#------------------------------------------------------------------------------
#$Date: 2022-10-01 01:31:35 +0300 (Sat, 01 Oct 2022) $
#$Revision: 278283 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/55/7245595.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_7245595
loop_
_publ_author_name
'Ward, Jas S.'
_publ_section_title
;
 The Solid-state Hierarchy and Iodination Potential of
 [bis(3-acetaminopyridine)iodine(I)]PF6
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE01225A
_journal_year                    2022
_chemical_formula_moiety         'C14 H16 I N4 O2, F6 P'
_chemical_formula_sum            'C14 H16 F6 I N4 O2 P'
_chemical_formula_weight         544.18
_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             2022-07-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-08-01 deposited with the CCDC.	2022-09-30 downloaded from the CCDC.
;
_cell_angle_alpha                103.504(3)
_cell_angle_beta                 99.401(2)
_cell_angle_gamma                90.172(2)
_cell_formula_units_Z            4
_cell_length_a                   9.9264(3)
_cell_length_b                   13.3351(4)
_cell_length_c                   14.6878(5)
_cell_measurement_reflns_used    12874
_cell_measurement_temperature    119.97(10)
_cell_measurement_theta_max      76.5810
_cell_measurement_theta_min      3.0770
_cell_volume                     1863.36(11)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_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      119.97(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3895
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -87.00  -6.00   1.00    1.00    --  -42.04 125.00-180.00   81
  2  ω   -117.00 -18.00   1.00    1.00    --  -42.04 -37.00  30.00   99
  3  ω    -75.00  34.00   1.00    1.00    --  -42.04  77.00 -60.00  109
  4  ω    -66.00  32.00   1.00    1.00    --  -42.04  37.00-150.00   98
  5  ω      9.00  42.00   1.00    1.00    --   42.04  80.00  41.77   33
  6  ω    103.00 178.00   1.00    3.00    --  112.00  77.00 -90.00   75
  7  ω     40.00 141.00   1.00    3.00    --  112.00 -61.00 -30.00  101
  8  ω     85.00 178.00   1.00    3.00    --  112.00  53.00  22.46   93
  9  ω     36.00 109.00   1.00    3.00    --  112.00-111.00  90.00   73
 10  ω     84.00 178.00   1.00    3.00    --  112.00  30.00-150.00   94
 11  ω     29.00 107.00   1.00    3.00    --  112.00 -94.00-120.00   78
 12  ω    103.00 178.00   1.00    3.00    --  112.00  77.00 -30.00   75
 13  ω     36.00 140.00   1.00    3.00    --  112.00 -30.00-150.00  104
 14  ω     29.00 107.00   1.00    3.00    --  112.00 -94.00 -60.00   78
 15  ω     36.00 109.00   1.00    3.00    --  112.00-111.00 150.00   73
 16  ω     59.00 178.00   1.00    3.00    --  112.00  15.00 150.00  119
 17  ω     36.00 109.00   1.00    3.00    --  112.00-111.00   0.00   73
 18  ω     29.00 107.00   1.00    3.00    --  112.00 -94.00-180.00   78
 19  ω    -87.00  -6.00   1.00    1.00    --  -42.04 125.00   0.00   81
 20  ω   -114.00 -14.00   1.00    1.00    --  -42.04 -57.00 150.00  100
 21  ω   -114.00 -14.00   1.00    1.00    --  -42.04 -57.00-120.00  100
 22  ω      7.00  33.00   1.00    1.00    --   42.04  84.00 176.97   26
 23  ω      8.00  42.00   1.00    1.00    --   42.04  82.00-139.48   34
 24  ω      8.00  34.00   1.00    1.00    --   42.04  83.00   4.59   26
 25  ω     59.00 178.00   1.00    3.00    --  112.00  15.00 -30.00  119
 26  ω     83.00 178.00   1.00    3.00    --  112.00  61.00-150.00   95
 27  ω     83.00 178.00   1.00    3.00    --  112.00  61.00 120.00   95
 28  ω     83.00 178.00   1.00    3.00    --  112.00  61.00 -30.00   95
 29  ω     83.00 178.00   1.00    3.00    --  112.00  61.00  60.00   95
 30  ω     83.00 178.00   1.00    3.00    --  112.00  61.00 150.00   95
 31  ω     83.00 178.00   1.00    3.00    --  112.00  61.00 -60.00   95
 32  ω     80.00 178.00   1.00    3.00    --  112.00  74.00-105.87   98
 33  ω     83.00 178.00   1.00    3.00    --  112.00  61.00   0.00   95
 34  ω     83.00 178.00   1.00    3.00    --  112.00  61.00  90.00   95
 35  ω     83.00 178.00   1.00    3.00    --  112.00  61.00  30.00   95
 36  ω     81.00 178.00   1.00    3.00    --  112.00  69.00-133.29   97
 37  ω   -117.00 -56.00   1.00    1.00    --  -42.04-156.00-109.00   61
 38  ω   -117.00 -18.00   1.00    1.00    --  -42.04 -37.00 -90.00   99
 39  ω      7.00  33.00   1.00    1.00    --   42.04  84.00 -45.14   26
 40  ω      9.00  42.00   1.00    1.00    --   42.04  81.00  81.06   33
 41  ω      9.00  42.00   1.00    1.00    --   42.04  81.00 -80.80   33
 42  ω      9.00  42.00   1.00    1.00    --   42.04  80.00 105.41   33
 43  ω     83.00 134.00   1.00    3.00    --  112.00  61.00-180.00   51
;
_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      0.1231079000
_diffrn_orient_matrix_UB_12      -0.0700443000
_diffrn_orient_matrix_UB_13      0.0009525000
_diffrn_orient_matrix_UB_21      0.0134750000
_diffrn_orient_matrix_UB_22      0.0171621000
_diffrn_orient_matrix_UB_23      0.1085798000
_diffrn_orient_matrix_UB_31      -0.0972369000
_diffrn_orient_matrix_UB_32      -0.0945592000
_diffrn_orient_matrix_UB_33      -0.0136429000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0543
_diffrn_reflns_av_unetI/netI     0.0350
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            37453
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.491
_diffrn_reflns_theta_min         3.139
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    15.056
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.165
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
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    1.940
_exptl_crystal_description       plate
_exptl_crystal_F_000             1064
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: MeCN'
_exptl_crystal_size_max          0.168
_exptl_crystal_size_mid          0.164
_exptl_crystal_size_min          0.014
_refine_diff_density_max         6.174
_refine_diff_density_min         -1.350
_refine_diff_density_rms         0.189
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     509
_refine_ls_number_reflns         7610
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0630
_refine_ls_R_factor_gt           0.0555
_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)+(0.0876P)²+7.4916P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1436
_refine_ls_wR_factor_ref         0.1512
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6527
_reflns_number_total             7610
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2ce01225a2.cif
_cod_data_source_block           3_2
_cod_original_cell_volume        1863.36(10)
_cod_database_code               7245595
_shelxl_version_number           2014/6
_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 99.53
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N7(H7), N17(H17), C2(H2), C4(H4), C5(H5), C6(H6), C12(H12), C14(H14),
 C15(H15), C16(H16), N27(H27), N37(H37), C22(H22), C24(H24), C25(H25), C26(H26),
  C32(H32), C34(H34), C35(H35), C36(H36)
2.b Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C20(H20A,H20B,H20C), C30(H30A,H30B,H30C), C40(H40A,H40B,
 H40C)
;
_ins_header
;
TITL OHD383_numabs in P-1 
REM P-1 (#2 in standard setting)
CELL 1.54184   9.926442  13.335083  14.687814 103.5037  99.4007  90.1715
ZERR    4.00   0.000255   0.000429   0.000523   0.0029   0.0025   0.0023
LATT  1
SFAC C H N O F P I
UNIT 56.00 64.00 16.00 8.00 24.00 4.00 4.00
TREF
HKLF 4
END
;
_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 1.320
_oxdiff_exptl_absorpt_empirical_full_min 0.794
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
I1 I 0.74123(3) 0.59090(2) 0.49488(2) 0.02103(12) Uani 1 1 d . . . . .
O9 O 1.0870(4) 0.4067(4) 0.0942(3) 0.0314(9) Uani 1 1 d . . . . .
O19 O 0.4186(4) 0.6058(3) 0.8994(3) 0.0273(9) Uani 1 1 d . . . . .
N1 N 0.8841(4) 0.5657(4) 0.3881(3) 0.0209(9) Uani 1 1 d . . . . .
N7 N 0.8825(5) 0.4598(4) 0.1364(3) 0.0217(9) Uani 1 1 d . . . . .
H7 H 0.7964 0.4612 0.1159 0.026 Uiso 1 1 calc R . . . .
N11 N 0.6018(5) 0.6242(4) 0.6037(3) 0.0222(9) Uani 1 1 d . . . . .
N17 N 0.6196(5) 0.6434(4) 0.8566(3) 0.0230(9) Uani 1 1 d . . . . .
H17 H 0.7058 0.6565 0.8758 0.028 Uiso 1 1 calc R . . . .
C2 C 0.8439(6) 0.5178(4) 0.2971(4) 0.0233(11) Uani 1 1 d . . . . .
H2 H 0.7557 0.4885 0.2776 0.028 Uiso 1 1 calc R . . . .
C3 C 0.9311(5) 0.5107(4) 0.2304(4) 0.0196(10) Uani 1 1 d . . . . .
C4 C 1.0621(6) 0.5578(4) 0.2617(4) 0.0238(11) Uani 1 1 d . . . . .
H4 H 1.1218 0.5571 0.2189 0.029 Uiso 1 1 calc R . . . .
C5 C 1.1021(6) 0.6053(5) 0.3569(4) 0.0262(12) Uani 1 1 d . . . . .
H5 H 1.1893 0.6359 0.3787 0.031 Uiso 1 1 calc R . . . .
C6 C 1.0112(6) 0.6070(5) 0.4198(4) 0.0264(12) Uani 1 1 d . . . . .
H6 H 1.0386 0.6369 0.4841 0.032 Uiso 1 1 calc R . . . .
C8 C 0.9621(5) 0.4075(4) 0.0743(4) 0.0224(11) Uani 1 1 d . . . . .
C10 C 0.8847(6) 0.3521(5) -0.0203(4) 0.0309(13) Uani 1 1 d . . . . .
H10A H 0.9345 0.3596 -0.0693 0.046 Uiso 1 1 calc GR . . . .
H10B H 0.7966 0.3810 -0.0307 0.046 Uiso 1 1 calc GR . . . .
H10C H 0.8733 0.2802 -0.0217 0.046 Uiso 1 1 calc GR . . . .
C12 C 0.6465(5) 0.6195(4) 0.6936(4) 0.0219(11) Uani 1 1 d . . . . .
H12 H 0.7334 0.5960 0.7095 0.026 Uiso 1 1 calc R . . . .
C13 C 0.5655(6) 0.6490(4) 0.7643(4) 0.0210(10) Uani 1 1 d . . . . .
C14 C 0.4360(5) 0.6861(4) 0.7384(4) 0.0233(11) Uani 1 1 d . . . . .
H14 H 0.3804 0.7089 0.7837 0.028 Uiso 1 1 calc R . . . .
C15 C 0.3927(6) 0.6881(5) 0.6448(5) 0.0279(12) Uani 1 1 d . . . . .
H15 H 0.3066 0.7115 0.6267 0.033 Uiso 1 1 calc R . . . .
C16 C 0.4759(6) 0.6557(5) 0.5772(4) 0.0263(12) Uani 1 1 d . . . . .
H16 H 0.4448 0.6558 0.5140 0.032 Uiso 1 1 calc R . . . .
C18 C 0.5437(6) 0.6182(4) 0.9184(4) 0.0240(11) Uani 1 1 d . . . . .
C20 C 0.6263(6) 0.6101(5) 1.0120(4) 0.0296(13) Uani 1 1 d . . . . .
H20A H 0.6062 0.6660 1.0616 0.044 Uiso 1 1 calc GR . . . .
H20B H 0.7219 0.6136 1.0086 0.044 Uiso 1 1 calc GR . . . .
H20C H 0.6033 0.5456 1.0253 0.044 Uiso 1 1 calc GR . . . .
I2 I 0.24591(3) 0.90438(2) 0.49850(2) 0.02091(12) Uani 1 1 d . . . . .
O29 O 0.7861(4) 1.0934(3) 0.8954(3) 0.0275(9) Uani 1 1 d . . . . .
O39 O -0.2944(4) 0.8883(4) 0.1003(3) 0.0319(9) Uani 1 1 d . . . . .
N21 N 0.4439(5) 0.9290(4) 0.6023(3) 0.0220(9) Uani 1 1 d . . . . .
N27 N 0.5632(5) 1.0358(4) 0.8538(3) 0.0225(9) Uani 1 1 d . . . . .
H27 H 0.4873 1.0335 0.8745 0.027 Uiso 1 1 calc R . . . .
N31 N 0.0491(5) 0.8733(4) 0.3933(3) 0.0230(9) Uani 1 1 d . . . . .
N37 N -0.0699(5) 0.8602(4) 0.1440(3) 0.0224(9) Uani 1 1 d . . . . .
H37 H 0.0075 0.8526 0.1247 0.027 Uiso 1 1 calc R . . . .
C22 C 0.4473(5) 0.9770(4) 0.6936(4) 0.0218(11) Uani 1 1 d . . . . .
H22 H 0.3685 1.0059 0.7130 0.026 Uiso 1 1 calc R . . . .
C23 C 0.5662(5) 0.9843(4) 0.7601(4) 0.0203(10) Uani 1 1 d . . . . .
C24 C 0.6831(6) 0.9375(4) 0.7299(4) 0.0236(11) Uani 1 1 d . . . . .
H24 H 0.7636 0.9389 0.7728 0.028 Uiso 1 1 calc R . . . .
C25 C 0.6753(6) 0.8889(5) 0.6342(4) 0.0262(12) Uani 1 1 d . . . . .
H25 H 0.7515 0.8579 0.6124 0.031 Uiso 1 1 calc R . . . .
C26 C 0.5550(6) 0.8865(5) 0.5717(4) 0.0265(12) Uani 1 1 d . . . . .
H26 H 0.5511 0.8552 0.5077 0.032 Uiso 1 1 calc R . . . .
C28 C 0.6723(6) 1.0901(4) 0.9159(4) 0.0232(11) Uani 1 1 d . . . . .
C30 C 0.6387(7) 1.1423(5) 1.0121(4) 0.0321(13) Uani 1 1 d . . . . .
H30A H 0.6950 1.1165 1.0605 0.048 Uiso 1 1 calc GR . . . .
H30B H 0.5442 1.1281 1.0133 0.048 Uiso 1 1 calc GR . . . .
H30C H 0.6556 1.2155 1.0236 0.048 Uiso 1 1 calc GR . . . .
C32 C 0.0455(5) 0.8790(4) 0.3034(4) 0.0229(11) Uani 1 1 d . . . . .
H32 H 0.1239 0.9010 0.2853 0.028 Uiso 1 1 calc R . . . .
C33 C -0.0729(5) 0.8528(4) 0.2361(4) 0.0200(10) Uani 1 1 d . . . . .
C34 C -0.1891(6) 0.8186(4) 0.2654(4) 0.0241(11) Uani 1 1 d . . . . .
H34 H -0.2695 0.7987 0.2222 0.029 Uiso 1 1 calc R . . . .
C35 C -0.1821(6) 0.8149(5) 0.3601(4) 0.0261(12) Uani 1 1 d . . . . .
H35 H -0.2583 0.7928 0.3806 0.031 Uiso 1 1 calc R . . . .
C36 C -0.0616(6) 0.8440(4) 0.4234(4) 0.0232(11) Uani 1 1 d . . . . .
H36 H -0.0575 0.8432 0.4870 0.028 Uiso 1 1 calc R . . . .
C38 C -0.1793(6) 0.8786(4) 0.0809(4) 0.0246(11) Uani 1 1 d . . . . .
C40 C -0.1449(7) 0.8847(5) -0.0142(4) 0.0323(13) Uani 1 1 d . . . . .
H40A H -0.2237 0.8633 -0.0626 0.048 Uiso 1 1 calc GR . . . .
H40B H -0.0714 0.8403 -0.0285 0.048 Uiso 1 1 calc GR . . . .
H40C H -0.1176 0.9545 -0.0119 0.048 Uiso 1 1 calc GR . . . .
P101 P 0.43210(14) 0.69036(11) 0.25776(10) 0.0213(3) Uani 1 1 d . . . . .
F102 F 0.4977(4) 0.7917(4) 0.3335(4) 0.0544(13) Uani 1 1 d . . . . .
F103 F 0.5812(3) 0.6439(3) 0.2572(3) 0.0302(7) Uani 1 1 d . . . . .
F104 F 0.3663(4) 0.5889(3) 0.1828(3) 0.0445(10) Uani 1 1 d . . . . .
F105 F 0.2839(3) 0.7363(3) 0.2592(3) 0.0313(8) Uani 1 1 d . . . . .
F106 F 0.4128(4) 0.6377(4) 0.3425(3) 0.0543(13) Uani 1 1 d . . . . .
F107 F 0.4533(5) 0.7431(3) 0.1745(3) 0.0460(11) Uani 1 1 d . . . . .
P111 P 0.05499(13) 0.81155(11) 0.74013(10) 0.0215(3) Uani 1 1 d . . . . .
F112 F 0.2042(3) 0.8591(3) 0.7431(3) 0.0312(8) Uani 1 1 d . . . . .
F113 F 0.0329(5) 0.9031(3) 0.8267(3) 0.0473(11) Uani 1 1 d . . . . .
F114 F -0.0945(3) 0.7636(3) 0.7366(3) 0.0330(8) Uani 1 1 d . . . . .
F115 F 0.0761(4) 0.7205(4) 0.6521(4) 0.0613(15) Uani 1 1 d . . . . .
F116 F 0.1187(4) 0.7438(3) 0.8106(4) 0.0498(12) Uani 1 1 d . . . . .
F117 F -0.0074(4) 0.8797(4) 0.6681(4) 0.0537(13) Uani 1 1 d . . . . .
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'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.3257 6.8362 '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'
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
0 0 9 0.0128
0 0 -9 0.0010
6 0 0 0.0668
-6 0 0 0.0967
0 -9 2 0.0888
0 9 -2 0.0748
-4 -7 2 0.0881
-2 8 -2 0.0872
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
N11 I1 N1 177.23(17) . . ?
C2 N1 I1 122.5(4) . . ?
C2 N1 C6 121.3(5) . . ?
C6 N1 I1 116.1(4) . . ?
C3 N7 H7 117.6 . . ?
C8 N7 H7 117.6 . . ?
C8 N7 C3 124.7(5) . . ?
C12 N11 I1 120.6(4) . . ?
C12 N11 C16 121.2(5) . . ?
C16 N11 I1 118.0(4) . . ?
C13 N17 H17 118.1 . . ?
C18 N17 H17 118.1 . . ?
C18 N17 C13 123.8(5) . . ?
N1 C2 H2 119.2 . . ?
N1 C2 C3 121.6(5) . . ?
C3 C2 H2 119.2 . . ?
N7 C3 C2 118.6(5) . . ?
N7 C3 C4 123.6(5) . . ?
C2 C3 C4 117.8(5) . . ?
C3 C4 H4 120.3 . . ?
C5 C4 C3 119.4(5) . . ?
C5 C4 H4 120.3 . . ?
C4 C5 H5 120.2 . . ?
C4 C5 C6 119.7(5) . . ?
C6 C5 H5 120.2 . . ?
N1 C6 C5 120.2(5) . . ?
N1 C6 H6 119.9 . . ?
C5 C6 H6 119.9 . . ?
O9 C8 N7 122.9(5) . . ?
O9 C8 C10 122.4(5) . . ?
N7 C8 C10 114.7(5) . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N11 C12 H12 119.3 . . ?
N11 C12 C13 121.5(5) . . ?
C13 C12 H12 119.3 . . ?
N17 C13 C12 118.3(5) . . ?
N17 C13 C14 123.8(5) . . ?
C12 C13 C14 117.8(5) . . ?
C13 C14 H14 120.6 . . ?
C15 C14 C13 118.9(5) . . ?
C15 C14 H14 120.6 . . ?
C14 C15 H15 119.6 . . ?
C14 C15 C16 120.9(5) . . ?
C16 C15 H15 119.6 . . ?
N11 C16 C15 119.6(5) . . ?
N11 C16 H16 120.2 . . ?
C15 C16 H16 120.2 . . ?
O19 C18 N17 122.4(5) . . ?
O19 C18 C20 123.4(5) . . ?
N17 C18 C20 114.2(5) . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N21 I2 N31 177.85(17) . . ?
C22 N21 I2 120.9(4) . . ?
C26 N21 I2 117.7(4) . . ?
C26 N21 C22 121.1(5) . . ?
C23 N27 H27 117.5 . . ?
C28 N27 H27 117.5 . . ?
C28 N27 C23 125.1(5) . . ?
C32 N31 I2 120.9(4) . . ?
C32 N31 C36 121.6(5) . . ?
C36 N31 I2 117.3(4) . . ?
C33 N37 H37 117.1 . . ?
C38 N37 H37 117.1 . . ?
C38 N37 C33 125.9(5) . . ?
N21 C22 H22 119.3 . . ?
N21 C22 C23 121.4(5) . . ?
C23 C22 H22 119.3 . . ?
N27 C23 C24 123.0(5) . . ?
C22 C23 N27 118.6(5) . . ?
C22 C23 C24 118.4(5) . . ?
C23 C24 H24 120.8 . . ?
C25 C24 C23 118.3(5) . . ?
C25 C24 H24 120.8 . . ?
C24 C25 H25 119.9 . . ?
C26 C25 C24 120.3(5) . . ?
C26 C25 H25 119.9 . . ?
N21 C26 C25 120.5(5) . . ?
N21 C26 H26 119.8 . . ?
C25 C26 H26 119.8 . . ?
O29 C28 N27 122.6(5) . . ?
O29 C28 C30 123.4(5) . . ?
N27 C28 C30 113.9(5) . . ?
C28 C30 H30A 109.5 . . ?
C28 C30 H30B 109.5 . . ?
C28 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
N31 C32 H32 119.3 . . ?
N31 C32 C33 121.5(5) . . ?
C33 C32 H32 119.3 . . ?
N37 C33 C32 118.7(5) . . ?
N37 C33 C34 123.4(5) . . ?
C32 C33 C34 117.9(5) . . ?
C33 C34 H34 120.5 . . ?
C35 C34 C33 119.0(5) . . ?
C35 C34 H34 120.5 . . ?
C34 C35 H35 120.1 . . ?
C36 C35 C34 119.9(5) . . ?
C36 C35 H35 120.1 . . ?
N31 C36 C35 120.0(5) . . ?
N31 C36 H36 120.0 . . ?
C35 C36 H36 120.0 . . ?
O39 C38 N37 122.4(5) . . ?
O39 C38 C40 123.4(5) . . ?
N37 C38 C40 114.1(5) . . ?
C38 C40 H40A 109.5 . . ?
C38 C40 H40B 109.5 . . ?
C38 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
F102 P101 F103 89.8(2) . . ?
F102 P101 F105 90.1(2) . . ?
F102 P101 F106 89.9(3) . . ?
F104 P101 F102 179.6(3) . . ?
F104 P101 F103 90.2(2) . . ?
F104 P101 F105 89.9(2) . . ?
F104 P101 F106 89.7(3) . . ?
F105 P101 F103 179.5(2) . . ?
F105 P101 F106 90.0(2) . . ?
F106 P101 F103 89.5(2) . . ?
F107 P101 F102 89.6(3) . . ?
F107 P101 F103 89.9(2) . . ?
F107 P101 F104 90.8(3) . . ?
F107 P101 F105 90.6(2) . . ?
F107 P101 F106 179.2(3) . . ?
F112 P111 F114 179.7(2) . . ?
F112 P111 F117 89.6(2) . . ?
F113 P111 F112 90.1(2) . . ?
F113 P111 F114 90.1(2) . . ?
F113 P111 F115 179.2(3) . . ?
F113 P111 F117 89.4(3) . . ?
F114 P111 F117 90.3(2) . . ?
F115 P111 F112 89.9(2) . . ?
F115 P111 F114 89.8(2) . . ?
F115 P111 F117 89.7(3) . . ?
F116 P111 F112 89.7(2) . . ?
F116 P111 F113 91.1(3) . . ?
F116 P111 F114 90.4(2) . . ?
F116 P111 F115 89.7(3) . . ?
F116 P111 F117 179.1(3) . . ?
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
I1 N1 2.251(4) . ?
I1 N11 2.250(4) . ?
O9 C8 1.228(7) . ?
O19 C18 1.229(7) . ?
N1 C2 1.333(7) . ?
N1 C6 1.340(8) . ?
N7 H7 0.8600 . ?
N7 C3 1.394(7) . ?
N7 C8 1.373(7) . ?
N11 C12 1.339(7) . ?
N11 C16 1.345(7) . ?
N17 H17 0.8600 . ?
N17 C13 1.393(7) . ?
N17 C18 1.366(7) . ?
C2 H2 0.9300 . ?
C2 C3 1.397(8) . ?
C3 C4 1.401(8) . ?
C4 H4 0.9300 . ?
C4 C5 1.385(8) . ?
C5 H5 0.9300 . ?
C5 C6 1.389(8) . ?
C6 H6 0.9300 . ?
C8 C10 1.495(8) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C12 H12 0.9300 . ?
C12 C13 1.402(7) . ?
C13 C14 1.405(8) . ?
C14 H14 0.9300 . ?
C14 C15 1.379(9) . ?
C15 H15 0.9300 . ?
C15 C16 1.387(8) . ?
C16 H16 0.9300 . ?
C18 C20 1.509(8) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
I2 N21 2.254(4) . ?
I2 N31 2.256(4) . ?
O29 C28 1.219(7) . ?
O39 C38 1.222(7) . ?
N21 C22 1.339(7) . ?
N21 C26 1.337(8) . ?
N27 H27 0.8600 . ?
N27 C23 1.392(7) . ?
N27 C28 1.376(7) . ?
N31 C32 1.335(8) . ?
N31 C36 1.339(8) . ?
N37 H37 0.8600 . ?
N37 C33 1.385(7) . ?
N37 C38 1.370(7) . ?
C22 H22 0.9300 . ?
C22 C23 1.391(7) . ?
C23 C24 1.406(8) . ?
C24 H24 0.9300 . ?
C24 C25 1.393(8) . ?
C25 H25 0.9300 . ?
C25 C26 1.377(8) . ?
C26 H26 0.9300 . ?
C28 C30 1.513(8) . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C32 H32 0.9300 . ?
C32 C33 1.392(8) . ?
C33 C34 1.405(8) . ?
C34 H34 0.9300 . ?
C34 C35 1.394(8) . ?
C35 H35 0.9300 . ?
C35 C36 1.382(8) . ?
C36 H36 0.9300 . ?
C38 C40 1.510(8) . ?
C40 H40A 0.9600 . ?
C40 H40B 0.9600 . ?
C40 H40C 0.9600 . ?
P101 F102 1.595(4) . ?
P101 F103 1.606(3) . ?
P101 F104 1.592(4) . ?
P101 F105 1.596(3) . ?
P101 F106 1.601(4) . ?
P101 F107 1.587(4) . ?
P111 F112 1.600(4) . ?
P111 F113 1.589(4) . ?
P111 F114 1.602(4) . ?
P111 F115 1.596(4) . ?
P111 F116 1.585(4) . ?
P111 F117 1.602(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
-0.4622 0.4235 9.1062 -0.0779 0.9898 -0.1193
0.4622 -0.4235 -9.1062 0.0779 -0.9898 0.1193
6.3722 -0.3890 -0.1474 0.8116 0.0632 -0.5808
-6.3757 -0.0310 0.2356 -0.7825 -0.0609 0.6197
-0.0620 -8.6458 1.8158 0.5997 0.0479 0.7988
0.0620 8.6458 -1.8158 -0.5997 -0.0479 -0.7988
-4.0216 -6.6584 1.5412 -0.0272 -0.0011 0.9996
-1.9978 8.0008 -2.0102 -0.8083 -0.1079 -0.5349
