
  5  ω     40.00 109.00   1.00   41.00    --  106.46 -94.00 -90.00   69
  6  ω     30.00  69.00   1.00   41.00    --  106.46 -30.00 150.00   39
  7  ω     46.00  77.00   1.00   41.00    --  106.46 -45.00 -30.00   31
  8  ω     41.00  99.00   1.00   41.00    --  106.46 -94.00-150.00   58
  9  ω     31.00  60.00   1.00   41.00    --  106.46 -30.00-150.00   29
 10  ω     33.00 121.00   1.00   41.00    --  106.46-125.00-150.00   88
 11  ω     43.00 109.00   1.00   41.00    --  106.46 -94.00   0.00   66
 12  ω     31.00 103.00   1.00   41.00    --  106.46 -94.00  90.00   72
 13  ω     77.00 158.00   1.00   41.00    --  106.46  61.00 -30.00   81
 14  ω     36.00  63.00   1.00   41.00    --  106.46 -30.00-180.00   27
 15  ω     78.00 148.00   1.00   41.00    --  106.46  61.00 120.00   70
 16  ω     39.00  66.00   1.00   41.00    --  106.46 -30.00 -60.00   27
 17  ω     27.00 154.00   1.00   41.00    --  106.46 -15.00 -30.00  127
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset/far, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1324738000
_diffrn_orient_matrix_UB_12      -0.0282701000
_diffrn_orient_matrix_UB_13      -0.0353568000
_diffrn_orient_matrix_UB_21      -0.1377250000
_diffrn_orient_matrix_UB_22      -0.0171372000
_diffrn_orient_matrix_UB_23      0.0259252000
_diffrn_orient_matrix_UB_31      0.0319888000
_diffrn_orient_matrix_UB_32      0.1524377000
_diffrn_orient_matrix_UB_33      0.0013644000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0299
_diffrn_reflns_av_unetI/netI     0.0484
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            20271
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.537
_diffrn_reflns_theta_min         3.776
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.458
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.845
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.21a (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            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.119
_exptl_crystal_description       plate
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.143
_exptl_crystal_size_mid          0.119
_exptl_crystal_size_min          0.044
_refine_diff_density_max         0.369
_refine_diff_density_min         -0.331
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     655
_refine_ls_number_reflns         11591
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0647
_refine_ls_R_factor_gt           0.0500
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0560P)²+1.3656P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1221
_refine_ls_wR_factor_ref         0.1317
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9222
_reflns_number_total             11591
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0cc07103j2.cif
_cod_data_source_block           gh436b_p
_cod_depositor_comments
'Adding full bibliography for 7127930--7127935.cif.'
_cod_original_cell_volume        2995.00(12)
_cod_database_code               7127933
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C31 H42 N2 P2'
_chemical_oxdiff_usercomment     'from n-hexane'
_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.
;
_reflns_odcompleteness_completeness 99.17
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C56(H56), C47(H47), C49(H49), C58(H58), C13(H13), C12(H12), C16(H16),
 C18(H18), C27(H27), C25(H25), C43(H43), C44(H44)
2.b Idealised Me refined as rotating group:
 C60(H60A,H60B,H60C), C40(H40A,H40B,H40C), C51(H51A,H51B,H51C), C53(H53A,H53B,
 H53C), C31(H31A,H31B,H31C), C30(H30A,H30B,H30C), C62(H62A,H62B,H62C), C52(H52A,
 H52B,H52C), C22(H22A,H22B,H22C), C35(H35A,H35B,H35C), C61(H61A,H61B,H61C),
 C29(H29A,H29B,H29C), C36(H36A,H36B,H36C), C41(H41A,H41B,H41C), C20(H20A,H20B,
 H20C), C37(H37A,H37B,H37C), C39(H39A,H39B,H39C), C6(H6A,H6B,H6C), C9(H9A,H9B,
 H9C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C8(H8A,H8B,H8C), C21(H21A,H21B,H21C),
 C10(H10A,H10B,H10C)
;
_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 1.282
_oxdiff_exptl_absorpt_empirical_full_min 0.793
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
P4 P 0.43674(7) 0.21912(5) 0.41673(2) 0.02836(12) Uani 1 1 d . . . . .
P3 P 0.52679(7) 0.21164(5) 0.36012(2) 0.03003(13) Uani 1 1 d . . . . .
P2 P 0.26102(8) 0.41706(5) 0.09311(2) 0.03552(14) Uani 1 1 d . . . . .
P1 P 0.42549(9) 0.48167(6) 0.14885(2) 0.04000(15) Uani 1 1 d . . . . .
N4 N 0.4589(2) -0.00116(17) 0.30500(5) 0.0325(4) Uani 1 1 d . . . . .
N1 N 0.3600(2) 0.73132(17) 0.14758(5) 0.0316(4) Uani 1 1 d . . . . .
N3 N 0.3534(2) -0.07911(17) 0.35519(5) 0.0321(4) Uani 1 1 d . . . . .
N2 N 0.5103(3) 0.71356(18) 0.19850(5) 0.0351(4) Uani 1 1 d . . . . .
C45 C 0.3117(3) -0.09292(19) 0.39297(6) 0.0297(4) Uani 1 1 d . . . . .
C55 C 0.7141(3) 0.1086(2) 0.27761(6) 0.0303(4) Uani 1 1 d . . . . .
C54 C 0.5458(3) 0.0874(2) 0.27891(6) 0.0296(4) Uani 1 1 d . . . . .
C50 C 0.4318(3) -0.1025(2) 0.42094(7) 0.0334(5) Uani 1 1 d . . . . .
C32 C 0.3546(3) 0.3579(2) 0.41318(6) 0.0279(4) Uani 1 1 d . . . . .
C14 C 0.2578(3) 0.71020(19) 0.11151(6) 0.0279(4) Uani 1 1 d . . . . .
C42 C 0.4418(3) 0.0400(2) 0.34138(6) 0.0277(4) Uani 1 1 d . . . . .
C56 C 0.7948(3) 0.1920(2) 0.25125(6) 0.0347(5) Uani 1 1 d . . . . .
H56 H 0.9079 0.2083 0.2500 0.042 Uiso 1 1 calc R . . . .
C2 C 0.1987(3) 0.2322(2) 0.09238(6) 0.0321(4) Uani 1 1 d . . . . .
C19 C 0.3354(3) 0.7577(2) 0.08025(6) 0.0331(5) Uani 1 1 d . . . . .
C47 C 0.1180(3) -0.1114(2) 0.43728(7) 0.0354(5) Uani 1 1 d . . . . .
H47 H 0.0142 -0.1125 0.4431 0.042 Uiso 1 1 calc R . . . .
C1 C 0.3297(3) 0.2819(2) 0.07515(6) 0.0335(5) Uani 1 1 d . . . . .
C33 C 0.5118(3) 0.4043(2) 0.42800(6) 0.0279(4) Uani 1 1 d . . . . .
C59 C 0.4560(3) 0.1450(2) 0.25503(6) 0.0357(5) Uani 1 1 d . . . . .
C46 C 0.1538(3) -0.0979(2) 0.40022(7) 0.0321(4) Uani 1 1 d . . . . .
C11 C 0.4247(3) 0.6435(2) 0.16380(6) 0.0309(4) Uani 1 1 d . . . . .
C49 C 0.3892(3) -0.1183(2) 0.45743(7) 0.0375(5) Uani 1 1 d . . . . .
H49 H 0.4670 -0.1257 0.4766 0.045 Uiso 1 1 calc R . . . .
C23 C 0.6014(3) 0.6651(2) 0.22634(6) 0.0350(5) Uani 1 1 d . . . . .
C57 C 0.7107(3) 0.2509(2) 0.22696(6) 0.0376(5) Uani 1 1 d . . . . .
C34 C 0.1989(3) 0.3807(2) 0.39809(7) 0.0349(5) Uani 1 1 d . . . . .
C58 C 0.5419(3) 0.2263(2) 0.22911(6) 0.0388(5) Uani 1 1 d . . . . .
H58 H 0.4848 0.2651 0.2128 0.047 Uiso 1 1 calc R . . . .
C48 C 0.2334(3) -0.1233(2) 0.46605(7) 0.0378(5) Uani 1 1 d . . . . .
C24 C 0.7767(3) 0.7168(2) 0.22985(7) 0.0395(5) Uani 1 1 d . . . . .
C60 C 0.8055(3) 0.0439(3) 0.30347(7) 0.0408(5) Uani 1 1 d . . . . .
H60A H 0.7977 0.0691 0.3295 0.061 Uiso 1 1 calc GR . . . .
H60B H 0.9215 0.0739 0.2996 0.061 Uiso 1 1 calc GR . . . .
H60C H 0.7556 -0.0528 0.2979 0.061 Uiso 1 1 calc GR . . . .
C13 C 0.5031(3) 0.8417(2) 0.20214(7) 0.0404(5) Uani 1 1 d . . . . .
H13 H 0.5540 0.9082 0.2226 0.049 Uiso 1 1 calc R . . . .
C12 C 0.4102(3) 0.8526(2) 0.17109(7) 0.0399(5) Uani 1 1 d . . . . .
H12 H 0.3836 0.9279 0.1660 0.048 Uiso 1 1 calc R . . . .
C38 C 0.6708(3) 0.5227(2) 0.44150(7) 0.0371(5) Uani 1 1 d . . . . .
C16 C -0.0116(3) 0.6390(2) 0.07463(8) 0.0424(5) Uani 1 1 d . . . . .
H16 H -0.1281 0.5992 0.0727 0.051 Uiso 1 1 calc R . . . .
C18 C 0.2329(3) 0.7442(2) 0.04611(7) 0.0392(5) Uani 1 1 d . . . . .
H18 H 0.2824 0.7758 0.0248 0.047 Uiso 1 1 calc R . . . .
C27 C 0.6082(3) 0.5288(2) 0.27674(7) 0.0408(5) Uani 1 1 d . . . . .
H27 H 0.5527 0.4666 0.2926 0.049 Uiso 1 1 calc R . . . .
C26 C 0.7819(3) 0.5757(2) 0.28060(7) 0.0419(5) Uani 1 1 d . . . . .
C25 C 0.8644(3) 0.6706(3) 0.25724(7) 0.0430(5) Uani 1 1 d . . . . .
H25 H 0.9813 0.7039 0.2600 0.052 Uiso 1 1 calc R . . . .
C17 C 0.0602(3) 0.6853(2) 0.04285(7) 0.0425(6) Uani 1 1 d . . . . .
C15 C 0.0843(3) 0.6499(2) 0.10947(7) 0.0350(5) Uani 1 1 d . . . . .
C40 C 0.6348(3) 0.6323(2) 0.46502(7) 0.0403(5) Uani 1 1 d . . . . .
H40A H 0.5540 0.6589 0.4502 0.060 Uiso 1 1 calc GR . . . .
H40B H 0.7371 0.7094 0.4721 0.060 Uiso 1 1 calc GR . . . .
H40C H 0.5908 0.5977 0.4875 0.060 Uiso 1 1 calc GR . . . .
C51 C 0.0292(3) -0.0848(2) 0.36919(7) 0.0396(5) Uani 1 1 d . . . . .
H51A H 0.0768 0.0002 0.3592 0.059 Uiso 1 1 calc GR . . . .
H51B H -0.0715 -0.0887 0.3794 0.059 Uiso 1 1 calc GR . . . .
H51C H 0.0029 -0.1575 0.3492 0.059 Uiso 1 1 calc GR . . . .
C3 C 0.4670(3) 0.2605(2) 0.05573(8) 0.0438(6) Uani 1 1 d . . . . .
C28 C 0.5138(3) 0.5719(2) 0.24984(6) 0.0387(5) Uani 1 1 d . . . . .
C7 C 0.0783(3) 0.1085(2) 0.10583(8) 0.0413(5) Uani 1 1 d . . . . .
C53 C 0.6027(3) -0.0914(3) 0.41117(8) 0.0437(6) Uani 1 1 d . . . . .
H53A H 0.5899 -0.1578 0.3902 0.066 Uiso 1 1 calc GR . . . .
H53B H 0.6674 -0.1069 0.4329 0.066 Uiso 1 1 calc GR . . . .
H53C H 0.6597 -0.0025 0.4042 0.066 Uiso 1 1 calc GR . . . .
C43 C 0.3853(4) -0.1407(2) 0.29724(8) 0.0474(6) Uani 1 1 d . . . . .
H43 H 0.3824 -0.1916 0.2747 0.057 Uiso 1 1 calc R . . . .
C31 C 0.3250(3) 0.5170(3) 0.24573(8) 0.0467(6) Uani 1 1 d . . . . .
H31A H 0.2842 0.5889 0.2416 0.070 Uiso 1 1 calc GR . . . .
H31B H 0.2891 0.4788 0.2685 0.070 Uiso 1 1 calc GR . . . .
H31C H 0.2812 0.4481 0.2244 0.070 Uiso 1 1 calc GR . . . .
C30 C 0.8797(4) 0.5228(3) 0.30904(8) 0.0501(6) Uani 1 1 d . . . . .
H30A H 0.9238 0.5870 0.3314 0.075 Uiso 1 1 calc GR . . . .
H30B H 0.9708 0.5094 0.2979 0.075 Uiso 1 1 calc GR . . . .
H30C H 0.8068 0.4382 0.3159 0.075 Uiso 1 1 calc GR . . . .
C44 C 0.3198(4) -0.1885(2) 0.32792(8) 0.0464(6) Uani 1 1 d . . . . .
H44 H 0.2619 -0.2789 0.3307 0.056 Uiso 1 1 calc R . . . .
C62 C 0.2752(3) 0.1225(3) 0.25774(8) 0.0498(6) Uani 1 1 d . . . . .
H62A H 0.2122 0.0271 0.2564 0.075 Uiso 1 1 calc GR . . . .
H62B H 0.2309 0.1592 0.2371 0.075 Uiso 1 1 calc GR . . . .
H62C H 0.2667 0.1666 0.2815 0.075 Uiso 1 1 calc GR . . . .
C52 C 0.1869(4) -0.1420(3) 0.50555(8) 0.0544(7) Uani 1 1 d . . . . .
H52A H 0.1413 -0.0755 0.5133 0.082 Uiso 1 1 calc GR . . . .
H52B H 0.2854 -0.1315 0.5229 0.082 Uiso 1 1 calc GR . . . .
H52C H 0.1045 -0.2310 0.5056 0.082 Uiso 1 1 calc GR . . . .
C22 C 0.5234(3) 0.8198(3) 0.08306(8) 0.0512(6) Uani 1 1 d . . . . .
H22A H 0.5648 0.8977 0.1017 0.077 Uiso 1 1 calc GR . . . .
H22B H 0.5541 0.8466 0.0588 0.077 Uiso 1 1 calc GR . . . .
H22C H 0.5715 0.7547 0.0904 0.077 Uiso 1 1 calc GR . . . .
C35 C 0.2159(3) 0.5273(3) 0.40901(9) 0.0492(6) Uani 1 1 d . . . . .
H35A H 0.2321 0.5459 0.4362 0.074 Uiso 1 1 calc GR . . . .
H35B H 0.1157 0.5404 0.3987 0.074 Uiso 1 1 calc GR . . . .
H35C H 0.3108 0.5876 0.3990 0.074 Uiso 1 1 calc GR . . . .
C61 C 0.8004(4) 0.3430(3) 0.19912(8) 0.0529(7) Uani 1 1 d . . . . .
H61A H 0.9181 0.3839 0.2086 0.079 Uiso 1 1 calc GR . . . .
H61B H 0.7542 0.4124 0.1961 0.079 Uiso 1 1 calc GR . . . .
H61C H 0.7860 0.2912 0.1750 0.079 Uiso 1 1 calc GR . . . .
C29 C 0.8681(4) 0.8190(3) 0.20458(8) 0.0493(6) Uani 1 1 d . . . . .
H29A H 0.8182 0.7887 0.1786 0.074 Uiso 1 1 calc GR . . . .
H29B H 0.9843 0.8284 0.2071 0.074 Uiso 1 1 calc GR . . . .
H29C H 0.8599 0.9048 0.2119 0.074 Uiso 1 1 calc GR . . . .
C36 C 0.1717(4) 0.3495(3) 0.35491(8) 0.0516(6) Uani 1 1 d . . . . .
H36A H 0.2604 0.4149 0.3444 0.077 Uiso 1 1 calc GR . . . .
H36B H 0.0655 0.3535 0.3448 0.077 Uiso 1 1 calc GR . . . .
H36C H 0.1720 0.2605 0.3483 0.077 Uiso 1 1 calc GR . . . .
C41 C 0.7929(4) 0.4765(3) 0.46607(10) 0.0601(8) Uani 1 1 d . . . . .
H41A H 0.7428 0.4397 0.4878 0.090 Uiso 1 1 calc GR . . . .
H41B H 0.8950 0.5524 0.4745 0.090 Uiso 1 1 calc GR . . . .
H41C H 0.8175 0.4084 0.4514 0.090 Uiso 1 1 calc GR . . . .
C20 C 0.0053(4) 0.5918(3) 0.14333(9) 0.0537(7) Uani 1 1 d . . . . .
H20A H 0.0219 0.5082 0.1467 0.081 Uiso 1 1 calc GR . . . .
H20B H -0.1129 0.5752 0.1392 0.081 Uiso 1 1 calc GR . . . .
H20C H 0.0566 0.6548 0.1657 0.081 Uiso 1 1 calc GR . . . .
C37 C 0.0498(3) 0.2835(3) 0.41443(10) 0.0535(7) Uani 1 1 d . . . . .
H37A H 0.0448 0.1924 0.4089 0.080 Uiso 1 1 calc GR . . . .
H37B H -0.0525 0.2913 0.4031 0.080 Uiso 1 1 calc GR . . . .
H37C H 0.0637 0.3059 0.4415 0.080 Uiso 1 1 calc GR . . . .
C39 C 0.7461(4) 0.5761(3) 0.40594(9) 0.0597(8) Uani 1 1 d . . . . .
H39A H 0.7639 0.5048 0.3911 0.090 Uiso 1 1 calc GR . . . .
H39B H 0.8515 0.6496 0.4134 0.090 Uiso 1 1 calc GR . . . .
H39C H 0.6701 0.6075 0.3911 0.090 Uiso 1 1 calc GR . . . .
C6 C 0.3996(4) 0.1225(3) 0.03219(9) 0.0559(8) Uani 1 1 d . . . . .
H6A H 0.3596 0.0530 0.0485 0.084 Uiso 1 1 calc GR . . . .
H6B H 0.4879 0.1092 0.0199 0.084 Uiso 1 1 calc GR . . . .
H6C H 0.3089 0.1183 0.0133 0.084 Uiso 1 1 calc GR . . . .
C9 C 0.1777(4) 0.0323(3) 0.12602(9) 0.0530(7) Uani 1 1 d . . . . .
H9A H 0.2447 0.0085 0.1089 0.080 Uiso 1 1 calc GR . . . .
H9B H 0.1011 -0.0484 0.1340 0.080 Uiso 1 1 calc GR . . . .
H9C H 0.2497 0.0891 0.1479 0.080 Uiso 1 1 calc GR . . . .
C4 C 0.6112(4) 0.2699(4) 0.08603(11) 0.0679(9) Uani 1 1 d . . . . .
H4A H 0.6470 0.3551 0.1016 0.102 Uiso 1 1 calc GR . . . .
H4B H 0.7034 0.2633 0.0739 0.102 Uiso 1 1 calc GR . . . .
H4C H 0.5739 0.1974 0.1016 0.102 Uiso 1 1 calc GR . . . .
C5 C 0.5308(4) 0.3723(3) 0.02967(10) 0.0583(7) Uani 1 1 d . . . . .
H5A H 0.4425 0.3635 0.0096 0.087 Uiso 1 1 calc GR . . . .
H5B H 0.6253 0.3639 0.0190 0.087 Uiso 1 1 calc GR . . . .
H5C H 0.5643 0.4593 0.0442 0.087 Uiso 1 1 calc GR . . . .
C8 C -0.0351(4) 0.0165(3) 0.07093(10) 0.0634(8) Uani 1 1 d . . . . .
H8A H -0.1002 0.0624 0.0583 0.095 Uiso 1 1 calc GR . . . .
H8B H -0.1093 -0.0654 0.0789 0.095 Uiso 1 1 calc GR . . . .
H8C H 0.0332 -0.0052 0.0537 0.095 Uiso 1 1 calc GR . . . .
C21 C -0.0472(4) 0.6728(3) 0.00539(9) 0.0648(9) Uani 1 1 d . . . . .
H21A H -0.1460 0.5922 0.0031 0.097 Uiso 1 1 calc GR . . . .
H21B H 0.0156 0.6679 -0.0151 0.097 Uiso 1 1 calc GR . . . .
H21C H -0.0797 0.7503 0.0044 0.097 Uiso 1 1 calc GR . . . .
C10 C -0.0253(4) 0.1486(3) 0.13282(11) 0.0636(8) Uani 1 1 d . . . . .
H10A H 0.0473 0.2027 0.1550 0.095 Uiso 1 1 calc GR . . . .
H10B H -0.1057 0.0687 0.1403 0.095 Uiso 1 1 calc GR . . . .
H10C H -0.0834 0.2000 0.1203 0.095 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 7 -1 0.0460
5 -3 5 0.0572
-1 -6 -1 0.0536
-5 0 -5 0.0466
0 0 -23 0.0197
0 0 23 0.0197
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
C32 P4 P3 100.70(7) . . ?
C33 P4 P3 98.58(7) . . ?
C33 P4 C32 41.20(10) . . ?
C42 P3 P4 105.49(7) . . ?
C2 P2 P1 99.40(7) . . ?
C1 P2 P1 99.19(7) . . ?
C1 P2 C2 41.31(10) . . ?
C11 P1 P2 105.30(7) . . ?
C42 N4 C54 124.91(17) . . ?
C42 N4 C43 110.72(18) . . ?
C43 N4 C54 124.34(18) . . ?
C11 N1 C14 127.89(17) . . ?
C11 N1 C12 110.35(18) . . ?
C12 N1 C14 121.74(18) . . ?
C42 N3 C45 126.06(17) . . ?
C42 N3 C44 110.42(18) . . ?
C44 N3 C45 123.35(18) . . ?
C11 N2 C23 125.73(18) . . ?
C13 N2 C11 110.44(19) . . ?
C13 N2 C23 123.77(18) . . ?
C50 C45 N3 118.0(2) . . ?
C46 C45 N3 119.1(2) . . ?
C46 C45 C50 122.8(2) . . ?
C54 C55 C56 117.5(2) . . ?
C54 C55 C60 121.1(2) . . ?
C56 C55 C60 121.4(2) . . ?
C55 C54 N4 118.5(2) . . ?
C55 C54 C59 122.7(2) . . ?
C59 C54 N4 118.7(2) . . ?
C45 C50 C53 119.7(2) . . ?
C49 C50 C45 117.6(2) . . ?
C49 C50 C53 122.6(2) . . ?
C33 C32 P4 68.97(13) . . ?
C33 C32 C34 150.7(2) . . ?
C34 C32 P4 140.15(16) . . ?
C19 C14 N1 118.60(19) . . ?
C19 C14 C15 122.3(2) . . ?
C15 C14 N1 119.01(19) . . ?
N4 C42 P3 121.58(15) . . ?
N4 C42 N3 103.67(17) . . ?
N3 C42 P3 134.74(16) . . ?
C57 C56 C55 121.8(2) . . ?
C1 C2 P2 69.10(13) . . ?
C1 C2 C7 146.6(2) . . ?
C7 C2 P2 144.18(18) . . ?
C14 C19 C18 117.6(2) . . ?
C14 C19 C22 121.2(2) . . ?
C18 C19 C22 121.2(2) . . ?
C46 C47 C48 121.7(2) . . ?
C2 C1 P2 69.59(14) . . ?
C2 C1 C3 148.9(2) . . ?
C3 C1 P2 141.31(17) . . ?
C32 C33 P4 69.83(12) . . ?
C32 C33 C38 149.3(2) . . ?
C38 C33 P4 140.37(17) . . ?
C54 C59 C62 121.4(2) . . ?
C58 C59 C54 117.4(2) . . ?
C58 C59 C62 121.2(2) . . ?
C45 C46 C51 120.9(2) . . ?
C47 C46 C45 117.4(2) . . ?
C47 C46 C51 121.7(2) . . ?
N1 C11 P1 134.65(16) . . ?
N1 C11 N2 103.84(17) . . ?
N2 C11 P1 121.43(16) . . ?
C48 C49 C50 121.6(2) . . ?
C24 C23 N2 118.1(2) . . ?
C24 C23 C28 122.2(2) . . ?
C28 C23 N2 119.7(2) . . ?
C56 C57 C58 118.8(2) . . ?
C56 C57 C61 121.2(2) . . ?
C58 C57 C61 120.1(2) . . ?
C32 C34 C35 110.71(19) . . ?
C32 C34 C36 108.06(19) . . ?
C32 C34 C37 108.7(2) . . ?
C36 C34 C35 110.0(2) . . ?
C36 C34 C37 109.2(2) . . ?
C37 C34 C35 110.1(2) . . ?
C57 C58 C59 121.8(2) . . ?
C47 C48 C52 119.8(2) . . ?
C49 C48 C47 118.8(2) . . ?
C49 C48 C52 121.4(2) . . ?
C23 C24 C29 121.1(2) . . ?
C25 C24 C23 117.8(2) . . ?
C25 C24 C29 121.0(2) . . ?
C12 C13 N2 107.6(2) . . ?
C13 C12 N1 107.7(2) . . ?
C33 C38 C40 110.74(19) . . ?
C33 C38 C41 109.6(2) . . ?
C33 C38 C39 106.8(2) . . ?
C40 C38 C41 108.9(2) . . ?
C40 C38 C39 110.7(2) . . ?
C41 C38 C39 110.0(2) . . ?
C17 C16 C15 122.1(2) . . ?
C17 C18 C19 122.0(2) . . ?
C26 C27 C28 122.1(2) . . ?
C27 C26 C25 118.7(2) . . ?
C27 C26 C30 120.6(2) . . ?
C25 C26 C30 120.7(2) . . ?
C24 C25 C26 121.7(2) . . ?
C16 C17 C21 120.9(3) . . ?
C18 C17 C16 118.5(2) . . ?
C18 C17 C21 120.6(3) . . ?
C14 C15 C20 120.8(2) . . ?
C16 C15 C14 117.5(2) . . ?
C16 C15 C20 121.6(2) . . ?
C1 C3 C6 109.8(2) . . ?
C1 C3 C4 108.6(2) . . ?
C1 C3 C5 109.1(2) . . ?
C6 C3 C4 110.6(3) . . ?
C6 C3 C5 109.7(2) . . ?
C4 C3 C5 109.0(3) . . ?
C23 C28 C31 121.6(2) . . ?
C27 C28 C23 117.5(2) . . ?
C27 C28 C31 120.9(2) . . ?
C2 C7 C9 109.1(2) . . ?
C2 C7 C8 108.4(2) . . ?
C2 C7 C10 110.1(2) . . ?
C9 C7 C8 108.6(2) . . ?
C10 C7 C9 109.9(2) . . ?
C10 C7 C8 110.7(3) . . ?
C44 C43 N4 107.5(2) . . ?
C43 C44 N3 107.7(2) . . ?
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
P4 P3 2.2342(7) . ?
P4 C32 1.852(2) . ?
P4 C33 1.841(2) . ?
P3 C42 1.760(2) . ?
P2 P1 2.2225(8) . ?
P2 C2 1.841(2) . ?
P2 C1 1.835(2) . ?
P1 C11 1.768(2) . ?
N4 C54 1.437(3) . ?
N4 C42 1.376(3) . ?
N4 C43 1.386(3) . ?
N1 C14 1.432(3) . ?
N1 C11 1.372(3) . ?
N1 C12 1.390(3) . ?
N3 C45 1.428(3) . ?
N3 C42 1.378(3) . ?
N3 C44 1.388(3) . ?
N2 C11 1.384(3) . ?
N2 C23 1.431(3) . ?
N2 C13 1.383(3) . ?
C45 C50 1.391(3) . ?
C45 C46 1.389(3) . ?
C55 C54 1.387(3) . ?
C55 C56 1.397(3) . ?
C55 C60 1.500(3) . ?
C54 C59 1.399(3) . ?
C50 C49 1.388(3) . ?
C50 C53 1.508(3) . ?
C32 C33 1.299(3) . ?
C32 C34 1.494(3) . ?
C14 C19 1.386(3) . ?
C14 C15 1.389(3) . ?
C56 C57 1.386(3) . ?
C2 C1 1.297(3) . ?
C2 C7 1.500(3) . ?
C19 C18 1.390(3) . ?
C19 C22 1.501(4) . ?
C47 C46 1.388(3) . ?
C47 C48 1.393(3) . ?
C1 C3 1.501(4) . ?
C33 C38 1.498(3) . ?
C59 C58 1.391(3) . ?
C59 C62 1.497(3) . ?
C46 C51 1.503(3) . ?
C49 C48 1.385(4) . ?
C23 C24 1.396(4) . ?
C23 C28 1.399(3) . ?
C57 C58 1.389(4) . ?
C57 C61 1.511(3) . ?
C34 C35 1.531(3) . ?
C34 C36 1.524(4) . ?
C34 C37 1.529(3) . ?
C48 C52 1.505(3) . ?
C24 C25 1.388(3) . ?
C24 C29 1.508(3) . ?
C13 C12 1.329(3) . ?
C38 C40 1.526(3) . ?
C38 C41 1.527(4) . ?
C38 C39 1.530(4) . ?
C16 C17 1.379(4) . ?
C16 C15 1.388(4) . ?
C18 C17 1.378(4) . ?
C27 C26 1.382(4) . ?
C27 C28 1.393(3) . ?
C26 C25 1.392(4) . ?
C26 C30 1.509(4) . ?
C17 C21 1.509(4) . ?
C15 C20 1.503(3) . ?
C3 C6 1.523(4) . ?
C3 C4 1.524(4) . ?
C3 C5 1.536(4) . ?
C28 C31 1.502(4) . ?
C7 C9 1.529(4) . ?
C7 C8 1.535(4) . ?
C7 C10 1.510(4) . ?
C43 C44 1.327(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
-0.6792 6.6899 -0.9343 -0.0661 -0.0453 0.9968
5.2795 -2.7123 5.0245 -0.8004 -0.5504 -0.2377
-1.0941 -5.7593 -0.7543 0.3344 0.2298 -0.9140
-4.9111 -0.0241 -4.5583 0.8124 0.5586 -0.1670
0.0938 0.1251 -22.8928 0.7935 -0.6086 -0.0092
-0.1649 0.3174 22.7444 -0.7913 0.6069 0.0741
