#------------------------------------------------------------------------------
#$Date: 2020-06-04 04:19:50 +0300 (Thu, 04 Jun 2020) $
#$Revision: 252620 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/49/4134979.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_4134979
loop_
_publ_author_name
'Asada, Takahiro'
'Hoshimoto, Yoichi'
'Ogoshi, Sensuke'
_publ_section_title
;
 Rotation-Triggered Transmetalation on a Heterobimetallic Cu/Al
 N-Phosphine-Oxide-Substituted Imidazolylidene Complex.
;
_journal_issue                   21
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9772
_journal_page_last               9784
_journal_paper_doi               10.1021/jacs.0c03252
_journal_volume                  142
_journal_year                    2020
_chemical_formula_moiety         'C41 H37 Al F15 N2 O P, C3 H3'
_chemical_formula_sum            'C44 H40 Al F15 N2 O P'
_chemical_formula_weight         955.75
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_Int_Tables_number      14
_atom_sites_solution_primary     dual
_audit_creation_date             2019-04-23
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 103.5030(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.47800(10)
_cell_length_b                   19.75960(10)
_cell_length_c                   21.5187(2)
_cell_measurement_reflns_used    34916
_cell_measurement_temperature    123.15
_cell_measurement_theta_max      74.0920
_cell_measurement_theta_min      4.3580
_cell_volume                     4332.10(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.43a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.43a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.43a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      123.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.9927
_diffrn_measured_fraction_theta_max 0.9927
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω    -47.00 -16.00   0.50    0.09    --  -42.80  87.00 -94.00   62
  2  ω    -29.00  76.00   0.50    0.09    --   42.80 -87.00 147.00  210
  3  ω     32.00  57.00   0.50    0.37    --   76.50 -87.00 147.00   50
  4  ω    -65.00 -39.00   0.50    0.37    -- -106.00  87.00 -94.00   52
  5  ω   -115.00 -79.00   0.50    0.37    -- -106.00  87.00 -94.00   72
  6  ω   -152.00-126.00   0.50    0.37    -- -106.00 -87.00 147.00   52
  7  ω     79.00 116.00   0.50    0.09    --   42.80 125.00 120.00   74
  8  ω     71.00  96.00   0.50    0.09    --   42.80 125.00 150.00   50
  9  ω     71.00 114.00   0.50    0.09    --   42.80 125.00-180.00   86
 10  ω     71.00 116.00   0.50    0.09    --   42.80 125.00 -60.00   90
 11  ω     73.00 117.00   0.50    0.09    --   42.80 125.00  30.00   88
 12  ω     72.00 117.00   0.50    0.09    --   42.80 125.00   0.00   90
 13  ω     89.00 114.00   0.50    0.37    --   76.50  87.00 -94.00   50
 14  ω   -135.00-109.00   0.50    0.37    -- -106.00 -99.00 -90.00   52
 15  ω   -177.00-140.00   0.50    0.37    -- -106.00 -99.00 -90.00   74
 16  ω   -120.00 -87.00   0.50    0.37    -- -106.00 -57.00-150.00   66
 17  ω   -150.00-124.00   0.50    0.37    -- -106.00  13.00  96.43   52
 18  ω   -118.00 -92.00   0.50    0.37    -- -106.00  63.00 -56.52   52
 19  ω   -127.00 -69.00   0.50    0.37    -- -106.00  57.00  60.00  116
 20  ω    -60.00 -33.00   0.50    0.37    -- -106.00  57.00  60.00   54
 21  ω    -65.00 -36.00   0.50    0.37    -- -106.00 125.00 120.00   58
 22  ω   -114.00 -73.00   0.50    0.37    -- -106.00 125.00 120.00   82
 23  ω   -177.00 -86.00   0.50    0.37    -- -106.00 -57.00-180.00  182
 24  ω    -97.00 -36.00   0.50    0.37    -- -106.00 125.00  30.00  122
 25  ω   -117.00 -91.00   0.50    0.37    -- -106.00  59.00-144.22   52
 26  ω    -87.00 -36.00   0.50    0.37    -- -106.00  57.00-150.00  102
 27  ω   -126.00 -96.00   0.50    0.37    -- -106.00  57.00 -30.00   60
 28  ω    -75.00 -33.00   0.50    0.37    -- -106.00  57.00 -30.00   84
 29  ω    -61.00 -35.00   0.50    0.37    -- -106.00  77.00-180.00   52
 30  ω   -111.00 -74.00   0.50    0.37    -- -106.00  13.00  96.43   74
 31  ω    -67.00 -29.00   0.50    0.37    -- -106.00  13.00  96.43   76
 32  ω   -123.00 -98.00   0.50    0.37    -- -106.00  57.00 150.00   50
 33  ω    -81.00 -33.00   0.50    0.37    -- -106.00  57.00 150.00   96
 34  ω   -106.00 -40.00   0.50    0.37    -- -106.00  92.00 -41.77  132
 35  ω   -125.00 -83.00   0.50    0.37    -- -106.00  57.00   0.00   84
 36  ω    -58.00 -33.00   0.50    0.37    -- -106.00  57.00   0.00   50
 37  ω   -164.00-139.00   0.50    0.37    -- -106.00 -77.00 -30.00   50
 38  ω    -66.00 -41.00   0.50    0.37    -- -106.00  54.00 119.61   50
 39  ω   -121.00 -87.00   0.50    0.37    -- -106.00  54.00 119.61   68
 40  ω   -171.00-146.00   0.50    0.37    -- -106.00 -99.00  90.00   50
 41  ω   -144.00-103.00   0.50    0.37    -- -106.00 -37.00-150.00   82
 42  ω   -134.00 -81.00   0.50    0.37    -- -106.00  19.00 -30.00  106
 43  ω   -111.00 -77.00   0.50    0.37    -- -106.00 -77.00 -30.00   68
 44  ω    -84.00 -58.00   0.50    0.37    -- -106.00 125.00  60.00   52
 45  ω   -141.00-113.00   0.50    0.37    -- -106.00 -57.00 -60.00   56
 46  ω   -145.00-119.00   0.50    0.37    -- -106.00 -99.00  60.00   52
 47  ω   -173.00-126.00   0.50    0.37    -- -106.00 -57.00 150.00   94
 48  ω    -67.00 -41.00   0.50    0.37    -- -106.00  57.00-120.00   52
 49  ω   -116.00 -90.00   0.50    0.37    -- -106.00  57.00 -60.00   52
 50  ω   -163.00-138.00   0.50    0.37    -- -106.00 -19.00  90.00   50
 51  ω   -175.00-150.00   0.50    0.37    -- -106.00 -19.00 150.00   50
 52  ω   -114.00 -89.00   0.50    0.37    -- -106.00 -19.00 150.00   50
 53  ω   -172.00 -80.00   0.50    0.37    -- -106.00 -77.00 120.00  184
 54  ω    -95.00 -69.00   0.50    0.37    -- -106.00  77.00-120.00   52
 55  ω   -173.00-145.00   0.50    0.37    -- -106.00 -57.00-150.00   56
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at offset/far, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0344322000
_diffrn_orient_matrix_UB_12      0.0623263000
_diffrn_orient_matrix_UB_13      -0.0437092000
_diffrn_orient_matrix_UB_21      -0.0732613000
_diffrn_orient_matrix_UB_22      0.0313336000
_diffrn_orient_matrix_UB_23      0.0472903000
_diffrn_orient_matrix_UB_31      0.1277455000
_diffrn_orient_matrix_UB_32      0.0347782000
_diffrn_orient_matrix_UB_33      0.0357075000
_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  0.0324
_diffrn_reflns_av_unetI/netI     0.0213
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            57416
_diffrn_reflns_theta_full        74.2693
_diffrn_reflns_theta_max         74.27
_diffrn_reflns_theta_min         4.23
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.680
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74166
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.43a (Rigaku Oxford Diffraction, 2019)
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    1.4653
_exptl_crystal_description       block
_exptl_crystal_F_000             1966.1892
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.3084
_refine_diff_density_min         -0.3614
_refine_diff_density_rms         0.0464
_refine_ls_d_res_high            0.8009
_refine_ls_d_res_low             10.4619
_refine_ls_goodness_of_fit_ref   1.0385
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    67
_refine_ls_number_parameters     615
_refine_ls_number_reflns         8754
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0385
_refine_ls_R_factor_all          0.0324
_refine_ls_R_factor_gt           0.0307
_refine_ls_shift/su_max          0.0001
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0350P)²+1.9609P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0775
_refine_ls_wR_factor_ref         0.0786
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              10
_reflns_limit_h_min              -13
_reflns_limit_k_max              24
_reflns_limit_k_min              0
_reflns_limit_l_max              26
_reflns_limit_l_min              -9
_reflns_number_gt                8250
_reflns_number_total             8754
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            ja0c03252_si_002.cif
_cod_data_source_block           5a
_cod_depositor_comments
'Adding full bibliography for 4134972--4134984.cif.'
_cod_original_sg_symbol_Hall     '-P 2ybc (x-z,y,z)'
_cod_database_code               4134979
_chemical_oxdiff_formula         'C41 H38 Al1 F15 N2 O1 P1'
_reflns_odcompleteness_completeness 98.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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. Restrained distances
3. Others
 Sof(C65a)=Sof(C66a)=Sof(C67a)=Sof(H65a)=Sof(H66a)=Sof(H67a)=1-FVAR(1)
 Sof(C65)=Sof(C66)=Sof(C67)=Sof(H65)=Sof(H66)=Sof(H67)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C25(H25), C22(H22)
4.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C5(H5), C3(H3), C4(H4), C65(H65), C66(H66), C67(H67),
 C65a(H65a), C66a(H66a), C67a(H67a)
4.c Idealised Me refined as rotating group:
 C14(H14a,H14b,H14c), C19(H19a,H19b,H19c), C15(H15a,H15b,H15c), C20(H20a,H20b,
 H20c), C27(H27a,H27b,H27c), C17(H17a,H17b,H17c), C18(H18a,H18b,H18c), C26(H26a,
 H26b,H26c), C24(H24a,H24b,H24c), C23(H23a,H23b,H23c)
;
_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 1.520
_oxdiff_exptl_absorpt_empirical_full_min 0.732
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x+1/2,y+1/2,-z+1/2
3 -x,-y,-z
4 x-1/2,-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_refinement_flags_posn
_atom_site_disorder_group
P12 P 0.43427(3) 0.322508(15) 0.726212(13) 0.01625(7) Uani 1.000000 . .
Al28 Al 0.42203(3) 0.244044(17) 0.600487(15) 0.01648(8) Uani 1.000000 . .
F39 F 0.61604(7) 0.35985(4) 0.57721(4) 0.02626(16) Uani 1.000000 . .
F36 F 0.18859(7) 0.28332(4) 0.47814(3) 0.02513(16) Uani 1.000000 . .
F50 F 0.27121(8) 0.13044(4) 0.66717(3) 0.02903(17) Uani 1.000000 . .
F61 F 0.65195(8) 0.24823(4) 0.50895(4) 0.02978(17) Uani 1.000000 . .
F48 F 0.36426(9) 0.17182(4) 0.46548(4) 0.03059(18) Uani 1.000000 . .
F47 F 0.16898(9) 0.00982(4) 0.62463(4) 0.03421(19) Uani 1.000000 . .
F59 F 0.56569(9) 0.13108(4) 0.68702(4) 0.03322(18) Uani 1.000000 . .
F35 F 0.17717(8) 0.37521(5) 0.38536(4) 0.0365(2) Uani 1.000000 . .
F58 F 0.87443(8) 0.17986(5) 0.52176(4) 0.0365(2) Uani 1.000000 . .
F37 F 0.60142(8) 0.45088(4) 0.48362(4) 0.03434(19) Uani 1.000000 . .
O21 O 0.49629(8) 0.28316(4) 0.67947(4) 0.01817(16) Uani 1.000000 . .
F38 F 0.38336(9) 0.45898(5) 0.38702(4) 0.0417(2) Uani 1.000000 . .
F49 F 0.25037(12) 0.05374(5) 0.42225(4) 0.0490(3) Uani 1.000000 . .
F60 F 0.78711(10) 0.06053(5) 0.69697(5) 0.0451(2) Uani 1.000000 . .
F57 F 0.94854(9) 0.08709(5) 0.61748(5) 0.0468(2) Uani 1.000000 . .
F46 F 0.15371(11) -0.02861(5) 0.50251(5) 0.0505(3) Uani 1.000000 . .
N10 N 0.24997(10) 0.27590(5) 0.63237(5) 0.01776(19) Uani 1.000000 . .
N7 N 0.13898(10) 0.31503(5) 0.70068(5) 0.0184(2) Uani 1.000000 . .
C11 C 0.26056(11) 0.30610(6) 0.68903(5) 0.0168(2) Uani 1.000000 . .
C54 C 0.59935(12) 0.19616(6) 0.59986(6) 0.0209(2) Uani 1.000000 . .
C32 C 0.50481(12) 0.36085(6) 0.52996(6) 0.0198(2) Uani 1.000000 . .
C8 C 0.04985(12) 0.28894(6) 0.64879(6) 0.0221(2) Uani 1.000000 . .
H8 H -0.04281(12) 0.28784(6) 0.64308(6) 0.0266(3) Uiso 1.000000 R .
C43 C 0.32063(12) 0.15760(6) 0.56806(6) 0.0197(2) Uani 1.000000 . .
C33 C 0.50046(13) 0.40854(6) 0.48267(6) 0.0240(3) Uani 1.000000 . .
C13 C 0.47325(12) 0.41295(6) 0.72156(6) 0.0202(2) Uani 1.000000 . .
C52 C 0.79785(13) 0.16836(7) 0.56315(7) 0.0267(3) Uani 1.000000 . .
C31 C 0.40405(12) 0.31596(6) 0.53189(5) 0.0180(2) Uani 1.000000 . .
C14 C 0.39342(12) 0.43917(6) 0.65692(6) 0.0224(2) Uani 1.000000 . .
H14a H 0.4099(8) 0.4104(3) 0.62253(7) 0.0336(4) Uiso 1.000000 GR .
H14b H 0.29971(14) 0.4381(5) 0.65650(19) 0.0336(4) Uiso 1.000000 GR .
H14c H 0.4197(7) 0.48576(19) 0.6505(2) 0.0336(4) Uiso 1.000000 GR .
C1 C 0.09849(12) 0.34420(6) 0.75529(6) 0.0210(2) Uani 1.000000 . .
C30 C 0.29560(12) 0.32357(6) 0.48153(6) 0.0200(2) Uani 1.000000 . .
C53 C 0.68183(12) 0.20396(6) 0.55850(6) 0.0225(2) Uani 1.000000 . .
C9 C 0.11900(12) 0.26504(6) 0.60724(6) 0.0211(2) Uani 1.000000 . .
H9 H 0.08237(12) 0.24419(6) 0.56727(6) 0.0253(3) Uiso 1.000000 R .
C42 C 0.26856(12) 0.11353(6) 0.60563(6) 0.0218(2) Uani 1.000000 . .
C19 C 0.44538(13) 0.20900(7) 0.79650(6) 0.0262(3) Uani 1.000000 . .
H19a H 0.3503(2) 0.20634(7) 0.7791(5) 0.0394(4) Uiso 1.000000 GR .
H19b H 0.4908(8) 0.18742(15) 0.7668(4) 0.0394(4) Uiso 1.000000 GR .
H19c H 0.4684(10) 0.18567(14) 0.83780(10) 0.0394(4) Uiso 1.000000 GR .
C44 C 0.31275(13) 0.13408(6) 0.50654(6) 0.0238(3) Uani 1.000000 . .
C29 C 0.28582(13) 0.37021(7) 0.43277(6) 0.0247(3) Uani 1.000000 . .
C55 C 0.64115(13) 0.14611(7) 0.64489(6) 0.0249(3) Uani 1.000000 . .
C2 C 0.08163(13) 0.30069(7) 0.80454(6) 0.0248(3) Uani 1.000000 . .
C25 C 0.05475(12) 0.45616(7) 0.69357(6) 0.0242(3) Uani 1.000000 . .
H25 H 0.10690(12) 0.43386(7) 0.66588(6) 0.0291(3) Uiso 1.000000 R .
C15 C 0.62063(12) 0.41999(7) 0.72328(6) 0.0259(3) Uani 1.000000 . .
H15a H 0.67252(12) 0.4059(5) 0.76529(19) 0.0388(4) Uiso 1.000000 GR .
H15b H 0.6425(3) 0.3913(4) 0.6901(4) 0.0388(4) Uiso 1.000000 GR .
H15c H 0.6405(2) 0.46728(12) 0.7155(5) 0.0388(4) Uiso 1.000000 GR .
C41 C 0.21441(13) 0.05133(7) 0.58532(6) 0.0257(3) Uani 1.000000 . .
C16 C 0.48710(12) 0.28363(7) 0.80559(6) 0.0227(2) Uani 1.000000 . .
C20 C 0.43864(14) 0.45404(7) 0.77567(6) 0.0267(3) Uani 1.000000 . .
H20a H 0.3501(4) 0.4420(4) 0.7796(4) 0.0401(4) Uiso 1.000000 GR .
H20b H 0.5019(7) 0.4440(4) 0.81592(11) 0.0401(4) Uiso 1.000000 GR .
H20c H 0.4418(11) 0.50243(7) 0.7662(3) 0.0401(4) Uiso 1.000000 GR .
C34 C 0.38989(14) 0.41298(7) 0.43343(6) 0.0267(3) Uani 1.000000 . .
C56 C 0.75419(14) 0.10837(7) 0.65140(7) 0.0308(3) Uani 1.000000 . .
C6 C 0.06694(12) 0.41342(7) 0.75342(6) 0.0238(3) Uani 1.000000 . .
C22 C 0.08935(14) 0.22397(7) 0.80001(6) 0.0277(3) Uani 1.000000 . .
H22 H 0.13913(14) 0.21269(7) 0.76698(6) 0.0333(3) Uiso 1.000000 R .
C45 C 0.25689(15) 0.07320(7) 0.48313(7) 0.0319(3) Uani 1.000000 . .
C51 C 0.83504(13) 0.12075(8) 0.61061(7) 0.0318(3) Uani 1.000000 . .
C40 C 0.20740(15) 0.03130(7) 0.52321(7) 0.0324(3) Uani 1.000000 . .
C5 C 0.03134(15) 0.44018(8) 0.80717(7) 0.0329(3) Uani 1.000000 . .
H5 H 0.01250(15) 0.48712(8) 0.80851(7) 0.0395(4) Uiso 1.000000 R .
C27 C 0.10512(15) 0.52853(7) 0.70680(8) 0.0334(3) Uani 1.000000 . .
H27a H 0.0487(7) 0.5530(2) 0.7296(5) 0.0501(5) Uiso 1.000000 GR .
H27b H 0.1952(5) 0.52757(7) 0.7330(5) 0.0501(5) Uiso 1.000000 GR .
H27c H 0.1038(11) 0.5514(2) 0.66625(8) 0.0501(5) Uiso 1.000000 GR .
C17 C 0.63818(13) 0.28748(8) 0.82511(7) 0.0326(3) Uani 1.000000 . .
H17a H 0.67458(14) 0.2713(6) 0.7898(2) 0.0489(5) Uiso 1.000000 GR .
H17b H 0.66532(14) 0.33447(13) 0.8351(6) 0.0489(5) Uiso 1.000000 GR .
H17c H 0.67067(15) 0.2591(5) 0.8629(4) 0.0489(5) Uiso 1.000000 GR .
C18 C 0.42907(15) 0.31617(8) 0.85780(6) 0.0305(3) Uani 1.000000 . .
H18a H 0.4684(9) 0.3609(3) 0.8685(4) 0.0457(4) Uiso 1.000000 GR .
H18b H 0.3339(2) 0.3209(5) 0.8422(2) 0.0457(4) Uiso 1.000000 GR .
H18c H 0.4480(10) 0.2874(3) 0.8960(2) 0.0457(4) Uiso 1.000000 GR .
C3 C 0.04511(15) 0.33049(8) 0.85655(7) 0.0335(3) Uani 1.000000 . .
H3 H 0.03515(15) 0.30299(8) 0.89132(7) 0.0402(4) Uiso 1.000000 R .
C26 C -0.08954(14) 0.45776(8) 0.65670(8) 0.0356(3) Uani 1.000000 . .
H26a H -0.1216(4) 0.41136(8) 0.6477(5) 0.0533(5) Uiso 1.000000 GR .
H26b H -0.1422(2) 0.4807(6) 0.6825(3) 0.0533(5) Uiso 1.000000 GR .
H26c H -0.0970(2) 0.4822(6) 0.6164(3) 0.0533(5) Uiso 1.000000 GR .
C24 C 0.15828(16) 0.18966(8) 0.86287(7) 0.0350(3) Uani 1.000000 . .
H24a H 0.2434(6) 0.2114(4) 0.8797(3) 0.0525(5) Uiso 1.000000 GR .
H24b H 0.1038(6) 0.1941(6) 0.8940(2) 0.0525(5) Uiso 1.000000 GR .
H24c H 0.1717(11) 0.14161(16) 0.85504(13) 0.0525(5) Uiso 1.000000 GR .
C4 C 0.02313(17) 0.39953(8) 0.85833(7) 0.0388(3) Uani 1.000000 . .
H4 H 0.00222(17) 0.41909(8) 0.89505(7) 0.0466(4) Uiso 1.000000 R .
C23 C -0.04993(17) 0.19525(9) 0.77776(9) 0.0434(4) Uani 1.000000 . .
H23a H -0.0999(5) 0.2050(6) 0.8100(3) 0.0652(6) Uiso 1.000000 GR .
H23b H -0.0936(5) 0.2163(5) 0.7371(4) 0.0652(6) Uiso 1.000000 GR .
H23c H -0.04526(17) 0.14618(14) 0.7720(7) 0.0652(6) Uiso 1.000000 GR .
C65 C 1.1289(5) 0.4801(5) 0.5216(3) 0.0361(14) Uani 0.65(2) . 1
C66 C 1.0306(9) 0.4330(3) 0.5025(5) 0.0433(19) Uani 0.65(2) . 1
C67 C 0.9004(7) 0.4517(4) 0.4817(4) 0.0431(16) Uani 0.65(2) . 1
C65a C 1.088(2) 0.4503(10) 0.5250(5) 0.048(4) Uani 0.35(2) . 2
C66a C 0.969(3) 0.4314(8) 0.4886(6) 0.063(5) Uani 0.35(2) . 2
C67a C 0.8828(9) 0.4834(12) 0.4638(4) 0.046(4) Uani 0.35(2) . 2
H65 H 1.2171(5) 0.4656(5) 0.5371(3) 0.0433(17) Uiso 0.65(2) R 1
H66 H 1.0528(9) 0.3863(3) 0.5038(5) 0.052(2) Uiso 0.65(2) R 1
H67 H 0.8333(7) 0.4187(4) 0.4699(4) 0.0518(19) Uiso 0.65(2) R 1
H65a H 1.151(2) 0.4167(10) 0.5425(5) 0.058(5) Uiso 0.35(2) R 2
H66a H 0.946(3) 0.3852(8) 0.4807(6) 0.075(6) Uiso 0.35(2) R 2
H67a H 0.7995(9) 0.4718(12) 0.4376(4) 0.055(5) Uiso 0.35(2) R 2
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
_atom_type_scat_dispersion_source
C 0.01920 0.00962 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870
51.65120 0.215599998832
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
F 0.07537 0.05506 3.53920 2.64120 1.51700 1.02430 10.28250 4.29440 0.26150
26.14760 0.277599990368
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236
57.79970 0.0030380000826
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
Al 0.21266 0.24195 6.42020 1.90020 1.59360 1.96460 3.03870 0.74260 31.54720
85.08860 1.11510002613
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
O 0.05239 0.03377 3.04850 2.28680 1.54630 0.86700 13.27710 5.70110 0.32390
32.90890 0.250800013542
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
N 0.03256 0.01839 12.21260 3.13220 2.01250 1.16630 0.00570 9.89330 28.99750
0.58260 -11.5290002823
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
P 0.30360 0.43703 6.43450 4.17910 1.78000 1.49080 1.90670 27.15700 0.52600
68.16450 1.11489999294
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
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
C11 P12 O21 98.83(5) . . ?
C13 P12 O21 108.89(5) . . ?
C13 P12 C11 110.94(5) . . ?
C16 P12 O21 108.46(5) . . ?
C16 P12 C11 112.57(5) . . ?
C16 P12 C13 115.73(6) . . ?
N10 Al28 O21 77.99(4) . . ?
C54 Al28 O21 90.64(4) . . ?
C54 Al28 N10 160.25(5) . . ?
C43 Al28 O21 136.89(5) . . ?
C43 Al28 N10 86.92(4) . . ?
C43 Al28 C54 90.66(5) . . ?
C31 Al28 O21 108.76(4) . . ?
C31 Al28 N10 94.84(4) . . ?
C31 Al28 C54 104.16(5) . . ?
C31 Al28 C43 112.62(5) . . ?
Al28 O21 P12 131.21(5) . . ?
C11 N10 Al28 121.31(8) . . ?
C9 N10 Al28 131.36(8) . . ?
C9 N10 C11 106.97(10) . . ?
C8 N7 C11 106.71(10) . . ?
C1 N7 C11 131.17(10) . . ?
C1 N7 C8 122.11(10) . . ?
N10 C11 P12 109.77(8) . . ?
N7 C11 P12 140.21(9) . . ?
N7 C11 N10 110.02(10) . . ?
C53 C54 Al28 130.01(9) . . ?
C55 C54 Al28 117.16(9) . . ?
C55 C54 C53 112.74(11) . . ?
C33 C32 F39 115.95(11) . . ?
C31 C32 F39 119.68(11) . . ?
C31 C32 C33 124.37(11) . . ?
H8 C8 N7 126.32(7) . . ?
C9 C8 N7 107.36(10) . . ?
C9 C8 H8 126.32(7) . . ?
C42 C43 Al28 124.76(9) . . ?
C44 C43 Al28 121.03(9) . . ?
C44 C43 C42 113.76(11) . . ?
C32 C33 F37 121.55(12) . . ?
C34 C33 F37 119.27(11) . . ?
C34 C33 C32 119.18(11) . . ?
C14 C13 P12 107.20(8) . . ?
C15 C13 P12 108.66(9) . . ?
C15 C13 C14 108.77(10) . . ?
C20 C13 P12 112.24(9) . . ?
C20 C13 C14 109.53(10) . . ?
C20 C13 C15 110.34(10) . . ?
C53 C52 F58 120.84(13) . . ?
C51 C52 F58 119.72(12) . . ?
C51 C52 C53 119.44(12) . . ?
C32 C31 Al28 121.90(9) . . ?
C30 C31 Al28 124.52(9) . . ?
C30 C31 C32 113.51(11) . . ?
H14a C14 C13 109.5 . . ?
H14b C14 C13 109.5 . . ?
H14b C14 H14a 109.5 . . ?
H14c C14 C13 109.5 . . ?
H14c C14 H14a 109.5 . . ?
H14c C14 H14b 109.5 . . ?
C2 C1 N7 118.46(11) . . ?
C6 C1 N7 118.19(11) . . ?
C6 C1 C2 123.09(11) . . ?
C31 C30 F36 119.58(10) . . ?
C29 C30 F36 115.74(11) . . ?
C29 C30 C31 124.68(11) . . ?
C54 C53 F61 120.78(11) . . ?
C52 C53 F61 114.87(11) . . ?
C52 C53 C54 124.35(12) . . ?
C8 C9 N10 108.94(10) . . ?
H9 C9 N10 125.53(6) . . ?
H9 C9 C8 125.53(7) . . ?
C43 C42 F50 119.54(11) . . ?
C41 C42 F50 116.13(11) . . ?
C41 C42 C43 124.32(11) . . ?
H19b C19 H19a 109.5 . . ?
H19c C19 H19a 109.5 . . ?
H19c C19 H19b 109.5 . . ?
C16 C19 H19a 109.5 . . ?
C16 C19 H19b 109.5 . . ?
C16 C19 H19c 109.5 . . ?
C43 C44 F48 119.47(11) . . ?
C45 C44 F48 116.06(11) . . ?
C45 C44 C43 124.47(12) . . ?
C30 C29 F35 121.68(11) . . ?
C34 C29 F35 119.43(11) . . ?
C34 C29 C30 118.89(12) . . ?
C54 C55 F59 118.85(11) . . ?
C56 C55 F59 115.54(12) . . ?
C56 C55 C54 125.61(13) . . ?
C22 C2 C1 122.83(11) . . ?
C3 C2 C1 116.91(12) . . ?
C3 C2 C22 120.02(12) . . ?
C6 C25 H25 108.08(7) . . ?
C27 C25 H25 108.08(7) . . ?
C27 C25 C6 113.89(11) . . ?
C26 C25 H25 108.08(8) . . ?
C26 C25 C6 109.10(11) . . ?
C26 C25 C27 109.43(12) . . ?
H15a C15 C13 109.5 . . ?
H15b C15 C13 109.5 . . ?
H15b C15 H15a 109.5 . . ?
H15c C15 C13 109.5 . . ?
H15c C15 H15a 109.5 . . ?
H15c C15 H15b 109.5 . . ?
C42 C41 F47 121.60(12) . . ?
C40 C41 F47 119.24(12) . . ?
C40 C41 C42 119.15(12) . . ?
C19 C16 P12 105.54(8) . . ?
C17 C16 P12 107.46(9) . . ?
C17 C16 C19 108.99(11) . . ?
C18 C16 P12 114.83(9) . . ?
C18 C16 C19 110.17(11) . . ?
C18 C16 C17 109.65(11) . . ?
H20a C20 C13 109.5 . . ?
H20b C20 C13 109.5 . . ?
H20b C20 H20a 109.5 . . ?
H20c C20 C13 109.5 . . ?
H20c C20 H20a 109.5 . . ?
H20c C20 H20b 109.5 . . ?
C33 C34 F38 120.23(12) . . ?
C29 C34 F38 120.40(12) . . ?
C29 C34 C33 119.37(12) . . ?
C55 C56 F60 121.41(13) . . ?
C51 C56 F60 119.83(13) . . ?
C51 C56 C55 118.76(13) . . ?
C25 C6 C1 122.52(11) . . ?
C5 C6 C1 116.77(12) . . ?
C5 C6 C25 120.29(12) . . ?
H22 C22 C2 108.17(7) . . ?
C24 C22 C2 113.86(12) . . ?
C24 C22 H22 108.17(8) . . ?
C23 C22 C2 109.10(12) . . ?
C23 C22 H22 108.17(9) . . ?
C23 C22 C24 109.22(12) . . ?
C44 C45 F49 121.52(12) . . ?
C40 C45 F49 119.55(12) . . ?
C40 C45 C44 118.92(12) . . ?
C52 C51 F57 120.74(14) . . ?
C56 C51 F57 120.26(14) . . ?
C56 C51 C52 119.00(12) . . ?
C41 C40 F46 119.90(13) . . ?
C45 C40 F46 120.75(13) . . ?
C45 C40 C41 119.35(12) . . ?
H5 C5 C6 119.43(8) . . ?
C4 C5 C6 121.14(13) . . ?
C4 C5 H5 119.43(8) . . ?
H27a C27 C25 109.5 . . ?
H27b C27 C25 109.5 . . ?
H27b C27 H27a 109.5 . . ?
H27c C27 C25 109.5 . . ?
H27c C27 H27a 109.5 . . ?
H27c C27 H27b 109.5 . . ?
H17a C17 C16 109.5 . . ?
H17b C17 C16 109.5 . . ?
H17b C17 H17a 109.5 . . ?
H17c C17 C16 109.5 . . ?
H17c C17 H17a 109.5 . . ?
H17c C17 H17b 109.5 . . ?
H18a C18 C16 109.5 . . ?
H18b C18 C16 109.5 . . ?
H18b C18 H18a 109.5 . . ?
H18c C18 C16 109.5 . . ?
H18c C18 H18a 109.5 . . ?
H18c C18 H18b 109.5 . . ?
H3 C3 C2 119.46(8) . . ?
C4 C3 C2 121.08(13) . . ?
C4 C3 H3 119.46(8) . . ?
H26a C26 C25 109.5 . . ?
H26b C26 C25 109.5 . . ?
H26b C26 H26a 109.5 . . ?
H26c C26 C25 109.5 . . ?
H26c C26 H26a 109.5 . . ?
H26c C26 H26b 109.5 . . ?
H24a C24 C22 109.5 . . ?
H24b C24 C22 109.5 . . ?
H24b C24 H24a 109.5 . . ?
H24c C24 C22 109.5 . . ?
H24c C24 H24a 109.5 . . ?
H24c C24 H24b 109.5 . . ?
C3 C4 C5 120.58(13) . . ?
H4 C4 C5 119.71(8) . . ?
H4 C4 C3 119.71(8) . . ?
H23a C23 C22 109.5 . . ?
H23b C23 C22 109.5 . . ?
H23b C23 H23a 109.5 . . ?
H23c C23 C22 109.5 . . ?
H23c C23 H23a 109.5 . . ?
H23c C23 H23b 109.5 . . ?
C67 C65 C66 120.1(4) 3_766 . ?
H65 C65 C66 119.9(5) . . ?
H65 C65 C67 119.9(5) . 3_766 ?
C67 C66 C65 121.8(5) . . ?
H66 C66 C65 119.1(5) . . ?
H66 C66 C67 119.1(5) . . ?
C66 C67 C65 118.0(4) . 3_766 ?
H67 C67 C65 121.0(5) . 3_766 ?
H67 C67 C66 121.0(5) . . ?
C67a C65a C66a 120.4(10) 3_766 . ?
H65a C65a C66a 119.8(13) . . ?
H65a C65a C67a 119.8(11) . 3_766 ?
C67a C66a C65a 116.4(11) . . ?
H66a C66a C65a 121.8(13) . . ?
H66a C66a C67a 121.8(11) . . ?
C66a C67a C65a 123.2(7) . 3_766 ?
H67a C67a C65a 118.4(11) . 3_766 ?
H67a C67a C66a 118.4(11) . . ?
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
P12 O21 1.5309(8) . ?
P12 C11 1.8380(12) . ?
P12 C13 1.8410(12) . ?
P12 C16 1.8365(12) . ?
Al28 O21 1.8639(9) . ?
Al28 N10 2.1667(10) . ?
Al28 C54 2.0878(12) . ?
Al28 C43 2.0463(13) . ?
Al28 C31 2.0258(12) . ?
F39 C32 1.3561(14) . ?
F36 C30 1.3627(14) . ?
F50 C42 1.3597(14) . ?
F61 C53 1.3581(15) . ?
F48 C44 1.3606(14) . ?
F47 C41 1.3428(15) . ?
F59 C55 1.3675(15) . ?
F35 C29 1.3432(15) . ?
F58 C52 1.3500(16) . ?
F37 C33 1.3452(15) . ?
F38 C34 1.3404(15) . ?
F49 C45 1.3518(16) . ?
F60 C56 1.3477(16) . ?
F57 C51 1.3403(16) . ?
F46 C40 1.3414(16) . ?
N10 C11 1.3386(15) . ?
N10 C9 1.3693(16) . ?
N7 C11 1.3661(15) . ?
N7 C8 1.3777(16) . ?
N7 C1 1.4580(15) . ?
C54 C53 1.3863(17) . ?
C54 C55 1.3823(18) . ?
C32 C33 1.3797(18) . ?
C32 C31 1.3870(17) . ?
C8 H8 0.9500 . ?
C8 C9 1.3600(17) . ?
C43 C42 1.3841(17) . ?
C43 C44 1.3872(17) . ?
C33 C34 1.3782(19) . ?
C13 C14 1.5362(17) . ?
C13 C15 1.5423(17) . ?
C13 C20 1.5309(16) . ?
C52 C53 1.3878(18) . ?
C52 C51 1.376(2) . ?
C31 C30 1.3832(17) . ?
C14 H14a 0.9800 . ?
C14 H14b 0.9800 . ?
C14 H14c 0.9800 . ?
C1 C2 1.4074(18) . ?
C1 C6 1.4055(18) . ?
C30 C29 1.3821(18) . ?
C9 H9 0.9500 . ?
C42 C41 1.3811(19) . ?
C19 H19a 0.9800 . ?
C19 H19b 0.9800 . ?
C19 H19c 0.9800 . ?
C19 C16 1.5376(18) . ?
C44 C45 1.3804(19) . ?
C29 C34 1.3770(19) . ?
C55 C56 1.3788(19) . ?
C2 C22 1.5226(19) . ?
C2 C3 1.3949(18) . ?
C25 H25 1.0000 . ?
C25 C6 1.5202(18) . ?
C25 C27 1.5279(19) . ?
C25 C26 1.5350(19) . ?
C15 H15a 0.9800 . ?
C15 H15b 0.9800 . ?
C15 H15c 0.9800 . ?
C41 C40 1.379(2) . ?
C16 C17 1.5420(18) . ?
C16 C18 1.5377(18) . ?
C20 H20a 0.9800 . ?
C20 H20b 0.9800 . ?
C20 H20c 0.9800 . ?
C56 C51 1.377(2) . ?
C6 C5 1.3993(18) . ?
C22 H22 1.0000 . ?
C22 C24 1.534(2) . ?
C22 C23 1.534(2) . ?
C45 C40 1.381(2) . ?
C5 H5 0.9500 . ?
C5 C4 1.382(2) . ?
C27 H27a 0.9800 . ?
C27 H27b 0.9800 . ?
C27 H27c 0.9800 . ?
C17 H17a 0.9800 . ?
C17 H17b 0.9800 . ?
C17 H17c 0.9800 . ?
C18 H18a 0.9800 . ?
C18 H18b 0.9800 . ?
C18 H18c 0.9800 . ?
C3 H3 0.9500 . ?
C3 C4 1.386(2) . ?
C26 H26a 0.9800 . ?
C26 H26b 0.9800 . ?
C26 H26c 0.9800 . ?
C24 H24a 0.9800 . ?
C24 H24b 0.9800 . ?
C24 H24c 0.9800 . ?
C4 H4 0.9500 . ?
C23 H23a 0.9800 . ?
C23 H23b 0.9800 . ?
C23 H23c 0.9800 . ?
C65 C66 1.378(6) . ?
C65 C67 1.379(6) 3_766 ?
C65 H65 0.9500 . ?
C66 C67 1.383(6) . ?
C66 H66 0.9500 . ?
C67 H67 0.9500 . ?
C65a C66a 1.362(12) . ?
C65a C67a 1.356(13) 3_766 ?
C65a H65a 0.9500 . ?
C66a C67a 1.388(16) . ?
C66a H66a 0.9500 . ?
C67a H67a 0.9500 . ?
