# Electronic Supplementary Material (ESI) for Organic Chemistry Frontiers.
# This journal is © the Partner Organisations 2021

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_202009166
_database_code_depnum_ccdc_archive 'CCDC 2051914'
loop_
_audit_author_name
_audit_author_address
'Rongqiang Tian'
;Zhengzhou University
China
;
_audit_update_record             
;
2020-12-22 deposited with the CCDC.	2021-05-07 downloaded from the CCDC.
;
_audit_creation_date             2020-12-22
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C36 H31 Mo N O4 P2'
_chemical_formula_sum            'C36 H31 Mo N O4 P2'
_chemical_formula_weight         699.50
_chemical_melting_point          ?
_chemical_oxdiff_formula         C14H15N2O1P1Mo1
_chemical_oxdiff_usercomment     r
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'
Mo Mo -0.0483 2.7339 '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'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   13.3804(4)
_cell_length_b                   15.4864(5)
_cell_length_c                   16.7675(6)
_cell_angle_alpha                105.320(3)
_cell_angle_beta                 91.827(3)
_cell_angle_gamma                92.381(3)
_cell_volume                     3344.8(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9982
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      70.9890
_cell_measurement_theta_min      4.1920
_shelx_estimated_absorpt_T_max   0.718
_shelx_estimated_absorpt_T_min   0.557
_exptl_absorpt_coefficient_mu    4.425
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67322
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            gray
_exptl_crystal_colour_primary    gray
_exptl_crystal_density_diffrn    1.389
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_av_unetI/netI     0.0481
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            25314
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.080
_diffrn_reflns_theta_max         67.080
_diffrn_reflns_theta_min         3.309
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2312
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -65.00 -32.00   1.00    2.25    --  -33.50 178.00  30.00   33
  2  ω    -86.00 -60.00   1.00    2.25    --  -33.50 -77.00-180.00   26
  3  ω   -107.00 -81.00   1.00    2.25    --  -33.50 178.00 150.00   26
  4  ω    -66.00 -22.00   1.00    2.25    --  -33.50 -57.00  60.00   44
  5  ω    -31.00  -6.00   1.00    2.25    --  -33.50 -77.00-180.00   25
  6  ω     14.00 106.00   1.00    2.25    --   36.47  77.00-180.00   92
  7  ω    -28.00   8.00   1.00    2.25    --   36.47 -57.00 -30.00   36
  8  ω     -1.00  77.00   1.00    2.25    --   36.47 -99.00  90.00   78
  9  ω     52.00 104.00   1.00    2.25    --   36.47  77.00-120.00   52
 10  ω      8.00  36.00   1.00    2.25    --   36.47  77.00-120.00   28
 11  ω     20.00 103.00   1.00    2.25    --   36.47  57.00 -60.00   83
 12  ω     32.00  77.00   1.00    2.25    --   36.47-131.00  10.00   45
 13  ω     74.00 100.00   1.00    2.25    --   36.47  37.00  60.00   26
 14  ω     21.00  49.00   1.00    2.25    --   36.47 -57.00 -30.00   28
 15  ω     43.00  77.00   1.00    2.25    --   36.47 -99.00-150.00   34
 16  ω      8.00  37.00   1.00    2.25    --   36.47 -99.00-150.00   29
 17  ω     33.00  70.00   1.00    2.25    --   36.47  57.00 150.00   37
 18  ω     30.00  64.00   1.00    2.25    --   36.47  57.00  30.00   34
 19  ω     75.00 105.00   1.00    2.25    --   36.47  57.00  30.00   30
 20  ω     69.00 101.00   1.00    2.25    --   36.47 178.00 150.00   32
 21  ω     88.00 123.00   1.00    6.50    --  108.00  61.00  90.00   35
 22  ω     42.00 118.00   1.00    6.50    --  108.00 -45.00 150.00   76
 23  ω     50.00 130.00   1.00    6.50    --  108.00 -30.00 -90.00   80
 24  ω     89.00 172.00   1.00    6.50    --  108.00  45.00 -30.00   83
 25  ω     89.00 127.00   1.00    6.50    --  108.00 -61.00-180.00   38
 26  ω     42.00 116.00   1.00    6.50    --  108.00 -77.00  60.00   74
 27  ω    129.00 167.00   1.00    6.50    --  108.00  61.00-150.00   38
 28  ω     39.00  65.00   1.00    6.50    --  108.00-111.00 150.00   26
 29  ω     90.00 150.00   1.00    6.50    --  108.00  77.00 -90.00   60
 30  ω     40.00 126.00   1.00    6.50    --  108.00 -61.00 -60.00   86
 31  ω    101.00 127.00   1.00    6.50    --  108.00-138.00-165.00   26
 32  ω     39.00  71.00   1.00    6.50    --  108.00-138.00-165.00   32
 33  ω     65.00  99.00   1.00    6.50    --  108.00 -94.00-150.00   34
 34  ω    130.00 173.00   1.00    6.50    --  108.00  61.00  90.00   43
 35  ω     73.00 108.00   1.00    6.50    --  108.00 -94.00   0.00   35
 36  ω    122.00 178.00   1.00    6.50    --  108.00 111.00 -60.00   56
 37  ω     90.00 116.00   1.00    6.50    --  108.00  77.00 150.00   26
 38  ω     71.00 105.00   1.00    6.50    --  108.00 -94.00 -90.00   34
 39  ω     37.00 132.00   1.00    6.50    --  108.00   0.00 -60.00   95
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0067811000
_diffrn_orient_matrix_UB_12      -0.0906647000
_diffrn_orient_matrix_UB_13      -0.0662861000
_diffrn_orient_matrix_UB_21      0.0033644000
_diffrn_orient_matrix_UB_22      0.0494480000
_diffrn_orient_matrix_UB_23      -0.0685105000
_diffrn_orient_matrix_UB_31      0.1151006000
_diffrn_orient_matrix_UB_32      -0.0014211000
_diffrn_orient_matrix_UB_33      0.0023482000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9873
_reflns_number_total             11932
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (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)'
_refine_diff_density_max         0.425
_refine_diff_density_min         -0.511
_refine_diff_density_rms         0.067
_refine_ls_extinction_coef       .
_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     797
_refine_ls_number_reflns         11932
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0371
_refine_ls_restrained_S_all      1.037
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0468P)²+0.1023P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0894
_refine_ls_wR_factor_ref         0.0977
_refine_special_details          ?
_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:
 C18(H18), C19(H19), C18'(H18'), C19'(H19')
2.b Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C23(H23A,H23B), C17'(H17C,H17D), C23'(H23C,H23D)
2.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C12(H12), C13(H13), C14(H14),
 C15(H15), C16(H16), C25(H25), C26(H26), C27(H27), C28(H28), C29(H29), C33(H33),
  C34(H34), C35(H35), C36(H36), C6'(H6'), C7'(H7'), C8'(H8'), C9'(H9'),
 C10'(H10'), C12'(H12'), C13'(H13'), C14'(H14'), C15'(H15'), C16'(H16'),
 C25'(H25'), C26'(H26'), C27'(H27'), C28'(H28'), C29'(H29'), C33'(H33'),
 C34'(H34'), C35'(H35'), C36'(H36')
2.d Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C30'(H30D,H30E,H30F), C31'(H31D,
 H31E,H31F)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.6426(3) 0.6134(3) 0.0695(2) 0.0498(8) Uani 1 1 d . . . . .
C2 C 0.6562(3) 0.7485(3) 0.2138(2) 0.0544(9) Uani 1 1 d . . . . .
C3 C 0.6287(3) 0.7980(3) 0.0651(3) 0.0743(13) Uani 1 1 d . . . . .
C4 C 0.4690(3) 0.6635(3) 0.0096(2) 0.0585(9) Uani 1 1 d . . . . .
C5 C 0.4667(2) 0.9478(2) 0.2230(2) 0.0471(8) Uani 1 1 d . . . . .
C6 C 0.5548(3) 0.9625(3) 0.2704(3) 0.0631(10) Uani 1 1 d . . . . .
H6 H 0.597904 0.916097 0.266231 0.076 Uiso 1 1 calc R . . . .
C7 C 0.5800(4) 1.0453(3) 0.3240(3) 0.0783(13) Uani 1 1 d . . . . .
H7 H 0.639511 1.053689 0.355869 0.094 Uiso 1 1 calc R . . . .
C8 C 0.5188(4) 1.1152(3) 0.3309(3) 0.0853(15) Uani 1 1 d . . . . .
H8 H 0.536542 1.171083 0.366608 0.102 Uiso 1 1 calc R . . . .
C9 C 0.4320(4) 1.1016(3) 0.2848(4) 0.0966(19) Uani 1 1 d . . . . .
H9 H 0.389680 1.148703 0.289514 0.116 Uiso 1 1 calc R . . . .
C10 C 0.4047(3) 1.0193(3) 0.2310(3) 0.0779(14) Uani 1 1 d . . . . .
H10 H 0.344639 1.011561 0.199828 0.094 Uiso 1 1 calc R . . . .
C11 C 0.3567(3) 0.8583(2) 0.0749(2) 0.0481(8) Uani 1 1 d . . . . .
C12 C 0.4056(4) 0.8927(4) 0.0179(3) 0.0836(15) Uani 1 1 d . . . . .
H12 H 0.475052 0.900946 0.022018 0.100 Uiso 1 1 calc R . . . .
C13 C 0.3519(5) 0.9155(4) -0.0460(3) 0.104(2) Uani 1 1 d . . . . .
H13 H 0.385840 0.938771 -0.083861 0.124 Uiso 1 1 calc R . . . .
C14 C 0.2502(5) 0.9037(4) -0.0533(3) 0.0962(19) Uani 1 1 d . . . . .
H14 H 0.214579 0.920286 -0.094946 0.115 Uiso 1 1 calc R . . . .
C15 C 0.2008(4) 0.8672(4) 0.0014(3) 0.0879(15) Uani 1 1 d . . . . .
H15 H 0.131582 0.857581 -0.004041 0.105 Uiso 1 1 calc R . . . .
C16 C 0.2533(3) 0.8448(3) 0.0646(3) 0.0663(11) Uani 1 1 d . . . . .
H16 H 0.218650 0.820034 0.101187 0.080 Uiso 1 1 calc R . . . .
C17 C 0.3358(2) 0.7990(2) 0.2244(2) 0.0383(6) Uani 1 1 d . . . . .
H17A H 0.360610 0.814393 0.281641 0.046 Uiso 1 1 calc R . . . .
H17B H 0.274334 0.829308 0.221528 0.046 Uiso 1 1 calc R . . . .
C18 C 0.3156(2) 0.6984(2) 0.19294(18) 0.0349(6) Uani 1 1 d . . . . .
H18 H 0.288444 0.685612 0.135825 0.042 Uiso 1 1 calc R . . . .
C19 C 0.2426(2) 0.6539(2) 0.24137(18) 0.0369(6) Uani 1 1 d . . . . .
H19 H 0.244061 0.692878 0.297967 0.044 Uiso 1 1 calc R . . . .
C20 C 0.2925(2) 0.5627(2) 0.2466(2) 0.0402(7) Uani 1 1 d . . . . .
C21 C 0.3679(2) 0.5986(2) 0.32005(19) 0.0376(6) Uani 1 1 d . . . . .
C22 C 0.4476(2) 0.6436(2) 0.30070(19) 0.0374(6) Uani 1 1 d . . . . .
C23 C 0.3595(2) 0.5349(2) 0.1718(2) 0.0438(7) Uani 1 1 d . . . . .
H23A H 0.321239 0.521125 0.119428 0.053 Uiso 1 1 calc R . . . .
H23B H 0.399557 0.484860 0.174309 0.053 Uiso 1 1 calc R . . . .
C24 C 0.1354(2) 0.6464(2) 0.2085(2) 0.0422(7) Uani 1 1 d . . . . .
C25 C 0.1064(3) 0.6069(3) 0.1262(2) 0.0604(10) Uani 1 1 d . . . . .
H25 H 0.153685 0.581382 0.088801 0.072 Uiso 1 1 calc R . . . .
C26 C 0.0063(3) 0.6055(4) 0.0996(3) 0.0752(13) Uani 1 1 d . . . . .
H26 H -0.012593 0.579143 0.044373 0.090 Uiso 1 1 calc R . . . .
C27 C -0.0643(3) 0.6425(4) 0.1538(3) 0.0796(15) Uani 1 1 d . . . . .
H27 H -0.130617 0.641896 0.135244 0.096 Uiso 1 1 calc R . . . .
C28 C -0.0374(3) 0.6804(3) 0.2352(3) 0.0741(13) Uani 1 1 d . . . . .
H28 H -0.085509 0.704581 0.272294 0.089 Uiso 1 1 calc R . . . .
C29 C 0.0626(3) 0.6827(3) 0.2625(2) 0.0546(9) Uani 1 1 d . . . . .
H29 H 0.080571 0.709151 0.317865 0.066 Uiso 1 1 calc R . . . .
C30 C 0.2180(3) 0.4896(2) 0.2555(2) 0.0525(8) Uani 1 1 d . . . . .
H30A H 0.253460 0.439687 0.263559 0.079 Uiso 1 1 calc GR . . . .
H30B H 0.175341 0.470317 0.206290 0.079 Uiso 1 1 calc GR . . . .
H30C H 0.178106 0.512448 0.302295 0.079 Uiso 1 1 calc GR . . . .
C31 C 0.3404(2) 0.5963(2) 0.4054(2) 0.0470(8) Uani 1 1 d . . . . .
H31A H 0.388226 0.632983 0.445242 0.071 Uiso 1 1 calc GR . . . .
H31B H 0.340317 0.535678 0.409710 0.071 Uiso 1 1 calc GR . . . .
H31C H 0.274888 0.618667 0.415921 0.071 Uiso 1 1 calc GR . . . .
C32 C 0.5205(2) 0.7009(2) 0.36203(19) 0.0396(7) Uani 1 1 d . . . . .
C33 C 0.5841(3) 0.6650(3) 0.4108(3) 0.0571(9) Uani 1 1 d . . . . .
H33 H 0.586213 0.603258 0.402138 0.069 Uiso 1 1 calc R . . . .
C34 C 0.6443(3) 0.7234(4) 0.4726(3) 0.0775(13) Uani 1 1 d . . . . .
H34 H 0.686532 0.701330 0.506924 0.093 Uiso 1 1 calc R . . . .
C35 C 0.6406(3) 0.8123(4) 0.4822(3) 0.0777(13) Uani 1 1 d . . . . .
H35 H 0.679598 0.852500 0.523623 0.093 Uiso 1 1 calc R . . . .
C36 C 0.5785(3) 0.8427(3) 0.4301(3) 0.0687(11) Uani 1 1 d . . . . .
H36 H 0.577972 0.904222 0.436507 0.082 Uiso 1 1 calc R . . . .
Mo1 Mo 0.55437(2) 0.71380(2) 0.11465(2) 0.03926(8) Uani 1 1 d . . . . .
N1 N 0.5184(2) 0.7888(2) 0.37033(19) 0.0518(7) Uani 1 1 d . . . . .
O1 O 0.6958(2) 0.5589(2) 0.04058(18) 0.0796(9) Uani 1 1 d . . . . .
O2 O 0.7189(2) 0.7638(3) 0.2628(2) 0.0873(10) Uani 1 1 d . . . . .
O3 O 0.6702(3) 0.8498(3) 0.0384(3) 0.138(2) Uani 1 1 d . . . . .
O4 O 0.4267(3) 0.6317(3) -0.0517(2) 0.1044(13) Uani 1 1 d . . . . .
P1 P 0.42965(6) 0.83508(5) 0.15988(5) 0.03774(17) Uani 1 1 d . . . . .
P2 P 0.43518(6) 0.64043(5) 0.19082(5) 0.03642(16) Uani 1 1 d . . . . .
C1' C 1.1426(2) 0.3937(2) 0.4496(2) 0.0444(7) Uani 1 1 d . . . . .
C2' C 1.1453(3) 0.2444(3) 0.3216(2) 0.0564(9) Uani 1 1 d . . . . .
C3' C 1.0918(3) 0.2257(3) 0.4866(2) 0.0529(9) Uani 1 1 d . . . . .
C4' C 0.9560(2) 0.3549(2) 0.5013(2) 0.0443(7) Uani 1 1 d . . . . .
C5' C 0.9485(2) 0.0560(2) 0.2892(2) 0.0430(7) Uani 1 1 d . . . . .
C6' C 1.0465(3) 0.0332(3) 0.2911(3) 0.0647(11) Uani 1 1 d . . . . .
H6' H 1.094264 0.072871 0.324620 0.078 Uiso 1 1 calc R . . . .
C7' C 1.0742(4) -0.0485(3) 0.2432(4) 0.0895(16) Uani 1 1 d . . . . .
H7' H 1.140747 -0.063236 0.244892 0.107 Uiso 1 1 calc R . . . .
C8' C 1.0057(4) -0.1081(3) 0.1936(3) 0.0814(14) Uani 1 1 d . . . . .
H8' H 1.025175 -0.163248 0.161967 0.098 Uiso 1 1 calc R . . . .
C9' C 0.9085(4) -0.0858(3) 0.1909(3) 0.0747(12) Uani 1 1 d . . . . .
H9' H 0.861346 -0.125678 0.156673 0.090 Uiso 1 1 calc R . . . .
C10' C 0.8794(3) -0.0044(3) 0.2387(2) 0.0598(10) Uani 1 1 d . . . . .
H10' H 0.812707 0.009805 0.236753 0.072 Uiso 1 1 calc R . . . .
C11' C 0.8428(2) 0.1302(2) 0.43389(19) 0.0392(7) Uani 1 1 d . . . . .
C12' C 0.8662(4) 0.0543(3) 0.4588(3) 0.0732(13) Uani 1 1 d . . . . .
H12' H 0.917342 0.019302 0.434017 0.088 Uiso 1 1 calc R . . . .
C13' C 0.8141(5) 0.0309(4) 0.5199(3) 0.099(2) Uani 1 1 d . . . . .
H13' H 0.830741 -0.019915 0.535990 0.119 Uiso 1 1 calc R . . . .
C14' C 0.7388(4) 0.0805(3) 0.5572(3) 0.0776(14) Uani 1 1 d . . . . .
H14' H 0.703285 0.062944 0.597571 0.093 Uiso 1 1 calc R . . . .
C15' C 0.7157(3) 0.1565(3) 0.5349(2) 0.0581(9) Uani 1 1 d . . . . .
H15' H 0.665199 0.191482 0.560892 0.070 Uiso 1 1 calc R . . . .
C16' C 0.7678(3) 0.1811(2) 0.4734(2) 0.0490(8) Uani 1 1 d . . . . .
H16' H 0.751845 0.232790 0.458608 0.059 Uiso 1 1 calc R . . . .
C17' C 0.8128(2) 0.19696(19) 0.28903(19) 0.0372(6) Uani 1 1 d . . . . .
H17C H 0.826884 0.175095 0.230958 0.045 Uiso 1 1 calc R . . . .
H17D H 0.748703 0.170114 0.297770 0.045 Uiso 1 1 calc R . . . .
C18' C 0.8082(2) 0.29827(19) 0.31193(17) 0.0340(6) Uani 1 1 d . . . . .
H18' H 0.784469 0.316718 0.368315 0.041 Uiso 1 1 calc R . . . .
C19' C 0.7392(2) 0.3389(2) 0.25714(18) 0.0357(6) Uani 1 1 d . . . . .
H19' H 0.733171 0.295902 0.202377 0.043 Uiso 1 1 calc R . . . .
C20' C 0.8007(2) 0.4264(2) 0.24648(19) 0.0389(7) Uani 1 1 d . . . . .
C21' C 0.8693(2) 0.3846(2) 0.17715(19) 0.0403(7) Uani 1 1 d . . . . .
C22' C 0.9434(2) 0.3411(2) 0.20276(18) 0.0392(7) Uani 1 1 d . . . . .
C23' C 0.8728(2) 0.4596(2) 0.32351(19) 0.0415(7) Uani 1 1 d . . . . .
H23C H 0.837484 0.477933 0.374388 0.050 Uiso 1 1 calc R . . . .
H23D H 0.919079 0.507781 0.318865 0.050 Uiso 1 1 calc R . . . .
C24' C 0.6340(2) 0.3516(2) 0.28790(19) 0.0374(6) Uani 1 1 d . . . . .
C25' C 0.6140(2) 0.3934(2) 0.3693(2) 0.0462(7) Uani 1 1 d . . . . .
H25' H 0.666599 0.417336 0.407371 0.055 Uiso 1 1 calc R . . . .
C26' C 0.5163(3) 0.3997(3) 0.3943(3) 0.0585(9) Uani 1 1 d . . . . .
H26' H 0.503897 0.427825 0.449046 0.070 Uiso 1 1 calc R . . . .
C27' C 0.4373(3) 0.3647(3) 0.3386(3) 0.0615(10) Uani 1 1 d . . . . .
H27' H 0.371803 0.368504 0.355781 0.074 Uiso 1 1 calc R . . . .
C28' C 0.4562(3) 0.3246(3) 0.2582(3) 0.0638(10) Uani 1 1 d . . . . .
H28' H 0.403076 0.302465 0.220158 0.077 Uiso 1 1 calc R . . . .
C29' C 0.5537(3) 0.3164(3) 0.2327(2) 0.0523(8) Uani 1 1 d . . . . .
H29' H 0.565401 0.287143 0.178078 0.063 Uiso 1 1 calc R . . . .
C30' C 0.7341(3) 0.4985(2) 0.2313(2) 0.0497(8) Uani 1 1 d . . . . .
H30D H 0.775071 0.546930 0.221975 0.075 Uiso 1 1 calc GR . . . .
H30E H 0.694915 0.520448 0.278695 0.075 Uiso 1 1 calc GR . . . .
H30F H 0.690320 0.473363 0.183514 0.075 Uiso 1 1 calc GR . . . .
C31' C 0.8403(3) 0.3821(3) 0.0892(2) 0.0523(8) Uani 1 1 d . . . . .
H31D H 0.886164 0.347029 0.052697 0.079 Uiso 1 1 calc GR . . . .
H31E H 0.842633 0.442040 0.083035 0.079 Uiso 1 1 calc GR . . . .
H31F H 0.773702 0.355686 0.075702 0.079 Uiso 1 1 calc GR . . . .
C32' C 1.0084(2) 0.2773(2) 0.1501(2) 0.0437(7) Uani 1 1 d . . . . .
C33' C 1.0686(3) 0.3016(3) 0.0932(2) 0.0595(10) Uani 1 1 d . . . . .
H33' H 1.071343 0.360071 0.088207 0.071 Uiso 1 1 calc R . . . .
C34' C 1.1250(4) 0.2368(4) 0.0437(3) 0.0786(14) Uani 1 1 d . . . . .
H34' H 1.165372 0.250914 0.004344 0.094 Uiso 1 1 calc R . . . .
C35' C 1.1203(4) 0.1518(3) 0.0535(3) 0.0816(14) Uani 1 1 d . . . . .
H35' H 1.157171 0.107104 0.021044 0.098 Uiso 1 1 calc R . . . .
C36' C 1.0593(3) 0.1340(3) 0.1127(3) 0.0648(10) Uani 1 1 d . . . . .
H36' H 1.057166 0.076393 0.119755 0.078 Uiso 1 1 calc R . . . .
Mo1' Mo 1.04193(2) 0.29253(2) 0.40788(2) 0.03563(7) Uani 1 1 d . . . . .
N1' N 1.0035(2) 0.1944(2) 0.16032(18) 0.0526(7) Uani 1 1 d . . . . .
O1' O 1.2045(2) 0.44824(19) 0.47412(17) 0.0667(7) Uani 1 1 d . . . . .
O2' O 1.2095(2) 0.2248(3) 0.2793(2) 0.0957(12) Uani 1 1 d . . . . .
O3' O 1.1137(3) 0.1886(3) 0.5344(2) 0.0920(11) Uani 1 1 d . . . . .
O4' O 0.9150(2) 0.3915(2) 0.55691(18) 0.0751(8) Uani 1 1 d . . . . .
P1' P 0.91209(5) 0.16439(5) 0.35336(5) 0.03526(16) Uani 1 1 d . . . . .
P2' P 0.93478(6) 0.35375(5) 0.31402(5) 0.03510(16) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 Mo1 1.993(3) . ?
C1 O1 1.144(4) . ?
C2 Mo1 2.057(4) . ?
C2 O2 1.128(5) . ?
C3 Mo1 1.975(4) . ?
C3 O3 1.148(5) . ?
C4 Mo1 2.022(4) . ?
C4 O4 1.136(5) . ?
C5 C6 1.377(5) . ?
C5 C10 1.392(5) . ?
C5 P1 1.825(3) . ?
C6 H6 0.9300 . ?
C6 C7 1.377(6) . ?
C7 H7 0.9300 . ?
C7 C8 1.368(7) . ?
C8 H8 0.9300 . ?
C8 C9 1.351(7) . ?
C9 H9 0.9300 . ?
C9 C10 1.381(6) . ?
C10 H10 0.9300 . ?
C11 C12 1.382(6) . ?
C11 C16 1.388(5) . ?
C11 P1 1.823(3) . ?
C12 H12 0.9300 . ?
C12 C13 1.401(7) . ?
C13 H13 0.9300 . ?
C13 C14 1.362(8) . ?
C14 H14 0.9300 . ?
C14 C15 1.370(8) . ?
C15 H15 0.9300 . ?
C15 C16 1.380(6) . ?
C16 H16 0.9300 . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C17 C18 1.517(4) . ?
C17 P1 1.846(3) . ?
C18 H18 0.9800 . ?
C18 C19 1.542(4) . ?
C18 P2 1.863(3) . ?
C19 H19 0.9800 . ?
C19 C20 1.609(4) . ?
C19 C24 1.509(4) . ?
C20 C21 1.535(4) . ?
C20 C23 1.544(4) . ?
C20 C30 1.517(4) . ?
C21 C22 1.345(4) . ?
C21 C31 1.498(4) . ?
C22 C32 1.476(4) . ?
C22 P2 1.832(3) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C23 P2 1.834(3) . ?
C24 C25 1.389(5) . ?
C24 C29 1.386(5) . ?
C25 H25 0.9300 . ?
C25 C26 1.395(5) . ?
C26 H26 0.9300 . ?
C26 C27 1.368(7) . ?
C27 H27 0.9300 . ?
C27 C28 1.365(7) . ?
C28 H28 0.9300 . ?
C28 C29 1.396(5) . ?
C29 H29 0.9300 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 C33 1.391(5) . ?
C32 N1 1.333(4) . ?
C33 H33 0.9300 . ?
C33 C34 1.391(6) . ?
C34 H34 0.9300 . ?
C34 C35 1.347(7) . ?
C35 H35 0.9300 . ?
C35 C36 1.372(6) . ?
C36 H36 0.9300 . ?
C36 N1 1.340(5) . ?
Mo1 P1 2.5448(8) . ?
Mo1 P2 2.4923(8) . ?
C1' Mo1' 1.986(3) . ?
C1' O1' 1.142(4) . ?
C2' Mo1' 2.051(4) . ?
C2' O2' 1.131(4) . ?
C3' Mo1' 1.995(4) . ?
C3' O3' 1.141(5) . ?
C4' Mo1' 2.029(3) . ?
C4' O4' 1.127(4) . ?
C5' C6' 1.373(5) . ?
C5' C10' 1.382(5) . ?
C5' P1' 1.833(3) . ?
C6' H6' 0.9300 . ?
C6' C7' 1.380(6) . ?
C7' H7' 0.9300 . ?
C7' C8' 1.363(7) . ?
C8' H8' 0.9300 . ?
C8' C9' 1.363(6) . ?
C9' H9' 0.9300 . ?
C9' C10' 1.382(5) . ?
C10' H10' 0.9300 . ?
C11' C12' 1.391(5) . ?
C11' C16' 1.378(4) . ?
C11' P1' 1.838(3) . ?
C12' H12' 0.9300 . ?
C12' C13' 1.373(6) . ?
C13' H13' 0.9300 . ?
C13' C14' 1.359(7) . ?
C14' H14' 0.9300 . ?
C14' C15' 1.370(6) . ?
C15' H15' 0.9300 . ?
C15' C16' 1.388(5) . ?
C16' H16' 0.9300 . ?
C17' H17C 0.9700 . ?
C17' H17D 0.9700 . ?
C17' C18' 1.518(4) . ?
C17' P1' 1.853(3) . ?
C18' H18' 0.9800 . ?
C18' C19' 1.546(4) . ?
C18' P2' 1.862(3) . ?
C19' H19' 0.9800 . ?
C19' C20' 1.610(4) . ?
C19' C24' 1.518(4) . ?
C20' C21' 1.528(4) . ?
C20' C23' 1.547(4) . ?
C20' C30' 1.524(4) . ?
C21' C22' 1.342(5) . ?
C21' C31' 1.503(4) . ?
C22' C32' 1.473(4) . ?
C22' P2' 1.831(3) . ?
C23' H23C 0.9700 . ?
C23' H23D 0.9700 . ?
C23' P2' 1.840(3) . ?
C24' C25' 1.387(5) . ?
C24' C29' 1.389(5) . ?
C25' H25' 0.9300 . ?
C25' C26' 1.384(5) . ?
C26' H26' 0.9300 . ?
C26' C27' 1.381(6) . ?
C27' H27' 0.9300 . ?
C27' C28' 1.363(6) . ?
C28' H28' 0.9300 . ?
C28' C29' 1.386(5) . ?
C29' H29' 0.9300 . ?
C30' H30D 0.9600 . ?
C30' H30E 0.9600 . ?
C30' H30F 0.9600 . ?
C31' H31D 0.9600 . ?
C31' H31E 0.9600 . ?
C31' H31F 0.9600 . ?
C32' C33' 1.385(5) . ?
C32' N1' 1.339(5) . ?
C33' H33' 0.9300 . ?
C33' C34' 1.389(6) . ?
C34' H34' 0.9300 . ?
C34' C35' 1.368(7) . ?
C35' H35' 0.9300 . ?
C35' C36' 1.379(6) . ?
C36' H36' 0.9300 . ?
C36' N1' 1.332(5) . ?
Mo1' P1' 2.5387(8) . ?
Mo1' P2' 2.4877(8) . ?

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
O1 C1 Mo1 175.7(4) . . ?
O2 C2 Mo1 173.2(3) . . ?
O3 C3 Mo1 177.2(5) . . ?
O4 C4 Mo1 175.0(4) . . ?
C6 C5 C10 117.7(4) . . ?
C6 C5 P1 119.9(3) . . ?
C10 C5 P1 122.2(3) . . ?
C5 C6 H6 119.6 . . ?
C5 C6 C7 120.8(4) . . ?
C7 C6 H6 119.6 . . ?
C6 C7 H7 119.5 . . ?
C8 C7 C6 121.0(4) . . ?
C8 C7 H7 119.5 . . ?
C7 C8 H8 120.6 . . ?
C9 C8 C7 118.8(4) . . ?
C9 C8 H8 120.6 . . ?
C8 C9 H9 119.3 . . ?
C8 C9 C10 121.4(4) . . ?
C10 C9 H9 119.3 . . ?
C5 C10 H10 119.8 . . ?
C9 C10 C5 120.3(4) . . ?
C9 C10 H10 119.8 . . ?
C12 C11 C16 117.4(4) . . ?
C12 C11 P1 118.9(3) . . ?
C16 C11 P1 123.7(3) . . ?
C11 C12 H12 119.7 . . ?
C11 C12 C13 120.7(5) . . ?
C13 C12 H12 119.7 . . ?
C12 C13 H13 119.7 . . ?
C14 C13 C12 120.5(5) . . ?
C14 C13 H13 119.7 . . ?
C13 C14 H14 120.3 . . ?
C13 C14 C15 119.4(5) . . ?
C15 C14 H14 120.3 . . ?
C14 C15 H15 119.8 . . ?
C14 C15 C16 120.4(5) . . ?
C16 C15 H15 119.8 . . ?
C11 C16 H16 119.2 . . ?
C15 C16 C11 121.5(5) . . ?
C15 C16 H16 119.2 . . ?
H17A C17 H17B 108.3 . . ?
C18 C17 H17A 109.9 . . ?
C18 C17 H17B 109.9 . . ?
C18 C17 P1 108.9(2) . . ?
P1 C17 H17A 109.9 . . ?
P1 C17 H17B 109.9 . . ?
C17 C18 H18 107.6 . . ?
C17 C18 C19 117.1(2) . . ?
C17 C18 P2 110.0(2) . . ?
C19 C18 H18 107.6 . . ?
C19 C18 P2 106.6(2) . . ?
P2 C18 H18 107.6 . . ?
C18 C19 H19 106.7 . . ?
C18 C19 C20 105.4(2) . . ?
C20 C19 H19 106.7 . . ?
C24 C19 C18 113.6(2) . . ?
C24 C19 H19 106.7 . . ?
C24 C19 C20 117.2(3) . . ?
C21 C20 C19 100.7(2) . . ?
C21 C20 C23 103.5(3) . . ?
C23 C20 C19 107.0(2) . . ?
C30 C20 C19 114.3(3) . . ?
C30 C20 C21 115.4(3) . . ?
C30 C20 C23 114.5(3) . . ?
C22 C21 C20 112.8(3) . . ?
C22 C21 C31 126.2(3) . . ?
C31 C21 C20 120.0(3) . . ?
C21 C22 C32 124.3(3) . . ?
C21 C22 P2 108.7(2) . . ?
C32 C22 P2 125.9(2) . . ?
C20 C23 H23A 112.3 . . ?
C20 C23 H23B 112.3 . . ?
C20 C23 P2 97.5(2) . . ?
H23A C23 H23B 109.9 . . ?
P2 C23 H23A 112.3 . . ?
P2 C23 H23B 112.3 . . ?
C25 C24 C19 123.3(3) . . ?
C29 C24 C19 118.5(3) . . ?
C29 C24 C25 118.2(3) . . ?
C24 C25 H25 120.0 . . ?
C24 C25 C26 120.1(4) . . ?
C26 C25 H25 120.0 . . ?
C25 C26 H26 119.6 . . ?
C27 C26 C25 120.8(4) . . ?
C27 C26 H26 119.6 . . ?
C26 C27 H27 120.0 . . ?
C28 C27 C26 120.0(4) . . ?
C28 C27 H27 120.0 . . ?
C27 C28 H28 120.1 . . ?
C27 C28 C29 119.8(4) . . ?
C29 C28 H28 120.1 . . ?
C24 C29 C28 121.1(4) . . ?
C24 C29 H29 119.4 . . ?
C28 C29 H29 119.4 . . ?
C20 C30 H30A 109.5 . . ?
C20 C30 H30B 109.5 . . ?
C20 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C21 C31 H31A 109.5 . . ?
C21 C31 H31B 109.5 . . ?
C21 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C33 C32 C22 121.5(3) . . ?
N1 C32 C22 116.1(3) . . ?
N1 C32 C33 122.3(3) . . ?
C32 C33 H33 120.7 . . ?
C34 C33 C32 118.6(4) . . ?
C34 C33 H33 120.7 . . ?
C33 C34 H34 120.5 . . ?
C35 C34 C33 119.0(4) . . ?
C35 C34 H34 120.5 . . ?
C34 C35 H35 120.4 . . ?
C34 C35 C36 119.2(4) . . ?
C36 C35 H35 120.4 . . ?
C35 C36 H36 118.2 . . ?
N1 C36 C35 123.7(4) . . ?
N1 C36 H36 118.2 . . ?
C1 Mo1 C2 85.28(14) . . ?
C1 Mo1 C4 85.44(15) . . ?
C1 Mo1 P1 174.22(11) . . ?
C1 Mo1 P2 100.65(11) . . ?
C2 Mo1 P1 100.47(10) . . ?
C2 Mo1 P2 92.40(11) . . ?
C3 Mo1 C1 93.63(16) . . ?
C3 Mo1 C2 88.49(19) . . ?
C3 Mo1 C4 91.9(2) . . ?
C3 Mo1 P1 87.10(12) . . ?
C3 Mo1 P2 165.71(12) . . ?
C4 Mo1 C2 170.72(15) . . ?
C4 Mo1 P1 88.80(12) . . ?
C4 Mo1 P2 89.51(11) . . ?
P2 Mo1 P1 78.71(2) . . ?
C32 N1 C36 117.2(3) . . ?
C5 P1 C17 101.41(15) . . ?
C5 P1 Mo1 122.64(11) . . ?
C11 P1 C5 101.99(16) . . ?
C11 P1 C17 104.73(16) . . ?
C11 P1 Mo1 114.28(12) . . ?
C17 P1 Mo1 109.76(10) . . ?
C18 P2 Mo1 106.71(9) . . ?
C22 P2 C18 98.46(13) . . ?
C22 P2 C23 89.39(14) . . ?
C22 P2 Mo1 125.73(10) . . ?
C23 P2 C18 87.53(14) . . ?
C23 P2 Mo1 137.84(11) . . ?
O1' C1' Mo1' 175.9(3) . . ?
O2' C2' Mo1' 172.4(3) . . ?
O3' C3' Mo1' 174.9(4) . . ?
O4' C4' Mo1' 174.6(3) . . ?
C6' C5' C10' 118.5(3) . . ?
C6' C5' P1' 119.9(3) . . ?
C10' C5' P1' 121.6(3) . . ?
C5' C6' H6' 119.9 . . ?
C5' C6' C7' 120.1(4) . . ?
C7' C6' H6' 119.9 . . ?
C6' C7' H7' 119.4 . . ?
C8' C7' C6' 121.2(4) . . ?
C8' C7' H7' 119.4 . . ?
C7' C8' H8' 120.5 . . ?
C9' C8' C7' 119.1(4) . . ?
C9' C8' H8' 120.5 . . ?
C8' C9' H9' 119.8 . . ?
C8' C9' C10' 120.4(4) . . ?
C10' C9' H9' 119.8 . . ?
C5' C10' H10' 119.7 . . ?
C9' C10' C5' 120.6(4) . . ?
C9' C10' H10' 119.7 . . ?
C12' C11' P1' 121.5(3) . . ?
C16' C11' C12' 117.9(3) . . ?
C16' C11' P1' 120.6(3) . . ?
C11' C12' H12' 119.8 . . ?
C13' C12' C11' 120.3(4) . . ?
C13' C12' H12' 119.8 . . ?
C12' C13' H13' 119.3 . . ?
C14' C13' C12' 121.3(4) . . ?
C14' C13' H13' 119.3 . . ?
C13' C14' H14' 120.3 . . ?
C13' C14' C15' 119.5(4) . . ?
C15' C14' H14' 120.3 . . ?
C14' C15' H15' 120.1 . . ?
C14' C15' C16' 119.8(4) . . ?
C16' C15' H15' 120.1 . . ?
C11' C16' C15' 121.2(3) . . ?
C11' C16' H16' 119.4 . . ?
C15' C16' H16' 119.4 . . ?
H17C C17' H17D 108.2 . . ?
C18' C17' H17C 109.7 . . ?
C18' C17' H17D 109.7 . . ?
C18' C17' P1' 109.9(2) . . ?
P1' C17' H17C 109.7 . . ?
P1' C17' H17D 109.7 . . ?
C17' C18' H18' 107.1 . . ?
C17' C18' C19' 117.4(2) . . ?
C17' C18' P2' 111.3(2) . . ?
C19' C18' H18' 107.1 . . ?
C19' C18' P2' 106.41(19) . . ?
P2' C18' H18' 107.1 . . ?
C18' C19' H19' 106.8 . . ?
C18' C19' C20' 105.5(2) . . ?
C20' C19' H19' 106.8 . . ?
C24' C19' C18' 113.4(2) . . ?
C24' C19' H19' 106.8 . . ?
C24' C19' C20' 116.9(2) . . ?
C21' C20' C19' 101.2(2) . . ?
C21' C20' C23' 103.8(2) . . ?
C23' C20' C19' 106.8(2) . . ?
C30' C20' C19' 113.7(3) . . ?
C30' C20' C21' 116.5(3) . . ?
C30' C20' C23' 113.6(3) . . ?
C22' C21' C20' 112.7(3) . . ?
C22' C21' C31' 126.8(3) . . ?
C31' C21' C20' 119.7(3) . . ?
C21' C22' C32' 126.8(3) . . ?
C21' C22' P2' 108.9(2) . . ?
C32' C22' P2' 123.1(2) . . ?
C20' C23' H23C 112.3 . . ?
C20' C23' H23D 112.3 . . ?
C20' C23' P2' 97.1(2) . . ?
H23C C23' H23D 109.9 . . ?
P2' C23' H23C 112.3 . . ?
P2' C23' H23D 112.3 . . ?
C25' C24' C19' 123.2(3) . . ?
C25' C24' C29' 118.3(3) . . ?
C29' C24' C19' 118.4(3) . . ?
C24' C25' H25' 119.8 . . ?
C26' C25' C24' 120.5(3) . . ?
C26' C25' H25' 119.8 . . ?
C25' C26' H26' 119.7 . . ?
C27' C26' C25' 120.6(4) . . ?
C27' C26' H26' 119.7 . . ?
C26' C27' H27' 120.3 . . ?
C28' C27' C26' 119.3(3) . . ?
C28' C27' H27' 120.3 . . ?
C27' C28' H28' 119.7 . . ?
C27' C28' C29' 120.7(4) . . ?
C29' C28' H28' 119.7 . . ?
C24' C29' H29' 119.7 . . ?
C28' C29' C24' 120.6(4) . . ?
C28' C29' H29' 119.7 . . ?
C20' C30' H30D 109.5 . . ?
C20' C30' H30E 109.5 . . ?
C20' C30' H30F 109.5 . . ?
H30D C30' H30E 109.5 . . ?
H30D C30' H30F 109.5 . . ?
H30E C30' H30F 109.5 . . ?
C21' C31' H31D 109.5 . . ?
C21' C31' H31E 109.5 . . ?
C21' C31' H31F 109.5 . . ?
H31D C31' H31E 109.5 . . ?
H31D C31' H31F 109.5 . . ?
H31E C31' H31F 109.5 . . ?
C33' C32' C22' 122.0(3) . . ?
N1' C32' C22' 115.3(3) . . ?
N1' C32' C33' 122.7(3) . . ?
C32' C33' H33' 120.7 . . ?
C32' C33' C34' 118.5(4) . . ?
C34' C33' H33' 120.7 . . ?
C33' C34' H34' 120.4 . . ?
C35' C34' C33' 119.2(4) . . ?
C35' C34' H34' 120.4 . . ?
C34' C35' H35' 120.9 . . ?
C34' C35' C36' 118.3(4) . . ?
C36' C35' H35' 120.9 . . ?
C35' C36' H36' 118.0 . . ?
N1' C36' C35' 123.9(4) . . ?
N1' C36' H36' 118.0 . . ?
C1' Mo1' C2' 84.31(14) . . ?
C1' Mo1' C3' 93.07(14) . . ?
C1' Mo1' C4' 86.98(14) . . ?
C1' Mo1' P1' 179.23(10) . . ?
C1' Mo1' P2' 100.86(10) . . ?
C2' Mo1' P1' 95.73(10) . . ?
C2' Mo1' P2' 95.11(12) . . ?
C3' Mo1' C2' 94.19(16) . . ?
C3' Mo1' C4' 85.30(15) . . ?
C3' Mo1' P1' 87.70(11) . . ?
C3' Mo1' P2' 163.94(11) . . ?
C4' Mo1' C2' 171.24(14) . . ?
C4' Mo1' P1' 92.99(10) . . ?
C4' Mo1' P2' 87.46(9) . . ?
P2' Mo1' P1' 78.37(2) . . ?
C36' N1' C32' 117.3(3) . . ?
C5' P1' C11' 101.53(14) . . ?
C5' P1' C17' 103.64(15) . . ?
C5' P1' Mo1' 120.63(11) . . ?
C11' P1' C17' 103.73(14) . . ?
C11' P1' Mo1' 114.56(10) . . ?
C17' P1' Mo1' 110.89(9) . . ?
C18' P2' Mo1' 105.64(9) . . ?
C22' P2' C18' 98.36(13) . . ?
C22' P2' C23' 89.36(14) . . ?
C22' P2' Mo1' 129.12(11) . . ?
C23' P2' C18' 87.75(14) . . ?
C23' P2' Mo1' 134.90(11) . . ?

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
C5 C6 C7 C8 -0.7(8) . . . . ?
C6 C5 C10 C9 0.0(7) . . . . ?
C6 C5 P1 C11 -150.9(3) . . . . ?
C6 C5 P1 C17 101.1(3) . . . . ?
C6 C5 P1 Mo1 -21.5(4) . . . . ?
C6 C7 C8 C9 0.8(9) . . . . ?
C7 C8 C9 C10 -0.5(10) . . . . ?
C8 C9 C10 C5 0.1(9) . . . . ?
C10 C5 C6 C7 0.3(7) . . . . ?
C10 C5 P1 C11 34.7(4) . . . . ?
C10 C5 P1 C17 -73.3(4) . . . . ?
C10 C5 P1 Mo1 164.1(3) . . . . ?
C11 C12 C13 C14 -0.2(9) . . . . ?
C12 C11 C16 C15 -1.8(7) . . . . ?
C12 C11 P1 C5 70.4(4) . . . . ?
C12 C11 P1 C17 175.8(4) . . . . ?
C12 C11 P1 Mo1 -64.1(4) . . . . ?
C12 C13 C14 C15 -1.6(9) . . . . ?
C13 C14 C15 C16 1.7(9) . . . . ?
C14 C15 C16 C11 0.1(8) . . . . ?
C16 C11 C12 C13 1.9(7) . . . . ?
C16 C11 P1 C5 -108.3(3) . . . . ?
C16 C11 P1 C17 -3.0(4) . . . . ?
C16 C11 P1 Mo1 117.2(3) . . . . ?
C17 C18 C19 C20 -138.1(3) . . . . ?
C17 C18 C19 C24 92.3(3) . . . . ?
C17 C18 P2 C22 80.2(2) . . . . ?
C17 C18 P2 C23 169.2(2) . . . . ?
C17 C18 P2 Mo1 -51.1(2) . . . . ?
C18 C17 P1 C5 -165.5(2) . . . . ?
C18 C17 P1 C11 88.7(2) . . . . ?
C18 C17 P1 Mo1 -34.4(2) . . . . ?
C18 C19 C20 C21 81.9(3) . . . . ?
C18 C19 C20 C23 -25.9(3) . . . . ?
C18 C19 C20 C30 -153.8(3) . . . . ?
C18 C19 C24 C25 53.3(4) . . . . ?
C18 C19 C24 C29 -124.9(3) . . . . ?
C19 C18 P2 C22 -47.7(2) . . . . ?
C19 C18 P2 C23 41.3(2) . . . . ?
C19 C18 P2 Mo1 -179.07(17) . . . . ?
C19 C20 C21 C22 -73.8(3) . . . . ?
C19 C20 C21 C31 95.4(3) . . . . ?
C19 C20 C23 P2 54.3(3) . . . . ?
C19 C24 C25 C26 -177.5(4) . . . . ?
C19 C24 C29 C28 178.0(4) . . . . ?
C20 C19 C24 C25 -70.1(4) . . . . ?
C20 C19 C24 C29 111.7(3) . . . . ?
C20 C21 C22 C32 166.7(3) . . . . ?
C20 C21 C22 P2 -1.9(3) . . . . ?
C20 C23 P2 C18 -54.0(2) . . . . ?
C20 C23 P2 C22 44.5(2) . . . . ?
C20 C23 P2 Mo1 -166.41(14) . . . . ?
C21 C20 C23 P2 -51.5(2) . . . . ?
C21 C22 C32 C33 67.0(4) . . . . ?
C21 C22 C32 N1 -110.1(4) . . . . ?
C21 C22 P2 C18 60.7(2) . . . . ?
C21 C22 P2 C23 -26.7(2) . . . . ?
C21 C22 P2 Mo1 178.38(17) . . . . ?
C22 C32 C33 C34 -174.1(3) . . . . ?
C22 C32 N1 C36 175.0(3) . . . . ?
C23 C20 C21 C22 36.8(3) . . . . ?
C23 C20 C21 C31 -154.1(3) . . . . ?
C24 C19 C20 C21 -150.6(3) . . . . ?
C24 C19 C20 C23 101.6(3) . . . . ?
C24 C19 C20 C30 -26.3(4) . . . . ?
C24 C25 C26 C27 -0.2(7) . . . . ?
C25 C24 C29 C28 -0.3(6) . . . . ?
C25 C26 C27 C28 -0.8(7) . . . . ?
C26 C27 C28 C29 1.2(7) . . . . ?
C27 C28 C29 C24 -0.6(7) . . . . ?
C29 C24 C25 C26 0.7(6) . . . . ?
C30 C20 C21 C22 162.7(3) . . . . ?
C30 C20 C21 C31 -28.2(4) . . . . ?
C30 C20 C23 P2 -178.0(2) . . . . ?
C31 C21 C22 C32 -1.7(5) . . . . ?
C31 C21 C22 P2 -170.2(3) . . . . ?
C32 C22 P2 C18 -107.7(3) . . . . ?
C32 C22 P2 C23 164.9(3) . . . . ?
C32 C22 P2 Mo1 10.1(3) . . . . ?
C32 C33 C34 C35 -1.3(7) . . . . ?
C33 C32 N1 C36 -2.1(5) . . . . ?
C33 C34 C35 C36 -0.8(8) . . . . ?
C34 C35 C36 N1 1.6(8) . . . . ?
C35 C36 N1 C32 -0.2(6) . . . . ?
N1 C32 C33 C34 2.9(6) . . . . ?
P1 C5 C6 C7 -174.3(4) . . . . ?
P1 C5 C10 C9 174.5(4) . . . . ?
P1 C11 C12 C13 -177.0(4) . . . . ?
P1 C11 C16 C15 176.9(4) . . . . ?
P1 C17 C18 C19 177.1(2) . . . . ?
P1 C17 C18 P2 55.3(2) . . . . ?
P2 C18 C19 C20 -14.5(3) . . . . ?
P2 C18 C19 C24 -144.1(2) . . . . ?
P2 C22 C32 C33 -126.4(3) . . . . ?
P2 C22 C32 N1 56.5(4) . . . . ?
C5' C6' C7' C8' -0.1(8) . . . . ?
C6' C5' C10' C9' -0.2(6) . . . . ?
C6' C5' P1' C11' -107.5(3) . . . . ?
C6' C5' P1' C17' 145.1(3) . . . . ?
C6' C5' P1' Mo1' 20.4(4) . . . . ?
C6' C7' C8' C9' 0.6(9) . . . . ?
C7' C8' C9' C10' -0.8(8) . . . . ?
C8' C9' C10' C5' 0.7(7) . . . . ?
C10' C5' C6' C7' -0.1(7) . . . . ?
C10' C5' P1' C11' 72.2(3) . . . . ?
C10' C5' P1' C17' -35.2(3) . . . . ?
C10' C5' P1' Mo1' -159.9(3) . . . . ?
C11' C12' C13' C14' 0.2(9) . . . . ?
C12' C11' C16' C15' -1.4(6) . . . . ?
C12' C11' P1' C5' 30.1(4) . . . . ?
C12' C11' P1' C17' 137.4(3) . . . . ?
C12' C11' P1' Mo1' -101.5(3) . . . . ?
C12' C13' C14' C15' -1.5(9) . . . . ?
C13' C14' C15' C16' 1.3(7) . . . . ?
C14' C15' C16' C11' 0.1(6) . . . . ?
C16' C11' C12' C13' 1.2(7) . . . . ?
C16' C11' P1' C5' -152.0(3) . . . . ?
C16' C11' P1' C17' -44.7(3) . . . . ?
C16' C11' P1' Mo1' 76.3(3) . . . . ?
C17' C18' C19' C20' -139.2(3) . . . . ?
C17' C18' C19' C24' 91.6(3) . . . . ?
C17' C18' P2' C22' 81.1(2) . . . . ?
C17' C18' P2' C23' 170.1(2) . . . . ?
C17' C18' P2' Mo1' -53.7(2) . . . . ?
C18' C17' P1' C5' -153.8(2) . . . . ?
C18' C17' P1' C11' 100.5(2) . . . . ?
C18' C17' P1' Mo1' -23.0(2) . . . . ?
C18' C19' C20' C21' 81.5(3) . . . . ?
C18' C19' C20' C23' -26.8(3) . . . . ?
C18' C19' C20' C30' -152.9(3) . . . . ?
C18' C19' C24' C25' 49.4(4) . . . . ?
C18' C19' C24' C29' -127.9(3) . . . . ?
C19' C18' P2' C22' -47.9(2) . . . . ?
C19' C18' P2' C23' 41.1(2) . . . . ?
C19' C18' P2' Mo1' 177.36(16) . . . . ?
C19' C20' C21' C22' -73.3(3) . . . . ?
C19' C20' C21' C31' 96.9(3) . . . . ?
C19' C20' C23' P2' 54.8(2) . . . . ?
C19' C24' C25' C26' -177.4(3) . . . . ?
C19' C24' C29' C28' 178.6(3) . . . . ?
C20' C19' C24' C25' -73.8(4) . . . . ?
C20' C19' C24' C29' 109.0(3) . . . . ?
C20' C21' C22' C32' 165.5(3) . . . . ?
C20' C21' C22' P2' -2.3(3) . . . . ?
C20' C23' P2' C18' -54.24(19) . . . . ?
C20' C23' P2' C22' 44.1(2) . . . . ?
C20' C23' P2' Mo1' -164.24(13) . . . . ?
C21' C20' C23' P2' -51.6(2) . . . . ?
C21' C22' C32' C33' 59.5(5) . . . . ?
C21' C22' C32' N1' -119.3(4) . . . . ?
C21' C22' P2' C18' 61.2(2) . . . . ?
C21' C22' P2' C23' -26.5(2) . . . . ?
C21' C22' P2' Mo1' 179.27(17) . . . . ?
C22' C32' C33' C34' -177.6(4) . . . . ?
C22' C32' N1' C36' 178.5(3) . . . . ?
C23' C20' C21' C22' 37.3(3) . . . . ?
C23' C20' C21' C31' -152.5(3) . . . . ?
C24' C19' C20' C21' -151.4(3) . . . . ?
C24' C19' C20' C23' 100.3(3) . . . . ?
C24' C19' C20' C30' -25.8(4) . . . . ?
C24' C25' C26' C27' -0.1(6) . . . . ?
C25' C24' C29' C28' 1.2(5) . . . . ?
C25' C26' C27' C28' -0.8(6) . . . . ?
C26' C27' C28' C29' 1.9(6) . . . . ?
C27' C28' C29' C24' -2.1(6) . . . . ?
C29' C24' C25' C26' -0.1(5) . . . . ?
C30' C20' C21' C22' 163.0(3) . . . . ?
C30' C20' C21' C31' -26.8(4) . . . . ?
C30' C20' C23' P2' -179.1(2) . . . . ?
C31' C21' C22' C32' -3.9(6) . . . . ?
C31' C21' C22' P2' -171.7(3) . . . . ?
C32' C22' P2' C18' -107.2(3) . . . . ?
C32' C22' P2' C23' 165.2(3) . . . . ?
C32' C22' P2' Mo1' 10.9(3) . . . . ?
C32' C33' C34' C35' -0.9(7) . . . . ?
C33' C32' N1' C36' -0.3(6) . . . . ?
C33' C34' C35' C36' -0.1(8) . . . . ?
C34' C35' C36' N1' 1.0(8) . . . . ?
C35' C36' N1' C32' -0.8(7) . . . . ?
N1' C32' C33' C34' 1.1(6) . . . . ?
P1' C5' C6' C7' 179.6(4) . . . . ?
P1' C5' C10' C9' -179.9(3) . . . . ?
P1' C11' C12' C13' 179.2(4) . . . . ?
P1' C11' C16' C15' -179.3(3) . . . . ?
P1' C17' C18' C19' 172.3(2) . . . . ?
P1' C17' C18' P2' 49.4(2) . . . . ?
P2' C18' C19' C20' -13.9(3) . . . . ?
P2' C18' C19' C24' -143.1(2) . . . . ?
P2' C22' C32' C33' -134.3(3) . . . . ?
P2' C22' C32' N1' 46.9(4) . . . . ?

_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 1.703
_oxdiff_exptl_absorpt_empirical_full_min 0.744
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_20200790
_database_code_depnum_ccdc_archive 'CCDC 2048634'
loop_
_audit_author_name
_audit_author_address
'Zhang keke'
;Zhengzhou University
China
;
_audit_update_record             
;
2020-12-07 deposited with the CCDC.	2021-05-07 downloaded from the CCDC.
;
_audit_creation_date             2020-07-15
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C21 H21 P S'
_chemical_formula_sum            'C21 H21 P S'
_chemical_formula_weight         336.41
_chemical_absolute_configuration ad
_chemical_melting_point          ?
_chemical_oxdiff_formula         C14H15N2O4
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'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'

_cell_length_a                   8.5974(3)
_cell_length_b                   10.8728(5)
_cell_length_c                   19.5450(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1827.02(13)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2726
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      70.2760
_cell_measurement_theta_min      4.1080
_shelx_estimated_absorpt_T_max   0.816
_shelx_estimated_absorpt_T_min   0.719
_exptl_absorpt_coefficient_mu    2.354
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83511
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.223
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0323
_diffrn_reflns_av_unetI/netI     0.0405
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7505
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.847
_diffrn_reflns_theta_min         4.525
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2312
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -97.00 -70.00   1.00    1.50    --  -33.50 178.00   0.00   27
  2  ω   -102.00 -37.00   1.00    1.50    --  -33.50 -57.00-120.00   65
  3  ω     68.00 104.00   1.00    1.50    --   36.47 178.00  30.00   36
  4  ω     48.00  74.00   1.00    1.50    --   36.47 -99.00 -30.00   26
  5  ω    -18.00  50.00   1.00    1.50    --   36.47 -77.00 150.00   68
  6  ω     43.00 101.00   1.00    7.50    --  108.00 -94.00   0.00   58
  7  ω     58.00 128.00   1.00    7.50    --  108.00 -45.00 120.00   70
  8  ω    133.00 159.00   1.00    7.50    --  108.00  61.00 -90.00   26
  9  ω    100.00 178.00   1.00    7.50    --  108.00 111.00-150.00   78
 10  ω     92.00 121.00   1.00    7.50    --  108.00  61.00 -90.00   29
 11  ω     91.00 163.00   1.00    7.50    --  108.00  61.00 150.00   72
 12  ω    135.00 161.00   1.00    7.50    --  108.00 111.00  90.00   26
 13  ω     39.00  65.00   1.00    2.50    --   36.47-151.00-121.00   26
 14  ω     60.00 108.00   1.00    2.50    --   36.47 178.00 -30.00   48
 15  ω     51.00  96.00   1.00    2.50    --   36.47  19.00 -90.00   45
 16  ω     78.00 104.00   1.00    2.50    --   36.47-151.00-121.00   26
 17  ω    124.00 177.00   1.00    7.50    --  108.00  45.00  90.00   53
 18  ω     72.00 100.00   1.00    7.50    --  108.00 -94.00-180.00   28
 19  ω     38.00  73.00   1.00    7.50    --  108.00 -94.00 150.00   35
 20  ω     39.00  70.00   1.00    7.50    --  108.00 -45.00   0.00   31
 21  ω     65.00 103.00   1.00    7.50    --  108.00 -94.00  30.00   38
 22  ω      2.00  28.00   1.00    2.50    --  -33.50  77.00  90.00   26
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1697694000
_diffrn_orient_matrix_UB_12      -0.0230753000
_diffrn_orient_matrix_UB_13      0.0217059000
_diffrn_orient_matrix_UB_21      0.0333918000
_diffrn_orient_matrix_UB_22      -0.1389764000
_diffrn_orient_matrix_UB_23      0.0048100000
_diffrn_orient_matrix_UB_31      0.0465075000
_diffrn_orient_matrix_UB_32      0.0154222000
_diffrn_orient_matrix_UB_33      0.0756148000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_reflns_Friedel_coverage         0.716
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.964
_reflns_number_gt                3087
_reflns_number_total             3456
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (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)'
_refine_diff_density_max         0.288
_refine_diff_density_min         -0.249
_refine_diff_density_rms         0.042
_refine_ls_abs_structure_details 
;
 Flack x determined using 1171 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.018(15)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     210
_refine_ls_number_reflns         3456
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0500
_refine_ls_R_factor_gt           0.0434
_refine_ls_restrained_S_all      1.024
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0651P)²+0.1551P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1104
_refine_ls_wR_factor_ref         0.1165
_refine_special_details          ?
_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:
 C2(H2)
2.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B)
2.c Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C11(H11), C12(H12), C13(H13), C17(H17), C18(H18), C19(H19),
 C20(H20), C21(H21)
2.d X=CH2 refined with riding coordinates:
 C7(H7A,H7B)
2.e Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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
S1 S 0.84428(13) 0.83915(10) 0.79086(6) 0.0622(3) Uani 1 1 d . . . . .
P1 P 0.64685(11) 0.77341(8) 0.75997(4) 0.0429(2) Uani 1 1 d . . . . .
C1 C 0.6421(5) 0.6459(3) 0.69906(17) 0.0463(7) Uani 1 1 d . . . . .
C2 C 0.4754(4) 0.6385(3) 0.67238(17) 0.0457(8) Uani 1 1 d . . . . .
H2 H 0.4309 0.5612 0.6891 0.055 Uiso 1 1 calc R . . . .
C3 C 0.3842(4) 0.7478(3) 0.70909(17) 0.0450(8) Uani 1 1 d . . . . .
C4 C 0.3694(4) 0.7073(3) 0.78439(18) 0.0459(8) Uani 1 1 d . . . . .
C5 C 0.5010(4) 0.7180(3) 0.82025(17) 0.0436(7) Uani 1 1 d . . . . .
C6 C 0.5001(4) 0.8563(3) 0.71159(19) 0.0472(8) Uani 1 1 d . . . . .
H6A H 0.4594 0.9269 0.7361 0.057 Uiso 1 1 calc R . . . .
H6B H 0.5362 0.8808 0.6666 0.057 Uiso 1 1 calc R . . . .
C7 C 0.7602(6) 0.5779(5) 0.6830(3) 0.0762(14) Uani 1 1 d . . . . .
H7A H 0.7488 0.5149 0.6512 0.091 Uiso 1 1 calc R . . . .
H7B H 0.8565 0.5922 0.7032 0.091 Uiso 1 1 calc R . . . .
C8 C 0.4636(5) 0.6370(4) 0.59477(18) 0.0483(8) Uani 1 1 d . . . . .
C9 C 0.5373(6) 0.7228(5) 0.5536(2) 0.0685(12) Uani 1 1 d . . . . .
H9 H 0.6010 0.7821 0.5734 0.082 Uiso 1 1 calc R . . . .
C10 C 0.5175(7) 0.7216(5) 0.4834(2) 0.0763(14) Uani 1 1 d . . . . .
H10 H 0.5638 0.7825 0.4569 0.092 Uiso 1 1 calc R . . . .
C11 C 0.4320(6) 0.6333(6) 0.4525(2) 0.0756(14) Uani 1 1 d . . . . .
H11 H 0.4210 0.6321 0.4052 0.091 Uiso 1 1 calc R . . . .
C12 C 0.3619(8) 0.5459(6) 0.4921(2) 0.0872(17) Uani 1 1 d . . . . .
H12 H 0.3036 0.4842 0.4715 0.105 Uiso 1 1 calc R . . . .
C13 C 0.3768(6) 0.5482(4) 0.5630(2) 0.0657(12) Uani 1 1 d . . . . .
H13 H 0.3270 0.4886 0.5891 0.079 Uiso 1 1 calc R . . . .
C14 C 0.2313(5) 0.7801(4) 0.6751(2) 0.0577(9) Uani 1 1 d . . . . .
H14A H 0.1685 0.7074 0.6711 0.087 Uiso 1 1 calc GR . . . .
H14B H 0.2509 0.8132 0.6304 0.087 Uiso 1 1 calc GR . . . .
H14C H 0.1774 0.8401 0.7023 0.087 Uiso 1 1 calc GR . . . .
C15 C 0.2229(5) 0.6477(5) 0.8091(2) 0.0588(10) Uani 1 1 d . . . . .
H15A H 0.1407 0.7074 0.8102 0.088 Uiso 1 1 calc GR . . . .
H15B H 0.2391 0.6154 0.8543 0.088 Uiso 1 1 calc GR . . . .
H15C H 0.1949 0.5820 0.7787 0.088 Uiso 1 1 calc GR . . . .
C16 C 0.5303(5) 0.6800(3) 0.89126(18) 0.0461(8) Uani 1 1 d . . . . .
C17 C 0.4381(5) 0.7271(5) 0.9435(2) 0.0598(10) Uani 1 1 d . . . . .
H17 H 0.3627 0.7856 0.9333 0.072 Uiso 1 1 calc R . . . .
C18 C 0.4571(7) 0.6878(5) 1.0105(2) 0.0738(14) Uani 1 1 d . . . . .
H18 H 0.3958 0.7215 1.0450 0.089 Uiso 1 1 calc R . . . .
C19 C 0.5646(7) 0.6004(5) 1.0262(2) 0.0746(14) Uani 1 1 d . . . . .
H19 H 0.5741 0.5721 1.0709 0.090 Uiso 1 1 calc R . . . .
C20 C 0.6593(7) 0.5542(4) 0.9756(2) 0.0716(13) Uani 1 1 d . . . . .
H20 H 0.7342 0.4955 0.9862 0.086 Uiso 1 1 calc R . . . .
C21 C 0.6431(6) 0.5951(4) 0.9083(2) 0.0572(9) Uani 1 1 d . . . . .
H21 H 0.7091 0.5649 0.8745 0.069 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
S1 P1 1.9381(14) . ?
P1 C1 1.828(3) . ?
P1 C5 1.823(4) . ?
P1 C6 1.816(4) . ?
C1 C2 1.527(5) . ?
C1 C7 1.295(6) . ?
C2 H2 0.9800 . ?
C2 C3 1.594(5) . ?
C2 C8 1.520(5) . ?
C3 C4 1.541(5) . ?
C3 C6 1.545(5) . ?
C3 C14 1.514(5) . ?
C4 C5 1.336(5) . ?
C4 C15 1.497(6) . ?
C5 C16 1.470(5) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 H7A 0.9300 . ?
C7 H7B 0.9300 . ?
C8 C9 1.386(6) . ?
C8 C13 1.370(6) . ?
C9 H9 0.9300 . ?
C9 C10 1.383(6) . ?
C10 H10 0.9300 . ?
C10 C11 1.351(8) . ?
C11 H11 0.9300 . ?
C11 C12 1.366(8) . ?
C12 H12 0.9300 . ?
C12 C13 1.391(6) . ?
C13 H13 0.9300 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 C17 1.389(6) . ?
C16 C21 1.380(6) . ?
C17 H17 0.9300 . ?
C17 C18 1.388(6) . ?
C18 H18 0.9300 . ?
C18 C19 1.361(7) . ?
C19 H19 0.9300 . ?
C19 C20 1.376(8) . ?
C20 H20 0.9300 . ?
C20 C21 1.395(6) . ?
C21 H21 0.9300 . ?

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
C1 P1 S1 120.15(14) . . ?
C5 P1 S1 121.53(13) . . ?
C5 P1 C1 98.89(17) . . ?
C6 P1 S1 125.97(14) . . ?
C6 P1 C1 91.25(17) . . ?
C6 P1 C5 91.31(18) . . ?
C2 C1 P1 106.4(2) . . ?
C7 C1 P1 125.0(4) . . ?
C7 C1 C2 128.6(4) . . ?
C1 C2 H2 107.3 . . ?
C1 C2 C3 105.6(3) . . ?
C3 C2 H2 107.3 . . ?
C8 C2 C1 113.8(3) . . ?
C8 C2 H2 107.3 . . ?
C8 C2 C3 115.1(3) . . ?
C4 C3 C2 104.9(3) . . ?
C4 C3 C6 104.0(3) . . ?
C6 C3 C2 105.4(3) . . ?
C14 C3 C2 113.7(3) . . ?
C14 C3 C4 114.4(3) . . ?
C14 C3 C6 113.4(3) . . ?
C5 C4 C3 114.0(3) . . ?
C5 C4 C15 125.5(3) . . ?
C15 C4 C3 120.1(3) . . ?
C4 C5 P1 105.8(3) . . ?
C4 C5 C16 128.1(3) . . ?
C16 C5 P1 125.8(3) . . ?
P1 C6 H6A 112.8 . . ?
P1 C6 H6B 112.8 . . ?
C3 C6 P1 94.9(2) . . ?
C3 C6 H6A 112.8 . . ?
C3 C6 H6B 112.8 . . ?
H6A C6 H6B 110.2 . . ?
C1 C7 H7A 120.0 . . ?
C1 C7 H7B 120.0 . . ?
H7A C7 H7B 120.0 . . ?
C9 C8 C2 122.8(4) . . ?
C13 C8 C2 119.8(4) . . ?
C13 C8 C9 117.4(4) . . ?
C8 C9 H9 119.6 . . ?
C10 C9 C8 120.9(5) . . ?
C10 C9 H9 119.6 . . ?
C9 C10 H10 119.4 . . ?
C11 C10 C9 121.2(5) . . ?
C11 C10 H10 119.4 . . ?
C10 C11 H11 120.6 . . ?
C10 C11 C12 118.7(4) . . ?
C12 C11 H11 120.6 . . ?
C11 C12 H12 119.6 . . ?
C11 C12 C13 120.8(5) . . ?
C13 C12 H12 119.6 . . ?
C8 C13 C12 120.9(5) . . ?
C8 C13 H13 119.5 . . ?
C12 C13 H13 119.5 . . ?
C3 C14 H14A 109.5 . . ?
C3 C14 H14B 109.5 . . ?
C3 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C4 C15 H15A 109.5 . . ?
C4 C15 H15B 109.5 . . ?
C4 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C17 C16 C5 119.5(3) . . ?
C21 C16 C5 122.4(3) . . ?
C21 C16 C17 118.1(4) . . ?
C16 C17 H17 119.6 . . ?
C18 C17 C16 120.9(4) . . ?
C18 C17 H17 119.6 . . ?
C17 C18 H18 119.7 . . ?
C19 C18 C17 120.5(5) . . ?
C19 C18 H18 119.7 . . ?
C18 C19 H19 120.2 . . ?
C18 C19 C20 119.6(4) . . ?
C20 C19 H19 120.2 . . ?
C19 C20 H20 119.9 . . ?
C19 C20 C21 120.2(5) . . ?
C21 C20 H20 119.9 . . ?
C16 C21 C20 120.7(4) . . ?
C16 C21 H21 119.6 . . ?
C20 C21 H21 119.6 . . ?

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
S1 P1 C1 C2 -166.18(19) . . . . ?
S1 P1 C1 C7 13.5(5) . . . . ?
S1 P1 C5 C4 165.7(2) . . . . ?
S1 P1 C5 C16 -20.6(4) . . . . ?
S1 P1 C6 C3 -178.66(15) . . . . ?
P1 C1 C2 C3 1.2(3) . . . . ?
P1 C1 C2 C8 128.4(3) . . . . ?
P1 C5 C16 C17 130.4(4) . . . . ?
P1 C5 C16 C21 -52.1(5) . . . . ?
C1 P1 C5 C4 -60.5(3) . . . . ?
C1 P1 C5 C16 113.2(3) . . . . ?
C1 P1 C6 C3 51.8(2) . . . . ?
C1 C2 C3 C4 -71.0(3) . . . . ?
C1 C2 C3 C6 38.4(4) . . . . ?
C1 C2 C3 C14 163.3(3) . . . . ?
C1 C2 C8 C9 -50.9(5) . . . . ?
C1 C2 C8 C13 129.3(4) . . . . ?
C2 C3 C4 C5 75.6(4) . . . . ?
C2 C3 C4 C15 -97.4(4) . . . . ?
C2 C3 C6 P1 -58.6(3) . . . . ?
C2 C8 C9 C10 -176.9(5) . . . . ?
C2 C8 C13 C12 178.9(5) . . . . ?
C3 C2 C8 C9 71.2(5) . . . . ?
C3 C2 C8 C13 -108.6(4) . . . . ?
C3 C4 C5 P1 -1.9(4) . . . . ?
C3 C4 C5 C16 -175.4(3) . . . . ?
C4 C3 C6 P1 51.5(3) . . . . ?
C4 C5 C16 C17 -57.4(6) . . . . ?
C4 C5 C16 C21 120.1(5) . . . . ?
C5 P1 C1 C2 59.2(3) . . . . ?
C5 P1 C1 C7 -121.2(4) . . . . ?
C5 P1 C6 C3 -47.1(2) . . . . ?
C5 C16 C17 C18 176.3(4) . . . . ?
C5 C16 C21 C20 -174.9(4) . . . . ?
C6 P1 C1 C2 -32.4(3) . . . . ?
C6 P1 C1 C7 147.3(4) . . . . ?
C6 P1 C5 C4 31.0(3) . . . . ?
C6 P1 C5 C16 -155.3(3) . . . . ?
C6 C3 C4 C5 -34.9(4) . . . . ?
C6 C3 C4 C15 152.2(4) . . . . ?
C7 C1 C2 C3 -178.4(5) . . . . ?
C7 C1 C2 C8 -51.2(6) . . . . ?
C8 C2 C3 C4 162.6(3) . . . . ?
C8 C2 C3 C6 -88.0(4) . . . . ?
C8 C2 C3 C14 36.8(5) . . . . ?
C8 C9 C10 C11 -3.3(9) . . . . ?
C9 C8 C13 C12 -0.9(8) . . . . ?
C9 C10 C11 C12 1.4(9) . . . . ?
C10 C11 C12 C13 0.7(10) . . . . ?
C11 C12 C13 C8 -0.9(10) . . . . ?
C13 C8 C9 C10 2.9(7) . . . . ?
C14 C3 C4 C5 -159.1(4) . . . . ?
C14 C3 C4 C15 27.9(5) . . . . ?
C14 C3 C6 P1 176.3(3) . . . . ?
C15 C4 C5 P1 170.5(3) . . . . ?
C15 C4 C5 C16 -3.0(6) . . . . ?
C16 C17 C18 C19 -1.3(8) . . . . ?
C17 C16 C21 C20 2.7(7) . . . . ?
C17 C18 C19 C20 2.5(8) . . . . ?
C18 C19 C20 C21 -1.1(8) . . . . ?
C19 C20 C21 C16 -1.5(8) . . . . ?
C21 C16 C17 C18 -1.3(7) . . . . ?

_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 1.384
_oxdiff_exptl_absorpt_empirical_full_min 0.812
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_202008137
_database_code_depnum_ccdc_archive 'CCDC 2048671'
loop_
_audit_author_name
_audit_author_address
'Zhang keke'
;Zhengzhou University
China
;
_audit_update_record             
;
2020-12-07 deposited with the CCDC.	2021-05-07 downloaded from the CCDC.
;
_audit_creation_date             2020-08-18
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C33 H32 Cl2 P2 Pd'
_chemical_formula_sum            'C33 H32 Cl2 P2 Pd'
_chemical_formula_weight         667.82
_chemical_melting_point          ?
_chemical_oxdiff_formula         C14H15N2O1P1Pd1
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'
Cl Cl 0.3639 0.7018 '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'
Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   11.55252(15)
_cell_length_b                   13.96012(19)
_cell_length_c                   18.4085(2)
_cell_angle_alpha                90
_cell_angle_beta                 94.0277(11)
_cell_angle_gamma                90
_cell_volume                     2961.49(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5053
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      70.7510
_cell_measurement_theta_min      3.9840
_shelx_estimated_absorpt_T_max   0.571
_shelx_estimated_absorpt_T_min   0.477
_exptl_absorpt_coefficient_mu    7.892
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45775
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.498
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0495
_diffrn_reflns_av_unetI/netI     0.0555
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            11646
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.070
_diffrn_reflns_theta_max         67.070
_diffrn_reflns_theta_min         3.978
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2312
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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 -56.00   0.50    3.00    --  -33.50 -77.00-180.00   62
  2  ω    -55.00 -12.00   0.50    3.00    --  -33.50 -77.00-180.00   86
  3  ω    -50.00 -19.00   0.50    3.00    --  -33.50  57.00 -30.00   62
  4  ω     47.00 109.00   0.50    3.00    --   36.47  19.00 -90.00  124
  5  ω     58.00 102.00   0.50    3.00    --   36.47 178.00 -90.00   88
  6  ω     80.00 110.00   0.50    3.00    --   36.47 178.00  90.00   60
  7  ω     60.00 108.00   0.50    3.00    --   36.47 178.00-180.00   96
  8  ω     17.00  87.00   0.50    3.00    --   36.47  37.00   0.00  140
  9  ω     79.00 110.00   0.50    3.00    --   36.47 178.00 150.00   62
 10  ω      0.00  35.00   0.50    3.00    --   36.47  19.00 -90.00   70
 11  ω    134.00 161.00   0.50   10.00    --  108.00  45.00-150.00   54
 12  ω     88.00 118.00   0.50   10.00    --  108.00  45.00-150.00   60
 13  ω     55.00 110.00   0.50   10.00    --  108.00 -94.00-150.00  110
 14  ω     39.00 137.00   0.50   10.00    --  108.00 -77.00   0.00  196
 15  ω     69.00 127.00   0.50   10.00    --  108.00 -61.00  90.00  116
 16  ω     83.00 171.00   0.50   10.00    --  108.00  77.00 120.00  176
 17  ω     38.00 128.00   0.50   10.00    --  108.00 -45.00-180.00  180
 18  ω     81.00 142.00   0.50   10.00    --  108.00 178.00  60.00  122
 19  ω    121.00 148.00   0.50   10.00    --  108.00  45.00 -90.00   54
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0390363000
_diffrn_orient_matrix_UB_12      0.0438822000
_diffrn_orient_matrix_UB_13      -0.0744830000
_diffrn_orient_matrix_UB_21      0.0583698000
_diffrn_orient_matrix_UB_22      0.0954208000
_diffrn_orient_matrix_UB_23      0.0234152000
_diffrn_orient_matrix_UB_31      0.1137897000
_diffrn_orient_matrix_UB_32      -0.0339081000
_diffrn_orient_matrix_UB_33      -0.0306272000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4623
_reflns_number_total             5279
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (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    
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max         1.278
_refine_diff_density_min         -1.173
_refine_diff_density_rms         0.142
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         5279
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0564
_refine_ls_R_factor_gt           0.0502
_refine_ls_restrained_S_all      1.058
_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)+(0.0889P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1284
_refine_ls_wR_factor_ref         0.1359
_refine_special_details          ?
_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:
 C4(H4), C5(H5)
2.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B)
2.c Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C11(H11), C12(H12), C13(H13), C17(H17), C18(H18), C19(H19),
 C20(H20), C21(H21), C23(H23), C24(H24), C25(H25), C26(H26), C27(H27), C29(H29),
  C30(H30), C31(H31), C32(H32), C33(H33)
2.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.8584(4) 0.4988(3) 0.3737(2) 0.0359(9) Uani 1 1 d . . . . .
C2 C 0.9707(4) 0.4819(4) 0.3614(2) 0.0397(10) Uani 1 1 d . . . . .
C3 C 1.0139(4) 0.5441(3) 0.3004(2) 0.0359(9) Uani 1 1 d . . . . .
C4 C 0.9526(3) 0.4968(3) 0.2279(2) 0.0309(8) Uani 1 1 d . . . . .
H4 H 0.9506 0.4273 0.2355 0.037 Uiso 1 1 calc R . . . .
C5 C 0.8257(3) 0.5334(3) 0.2237(2) 0.0284(8) Uani 1 1 d . . . . .
H5 H 0.8174 0.5819 0.1852 0.034 Uiso 1 1 calc R . . . .
C6 C 0.7248(3) 0.4635(3) 0.2122(2) 0.0325(8) Uani 1 1 d . . . . .
H6A H 0.7333 0.4114 0.2471 0.039 Uiso 1 1 calc R . . . .
H6B H 0.7221 0.4369 0.1635 0.039 Uiso 1 1 calc R . . . .
C7 C 0.9551(4) 0.6428(3) 0.3107(3) 0.0376(10) Uani 1 1 d . . . . .
H7A H 0.9639 0.6861 0.2703 0.045 Uiso 1 1 calc R . . . .
H7B H 0.9806 0.6734 0.3563 0.045 Uiso 1 1 calc R . . . .
C8 C 0.7809(4) 0.4438(4) 0.4192(2) 0.0391(10) Uani 1 1 d . . . . .
C9 C 0.7155(5) 0.4893(4) 0.4688(2) 0.0477(11) Uani 1 1 d . . . . .
H9 H 0.7198 0.5555 0.4740 0.057 Uiso 1 1 calc R . . . .
C10 C 0.6433(5) 0.4369(5) 0.5109(3) 0.0597(15) Uani 1 1 d . . . . .
H10 H 0.6007 0.4681 0.5448 0.072 Uiso 1 1 calc R . . . .
C11 C 0.6344(6) 0.3395(5) 0.5029(3) 0.0638(16) Uani 1 1 d . . . . .
H11 H 0.5860 0.3049 0.5315 0.077 Uiso 1 1 calc R . . . .
C12 C 0.6961(6) 0.2935(5) 0.4535(3) 0.0619(15) Uani 1 1 d . . . . .
H12 H 0.6889 0.2275 0.4478 0.074 Uiso 1 1 calc R . . . .
C13 C 0.7703(5) 0.3449(4) 0.4110(3) 0.0525(13) Uani 1 1 d . . . . .
H13 H 0.8126 0.3131 0.3772 0.063 Uiso 1 1 calc R . . . .
C14 C 1.0448(5) 0.4032(5) 0.3949(4) 0.0646(16) Uani 1 1 d . . . . .
H14A H 1.0083 0.3769 0.4357 0.097 Uiso 1 1 calc GR . . . .
H14B H 1.1195 0.4285 0.4111 0.097 Uiso 1 1 calc GR . . . .
H14C H 1.0541 0.3539 0.3595 0.097 Uiso 1 1 calc GR . . . .
C15 C 1.1453(4) 0.5524(4) 0.3001(3) 0.0511(12) Uani 1 1 d . . . . .
H15A H 1.1779 0.4905 0.2918 0.077 Uiso 1 1 calc GR . . . .
H15B H 1.1763 0.5766 0.3463 0.077 Uiso 1 1 calc GR . . . .
H15C H 1.1647 0.5955 0.2622 0.077 Uiso 1 1 calc GR . . . .
C16 C 1.0151(3) 0.5150(3) 0.1595(2) 0.0324(8) Uani 1 1 d . . . . .
C17 C 1.0715(4) 0.4393(4) 0.1279(3) 0.0420(10) Uani 1 1 d . . . . .
H17 H 1.0691 0.3785 0.1484 0.050 Uiso 1 1 calc R . . . .
C18 C 1.1309(5) 0.4536(4) 0.0664(3) 0.0514(12) Uani 1 1 d . . . . .
H18 H 1.1694 0.4024 0.0465 0.062 Uiso 1 1 calc R . . . .
C19 C 1.1342(5) 0.5421(4) 0.0340(3) 0.0525(13) Uani 1 1 d . . . . .
H19 H 1.1739 0.5506 -0.0078 0.063 Uiso 1 1 calc R . . . .
C20 C 1.0776(5) 0.6189(4) 0.0644(3) 0.0503(12) Uani 1 1 d . . . . .
H20 H 1.0788 0.6793 0.0431 0.060 Uiso 1 1 calc R . . . .
C21 C 1.0192(4) 0.6039(3) 0.1268(3) 0.0421(10) Uani 1 1 d . . . . .
H21 H 0.9818 0.6552 0.1472 0.051 Uiso 1 1 calc R . . . .
C22 C 0.5424(4) 0.5804(3) 0.1366(2) 0.0323(8) Uani 1 1 d . . . . .
C23 C 0.6139(4) 0.5796(5) 0.0789(3) 0.0527(13) Uani 1 1 d . . . . .
H23 H 0.6872 0.5519 0.0849 0.063 Uiso 1 1 calc R . . . .
C24 C 0.5772(5) 0.6194(6) 0.0131(3) 0.0692(19) Uani 1 1 d . . . . .
H24 H 0.6266 0.6200 -0.0247 0.083 Uiso 1 1 calc R . . . .
C25 C 0.4680(5) 0.6586(4) 0.0025(3) 0.0570(15) Uani 1 1 d . . . . .
H25 H 0.4426 0.6834 -0.0428 0.068 Uiso 1 1 calc R . . . .
C26 C 0.3966(5) 0.6609(4) 0.0593(3) 0.0493(12) Uani 1 1 d . . . . .
H26 H 0.3236 0.6890 0.0530 0.059 Uiso 1 1 calc R . . . .
C27 C 0.4336(5) 0.6212(4) 0.1258(3) 0.0443(10) Uani 1 1 d . . . . .
H27 H 0.3845 0.6221 0.1638 0.053 Uiso 1 1 calc R . . . .
C28 C 0.4833(3) 0.4455(3) 0.2496(2) 0.0298(8) Uani 1 1 d . . . . .
C29 C 0.4109(4) 0.4005(3) 0.1973(2) 0.0392(10) Uani 1 1 d . . . . .
H29 H 0.4150 0.4159 0.1484 0.047 Uiso 1 1 calc R . . . .
C30 C 0.3311(4) 0.3315(4) 0.2178(3) 0.0482(11) Uani 1 1 d . . . . .
H30 H 0.2832 0.3002 0.1827 0.058 Uiso 1 1 calc R . . . .
C31 C 0.3242(4) 0.3106(4) 0.2902(3) 0.0500(12) Uani 1 1 d . . . . .
H31 H 0.2702 0.2662 0.3043 0.060 Uiso 1 1 calc R . . . .
C32 C 0.3971(5) 0.3551(4) 0.3421(3) 0.0518(13) Uani 1 1 d . . . . .
H32 H 0.3934 0.3392 0.3910 0.062 Uiso 1 1 calc R . . . .
C33 C 0.4759(4) 0.4234(4) 0.3223(3) 0.0429(10) Uani 1 1 d . . . . .
H33 H 0.5235 0.4543 0.3578 0.051 Uiso 1 1 calc R . . . .
Cl1 Cl 0.69056(11) 0.75803(9) 0.40172(6) 0.0505(3) Uani 1 1 d . . . . .
Cl2 Cl 0.43326(10) 0.68782(10) 0.30568(7) 0.0513(3) Uani 1 1 d . . . . .
P1 P 0.80993(8) 0.59326(7) 0.31120(5) 0.0275(2) Uani 1 1 d . . . . .
P2 P 0.59061(8) 0.53236(7) 0.22553(5) 0.0266(2) Uani 1 1 d . . . . .
Pd1 Pd 0.63055(2) 0.64611(2) 0.31116(2) 0.02641(13) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.353(6) . ?
C1 C8 1.483(6) . ?
C1 P1 1.813(4) . ?
C2 C3 1.530(6) . ?
C2 C14 1.499(7) . ?
C3 C4 1.608(6) . ?
C3 C7 1.554(6) . ?
C3 C15 1.523(6) . ?
C4 H4 0.9800 . ?
C4 C5 1.549(5) . ?
C4 C16 1.517(6) . ?
C5 H5 0.9800 . ?
C5 C6 1.523(5) . ?
C5 P1 1.836(4) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 P2 1.854(4) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 P1 1.814(5) . ?
C8 C9 1.380(7) . ?
C8 C13 1.393(7) . ?
C9 H9 0.9300 . ?
C9 C10 1.386(8) . ?
C10 H10 0.9300 . ?
C10 C11 1.371(9) . ?
C11 H11 0.9300 . ?
C11 C12 1.357(9) . ?
C12 H12 0.9300 . ?
C12 C13 1.399(8) . ?
C13 H13 0.9300 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 C17 1.390(6) . ?
C16 C21 1.381(6) . ?
C17 H17 0.9300 . ?
C17 C18 1.378(7) . ?
C18 H18 0.9300 . ?
C18 C19 1.373(8) . ?
C19 H19 0.9300 . ?
C19 C20 1.394(8) . ?
C20 H20 0.9300 . ?
C20 C21 1.388(7) . ?
C21 H21 0.9300 . ?
C22 C23 1.392(6) . ?
C22 C27 1.382(7) . ?
C22 P2 1.819(4) . ?
C23 H23 0.9300 . ?
C23 C24 1.372(8) . ?
C24 H24 0.9300 . ?
C24 C25 1.376(9) . ?
C25 H25 0.9300 . ?
C25 C26 1.378(9) . ?
C26 H26 0.9300 . ?
C26 C27 1.383(7) . ?
C27 H27 0.9300 . ?
C28 C29 1.381(6) . ?
C28 C33 1.383(6) . ?
C28 P2 1.811(4) . ?
C29 H29 0.9300 . ?
C29 C30 1.404(7) . ?
C30 H30 0.9300 . ?
C30 C31 1.371(8) . ?
C31 H31 0.9300 . ?
C31 C32 1.377(8) . ?
C32 H32 0.9300 . ?
C32 C33 1.384(7) . ?
C33 H33 0.9300 . ?
Cl1 Pd1 2.3534(11) . ?
Cl2 Pd1 2.3477(11) . ?
P1 Pd1 2.1996(10) . ?
P2 Pd1 2.2622(10) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C8 128.9(4) . . ?
C2 C1 P1 106.1(3) . . ?
C8 C1 P1 124.3(3) . . ?
C1 C2 C3 113.0(4) . . ?
C1 C2 C14 125.8(4) . . ?
C14 C2 C3 120.8(4) . . ?
C2 C3 C4 103.2(3) . . ?
C2 C3 C7 104.2(4) . . ?
C7 C3 C4 107.1(3) . . ?
C15 C3 C2 115.0(4) . . ?
C15 C3 C4 114.2(4) . . ?
C15 C3 C7 112.2(4) . . ?
C3 C4 H4 107.6 . . ?
C5 C4 C3 105.4(3) . . ?
C5 C4 H4 107.6 . . ?
C16 C4 C3 114.3(3) . . ?
C16 C4 H4 107.6 . . ?
C16 C4 C5 114.0(3) . . ?
C4 C5 H5 108.0 . . ?
C4 C5 P1 105.0(3) . . ?
C6 C5 C4 120.6(3) . . ?
C6 C5 H5 108.0 . . ?
C6 C5 P1 106.9(3) . . ?
P1 C5 H5 108.0 . . ?
C5 C6 H6A 110.4 . . ?
C5 C6 H6B 110.4 . . ?
C5 C6 P2 106.8(3) . . ?
H6A C6 H6B 108.6 . . ?
P2 C6 H6A 110.4 . . ?
P2 C6 H6B 110.4 . . ?
C3 C7 H7A 112.9 . . ?
C3 C7 H7B 112.9 . . ?
C3 C7 P1 94.3(3) . . ?
H7A C7 H7B 110.3 . . ?
P1 C7 H7A 112.9 . . ?
P1 C7 H7B 112.9 . . ?
C9 C8 C1 121.0(5) . . ?
C9 C8 C13 118.7(5) . . ?
C13 C8 C1 120.2(4) . . ?
C8 C9 H9 119.8 . . ?
C8 C9 C10 120.4(5) . . ?
C10 C9 H9 119.8 . . ?
C9 C10 H10 119.8 . . ?
C11 C10 C9 120.5(5) . . ?
C11 C10 H10 119.8 . . ?
C10 C11 H11 119.9 . . ?
C12 C11 C10 120.2(5) . . ?
C12 C11 H11 119.9 . . ?
C11 C12 H12 119.9 . . ?
C11 C12 C13 120.3(6) . . ?
C13 C12 H12 119.9 . . ?
C8 C13 C12 120.0(5) . . ?
C8 C13 H13 120.0 . . ?
C12 C13 H13 120.0 . . ?
C2 C14 H14A 109.5 . . ?
C2 C14 H14B 109.5 . . ?
C2 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C3 C15 H15A 109.5 . . ?
C3 C15 H15B 109.5 . . ?
C3 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C17 C16 C4 119.0(4) . . ?
C21 C16 C4 123.0(4) . . ?
C21 C16 C17 118.0(4) . . ?
C16 C17 H17 119.7 . . ?
C18 C17 C16 120.6(5) . . ?
C18 C17 H17 119.7 . . ?
C17 C18 H18 119.4 . . ?
C19 C18 C17 121.2(5) . . ?
C19 C18 H18 119.4 . . ?
C18 C19 H19 120.4 . . ?
C18 C19 C20 119.3(4) . . ?
C20 C19 H19 120.4 . . ?
C19 C20 H20 120.5 . . ?
C21 C20 C19 119.0(5) . . ?
C21 C20 H20 120.5 . . ?
C16 C21 C20 122.0(5) . . ?
C16 C21 H21 119.0 . . ?
C20 C21 H21 119.0 . . ?
C23 C22 P2 121.6(4) . . ?
C27 C22 C23 118.4(4) . . ?
C27 C22 P2 120.0(3) . . ?
C22 C23 H23 119.8 . . ?
C24 C23 C22 120.5(5) . . ?
C24 C23 H23 119.8 . . ?
C23 C24 H24 119.7 . . ?
C23 C24 C25 120.7(5) . . ?
C25 C24 H24 119.7 . . ?
C24 C25 H25 120.2 . . ?
C24 C25 C26 119.5(5) . . ?
C26 C25 H25 120.2 . . ?
C25 C26 H26 120.0 . . ?
C25 C26 C27 119.9(5) . . ?
C27 C26 H26 120.0 . . ?
C22 C27 C26 121.0(5) . . ?
C22 C27 H27 119.5 . . ?
C26 C27 H27 119.5 . . ?
C29 C28 C33 119.8(4) . . ?
C29 C28 P2 121.8(3) . . ?
C33 C28 P2 118.4(3) . . ?
C28 C29 H29 119.9 . . ?
C28 C29 C30 120.2(4) . . ?
C30 C29 H29 119.9 . . ?
C29 C30 H30 120.3 . . ?
C31 C30 C29 119.4(5) . . ?
C31 C30 H30 120.3 . . ?
C30 C31 H31 119.9 . . ?
C30 C31 C32 120.3(5) . . ?
C32 C31 H31 119.9 . . ?
C31 C32 H32 119.7 . . ?
C31 C32 C33 120.6(5) . . ?
C33 C32 H32 119.7 . . ?
C28 C33 C32 119.7(5) . . ?
C28 C33 H33 120.1 . . ?
C32 C33 H33 120.1 . . ?
C1 P1 C5 100.41(19) . . ?
C1 P1 C7 92.1(2) . . ?
C1 P1 Pd1 119.54(15) . . ?
C5 P1 Pd1 107.70(13) . . ?
C7 P1 C5 91.2(2) . . ?
C7 P1 Pd1 138.01(15) . . ?
C6 P2 Pd1 108.91(14) . . ?
C22 P2 C6 106.16(19) . . ?
C22 P2 Pd1 113.75(14) . . ?
C28 P2 C6 106.16(19) . . ?
C28 P2 C22 107.15(19) . . ?
C28 P2 Pd1 114.16(13) . . ?
Cl2 Pd1 Cl1 95.89(4) . . ?
P1 Pd1 Cl1 89.53(4) . . ?
P1 Pd1 Cl2 174.23(4) . . ?
P1 Pd1 P2 84.88(4) . . ?
P2 Pd1 Cl1 174.37(4) . . ?
P2 Pd1 Cl2 89.67(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 -73.8(5) . . . . ?
C1 C2 C3 C7 38.0(5) . . . . ?
C1 C2 C3 C15 161.2(4) . . . . ?
C1 C8 C9 C10 179.9(5) . . . . ?
C1 C8 C13 C12 -179.2(5) . . . . ?
C2 C1 C8 C9 131.7(6) . . . . ?
C2 C1 C8 C13 -50.3(7) . . . . ?
C2 C1 P1 C5 62.8(4) . . . . ?
C2 C1 P1 C7 -28.8(4) . . . . ?
C2 C1 P1 Pd1 -179.9(3) . . . . ?
C2 C3 C4 C5 78.1(4) . . . . ?
C2 C3 C4 C16 -155.8(3) . . . . ?
C2 C3 C7 P1 -52.6(3) . . . . ?
C3 C4 C5 C6 -129.7(4) . . . . ?
C3 C4 C5 P1 -9.3(3) . . . . ?
C3 C4 C16 C17 109.7(4) . . . . ?
C3 C4 C16 C21 -70.2(5) . . . . ?
C3 C7 P1 C1 46.3(3) . . . . ?
C3 C7 P1 C5 -54.1(3) . . . . ?
C3 C7 P1 Pd1 -172.64(17) . . . . ?
C4 C3 C7 P1 56.4(3) . . . . ?
C4 C5 C6 P2 170.9(3) . . . . ?
C4 C5 P1 C1 -53.3(3) . . . . ?
C4 C5 P1 C7 39.0(3) . . . . ?
C4 C5 P1 Pd1 -179.1(2) . . . . ?
C4 C16 C17 C18 -178.9(4) . . . . ?
C4 C16 C21 C20 179.7(5) . . . . ?
C5 C4 C16 C17 -128.9(4) . . . . ?
C5 C4 C16 C21 51.3(6) . . . . ?
C5 C6 P2 C22 89.5(3) . . . . ?
C5 C6 P2 C28 -156.7(3) . . . . ?
C5 C6 P2 Pd1 -33.4(3) . . . . ?
C6 C5 P1 C1 75.8(3) . . . . ?
C6 C5 P1 C7 168.1(3) . . . . ?
C6 C5 P1 Pd1 -50.0(3) . . . . ?
C7 C3 C4 C5 -31.5(4) . . . . ?
C7 C3 C4 C16 94.6(4) . . . . ?
C8 C1 C2 C3 169.5(4) . . . . ?
C8 C1 C2 C14 -2.8(9) . . . . ?
C8 C1 P1 C5 -108.6(4) . . . . ?
C8 C1 P1 C7 159.8(4) . . . . ?
C8 C1 P1 Pd1 8.7(4) . . . . ?
C8 C9 C10 C11 -1.2(9) . . . . ?
C9 C8 C13 C12 -1.2(8) . . . . ?
C9 C10 C11 C12 -0.2(10) . . . . ?
C10 C11 C12 C13 0.9(10) . . . . ?
C11 C12 C13 C8 -0.2(10) . . . . ?
C13 C8 C9 C10 1.8(8) . . . . ?
C14 C2 C3 C4 98.9(5) . . . . ?
C14 C2 C3 C7 -149.3(5) . . . . ?
C14 C2 C3 C15 -26.1(7) . . . . ?
C15 C3 C4 C5 -156.4(4) . . . . ?
C15 C3 C4 C16 -30.3(5) . . . . ?
C15 C3 C7 P1 -177.5(3) . . . . ?
C16 C4 C5 C6 104.0(4) . . . . ?
C16 C4 C5 P1 -135.5(3) . . . . ?
C16 C17 C18 C19 -1.2(8) . . . . ?
C17 C16 C21 C20 -0.2(7) . . . . ?
C17 C18 C19 C20 0.7(9) . . . . ?
C18 C19 C20 C21 0.1(8) . . . . ?
C19 C20 C21 C16 -0.4(8) . . . . ?
C21 C16 C17 C18 1.0(7) . . . . ?
C22 C23 C24 C25 -1.7(10) . . . . ?
C23 C22 C27 C26 -0.3(8) . . . . ?
C23 C22 P2 C6 -13.1(5) . . . . ?
C23 C22 P2 C28 -126.2(4) . . . . ?
C23 C22 P2 Pd1 106.7(4) . . . . ?
C23 C24 C25 C26 2.4(10) . . . . ?
C24 C25 C26 C27 -2.0(9) . . . . ?
C25 C26 C27 C22 1.0(8) . . . . ?
C27 C22 C23 C24 0.6(9) . . . . ?
C27 C22 P2 C6 168.8(4) . . . . ?
C27 C22 P2 C28 55.6(4) . . . . ?
C27 C22 P2 Pd1 -71.5(4) . . . . ?
C28 C29 C30 C31 1.2(8) . . . . ?
C29 C28 C33 C32 1.1(7) . . . . ?
C29 C28 P2 C6 -89.8(4) . . . . ?
C29 C28 P2 C22 23.3(4) . . . . ?
C29 C28 P2 Pd1 150.2(3) . . . . ?
C29 C30 C31 C32 -1.7(8) . . . . ?
C30 C31 C32 C33 1.8(8) . . . . ?
C31 C32 C33 C28 -1.5(8) . . . . ?
C33 C28 C29 C30 -0.9(7) . . . . ?
C33 C28 P2 C6 89.3(4) . . . . ?
C33 C28 P2 C22 -157.6(3) . . . . ?
C33 C28 P2 Pd1 -30.7(4) . . . . ?
P1 C1 C2 C3 -1.4(5) . . . . ?
P1 C1 C2 C14 -173.7(5) . . . . ?
P1 C1 C8 C9 -59.0(6) . . . . ?
P1 C1 C8 C13 119.1(5) . . . . ?
P1 C5 C6 P2 51.4(3) . . . . ?
P2 C22 C23 C24 -177.6(5) . . . . ?
P2 C22 C27 C26 178.0(4) . . . . ?
P2 C28 C29 C30 178.1(4) . . . . ?
P2 C28 C33 C32 -178.0(4) . . . . ?

_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 1.816
_oxdiff_exptl_absorpt_empirical_full_min 0.625
_chemical_properties_physical    Oxygen-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_202008152
_database_code_depnum_ccdc_archive 'CCDC 2048674'
loop_
_audit_author_name
_audit_author_address
'Zhang keke'
;Zhengzhou University
China
;
_audit_update_record             
;
2020-12-07 deposited with the CCDC.	2021-05-07 downloaded from the CCDC.
;
_audit_creation_date             2020-08-28
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C32 H31 N P2'
_chemical_formula_sum            'C32 H31 N P2'
_chemical_formula_weight         491.52
_chemical_melting_point          ?
_chemical_oxdiff_formula         C14H15N2O1P2
_chemical_oxdiff_usercomment     r
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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   11.9742(2)
_cell_length_b                   10.3221(2)
_cell_length_c                   21.5772(4)
_cell_angle_alpha                90
_cell_angle_beta                 97.4710(19)
_cell_angle_gamma                90
_cell_volume                     2644.31(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2864
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      70.5530
_cell_measurement_theta_min      3.9990
_shelx_estimated_absorpt_T_max   0.853
_shelx_estimated_absorpt_T_min   0.780
_exptl_absorpt_coefficient_mu    1.638
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92943
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.235
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0319
_diffrn_reflns_av_unetI/netI     0.0441
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            9907
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.068
_diffrn_reflns_theta_max         67.068
_diffrn_reflns_theta_min         4.017
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2312
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -43.00 -11.80   0.80    1.75    --  -33.50 -77.00   0.00   39
  2  ω   -103.00 -72.60   0.80    1.75    --  -33.50 -77.00   0.00   38
  3  ω     13.00  39.40   0.80    1.75    --   36.47 -57.00  60.00   33
  4  ω     19.00 104.60   0.80    1.75    --   36.47  57.00-150.00  107
  5  ω    -31.00  -0.60   0.80    1.75    --   36.47 -57.00  60.00   38
  6  ω    -23.00  58.60   0.80    1.75    --   36.47 -37.00  60.00  102
  7  ω    -27.00   3.40   0.80    1.75    --   36.47 -57.00  30.00   38
  8  ω      9.00  48.20   0.80    1.75    --   36.47 -57.00  30.00   49
  9  ω      6.00  47.60   0.80    1.75    --   36.47 -57.00 -30.00   52
 10  ω     83.00 107.80   0.80    1.75    --   36.47 178.00-180.00   31
 11  ω    -31.00  -4.60   0.80    1.75    --   36.47 -57.00 -30.00   33
 12  ω     93.00 173.00   0.80    6.50    --  108.00  61.00 -90.00  100
 13  ω     38.00 151.60   0.80    6.50    --  108.00 -15.00  90.00  142
 14  ω     43.00 123.00   0.80    6.50    --  108.00 -61.00 150.00  100
 15  ω     38.00 105.20   0.80    6.50    --  108.00 -94.00 -30.00   84
 16  ω     40.00 106.40   0.80    6.50    --  108.00-111.00-180.00   83
 17  ω     50.00 126.00   0.80    6.50    --  108.00 -61.00   0.00   95
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0862557000
_diffrn_orient_matrix_UB_12      0.0403814000
_diffrn_orient_matrix_UB_13      -0.0434848000
_diffrn_orient_matrix_UB_21      -0.0949002000
_diffrn_orient_matrix_UB_22      0.0068025000
_diffrn_orient_matrix_UB_23      -0.0554503000
_diffrn_orient_matrix_UB_31      -0.0197480000
_diffrn_orient_matrix_UB_32      0.1435053000
_diffrn_orient_matrix_UB_33      0.0148765000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3582
_reflns_number_total             4727
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (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)'
_refine_diff_density_max         0.323
_refine_diff_density_min         -0.176
_refine_diff_density_rms         0.040
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         4727
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0620
_refine_ls_R_factor_gt           0.0447
_refine_ls_restrained_S_all      1.040
_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)+(0.0557P)²+0.1812P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1095
_refine_ls_wR_factor_ref         0.1238
_refine_special_details          ?
_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:
 C14(H14), C15(H15)
2.b Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C19(H19A,H19B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25), C29(H29), C30(H30),
  C31(H31), C32(H32)
2.d Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C27(H27A,H27B,H27C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.19561(19) 0.6452(2) 0.33991(10) 0.0445(5) Uani 1 1 d . . . . .
C2 C 0.2826(2) 0.6830(3) 0.38502(13) 0.0665(7) Uani 1 1 d . . . . .
H2 H 0.3483 0.7169 0.3727 0.080 Uiso 1 1 calc R . . . .
C3 C 0.2734(3) 0.6712(3) 0.44803(13) 0.0769(9) Uani 1 1 d . . . . .
H3 H 0.3333 0.6956 0.4776 0.092 Uiso 1 1 calc R . . . .
C4 C 0.1768(3) 0.6240(3) 0.46718(13) 0.0701(8) Uani 1 1 d . . . . .
H4 H 0.1707 0.6159 0.5095 0.084 Uiso 1 1 calc R . . . .
C5 C 0.0892(3) 0.5887(3) 0.42322(13) 0.0676(7) Uani 1 1 d . . . . .
H5 H 0.0230 0.5574 0.4359 0.081 Uiso 1 1 calc R . . . .
C6 C 0.0982(2) 0.5990(3) 0.36007(12) 0.0547(6) Uani 1 1 d . . . . .
H6 H 0.0378 0.5746 0.3308 0.066 Uiso 1 1 calc R . . . .
C7 C 0.09129(18) 0.5824(2) 0.21575(10) 0.0433(5) Uani 1 1 d . . . . .
C8 C 0.0092(2) 0.6584(3) 0.18170(11) 0.0554(6) Uani 1 1 d . . . . .
H8 H 0.0179 0.7478 0.1803 0.067 Uiso 1 1 calc R . . . .
C9 C -0.0862(2) 0.6000(3) 0.14978(14) 0.0721(8) Uani 1 1 d . . . . .
H9 H -0.1412 0.6507 0.1271 0.086 Uiso 1 1 calc R . . . .
C10 C -0.0996(3) 0.4678(3) 0.15149(15) 0.0752(9) Uani 1 1 d . . . . .
H10 H -0.1639 0.4295 0.1305 0.090 Uiso 1 1 calc R . . . .
C11 C -0.0180(2) 0.3929(3) 0.18423(15) 0.0687(8) Uani 1 1 d . . . . .
H11 H -0.0267 0.3034 0.1849 0.082 Uiso 1 1 calc R . . . .
C12 C 0.0768(2) 0.4490(2) 0.21626(13) 0.0569(6) Uani 1 1 d . . . . .
H12 H 0.1316 0.3970 0.2384 0.068 Uiso 1 1 calc R . . . .
C13 C 0.33259(18) 0.5529(2) 0.25518(10) 0.0434(5) Uani 1 1 d . . . . .
H13A H 0.3984 0.5889 0.2802 0.052 Uiso 1 1 calc R . . . .
H13B H 0.3140 0.4727 0.2749 0.052 Uiso 1 1 calc R . . . .
C14 C 0.36376(18) 0.5209(2) 0.19048(10) 0.0423(5) Uani 1 1 d . . . . .
H14 H 0.3044 0.4645 0.1698 0.051 Uiso 1 1 calc R . . . .
C15 C 0.37454(19) 0.6381(2) 0.14616(10) 0.0434(5) Uani 1 1 d . . . . .
H15 H 0.3829 0.7162 0.1722 0.052 Uiso 1 1 calc R . . . .
C16 C 0.4896(2) 0.6186(2) 0.11757(11) 0.0495(5) Uani 1 1 d . . . . .
C17 C 0.5787(2) 0.6590(2) 0.17125(11) 0.0492(5) Uani 1 1 d . . . . .
C18 C 0.59293(19) 0.5681(2) 0.21708(12) 0.0478(5) Uani 1 1 d . . . . .
C19 C 0.5048(2) 0.4713(3) 0.11280(12) 0.0590(6) Uani 1 1 d . . . . .
H19A H 0.5763 0.4488 0.0990 0.071 Uiso 1 1 calc R . . . .
H19B H 0.4438 0.4315 0.0853 0.071 Uiso 1 1 calc R . . . .
C20 C 0.2729(2) 0.6583(2) 0.09778(11) 0.0513(6) Uani 1 1 d . . . . .
C21 C 0.2248(2) 0.7794(3) 0.08947(13) 0.0637(7) Uani 1 1 d . . . . .
H21 H 0.2543 0.8477 0.1145 0.076 Uiso 1 1 calc R . . . .
C22 C 0.1331(3) 0.8010(4) 0.04436(16) 0.0847(10) Uani 1 1 d . . . . .
H22 H 0.1008 0.8829 0.0399 0.102 Uiso 1 1 calc R . . . .
C23 C 0.0899(3) 0.7018(5) 0.00634(17) 0.0959(12) Uani 1 1 d . . . . .
H23 H 0.0303 0.7171 -0.0249 0.115 Uiso 1 1 calc R . . . .
C24 C 0.1347(3) 0.5806(4) 0.01452(15) 0.0903(11) Uani 1 1 d . . . . .
H24 H 0.1042 0.5125 -0.0104 0.108 Uiso 1 1 calc R . . . .
C25 C 0.2252(3) 0.5588(3) 0.05989(13) 0.0685(8) Uani 1 1 d . . . . .
H25 H 0.2548 0.4757 0.0652 0.082 Uiso 1 1 calc R . . . .
C26 C 0.4941(3) 0.6906(3) 0.05605(12) 0.0686(8) Uani 1 1 d . . . . .
H26A H 0.4383 0.6558 0.0245 0.103 Uiso 1 1 calc GR . . . .
H26B H 0.5674 0.6803 0.0432 0.103 Uiso 1 1 calc GR . . . .
H26C H 0.4795 0.7810 0.0618 0.103 Uiso 1 1 calc GR . . . .
C27 C 0.6247(2) 0.7940(3) 0.17314(14) 0.0624(7) Uani 1 1 d . . . . .
H27A H 0.6804 0.8007 0.1451 0.094 Uiso 1 1 calc GR . . . .
H27B H 0.6586 0.8138 0.2149 0.094 Uiso 1 1 calc GR . . . .
H27C H 0.5647 0.8540 0.1607 0.094 Uiso 1 1 calc GR . . . .
C28 C 0.65499(19) 0.5799(2) 0.27991(12) 0.0490(5) Uani 1 1 d . . . . .
C29 C 0.7570(2) 0.6459(3) 0.29338(13) 0.0579(6) Uani 1 1 d . . . . .
H29 H 0.7936 0.6787 0.2613 0.070 Uiso 1 1 calc R . . . .
C30 C 0.8025(2) 0.6616(3) 0.35475(14) 0.0655(7) Uani 1 1 d . . . . .
H30 H 0.8690 0.7080 0.3646 0.079 Uiso 1 1 calc R . . . .
C31 C 0.7494(3) 0.6087(3) 0.40131(15) 0.0720(8) Uani 1 1 d . . . . .
H31 H 0.7781 0.6192 0.4432 0.086 Uiso 1 1 calc R . . . .
C32 C 0.6528(3) 0.5400(3) 0.38404(14) 0.0727(8) Uani 1 1 d . . . . .
H32 H 0.6180 0.5020 0.4156 0.087 Uiso 1 1 calc R . . . .
N1 N 0.60475(18) 0.5235(2) 0.32523(11) 0.0599(6) Uani 1 1 d . . . . .
P1 P 0.21330(5) 0.66784(5) 0.25701(3) 0.04238(15) Uani 1 1 d . . . . .
P2 P 0.50050(5) 0.42755(6) 0.19553(3) 0.04920(17) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.386(4) . ?
C1 C6 1.382(3) . ?
C1 P1 1.843(2) . ?
C2 H2 0.9300 . ?
C2 C3 1.384(4) . ?
C3 H3 0.9300 . ?
C3 C4 1.368(4) . ?
C4 H4 0.9300 . ?
C4 C5 1.369(4) . ?
C5 H5 0.9300 . ?
C5 C6 1.385(4) . ?
C6 H6 0.9300 . ?
C7 C8 1.391(3) . ?
C7 C12 1.388(3) . ?
C7 P1 1.835(2) . ?
C8 H8 0.9300 . ?
C8 C9 1.392(4) . ?
C9 H9 0.9300 . ?
C9 C10 1.374(5) . ?
C10 H10 0.9300 . ?
C10 C11 1.368(4) . ?
C11 H11 0.9300 . ?
C11 C12 1.378(4) . ?
C12 H12 0.9300 . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 C14 1.527(3) . ?
C13 P1 1.861(2) . ?
C14 H14 0.9800 . ?
C14 C15 1.559(3) . ?
C14 P2 1.890(2) . ?
C15 H15 0.9800 . ?
C15 C16 1.594(3) . ?
C15 C20 1.511(3) . ?
C16 C17 1.527(3) . ?
C16 C19 1.537(3) . ?
C16 C26 1.528(3) . ?
C17 C18 1.358(3) . ?
C17 C27 1.497(3) . ?
C18 C28 1.464(3) . ?
C18 P2 1.848(2) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C19 P2 1.848(3) . ?
C20 C21 1.378(4) . ?
C20 C25 1.388(4) . ?
C21 H21 0.9300 . ?
C21 C22 1.387(4) . ?
C22 H22 0.9300 . ?
C22 C23 1.371(5) . ?
C23 H23 0.9300 . ?
C23 C24 1.363(5) . ?
C24 H24 0.9300 . ?
C24 C25 1.381(4) . ?
C25 H25 0.9300 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 C29 1.396(3) . ?
C28 N1 1.345(3) . ?
C29 H29 0.9300 . ?
C29 C30 1.374(4) . ?
C30 H30 0.9300 . ?
C30 C31 1.370(4) . ?
C31 H31 0.9300 . ?
C31 C32 1.367(4) . ?
C32 H32 0.9300 . ?
C32 N1 1.334(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 P1 118.36(19) . . ?
C6 C1 C2 117.7(2) . . ?
C6 C1 P1 123.88(19) . . ?
C1 C2 H2 119.5 . . ?
C3 C2 C1 121.1(3) . . ?
C3 C2 H2 119.5 . . ?
C2 C3 H3 119.8 . . ?
C4 C3 C2 120.5(3) . . ?
C4 C3 H3 119.8 . . ?
C3 C4 H4 120.4 . . ?
C3 C4 C5 119.2(3) . . ?
C5 C4 H4 120.4 . . ?
C4 C5 H5 119.6 . . ?
C4 C5 C6 120.7(3) . . ?
C6 C5 H5 119.6 . . ?
C1 C6 C5 120.9(3) . . ?
C1 C6 H6 119.6 . . ?
C5 C6 H6 119.6 . . ?
C8 C7 P1 116.68(18) . . ?
C12 C7 C8 118.9(2) . . ?
C12 C7 P1 124.44(19) . . ?
C7 C8 H8 120.2 . . ?
C7 C8 C9 119.7(3) . . ?
C9 C8 H8 120.2 . . ?
C8 C9 H9 119.7 . . ?
C10 C9 C8 120.5(3) . . ?
C10 C9 H9 119.7 . . ?
C9 C10 H10 120.1 . . ?
C11 C10 C9 119.8(3) . . ?
C11 C10 H10 120.1 . . ?
C10 C11 H11 119.7 . . ?
C10 C11 C12 120.5(3) . . ?
C12 C11 H11 119.7 . . ?
C7 C12 H12 119.7 . . ?
C11 C12 C7 120.6(3) . . ?
C11 C12 H12 119.7 . . ?
H13A C13 H13B 107.4 . . ?
C14 C13 H13A 108.3 . . ?
C14 C13 H13B 108.3 . . ?
C14 C13 P1 115.90(16) . . ?
P1 C13 H13A 108.3 . . ?
P1 C13 H13B 108.3 . . ?
C13 C14 H14 107.2 . . ?
C13 C14 C15 116.25(18) . . ?
C13 C14 P2 111.74(15) . . ?
C15 C14 H14 107.2 . . ?
C15 C14 P2 106.91(14) . . ?
P2 C14 H14 107.2 . . ?
C14 C15 H15 107.3 . . ?
C14 C15 C16 106.50(18) . . ?
C16 C15 H15 107.3 . . ?
C20 C15 C14 114.03(18) . . ?
C20 C15 H15 107.3 . . ?
C20 C15 C16 114.17(19) . . ?
C17 C16 C15 103.06(18) . . ?
C17 C16 C19 104.1(2) . . ?
C17 C16 C26 115.2(2) . . ?
C19 C16 C15 105.47(19) . . ?
C26 C16 C15 113.9(2) . . ?
C26 C16 C19 113.9(2) . . ?
C18 C17 C16 111.9(2) . . ?
C18 C17 C27 127.8(2) . . ?
C27 C17 C16 119.6(2) . . ?
C17 C18 C28 128.2(2) . . ?
C17 C18 P2 110.18(19) . . ?
C28 C18 P2 120.90(17) . . ?
C16 C19 H19A 111.9 . . ?
C16 C19 H19B 111.9 . . ?
C16 C19 P2 99.13(15) . . ?
H19A C19 H19B 109.6 . . ?
P2 C19 H19A 111.9 . . ?
P2 C19 H19B 111.9 . . ?
C21 C20 C15 120.0(2) . . ?
C21 C20 C25 117.5(3) . . ?
C25 C20 C15 122.5(2) . . ?
C20 C21 H21 119.5 . . ?
C20 C21 C22 121.1(3) . . ?
C22 C21 H21 119.5 . . ?
C21 C22 H22 119.9 . . ?
C23 C22 C21 120.2(3) . . ?
C23 C22 H22 119.9 . . ?
C22 C23 H23 120.1 . . ?
C24 C23 C22 119.8(3) . . ?
C24 C23 H23 120.1 . . ?
C23 C24 H24 120.0 . . ?
C23 C24 C25 120.0(3) . . ?
C25 C24 H24 120.0 . . ?
C20 C25 H25 119.3 . . ?
C24 C25 C20 121.5(3) . . ?
C24 C25 H25 119.3 . . ?
C16 C26 H26A 109.5 . . ?
C16 C26 H26B 109.5 . . ?
C16 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C17 C27 H27A 109.5 . . ?
C17 C27 H27B 109.5 . . ?
C17 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C29 C28 C18 123.9(2) . . ?
N1 C28 C18 114.6(2) . . ?
N1 C28 C29 121.4(2) . . ?
C28 C29 H29 120.5 . . ?
C30 C29 C28 119.0(3) . . ?
C30 C29 H29 120.5 . . ?
C29 C30 H30 120.1 . . ?
C31 C30 C29 119.7(3) . . ?
C31 C30 H30 120.1 . . ?
C30 C31 H31 121.2 . . ?
C32 C31 C30 117.6(3) . . ?
C32 C31 H31 121.2 . . ?
C31 C32 H32 117.6 . . ?
N1 C32 C31 124.8(3) . . ?
N1 C32 H32 117.6 . . ?
C32 N1 C28 117.3(2) . . ?
C1 P1 C13 97.19(10) . . ?
C7 P1 C1 103.02(10) . . ?
C7 P1 C13 104.36(10) . . ?
C18 P2 C14 95.76(10) . . ?
C18 P2 C19 87.72(12) . . ?
C19 P2 C14 87.28(11) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 -1.2(5) . . . . ?
C2 C1 C6 C5 -1.3(4) . . . . ?
C2 C1 P1 C7 171.3(2) . . . . ?
C2 C1 P1 C13 64.7(2) . . . . ?
C2 C3 C4 C5 -0.1(5) . . . . ?
C3 C4 C5 C6 0.7(5) . . . . ?
C4 C5 C6 C1 0.0(4) . . . . ?
C6 C1 C2 C3 1.9(4) . . . . ?
C6 C1 P1 C7 -12.3(2) . . . . ?
C6 C1 P1 C13 -118.9(2) . . . . ?
C7 C8 C9 C10 -0.2(4) . . . . ?
C8 C7 C12 C11 -0.8(4) . . . . ?
C8 C7 P1 C1 111.59(19) . . . . ?
C8 C7 P1 C13 -147.35(18) . . . . ?
C8 C9 C10 C11 -0.8(5) . . . . ?
C9 C10 C11 C12 0.9(5) . . . . ?
C10 C11 C12 C7 -0.1(4) . . . . ?
C12 C7 C8 C9 1.0(4) . . . . ?
C12 C7 P1 C1 -68.8(2) . . . . ?
C12 C7 P1 C13 32.3(2) . . . . ?
C13 C14 C15 C16 132.6(2) . . . . ?
C13 C14 C15 C20 -100.6(2) . . . . ?
C13 C14 P2 C18 -75.74(17) . . . . ?
C13 C14 P2 C19 -163.17(17) . . . . ?
C14 C13 P1 C1 169.46(17) . . . . ?
C14 C13 P1 C7 63.99(18) . . . . ?
C14 C15 C16 C17 -76.9(2) . . . . ?
C14 C15 C16 C19 32.0(2) . . . . ?
C14 C15 C16 C26 157.6(2) . . . . ?
C14 C15 C20 C21 130.6(2) . . . . ?
C14 C15 C20 C25 -50.2(3) . . . . ?
C15 C14 P2 C18 52.50(16) . . . . ?
C15 C14 P2 C19 -34.93(16) . . . . ?
C15 C16 C17 C18 74.2(2) . . . . ?
C15 C16 C17 C27 -96.4(2) . . . . ?
C15 C16 C19 P2 -56.9(2) . . . . ?
C15 C20 C21 C22 178.5(2) . . . . ?
C15 C20 C25 C24 -177.7(3) . . . . ?
C16 C15 C20 C21 -106.7(3) . . . . ?
C16 C15 C20 C25 72.5(3) . . . . ?
C16 C17 C18 C28 -168.5(2) . . . . ?
C16 C17 C18 P2 1.4(2) . . . . ?
C16 C19 P2 C14 52.39(17) . . . . ?
C16 C19 P2 C18 -43.49(17) . . . . ?
C17 C16 C19 P2 51.20(19) . . . . ?
C17 C18 C28 C29 -39.0(4) . . . . ?
C17 C18 C28 N1 139.7(3) . . . . ?
C17 C18 P2 C14 -60.89(18) . . . . ?
C17 C18 P2 C19 26.14(19) . . . . ?
C18 C28 C29 C30 173.8(2) . . . . ?
C18 C28 N1 C32 -174.7(2) . . . . ?
C19 C16 C17 C18 -35.7(3) . . . . ?
C19 C16 C17 C27 153.7(2) . . . . ?
C20 C15 C16 C17 156.4(2) . . . . ?
C20 C15 C16 C19 -94.7(2) . . . . ?
C20 C15 C16 C26 30.9(3) . . . . ?
C20 C21 C22 C23 -1.2(5) . . . . ?
C21 C20 C25 C24 1.5(4) . . . . ?
C21 C22 C23 C24 2.5(6) . . . . ?
C22 C23 C24 C25 -1.8(6) . . . . ?
C23 C24 C25 C20 -0.3(5) . . . . ?
C25 C20 C21 C22 -0.8(4) . . . . ?
C26 C16 C17 C18 -161.2(2) . . . . ?
C26 C16 C17 C27 28.3(3) . . . . ?
C26 C16 C19 P2 177.47(19) . . . . ?
C27 C17 C18 C28 1.1(4) . . . . ?
C27 C17 C18 P2 171.1(2) . . . . ?
C28 C18 P2 C14 109.93(19) . . . . ?
C28 C18 P2 C19 -163.0(2) . . . . ?
C28 C29 C30 C31 2.3(4) . . . . ?
C29 C28 N1 C32 4.0(4) . . . . ?
C29 C30 C31 C32 0.9(4) . . . . ?
C30 C31 C32 N1 -1.8(5) . . . . ?
C31 C32 N1 C28 -0.6(5) . . . . ?
N1 C28 C29 C30 -4.9(4) . . . . ?
P1 C1 C2 C3 178.5(2) . . . . ?
P1 C1 C6 C5 -177.7(2) . . . . ?
P1 C7 C8 C9 -179.4(2) . . . . ?
P1 C7 C12 C11 179.5(2) . . . . ?
P1 C13 C14 C15 47.0(2) . . . . ?
P1 C13 C14 P2 170.07(11) . . . . ?
P2 C14 C15 C16 7.0(2) . . . . ?
P2 C14 C15 C20 133.84(17) . . . . ?
P2 C18 C28 C29 152.0(2) . . . . ?
P2 C18 C28 N1 -29.3(3) . . . . ?


_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 1.256
_oxdiff_exptl_absorpt_empirical_full_min 0.920
_chemical_properties_physical    Oxygen-sensitive
