# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_compound1b
_database_code_depnum_ccdc_archive 'CCDC 1939608'
loop_
_audit_author_name
_audit_author_address
'Hans Georg Stammler'
;University of Bielefeld
Germany
;
_audit_update_record             
;
2019-07-10 deposited with the CCDC.	2019-10-18 downloaded from the CCDC.
;



_audit_creation_date             2019-04-15
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2018.12.18 svn.r3554 for Rigaku Oxford Diffraction, GUI svn.r1)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br, C34 H43 N2'
_chemical_formula_sum            'C34 H43 Br N2'
_chemical_formula_weight         559.61
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 '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/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   10.3786(2)
_cell_length_b                   15.7209(3)
_cell_length_c                   19.3197(3)
_cell_angle_alpha                90
_cell_angle_beta                 100.6678(18)
_cell_angle_gamma                90
_cell_volume                     3097.75(10)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    22413
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      30.9030
_cell_measurement_theta_min      1.6990
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.350
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79577
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.47a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.200
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1184
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 1 0.0336
0 0 -1 0.0336
-1 0 -1 0.0781
1 0 1 0.0781
0 -1 1 0.0712
0 1 -1 0.0712
-3 5 1 0.0945
3 -5 -1 0.0945

_exptl_crystal_size_max          0.268
_exptl_crystal_size_mid          0.189
_exptl_crystal_size_min          0.067
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0379
_diffrn_reflns_av_unetI/netI     0.0268
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.950
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            76135
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.162
_diffrn_reflns_theta_min         1.682
_diffrn_ambient_temperature      100.0(1)
_diffrn_detector_area_resol_mean 8.0951
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -4.00  96.00   1.00   29.96    --   26.03  77.00 -90.00  100
  2  ω      1.00  98.00   1.00   29.96    --   26.03  38.00-150.00   97
  3  ω      6.00  95.00   1.00   29.96    --   26.03  57.00  30.00   89
  4  ω     -4.00  96.00   1.00   29.96    --   26.03  77.00 120.00  100
  5  ω    -20.00  68.00   1.00   29.96    --   26.03 -99.00-120.00   88
  6  ω    -46.00  52.00   1.00   29.96    --   26.03 -38.00 120.00   98
  7  ω      6.00  95.00   1.00   29.96    --   26.03  57.00-120.00   89
  8  ω    -20.00  68.00   1.00   29.96    --   26.03 -99.00   0.00   88
  9  ω    -20.00  68.00   1.00   29.96    --   26.03 -99.00  90.00   88
 10  ω    -47.00  70.00   1.00   29.96    --   26.03 -19.00-150.00  117
 11  ω    -99.00 -42.00   1.00   29.96    --  -23.50-178.00 150.00   57
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8477
_reflns_number_total             10359
_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 1.171.40.47a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.47a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.47a (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         0.958
_refine_diff_density_min         -0.677
_refine_diff_density_rms         0.060
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     342
_refine_ls_number_reflns         10359
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0510
_refine_ls_R_factor_gt           0.0357
_refine_ls_restrained_S_all      1.043
_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)+(0.0348P)²+1.8602P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0815
_refine_ls_wR_factor_ref         0.0874
_refine_special_details          
'Hydrgen atoms taken into account using a riding model. Methyl group C10  disordered in ratio 1:1.'
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H,H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: H10A(0.5) H10B(0.5) H10C(0.5) H10D(0.5) H10E(0.5) H10F(0.5)
3.a Ternary CH refined with riding coordinates:
 C17(H17), C20(H20), C29(H29), C32(H32)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C7(H7), C8(H8), C9(H9), C13(H13), C14(H14), C15(H15),
 C25(H25), C26(H26), C27(H27)
3.c Disordered Me refined with riding coordinates:
 C10(H10A,H10B,H10C,H10D,H10E,H10F)
3.d Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C33(H33A,H33B,H33C), C34(H34A,
 H34B,H34C)
;
_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
Br1 Br 0.25939(2) 0.74035(2) 0.06482(2) 0.02525(5) Uani 1 1 d . . . . .
N1 N 0.36755(11) 0.53383(7) 0.27048(6) 0.0165(2) Uani 1 1 d . . . . .
N2 N 0.25555(11) 0.47251(7) 0.17828(6) 0.0156(2) Uani 1 1 d . . . . .
C1 C 0.30865(13) 0.46055(8) 0.24672(6) 0.0149(2) Uani 1 1 d . . . . .
C2 C 0.34991(14) 0.59311(9) 0.21644(7) 0.0201(3) Uani 1 1 d . . . . .
H2 H 0.380737 0.650131 0.219394 0.024 Uiso 1 1 calc R . . . .
C3 C 0.28073(14) 0.55468(8) 0.15881(7) 0.0197(3) Uani 1 1 d . . . . .
H3 H 0.254373 0.579365 0.113513 0.024 Uiso 1 1 calc R . . . .
C4 C 0.29745(13) 0.38364(8) 0.28814(6) 0.0149(2) Uani 1 1 d . . . . .
C5 C 0.17279(14) 0.35046(9) 0.28889(7) 0.0191(3) Uani 1 1 d . . . . .
H5 H 0.098063 0.377372 0.261917 0.023 Uiso 1 1 calc R . . . .
C6 C 0.15624(14) 0.27864(9) 0.32848(7) 0.0210(3) Uani 1 1 d . . . . .
C7 C 0.26809(15) 0.24083(9) 0.36746(7) 0.0203(3) Uani 1 1 d . . . . .
H7 H 0.258866 0.192073 0.395180 0.024 Uiso 1 1 calc R . . . .
C8 C 0.39248(14) 0.27265(9) 0.36677(7) 0.0193(3) Uani 1 1 d . . . . .
H8 H 0.467156 0.245187 0.393278 0.023 Uiso 1 1 calc R . . . .
C9 C 0.40812(13) 0.34465(8) 0.32737(7) 0.0168(2) Uani 1 1 d . . . . .
H9 H 0.493080 0.367022 0.327163 0.020 Uiso 1 1 calc R . . . .
C10 C 0.02139(17) 0.24337(12) 0.32883(10) 0.0349(4) Uani 1 1 d . . . . .
H10A H 0.028439 0.193131 0.359326 0.042 Uiso 0.5 1 calc R . P . .
H10B H -0.032148 0.286669 0.346580 0.042 Uiso 0.5 1 calc R . P . .
H10C H -0.019824 0.227365 0.280795 0.042 Uiso 0.5 1 calc R . P . .
H10D H -0.044128 0.278313 0.298475 0.042 Uiso 0.5 1 calc R . P . .
H10E H 0.016459 0.184775 0.311220 0.042 Uiso 0.5 1 calc R . P . .
H10F H 0.004135 0.244078 0.377006 0.042 Uiso 0.5 1 calc R . P . .
C11 C 0.42990(13) 0.55243(8) 0.34253(7) 0.0162(2) Uani 1 1 d . . . . .
C12 C 0.34946(13) 0.57668(8) 0.38978(7) 0.0180(2) Uani 1 1 d . . . . .
C13 C 0.41195(14) 0.60084(9) 0.45723(7) 0.0201(3) Uani 1 1 d . . . . .
H13 H 0.361081 0.618578 0.490746 0.024 Uiso 1 1 calc R . . . .
C14 C 0.54731(14) 0.59918(9) 0.47572(7) 0.0203(3) Uani 1 1 d . . . . .
H14 H 0.588288 0.615765 0.521838 0.024 Uiso 1 1 calc R . . . .
C15 C 0.62381(14) 0.57365(9) 0.42781(7) 0.0198(3) Uani 1 1 d . . . . .
H15 H 0.716513 0.572430 0.441697 0.024 Uiso 1 1 calc R . . . .
C16 C 0.56667(13) 0.54974(8) 0.35953(7) 0.0171(2) Uani 1 1 d . . . . .
C17 C 0.20105(14) 0.58030(10) 0.36984(8) 0.0233(3) Uani 1 1 d . . . . .
H17 H 0.174186 0.550719 0.323590 0.028 Uiso 1 1 calc R . . . .
C18 C 0.15617(18) 0.67274(12) 0.36076(10) 0.0367(4) Uani 1 1 d . . . . .
H18A H 0.185510 0.703667 0.404904 0.055 Uiso 1 1 calc GR . . . .
H18B H 0.060276 0.674754 0.348438 0.055 Uiso 1 1 calc GR . . . .
H18C H 0.193893 0.699151 0.323103 0.055 Uiso 1 1 calc GR . . . .
C19 C 0.13568(18) 0.53500(17) 0.42418(11) 0.0491(6) Uani 1 1 d . . . . .
H19A H 0.167108 0.476167 0.429680 0.074 Uiso 1 1 calc GR . . . .
H19B H 0.040383 0.535200 0.408232 0.074 Uiso 1 1 calc GR . . . .
H19C H 0.157621 0.564583 0.469481 0.074 Uiso 1 1 calc GR . . . .
C20 C 0.65346(15) 0.52473(9) 0.30737(7) 0.0218(3) Uani 1 1 d . . . . .
H20 H 0.596675 0.497883 0.265625 0.026 Uiso 1 1 calc R . . . .
C21 C 0.75855(16) 0.46012(11) 0.33885(9) 0.0287(3) Uani 1 1 d . . . . .
H21A H 0.818200 0.486159 0.378434 0.043 Uiso 1 1 calc GR . . . .
H21B H 0.808177 0.442593 0.302760 0.043 Uiso 1 1 calc GR . . . .
H21C H 0.716511 0.410251 0.355508 0.043 Uiso 1 1 calc GR . . . .
C22 C 0.71727(19) 0.60411(12) 0.28201(10) 0.0370(4) Uani 1 1 d . . . . .
H22A H 0.648844 0.642675 0.258378 0.055 Uiso 1 1 calc GR . . . .
H22B H 0.773748 0.587221 0.248951 0.055 Uiso 1 1 calc GR . . . .
H22C H 0.769979 0.633099 0.322494 0.055 Uiso 1 1 calc GR . . . .
C23 C 0.20294(13) 0.40569(8) 0.12918(6) 0.0145(2) Uani 1 1 d . . . . .
C24 C 0.29349(13) 0.35481(8) 0.10300(7) 0.0172(2) Uani 1 1 d . . . . .
C25 C 0.24267(14) 0.28974(9) 0.05660(7) 0.0209(3) Uani 1 1 d . . . . .
H25 H 0.300819 0.252780 0.038486 0.025 Uiso 1 1 calc R . . . .
C26 C 0.10864(15) 0.27849(9) 0.03673(7) 0.0212(3) Uani 1 1 d . . . . .
H26 H 0.075827 0.233474 0.005601 0.025 Uiso 1 1 calc R . . . .
C27 C 0.02186(14) 0.33218(9) 0.06175(7) 0.0190(3) Uani 1 1 d . . . . .
H27 H -0.069798 0.324629 0.046407 0.023 Uiso 1 1 calc R . . . .
C28 C 0.06723(13) 0.39719(8) 0.10916(7) 0.0158(2) Uani 1 1 d . . . . .
C29 C 0.44037(14) 0.37017(10) 0.11976(8) 0.0229(3) Uani 1 1 d . . . . .
H29 H 0.457173 0.420105 0.152235 0.027 Uiso 1 1 calc R . . . .
C30 C 0.51478(16) 0.29392(11) 0.15647(9) 0.0294(3) Uani 1 1 d . . . . .
H30A H 0.480527 0.280104 0.199102 0.044 Uiso 1 1 calc GR . . . .
H30B H 0.608200 0.307852 0.169268 0.044 Uiso 1 1 calc GR . . . .
H30C H 0.503350 0.244895 0.124590 0.044 Uiso 1 1 calc GR . . . .
C31 C 0.48980(19) 0.39236(18) 0.05202(11) 0.0538(6) Uani 1 1 d . . . . .
H31A H 0.479836 0.342839 0.020670 0.081 Uiso 1 1 calc GR . . . .
H31B H 0.582511 0.408463 0.063620 0.081 Uiso 1 1 calc GR . . . .
H31C H 0.438661 0.439984 0.028419 0.081 Uiso 1 1 calc GR . . . .
C32 C -0.02974(14) 0.45715(9) 0.13420(7) 0.0204(3) Uani 1 1 d . . . . .
H32 H 0.017025 0.487994 0.176793 0.024 Uiso 1 1 calc R . . . .
C33 C -0.07957(19) 0.52295(11) 0.07709(9) 0.0351(4) Uani 1 1 d . . . . .
H33A H -0.005641 0.556748 0.067297 0.053 Uiso 1 1 calc GR . . . .
H33B H -0.143167 0.560513 0.093383 0.053 Uiso 1 1 calc GR . . . .
H33C H -0.121788 0.493726 0.034022 0.053 Uiso 1 1 calc GR . . . .
C34 C -0.14558(15) 0.40904(11) 0.15450(9) 0.0296(3) Uani 1 1 d . . . . .
H34A H -0.195983 0.381276 0.112682 0.044 Uiso 1 1 calc GR . . . .
H34B H -0.202123 0.449107 0.173752 0.044 Uiso 1 1 calc GR . . . .
H34C H -0.112742 0.365940 0.190058 0.044 Uiso 1 1 calc GR . . . .


_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
N1 C1 1.3445(16) . ?
N1 C2 1.3860(17) . ?
N1 C11 1.4521(16) . ?
N2 C1 1.3481(16) . ?
N2 C3 1.3839(17) . ?
N2 C23 1.4524(16) . ?
C1 C4 1.4663(17) . ?
C2 H2 0.9500 . ?
C2 C3 1.3507(19) . ?
C3 H3 0.9500 . ?
C4 C5 1.3976(18) . ?
C4 C9 1.3955(18) . ?
C5 H5 0.9500 . ?
C5 C6 1.3921(19) . ?
C6 C7 1.394(2) . ?
C6 C10 1.507(2) . ?
C7 H7 0.9500 . ?
C7 C8 1.387(2) . ?
C8 H8 0.9500 . ?
C8 C9 1.3902(18) . ?
C9 H9 0.9500 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C10 H10D 0.9800 . ?
C10 H10E 0.9800 . ?
C10 H10F 0.9800 . ?
C11 C12 1.3993(19) . ?
C11 C16 1.3971(19) . ?
C12 C13 1.3963(19) . ?
C12 C17 1.518(2) . ?
C13 H13 0.9500 . ?
C13 C14 1.384(2) . ?
C14 H14 0.9500 . ?
C14 C15 1.386(2) . ?
C15 H15 0.9500 . ?
C15 C16 1.3942(18) . ?
C16 C20 1.5223(19) . ?
C17 H17 1.0000 . ?
C17 C18 1.526(2) . ?
C17 C19 1.527(2) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20 1.0000 . ?
C20 C21 1.532(2) . ?
C20 C22 1.535(2) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C24 1.3982(18) . ?
C23 C28 1.3962(18) . ?
C24 C25 1.3975(19) . ?
C24 C29 1.5179(19) . ?
C25 H25 0.9500 . ?
C25 C26 1.384(2) . ?
C26 H26 0.9500 . ?
C26 C27 1.385(2) . ?
C27 H27 0.9500 . ?
C27 C28 1.3949(18) . ?
C28 C32 1.5218(18) . ?
C29 H29 1.0000 . ?
C29 C30 1.528(2) . ?
C29 C31 1.532(2) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32 1.0000 . ?
C32 C33 1.531(2) . ?
C32 C34 1.532(2) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?

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 N1 C2 109.31(11) . . ?
C1 N1 C11 126.42(11) . . ?
C2 N1 C11 124.05(11) . . ?
C1 N2 C3 109.47(11) . . ?
C1 N2 C23 125.15(11) . . ?
C3 N2 C23 124.38(11) . . ?
N1 C1 N2 107.03(11) . . ?
N1 C1 C4 126.66(11) . . ?
N2 C1 C4 126.22(11) . . ?
N1 C2 H2 126.4 . . ?
C3 C2 N1 107.23(12) . . ?
C3 C2 H2 126.4 . . ?
N2 C3 H3 126.5 . . ?
C2 C3 N2 106.96(11) . . ?
C2 C3 H3 126.5 . . ?
C5 C4 C1 118.72(12) . . ?
C9 C4 C1 121.21(12) . . ?
C9 C4 C5 120.06(12) . . ?
C4 C5 H5 119.4 . . ?
C6 C5 C4 121.14(13) . . ?
C6 C5 H5 119.4 . . ?
C5 C6 C7 117.87(13) . . ?
C5 C6 C10 120.67(13) . . ?
C7 C6 C10 121.46(13) . . ?
C6 C7 H7 119.2 . . ?
C8 C7 C6 121.63(13) . . ?
C8 C7 H7 119.2 . . ?
C7 C8 H8 119.9 . . ?
C7 C8 C9 120.15(13) . . ?
C9 C8 H8 119.9 . . ?
C4 C9 H9 120.4 . . ?
C8 C9 C4 119.16(12) . . ?
C8 C9 H9 120.4 . . ?
C6 C10 H10A 109.5 . . ?
C6 C10 H10B 109.5 . . ?
C6 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
H10D C10 H10E 109.5 . . ?
H10D C10 H10F 109.5 . . ?
H10E C10 H10F 109.5 . . ?
C12 C11 N1 117.81(12) . . ?
C16 C11 N1 118.19(12) . . ?
C16 C11 C12 123.91(12) . . ?
C11 C12 C17 122.99(12) . . ?
C13 C12 C11 116.92(13) . . ?
C13 C12 C17 120.06(12) . . ?
C12 C13 H13 119.7 . . ?
C14 C13 C12 120.64(13) . . ?
C14 C13 H13 119.7 . . ?
C13 C14 H14 119.6 . . ?
C13 C14 C15 120.84(13) . . ?
C15 C14 H14 119.6 . . ?
C14 C15 H15 119.5 . . ?
C14 C15 C16 120.94(13) . . ?
C16 C15 H15 119.5 . . ?
C11 C16 C20 123.51(12) . . ?
C15 C16 C11 116.74(12) . . ?
C15 C16 C20 119.72(13) . . ?
C12 C17 H17 108.1 . . ?
C12 C17 C18 109.79(13) . . ?
C12 C17 C19 111.52(13) . . ?
C18 C17 H17 108.1 . . ?
C18 C17 C19 110.97(16) . . ?
C19 C17 H17 108.1 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C16 C20 H20 108.1 . . ?
C16 C20 C21 111.93(12) . . ?
C16 C20 C22 110.16(12) . . ?
C21 C20 H20 108.1 . . ?
C21 C20 C22 110.38(13) . . ?
C22 C20 H20 108.1 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C24 C23 N2 116.96(11) . . ?
C28 C23 N2 119.22(11) . . ?
C28 C23 C24 123.79(12) . . ?
C23 C24 C29 123.21(12) . . ?
C25 C24 C23 116.85(12) . . ?
C25 C24 C29 119.87(12) . . ?
C24 C25 H25 119.6 . . ?
C26 C25 C24 120.80(13) . . ?
C26 C25 H25 119.6 . . ?
C25 C26 H26 119.7 . . ?
C25 C26 C27 120.68(13) . . ?
C27 C26 H26 119.7 . . ?
C26 C27 H27 119.6 . . ?
C26 C27 C28 120.89(13) . . ?
C28 C27 H27 119.6 . . ?
C23 C28 C32 123.04(12) . . ?
C27 C28 C23 116.91(12) . . ?
C27 C28 C32 119.99(12) . . ?
C24 C29 H29 108.1 . . ?
C24 C29 C30 112.07(12) . . ?
C24 C29 C31 109.63(13) . . ?
C30 C29 H29 108.1 . . ?
C30 C29 C31 110.79(15) . . ?
C31 C29 H29 108.1 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C28 C32 H32 108.2 . . ?
C28 C32 C33 110.15(12) . . ?
C28 C32 C34 111.85(12) . . ?
C33 C32 H32 108.2 . . ?
C33 C32 C34 109.99(13) . . ?
C34 C32 H32 108.2 . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C32 C34 H34A 109.5 . . ?
C32 C34 H34B 109.5 . . ?
C32 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?

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
N1 C1 C4 C5 123.93(15) . . . . ?
N1 C1 C4 C9 -54.85(19) . . . . ?
N1 C2 C3 N2 0.58(16) . . . . ?
N1 C11 C12 C13 -175.03(11) . . . . ?
N1 C11 C12 C17 2.89(19) . . . . ?
N1 C11 C16 C15 175.67(11) . . . . ?
N1 C11 C16 C20 -2.68(19) . . . . ?
N2 C1 C4 C5 -52.27(19) . . . . ?
N2 C1 C4 C9 128.95(14) . . . . ?
N2 C23 C24 C25 179.05(11) . . . . ?
N2 C23 C24 C29 -4.11(18) . . . . ?
N2 C23 C28 C27 179.82(11) . . . . ?
N2 C23 C28 C32 2.47(18) . . . . ?
C1 N1 C2 C3 -0.83(16) . . . . ?
C1 N1 C11 C12 -81.18(17) . . . . ?
C1 N1 C11 C16 102.37(16) . . . . ?
C1 N2 C3 C2 -0.15(16) . . . . ?
C1 N2 C23 C24 -76.82(16) . . . . ?
C1 N2 C23 C28 105.07(15) . . . . ?
C1 C4 C5 C6 -178.64(12) . . . . ?
C1 C4 C9 C8 178.94(12) . . . . ?
C2 N1 C1 N2 0.73(15) . . . . ?
C2 N1 C1 C4 -176.07(13) . . . . ?
C2 N1 C11 C12 92.77(16) . . . . ?
C2 N1 C11 C16 -83.69(17) . . . . ?
C3 N2 C1 N1 -0.36(15) . . . . ?
C3 N2 C1 C4 176.45(13) . . . . ?
C3 N2 C23 C24 90.49(16) . . . . ?
C3 N2 C23 C28 -87.62(16) . . . . ?
C4 C5 C6 C7 0.0(2) . . . . ?
C4 C5 C6 C10 -179.93(14) . . . . ?
C5 C4 C9 C8 0.17(19) . . . . ?
C5 C6 C7 C8 -0.6(2) . . . . ?
C6 C7 C8 C9 0.9(2) . . . . ?
C7 C8 C9 C4 -0.7(2) . . . . ?
C9 C4 C5 C6 0.2(2) . . . . ?
C10 C6 C7 C8 179.40(15) . . . . ?
C11 N1 C1 N2 175.42(12) . . . . ?
C11 N1 C1 C4 -1.4(2) . . . . ?
C11 N1 C2 C3 -175.67(13) . . . . ?
C11 C12 C13 C14 -0.9(2) . . . . ?
C11 C12 C17 C18 -105.16(16) . . . . ?
C11 C12 C17 C19 131.42(17) . . . . ?
C11 C16 C20 C21 -132.75(14) . . . . ?
C11 C16 C20 C22 104.03(16) . . . . ?
C12 C11 C16 C15 -0.6(2) . . . . ?
C12 C11 C16 C20 -178.90(13) . . . . ?
C12 C13 C14 C15 0.1(2) . . . . ?
C13 C12 C17 C18 72.70(17) . . . . ?
C13 C12 C17 C19 -50.7(2) . . . . ?
C13 C14 C15 C16 0.6(2) . . . . ?
C14 C15 C16 C11 -0.4(2) . . . . ?
C14 C15 C16 C20 178.03(13) . . . . ?
C15 C16 C20 C21 48.95(18) . . . . ?
C15 C16 C20 C22 -74.26(17) . . . . ?
C16 C11 C12 C13 1.2(2) . . . . ?
C16 C11 C12 C17 179.13(13) . . . . ?
C17 C12 C13 C14 -178.92(13) . . . . ?
C23 N2 C1 N1 168.55(12) . . . . ?
C23 N2 C1 C4 -14.6(2) . . . . ?
C23 N2 C3 C2 -169.17(13) . . . . ?
C23 C24 C25 C26 1.6(2) . . . . ?
C23 C24 C29 C30 120.29(15) . . . . ?
C23 C24 C29 C31 -116.26(17) . . . . ?
C23 C28 C32 C33 99.94(16) . . . . ?
C23 C28 C32 C34 -137.41(13) . . . . ?
C24 C23 C28 C27 1.85(19) . . . . ?
C24 C23 C28 C32 -175.50(12) . . . . ?
C24 C25 C26 C27 0.8(2) . . . . ?
C25 C24 C29 C30 -62.96(17) . . . . ?
C25 C24 C29 C31 60.50(19) . . . . ?
C25 C26 C27 C28 -2.0(2) . . . . ?
C26 C27 C28 C23 0.67(19) . . . . ?
C26 C27 C28 C32 178.10(13) . . . . ?
C27 C28 C32 C33 -77.33(17) . . . . ?
C27 C28 C32 C34 45.32(17) . . . . ?
C28 C23 C24 C25 -2.94(19) . . . . ?
C28 C23 C24 C29 173.90(12) . . . . ?
C29 C24 C25 C26 -175.39(13) . . . . ?

_olex2_date_sample_data_collection 2019-04-12
_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
;
####################################################################### 
# 
# 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_compound4a
_database_code_depnum_ccdc_archive 'CCDC 1939609'
loop_
_audit_author_name
_audit_author_address
'Hans Georg Stammler'
;University of Bielefeld
Germany
;
_audit_update_record             
;
2019-07-10 deposited with the CCDC.	2019-10-18 downloaded from the CCDC.
;


_audit_creation_date             2018-11-05
_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         'C33 H39 N2 P3'
_chemical_formula_sum            'C33 H39 N2 P3'
_chemical_formula_weight         556.57
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C33 H39 N2 P3'
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           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   10.5947(8)
_cell_length_b                   16.2615(8)
_cell_length_c                   17.8991(13)
_cell_angle_alpha                90
_cell_angle_beta                 97.414(7)
_cell_angle_gamma                90
_cell_volume                     3058.0(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2925
_cell_measurement_temperature    99.9(3)
_cell_measurement_theta_max      76.4040
_cell_measurement_theta_min      5.0190
_shelx_estimated_absorpt_T_max   0.962
_shelx_estimated_absorpt_T_min   0.727
_exptl_absorpt_coefficient_mu    1.959
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.755
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.209
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1184
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 0 0.0838
-1 0 0 0.0838
0 -1 1 0.0098
0 1 -1 0.0098
0 1 1 0.0151
0 -1 -1 0.0151

_exptl_crystal_size_max          0.174
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.9995 -0.0038 -0.4356 0.0199 0.1409 0.0350
-0.9995 0.0038 0.4356 -0.0199 -0.1409 -0.0350
-0.0018 -0.9997 0.9986 -0.1283 0.0066 -0.0005
0.0018 0.9997 -0.9986 0.1283 -0.0066 0.0005
0.0016 0.9978 0.9975 0.0126 0.0180 -0.1262
-0.0016 -0.9978 -0.9975 -0.0126 -0.0180 0.1262

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?

_diffrn_reflns_number            17147
_diffrn_reflns_av_R_equivalents  0.0747
_diffrn_reflns_av_sigmaI/netI    0.0869

_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.546
_diffrn_reflns_theta_min         4.983
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.9(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -88.00 -15.00   1.00   55.50    --  -38.50 -57.00 -60.00   73
  2  ω   -115.00 -26.00   1.00   55.50    --  -38.50 -19.00   0.00   89
  3  ω    -63.00  29.00   1.00   55.50    --  -38.50  57.00 120.00   92
  4  ω     19.00  54.00   1.00   55.50    --   43.20  77.00 -60.00   35
  5  ω     57.00 127.00   1.00   55.50    --   43.20 178.00 -60.00   70
  6  ω     88.00 115.00   1.00   55.50    --   43.20  77.00 -60.00   27
  7  ω    102.00 127.00   1.00   55.50    --   43.20 178.00-180.00   25
  8  ω     69.00 117.00   1.00  111.00    --  111.00-125.00 150.00   48
  9  ω     42.00  67.00   1.00  111.00    --  111.00-125.00 -60.00   25
 10  ω     56.00 105.00   1.00  111.00    --  111.00 -77.00   0.00   49
 11  ω     41.00 117.00   1.00  111.00    --  111.00-125.00-150.00   76
 12  ω     38.00 118.00   1.00  111.00    --  111.00 -30.00 -60.00   80
 13  ω     90.00 152.00   1.00  111.00    --  111.00  30.00-120.00   62
 14  ω     82.00 172.00   1.00  111.00    --  111.00  77.00 -90.00   90
 15  ω     45.00 135.00   1.00  111.00    --  111.00 -61.00-150.00   90
 16  ω     61.00 117.00   1.00  111.00    --  111.00-125.00  30.00   56
 17  ω     45.00 120.00   1.00  111.00    --  111.00 -45.00  30.00   75
 18  ω    129.00 155.00   1.00  111.00    --  111.00  30.00-150.00   26
 19  ω    102.00 178.00   1.00  111.00    --  111.00  45.00 -30.00   76
 20  ω     90.00 117.00   1.00  111.00    --  111.00-125.00 -30.00   27
 21  ω     95.00 127.00   1.00  111.00    --  111.00 125.00-150.00   32
 22  ω     43.00 106.00   1.00  111.00    --  111.00 -77.00-180.00   63
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0050853000
_diffrn_orient_matrix_UB_12      0.0705067000
_diffrn_orient_matrix_UB_13      -0.0578821000
_diffrn_orient_matrix_UB_21      0.1463634000
_diffrn_orient_matrix_UB_22      0.0054573000
_diffrn_orient_matrix_UB_23      0.0123777000
_diffrn_orient_matrix_UB_31      0.0070472000
_diffrn_orient_matrix_UB_32      -0.0630012000
_diffrn_orient_matrix_UB_33      -0.0635574000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3981
_reflns_number_total             5324
_reflns_special_details          
;
 _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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.323
_refine_diff_density_min         -0.312
_refine_diff_density_rms         0.069
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         5324
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0610
_refine_ls_R_factor_gt           0.0437
_refine_ls_restrained_S_all      1.068
_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)+(0.0735P)²+0.0459P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1184
_refine_ls_wR_factor_ref         0.1298
_refine_special_details          
'Refined as a 2-component twin. Component 2 rotated by 179.8773°  around [0.98 0.00 -0.21] (reciprocal) or [1.00 -0.00 0.00] (direct). BASF 0.4067'
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.5933(14)
 0.4067(14)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Ternary CH refined with riding coordinates:
 C9(H9), C12(H12)
3.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C16(H16), C17(H17), C18(H18)
3.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C13(H13A,H13B,H13C), C14(H14A,H14B,
 H14C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
P1 P 0.48047(8) 0.83165(5) 0.65664(4) 0.02415(18) Uani 1 1 d . . . . .
P2 P 0.500000 0.91130(7) 0.750000 0.0256(2) Uani 1 2 d S T P . .
N1 N 0.4870(2) 0.65824(14) 0.68872(11) 0.0186(4) Uani 1 1 d . . . . .
C1 C 0.4918(3) 0.74116(16) 0.71069(14) 0.0191(5) Uani 1 1 d . . . . .
C2 C 0.500000 0.6097(2) 0.750000 0.0186(7) Uani 1 2 d S T P . .
C3 C 0.4830(3) 0.63244(16) 0.61097(14) 0.0187(5) Uani 1 1 d . . . . .
C4 C 0.3646(3) 0.61729(17) 0.56898(15) 0.0207(6) Uani 1 1 d . . . . .
C5 C 0.3645(3) 0.60067(18) 0.49241(15) 0.0227(6) Uani 1 1 d . . . . .
H5 H 0.287798 0.590730 0.462272 0.027 Uiso 1 1 calc R . . . .
C6 C 0.4765(3) 0.59877(19) 0.46085(15) 0.0238(6) Uani 1 1 d . . . . .
H6 H 0.474247 0.588180 0.409636 0.029 Uiso 1 1 calc R . . . .
C7 C 0.5921(3) 0.61242(18) 0.50444(15) 0.0225(6) Uani 1 1 d . . . . .
H7 H 0.666799 0.610214 0.482306 0.027 Uiso 1 1 calc R . . . .
C8 C 0.5981(3) 0.62944(17) 0.58113(15) 0.0201(6) Uani 1 1 d . . . . .
C9 C 0.2405(3) 0.62023(19) 0.60283(16) 0.0240(6) Uani 1 1 d . . . . .
H9 H 0.261699 0.621623 0.657754 0.029 Uiso 1 1 calc R . . . .
C10 C 0.1656(3) 0.6980(2) 0.57927(18) 0.0319(7) Uani 1 1 d . . . . .
H10A H 0.216784 0.745381 0.594266 0.048 Uiso 1 1 calc GR . . . .
H10B H 0.089504 0.699423 0.603149 0.048 Uiso 1 1 calc GR . . . .
H10C H 0.143263 0.698319 0.525559 0.048 Uiso 1 1 calc GR . . . .
C11 C 0.1600(3) 0.5435(2) 0.58289(19) 0.0332(7) Uani 1 1 d . . . . .
H11A H 0.127327 0.544601 0.530314 0.050 Uiso 1 1 calc GR . . . .
H11B H 0.090451 0.542248 0.612337 0.050 Uiso 1 1 calc GR . . . .
H11C H 0.211682 0.495338 0.593469 0.050 Uiso 1 1 calc GR . . . .
C12 C 0.7257(3) 0.6453(2) 0.62813(16) 0.0256(6) Uani 1 1 d . . . . .
H12 H 0.710365 0.653706 0.680421 0.031 Uiso 1 1 calc R . . . .
C13 C 0.7897(3) 0.7227(2) 0.60245(19) 0.0336(7) Uani 1 1 d . . . . .
H13A H 0.813490 0.713856 0.553099 0.050 Uiso 1 1 calc GR . . . .
H13B H 0.864371 0.734636 0.637126 0.050 Uiso 1 1 calc GR . . . .
H13C H 0.731611 0.768088 0.601007 0.050 Uiso 1 1 calc GR . . . .
C14 C 0.8143(3) 0.5714(2) 0.62635(18) 0.0341(7) Uani 1 1 d . . . . .
H14A H 0.771755 0.522685 0.640293 0.051 Uiso 1 1 calc GR . . . .
H14B H 0.889879 0.580116 0.661202 0.051 Uiso 1 1 calc GR . . . .
H14C H 0.836913 0.564915 0.576449 0.051 Uiso 1 1 calc GR . . . .
C15 C 0.500000 0.5189(2) 0.750000 0.0191(7) Uani 1 2 d S T P . .
C16 C 0.3852(3) 0.47573(17) 0.74265(16) 0.0242(6) Uani 1 1 d . . . . .
H16 H 0.308408 0.504125 0.737792 0.029 Uiso 1 1 calc R . . . .
C17 C 0.3857(3) 0.39082(18) 0.74259(17) 0.0281(6) Uani 1 1 d . . . . .
H17 H 0.309199 0.362105 0.737574 0.034 Uiso 1 1 calc R . . . .
C18 C 0.500000 0.3483(2) 0.750000 0.0261(8) Uani 1 2 d S T P . .
H18 H 0.500002 0.291084 0.750000 0.031 Uiso 1 2 calc RS T P . .


_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
P1 P2 2.1032(10) . ?
P1 C1 1.757(3) . ?
N1 C1 1.404(3) . ?
N1 C2 1.344(3) . ?
N1 C3 1.449(3) . ?
C1 C1 1.395(5) 2_656 ?
C2 C15 1.476(5) . ?
C3 C4 1.399(4) . ?
C3 C8 1.394(4) . ?
C4 C5 1.397(4) . ?
C4 C9 1.518(4) . ?
C5 H5 0.9300 . ?
C5 C6 1.379(4) . ?
C6 H6 0.9300 . ?
C6 C7 1.383(4) . ?
C7 H7 0.9300 . ?
C7 C8 1.394(4) . ?
C8 C12 1.519(4) . ?
C9 H9 0.9800 . ?
C9 C10 1.524(4) . ?
C9 C11 1.527(4) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 H12 0.9800 . ?
C12 C13 1.528(4) . ?
C12 C14 1.528(4) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 C16 1.396(3) 2_656 ?
C15 C16 1.396(3) . ?
C16 H16 0.9300 . ?
C16 C17 1.381(4) . ?
C17 H17 0.9300 . ?
C17 C18 1.386(4) . ?
C18 H18 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 P2 94.91(9) . . ?
P1 P2 P1 103.98(6) . 2_656 ?
C1 N1 C3 122.9(2) . . ?
C2 N1 C1 109.8(2) . . ?
C2 N1 C3 127.0(2) . . ?
N1 C1 P1 130.76(19) . . ?
C1 C1 P1 123.11(9) 2_656 . ?
C1 C1 N1 106.13(13) 2_656 . ?
N1 C2 N1 108.1(3) . 2_656 ?
N1 C2 C15 125.95(16) 2_656 . ?
N1 C2 C15 125.95(16) . . ?
C4 C3 N1 118.7(2) . . ?
C8 C3 N1 117.4(2) . . ?
C8 C3 C4 123.8(2) . . ?
C3 C4 C9 122.9(2) . . ?
C5 C4 C3 116.6(3) . . ?
C5 C4 C9 120.5(3) . . ?
C4 C5 H5 119.5 . . ?
C6 C5 C4 121.0(3) . . ?
C6 C5 H5 119.5 . . ?
C5 C6 H6 119.6 . . ?
C5 C6 C7 120.8(3) . . ?
C7 C6 H6 119.6 . . ?
C6 C7 H7 119.6 . . ?
C6 C7 C8 120.8(3) . . ?
C8 C7 H7 119.6 . . ?
C3 C8 C7 117.0(3) . . ?
C3 C8 C12 122.8(2) . . ?
C7 C8 C12 120.2(3) . . ?
C4 C9 H9 107.6 . . ?
C4 C9 C10 111.3(3) . . ?
C4 C9 C11 111.5(3) . . ?
C10 C9 H9 107.6 . . ?
C10 C9 C11 111.0(3) . . ?
C11 C9 H9 107.6 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C8 C12 H12 107.9 . . ?
C8 C12 C13 111.8(2) . . ?
C8 C12 C14 111.1(3) . . ?
C13 C12 H12 107.9 . . ?
C13 C12 C14 110.1(3) . . ?
C14 C12 H12 107.9 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C16 C15 C2 120.23(18) 2_656 . ?
C16 C15 C2 120.23(18) . . ?
C16 C15 C16 119.5(4) 2_656 . ?
C15 C16 H16 120.0 . . ?
C17 C16 C15 120.0(3) . . ?
C17 C16 H16 120.0 . . ?
C16 C17 H17 119.9 . . ?
C16 C17 C18 120.2(3) . . ?
C18 C17 H17 119.9 . . ?
C17 C18 C17 120.1(4) . 2_656 ?
C17 C18 H18 120.0 . . ?
C17 C18 H18 120.0 2_656 . ?

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
P2 P1 C1 N1 179.9(3) . . . . ?
P2 P1 C1 C1 0.0(3) . . . 2_656 ?
N1 C2 C15 C16 96.02(18) . . . 2_656 ?
N1 C2 C15 C16 -83.98(18) 2_656 . . 2_656 ?
N1 C2 C15 C16 -83.98(18) . . . . ?
N1 C2 C15 C16 96.02(18) 2_656 . . . ?
N1 C3 C4 C5 173.7(2) . . . . ?
N1 C3 C4 C9 -4.9(4) . . . . ?
N1 C3 C8 C7 -173.9(2) . . . . ?
N1 C3 C8 C12 4.9(4) . . . . ?
C1 N1 C2 N1 0.07(14) . . . 2_656 ?
C1 N1 C2 C15 -179.93(14) . . . . ?
C1 N1 C3 C4 -94.4(3) . . . . ?
C1 N1 C3 C8 81.5(3) . . . . ?
C2 N1 C1 P1 179.96(18) . . . . ?
C2 N1 C1 C1 -0.2(4) . . . 2_656 ?
C2 N1 C3 C4 93.0(3) . . . . ?
C2 N1 C3 C8 -91.0(3) . . . . ?
C2 C15 C16 C17 179.9(2) . . . . ?
C3 N1 C1 P1 6.3(4) . . . . ?
C3 N1 C1 C1 -173.8(3) . . . 2_656 ?
C3 N1 C2 N1 173.4(3) . . . 2_656 ?
C3 N1 C2 C15 -6.6(3) . . . . ?
C3 C4 C5 C6 0.6(4) . . . . ?
C3 C4 C9 C10 105.1(3) . . . . ?
C3 C4 C9 C11 -130.3(3) . . . . ?
C3 C8 C12 C13 -115.0(3) . . . . ?
C3 C8 C12 C14 121.6(3) . . . . ?
C4 C3 C8 C7 1.8(4) . . . . ?
C4 C3 C8 C12 -179.4(3) . . . . ?
C4 C5 C6 C7 0.7(5) . . . . ?
C5 C4 C9 C10 -73.4(4) . . . . ?
C5 C4 C9 C11 51.1(4) . . . . ?
C5 C6 C7 C8 -0.8(5) . . . . ?
C6 C7 C8 C3 -0.4(4) . . . . ?
C6 C7 C8 C12 -179.3(3) . . . . ?
C7 C8 C12 C13 63.8(4) . . . . ?
C7 C8 C12 C14 -59.6(4) . . . . ?
C8 C3 C4 C5 -1.9(4) . . . . ?
C8 C3 C4 C9 179.5(3) . . . . ?
C9 C4 C5 C6 179.3(3) . . . . ?
C15 C16 C17 C18 0.2(4) . . . . ?
C16 C15 C16 C17 -0.1(2) 2_656 . . . ?
C16 C17 C18 C17 -0.1(2) . . . 2_656 ?

_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 1.345
_oxdiff_exptl_absorpt_empirical_full_min 0.833
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_oxdiff_twin_reflns_isolated
_oxdiff_twin_reflns_overlapped
_twin_individual_twin_lattice_type
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.5933(14) 4914 7329 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000
0.0000 1.0000
2 0.4067(14) 4904 7329 nmt 1.0004 0.0000 -0.0000 -0.0000 -1.0001 -0.0010
-0.4354 0.0023 -0.9992

_twin_special_details            
;
Component 2 rotated by 179.8773° 
 around [0.98 0.00 -0.21] (reciprocal) or [1.00 -0.00 0.00] (direct)
;
####################################################################### 
# 
# 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_compound4c
_database_code_depnum_ccdc_archive 'CCDC 1939611'
loop_
_audit_author_name
_audit_author_address
'Hans Georg Stammler'
;University of Bielefeld
Germany
;
_audit_update_record             
;
2019-07-10 deposited with the CCDC.	2019-10-18 downloaded from the CCDC.
;



_audit_creation_date             2018-10-23
_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         'C34 H41 N2 P3, C7 H8'
_chemical_formula_sum            'C41 H49 N2 P3'
_chemical_formula_weight         662.73
_chemical_absolute_configuration ad
_chemical_melting_point          ?
_chemical_oxdiff_formula         C41H49N2P3
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      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, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   11.1499(5)
_cell_length_b                   17.6614(8)
_cell_length_c                   19.2232(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3785.5(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    14670
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      76.1140
_cell_measurement_theta_min      3.3750
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.659
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.855
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.163
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1416
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
2 -11 -2 0.0561
3 -10 3 0.0586
1 7 9 0.0740
-3 10 -2 0.0441
-3 6 -9 0.0531
-2 -3 -12 0.0555
-1 -8 9 0.0653
5 6 -7 0.0140
-7 2 -1 0.0351
3 -7 8 0.0772
-6 -3 -6 0.0486
6 -2 8 0.0837
7 -3 1 0.0498
-1 -4 12 0.0695

_exptl_crystal_size_max          0.153
_exptl_crystal_size_mid          0.108
_exptl_crystal_size_min          0.087
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
1.8140 -10.9341 -2.1511 0.2225 -0.7515 0.6211
2.8642 -10.1880 2.9969 0.1241 -0.4212 0.8984
0.6112 7.4909 9.3723 -0.2838 0.9556 0.0795
-2.7061 10.4883 -2.0521 -0.1450 0.4912 -0.8589
-3.3681 5.9567 -8.9668 0.0474 -0.1563 -0.9866
-2.1472 -2.6583 -11.5492 0.2374 -0.7979 -0.5540
-1.3352 -7.8708 8.7717 -0.5952 -0.1759 0.7841
4.7629 5.7977 -6.9309 0.8946 0.2652 -0.3597
-7.1385 1.7235 -0.9973 -0.7666 -0.2282 -0.6001
2.9879 -6.9989 8.0047 -0.0568 0.0268 0.9734
-5.9886 -3.0158 -6.0004 -0.4504 -0.7262 -0.5071
5.9858 -1.9882 8.0032 0.3257 0.4851 0.8846
6.9914 -2.9863 1.0058 0.7400 0.1384 0.6617
-1.0114 -4.0060 11.9996 -0.6703 0.2435 0.7470

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0500
_diffrn_reflns_av_unetI/netI     0.0417
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            31369
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.768
_diffrn_reflns_theta_min         3.398
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -122.00 -35.00   1.00    8.00    --  -38.50-178.00  30.00   87
  2  ω   -110.00 -18.00   1.00    8.00    --  -38.50 -38.00 150.00   92
  3  ω   -123.00 -34.00   1.00    8.00    --  -38.50 178.00 150.00   89
  4  ω     57.00 127.00   1.00    8.00    --   43.20 178.00  90.00   70
  5  ω     85.00 178.00   1.00   32.00    --  111.00  61.00 120.00   93
  6  ω     31.00 110.00   1.00   32.00    --  111.00 -94.00  60.00   79
  7  ω     94.00 178.00   1.00   32.00    --  111.00 125.00 -90.00   84
  8  ω     81.00 178.00   1.00   32.00    --  111.00  77.00-180.00   97
  9  ω     41.00 118.00   1.00   32.00    --  111.00-125.00 -30.00   77
 10  ω     41.00 118.00   1.00   32.00    --  111.00-125.00-150.00   77
 11  ω     31.00 110.00   1.00   32.00    --  111.00 -94.00-180.00   79
 12  ω     90.00 178.00   1.00   32.00    --  111.00  30.00-120.00   88
 13  ω     13.00 115.00   1.00    8.00    --   43.20  77.00   0.00  102
 14  ω     18.00 112.00   1.00    8.00    --   43.20  57.00 120.00   94
 15  ω     18.00 112.00   1.00    8.00    --   43.20  57.00 -90.00   94
 16  ω     71.00 141.00   1.00   32.00    --  111.00  15.00  60.00   70
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1152783000
_diffrn_orient_matrix_UB_12      0.0073722000
_diffrn_orient_matrix_UB_13      -0.0436866000
_diffrn_orient_matrix_UB_21      0.0416141000
_diffrn_orient_matrix_UB_22      0.0665810000
_diffrn_orient_matrix_UB_23      0.0460297000
_diffrn_orient_matrix_UB_31      0.0637426000
_diffrn_orient_matrix_UB_32      -0.0558597000
_diffrn_orient_matrix_UB_33      0.0489742000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.780
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.963
_reflns_number_gt                7012
_reflns_number_total             7770
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_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 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.295
_refine_diff_density_min         -0.446
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details 
;
 Flack x determined using 2682 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.024(12)
_refine_ls_extinction_coef       0.00082(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     491
_refine_ls_number_reflns         7770
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.0509
_refine_ls_restrained_S_all      1.037
_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)+(0.0492P)²+2.6152P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1214
_refine_ls_wR_factor_ref         0.1253
_refine_special_details          
'Hydrogen atoms were taken into account using a riding model. One solvent toluene molecule is disordered with ratio 58:42'
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(C35B)=Sof(C36B)=Sof(H36B)=Sof(C37B)=Sof(H37B)=Sof(C38B)=Sof(H38B)=
 Sof(C39B)=Sof(H39B)=Sof(C40B)=Sof(H40B)=Sof(C41B)=Sof(H41D)=Sof(H41E)=
 Sof(H41F)=1-FVAR(1)
 Sof(C35A)=Sof(C36A)=Sof(H36A)=Sof(C37A)=Sof(H37A)=Sof(C38A)=Sof(H38A)=
 Sof(C39A)=Sof(H39A)=Sof(C40A)=Sof(H40A)=Sof(C41A)=Sof(H41A)=Sof(H41B)=
 Sof(H41C)=FVAR(1)
3.a Ternary CH refined with riding coordinates:
 C17(H17), C20(H20), C29(H29), C32(H32)
3.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C8(H8), C9(H9), C13(H13), C14(H14), C15(H15), C25(H25),
 C26(H26), C27(H27), C36A(H36A), C37A(H37A), C38A(H38A), C39A(H39A), C40A(H40A),
  C36B(H36B), C37B(H37B), C38B(H38B), C39B(H39B), C40B(H40B)
3.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C21(H21A,H21B,
 H21C), C22(H22A,H22B,H22C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C33(H33A,
 H33B,H33C), C34(H34A,H34B,H34C), C41A(H41A,H41B,H41C), C41B(H41D,H41E,H41F)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
P1 P 0.72514(11) 0.33363(7) 0.62759(5) 0.0381(3) Uani 1 1 d . . . . .
P2 P 0.76861(11) 0.35151(7) 0.73303(5) 0.0424(3) Uani 1 1 d . . . . .
P3 P 0.63658(11) 0.42865(7) 0.76650(5) 0.0389(3) Uani 1 1 d . . . . .
N1 N 0.5176(3) 0.41081(18) 0.57443(14) 0.0289(7) Uani 1 1 d . . . . .
N2 N 0.4638(3) 0.47753(19) 0.66490(15) 0.0309(7) Uani 1 1 d . . . . .
C1 C 0.4358(4) 0.4624(2) 0.59772(17) 0.0292(8) Uani 1 1 d . . . . .
C2 C 0.6010(4) 0.3940(2) 0.62733(18) 0.0297(8) Uani 1 1 d . . . . .
C3 C 0.5641(4) 0.4348(2) 0.68569(18) 0.0327(8) Uani 1 1 d . . . . .
C4 C 0.3374(4) 0.4967(2) 0.55818(18) 0.0329(9) Uani 1 1 d . . . . .
C5 C 0.2777(4) 0.4572(2) 0.50567(18) 0.0344(8) Uani 1 1 d . . . . .
H5 H 0.299692 0.407698 0.495004 0.041 Uiso 1 1 calc R . . . .
C6 C 0.1848(4) 0.4923(3) 0.4693(2) 0.0369(9) Uani 1 1 d . . . . .
H6 H 0.145484 0.465743 0.434317 0.044 Uiso 1 1 calc R . . . .
C7 C 0.1496(5) 0.5662(3) 0.4840(2) 0.0420(10) Uani 1 1 d . . . . .
C8 C 0.2073(6) 0.6035(3) 0.5370(2) 0.0559(15) Uani 1 1 d . . . . .
H8 H 0.183116 0.652254 0.548841 0.067 Uiso 1 1 calc R . . . .
C9 C 0.3004(5) 0.5701(3) 0.5729(2) 0.0497(13) Uani 1 1 d . . . . .
H9 H 0.339147 0.597264 0.607774 0.060 Uiso 1 1 calc R . . . .
C10 C 0.0476(5) 0.6027(3) 0.4456(2) 0.0510(12) Uani 1 1 d . . . . .
H10A H 0.028671 0.573256 0.405063 0.076 Uiso 1 1 calc GR . . . .
H10B H 0.070306 0.652893 0.431783 0.076 Uiso 1 1 calc GR . . . .
H10C H -0.021346 0.605183 0.475408 0.076 Uiso 1 1 calc GR . . . .
C11 C 0.5246(4) 0.3800(2) 0.50472(17) 0.0314(8) Uani 1 1 d . . . . .
C12 C 0.5670(4) 0.4264(2) 0.45166(18) 0.0344(9) Uani 1 1 d . . . . .
C13 C 0.5693(4) 0.3956(3) 0.38410(18) 0.0374(9) Uani 1 1 d . . . . .
H13 H 0.596900 0.425000 0.347271 0.045 Uiso 1 1 calc R . . . .
C14 C 0.5315(4) 0.3231(3) 0.37187(19) 0.0374(9) Uani 1 1 d . . . . .
H14 H 0.531938 0.304061 0.326760 0.045 Uiso 1 1 calc R . . . .
C15 C 0.4924(4) 0.2778(3) 0.4263(2) 0.0349(9) Uani 1 1 d . . . . .
H15 H 0.468738 0.228244 0.417244 0.042 Uiso 1 1 calc R . . . .
C16 C 0.4880(4) 0.3050(2) 0.49461(18) 0.0309(8) Uani 1 1 d . . . . .
C17 C 0.6150(5) 0.5053(3) 0.4640(2) 0.0438(11) Uani 1 1 d . . . . .
H17 H 0.604058 0.517056 0.513392 0.053 Uiso 1 1 calc R . . . .
C18 C 0.5468(7) 0.5652(3) 0.4218(3) 0.0709(18) Uani 1 1 d . . . . .
H18A H 0.557878 0.555813 0.373041 0.106 Uiso 1 1 calc GR . . . .
H18B H 0.577043 0.614585 0.433135 0.106 Uiso 1 1 calc GR . . . .
H18C H 0.462975 0.562692 0.432879 0.106 Uiso 1 1 calc GR . . . .
C19 C 0.7492(6) 0.5079(3) 0.4485(3) 0.0636(16) Uani 1 1 d . . . . .
H19A H 0.790063 0.471432 0.476926 0.095 Uiso 1 1 calc GR . . . .
H19B H 0.779452 0.557649 0.458536 0.095 Uiso 1 1 calc GR . . . .
H19C H 0.762562 0.496416 0.400315 0.095 Uiso 1 1 calc GR . . . .
C20 C 0.4440(4) 0.2541(2) 0.55350(19) 0.0343(9) Uani 1 1 d . . . . .
H20 H 0.474764 0.274824 0.597273 0.041 Uiso 1 1 calc R . . . .
C21 C 0.4932(5) 0.1740(3) 0.5459(2) 0.0488(12) Uani 1 1 d . . . . .
H21A H 0.578687 0.176124 0.540256 0.073 Uiso 1 1 calc GR . . . .
H21B H 0.457846 0.150319 0.505967 0.073 Uiso 1 1 calc GR . . . .
H21C H 0.474144 0.145261 0.586835 0.073 Uiso 1 1 calc GR . . . .
C22 C 0.3084(4) 0.2530(3) 0.5582(2) 0.0421(10) Uani 1 1 d . . . . .
H22A H 0.279651 0.303128 0.567940 0.063 Uiso 1 1 calc GR . . . .
H22B H 0.284096 0.219396 0.594879 0.063 Uiso 1 1 calc GR . . . .
H22C H 0.275477 0.235771 0.514884 0.063 Uiso 1 1 calc GR . . . .
C23 C 0.3947(4) 0.5214(2) 0.71367(17) 0.0313(8) Uani 1 1 d . . . . .
C24 C 0.2890(4) 0.4886(2) 0.74133(19) 0.0345(9) Uani 1 1 d . . . . .
C25 C 0.2239(4) 0.5317(3) 0.78841(19) 0.0378(9) Uani 1 1 d . . . . .
H25 H 0.154451 0.511820 0.807949 0.045 Uiso 1 1 calc R . . . .
C26 C 0.2608(4) 0.6039(3) 0.80681(19) 0.0400(10) Uani 1 1 d . . . . .
H26 H 0.215227 0.632201 0.837935 0.048 Uiso 1 1 calc R . . . .
C27 C 0.3643(4) 0.6342(2) 0.77935(19) 0.0370(9) Uani 1 1 d . . . . .
H27 H 0.387676 0.682680 0.792424 0.044 Uiso 1 1 calc R . . . .
C28 C 0.4349(4) 0.5937(2) 0.73232(19) 0.0335(8) Uani 1 1 d . . . . .
C29 C 0.2481(4) 0.4089(2) 0.7222(2) 0.0394(10) Uani 1 1 d . . . . .
H29 H 0.305886 0.388278 0.688792 0.047 Uiso 1 1 calc R . . . .
C30 C 0.2497(6) 0.3585(3) 0.7864(3) 0.0631(16) Uani 1 1 d . . . . .
H30A H 0.222942 0.308618 0.774142 0.095 Uiso 1 1 calc GR . . . .
H30B H 0.197411 0.379299 0.821197 0.095 Uiso 1 1 calc GR . . . .
H30C H 0.329906 0.355808 0.804500 0.095 Uiso 1 1 calc GR . . . .
C31 C 0.1256(5) 0.4092(3) 0.6876(3) 0.0533(12) Uani 1 1 d . . . . .
H31A H 0.126155 0.443859 0.649115 0.080 Uiso 1 1 calc GR . . . .
H31B H 0.065987 0.424759 0.720702 0.080 Uiso 1 1 calc GR . . . .
H31C H 0.107190 0.359240 0.671146 0.080 Uiso 1 1 calc GR . . . .
C32 C 0.5492(4) 0.6286(3) 0.7033(2) 0.0397(10) Uani 1 1 d . . . . .
H32 H 0.586171 0.591754 0.671696 0.048 Uiso 1 1 calc R . . . .
C33 C 0.5242(6) 0.7013(3) 0.6619(3) 0.0590(14) Uani 1 1 d . . . . .
H33A H 0.468266 0.690531 0.625220 0.089 Uiso 1 1 calc GR . . . .
H33B H 0.597745 0.719765 0.642220 0.089 Uiso 1 1 calc GR . . . .
H33C H 0.491016 0.738906 0.692311 0.089 Uiso 1 1 calc GR . . . .
C34 C 0.6389(5) 0.6459(3) 0.7613(2) 0.0484(11) Uani 1 1 d . . . . .
H34A H 0.608126 0.685933 0.790046 0.073 Uiso 1 1 calc GR . . . .
H34B H 0.713911 0.661329 0.741314 0.073 Uiso 1 1 calc GR . . . .
H34C H 0.650958 0.601395 0.789118 0.073 Uiso 1 1 calc GR . . . .
C35A C 0.8759(16) 0.6912(15) 0.5928(12) 0.047(6) Uani 0.584(12) 1 d . . P A 1
C36A C 0.8177(10) 0.6219(7) 0.6013(5) 0.053(3) Uani 0.584(12) 1 d . . P A 1
H36A H 0.748027 0.609953 0.577164 0.063 Uiso 0.584(12) 1 calc R . P A 1
C37A C 0.8709(12) 0.5712(7) 0.6488(6) 0.055(3) Uani 0.584(12) 1 d . . P A 1
H37A H 0.839443 0.522624 0.652961 0.066 Uiso 0.584(12) 1 calc R . P A 1
C38A C 0.965(2) 0.5907(11) 0.6880(10) 0.065(5) Uani 0.584(12) 1 d . . P A 1
H38A H 0.997700 0.557668 0.720663 0.078 Uiso 0.584(12) 1 calc R . P A 1
C39A C 1.0124(17) 0.6624(16) 0.6778(12) 0.075(10) Uani 0.584(12) 1 d . . P A 1
H39A H 1.078616 0.676676 0.704095 0.090 Uiso 0.584(12) 1 calc R . P A 1
C40A C 0.9694(11) 0.7109(7) 0.6336(6) 0.056(3) Uani 0.584(12) 1 d . . P A 1
H40A H 1.002890 0.758939 0.630008 0.067 Uiso 0.584(12) 1 calc R . P A 1
C41A C 0.8188(12) 0.7477(7) 0.5415(5) 0.079(4) Uani 0.584(12) 1 d . . P A 1
H41A H 0.754782 0.723357 0.516747 0.119 Uiso 0.584(12) 1 calc GR . P A 1
H41B H 0.878438 0.764753 0.509013 0.119 Uiso 0.584(12) 1 calc GR . P A 1
H41C H 0.787741 0.790343 0.566722 0.119 Uiso 0.584(12) 1 calc GR . P A 1
C35B C 0.9003(12) 0.6101(9) 0.6308(7) 0.043(3) Uani 0.416(12) 1 d . . P A 2
C36B C 0.988(2) 0.6220(15) 0.6780(10) 0.048(7) Uani 0.416(12) 1 d . . P A 2
H36B H 1.008563 0.582758 0.707856 0.057 Uiso 0.416(12) 1 calc R . P A 2
C37B C 1.0461(19) 0.6883(15) 0.6835(12) 0.047(5) Uani 0.416(12) 1 d . . P A 2
H37B H 1.112600 0.693526 0.712333 0.056 Uiso 0.416(12) 1 calc R . P A 2
C38B C 1.0025(17) 0.7498(11) 0.6437(6) 0.055(4) Uani 0.416(12) 1 d . . P A 2
H38B H 1.036055 0.797525 0.650213 0.066 Uiso 0.416(12) 1 calc R . P A 2
C39B C 0.9125(17) 0.7413(10) 0.5960(7) 0.054(4) Uani 0.416(12) 1 d . . P A 2
H39B H 0.895677 0.781279 0.566101 0.064 Uiso 0.416(12) 1 calc R . P A 2
C40B C 0.843(3) 0.674(2) 0.5902(18) 0.052(7) Uani 0.416(12) 1 d . . P A 2
H40B H 0.772611 0.669459 0.564743 0.063 Uiso 0.416(12) 1 calc R . P A 2
C41B C 0.8447(14) 0.5328(10) 0.6236(8) 0.060(4) Uani 0.416(12) 1 d . . P A 2
H41D H 0.900607 0.499254 0.601409 0.090 Uiso 0.416(12) 1 calc GR . P A 2
H41E H 0.773199 0.536333 0.596031 0.090 Uiso 0.416(12) 1 calc GR . P A 2
H41F H 0.824963 0.513499 0.668894 0.090 Uiso 0.416(12) 1 calc GR . P A 2


_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
P1 P2 2.1078(14) . ?
P1 C2 1.747(4) . ?
P2 P3 2.1066(17) . ?
P3 C3 1.755(4) . ?
N1 C1 1.365(5) . ?
N1 C2 1.410(5) . ?
N1 C11 1.448(4) . ?
N2 C1 1.355(4) . ?
N2 C3 1.406(5) . ?
N2 C23 1.440(5) . ?
C1 C4 1.465(6) . ?
C2 C3 1.395(5) . ?
C4 C5 1.396(5) . ?
C4 C9 1.391(6) . ?
C5 H5 0.9300 . ?
C5 C6 1.396(6) . ?
C6 H6 0.9300 . ?
C6 C7 1.391(7) . ?
C7 C8 1.374(6) . ?
C7 C10 1.500(6) . ?
C8 H8 0.9300 . ?
C8 C9 1.380(7) . ?
C9 H9 0.9300 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 C12 1.392(5) . ?
C11 C16 1.398(6) . ?
C12 C13 1.408(5) . ?
C12 C17 1.510(6) . ?
C13 H13 0.9300 . ?
C13 C14 1.369(6) . ?
C14 H14 0.9300 . ?
C14 C15 1.388(6) . ?
C15 H15 0.9300 . ?
C15 C16 1.399(5) . ?
C16 C20 1.528(5) . ?
C17 H17 0.9800 . ?
C17 C18 1.534(7) . ?
C17 C19 1.527(8) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 H20 0.9800 . ?
C20 C21 1.523(6) . ?
C20 C22 1.515(6) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 C24 1.417(6) . ?
C23 C28 1.399(6) . ?
C24 C25 1.388(6) . ?
C24 C29 1.523(6) . ?
C25 H25 0.9300 . ?
C25 C26 1.386(6) . ?
C26 H26 0.9300 . ?
C26 C27 1.377(7) . ?
C27 H27 0.9300 . ?
C27 C28 1.396(5) . ?
C28 C32 1.522(6) . ?
C29 H29 0.9800 . ?
C29 C30 1.523(6) . ?
C29 C31 1.519(7) . ?
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 H32 0.9800 . ?
C32 C33 1.536(7) . ?
C32 C34 1.530(6) . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C35A C36A 1.39(2) . ?
C35A C40A 1.35(2) . ?
C35A C41A 1.54(3) . ?
C36A H36A 0.9300 . ?
C36A C37A 1.409(16) . ?
C37A H37A 0.9300 . ?
C37A C38A 1.34(3) . ?
C38A H38A 0.9300 . ?
C38A C39A 1.38(2) . ?
C39A H39A 0.9300 . ?
C39A C40A 1.30(3) . ?
C40A H40A 0.9300 . ?
C41A H41A 0.9600 . ?
C41A H41B 0.9600 . ?
C41A H41C 0.9600 . ?
C35B C36B 1.35(3) . ?
C35B C40B 1.51(4) . ?
C35B C41B 1.51(2) . ?
C36B H36B 0.9300 . ?
C36B C37B 1.34(4) . ?
C37B H37B 0.9300 . ?
C37B C38B 1.41(3) . ?
C38B H38B 0.9300 . ?
C38B C39B 1.37(2) . ?
C39B H39B 0.9300 . ?
C39B C40B 1.42(3) . ?
C40B H40B 0.9300 . ?
C41B H41D 0.9600 . ?
C41B H41E 0.9600 . ?
C41B H41F 0.9600 . ?

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 P1 P2 95.37(13) . . ?
P3 P2 P1 103.29(6) . . ?
C3 P3 P2 95.27(15) . . ?
C1 N1 C2 110.2(3) . . ?
C1 N1 C11 126.2(3) . . ?
C2 N1 C11 123.6(3) . . ?
C1 N2 C3 110.4(3) . . ?
C1 N2 C23 127.1(3) . . ?
C3 N2 C23 121.9(3) . . ?
N1 C1 C4 127.3(3) . . ?
N2 C1 N1 106.8(3) . . ?
N2 C1 C4 125.9(4) . . ?
N1 C2 P1 130.8(3) . . ?
C3 C2 P1 123.1(3) . . ?
C3 C2 N1 106.1(3) . . ?
N2 C3 P3 130.6(3) . . ?
C2 C3 P3 122.9(3) . . ?
C2 C3 N2 106.4(3) . . ?
C5 C4 C1 121.7(4) . . ?
C9 C4 C1 120.1(4) . . ?
C9 C4 C5 118.2(4) . . ?
C4 C5 H5 120.2 . . ?
C6 C5 C4 119.6(4) . . ?
C6 C5 H5 120.2 . . ?
C5 C6 H6 119.1 . . ?
C7 C6 C5 121.7(4) . . ?
C7 C6 H6 119.1 . . ?
C6 C7 C10 121.1(4) . . ?
C8 C7 C6 117.9(4) . . ?
C8 C7 C10 120.9(4) . . ?
C7 C8 H8 119.4 . . ?
C7 C8 C9 121.2(4) . . ?
C9 C8 H8 119.4 . . ?
C4 C9 H9 119.3 . . ?
C8 C9 C4 121.3(4) . . ?
C8 C9 H9 119.3 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 N1 118.3(3) . . ?
C12 C11 C16 123.7(3) . . ?
C16 C11 N1 117.9(3) . . ?
C11 C12 C13 117.0(4) . . ?
C11 C12 C17 123.3(3) . . ?
C13 C12 C17 119.6(4) . . ?
C12 C13 H13 119.5 . . ?
C14 C13 C12 120.9(4) . . ?
C14 C13 H13 119.5 . . ?
C13 C14 H14 119.8 . . ?
C13 C14 C15 120.5(4) . . ?
C15 C14 H14 119.8 . . ?
C14 C15 H15 119.3 . . ?
C14 C15 C16 121.3(4) . . ?
C16 C15 H15 119.3 . . ?
C11 C16 C15 116.5(4) . . ?
C11 C16 C20 123.3(3) . . ?
C15 C16 C20 120.2(4) . . ?
C12 C17 H17 107.7 . . ?
C12 C17 C18 112.2(4) . . ?
C12 C17 C19 110.2(4) . . ?
C18 C17 H17 107.7 . . ?
C19 C17 H17 107.7 . . ?
C19 C17 C18 111.2(5) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C16 C20 H20 107.6 . . ?
C21 C20 C16 111.1(3) . . ?
C21 C20 H20 107.6 . . ?
C22 C20 C16 111.9(4) . . ?
C22 C20 H20 107.6 . . ?
C22 C20 C21 110.7(4) . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C24 C23 N2 118.0(4) . . ?
C28 C23 N2 119.1(4) . . ?
C28 C23 C24 122.9(4) . . ?
C23 C24 C29 122.4(4) . . ?
C25 C24 C23 117.0(4) . . ?
C25 C24 C29 120.5(4) . . ?
C24 C25 H25 119.4 . . ?
C26 C25 C24 121.1(4) . . ?
C26 C25 H25 119.4 . . ?
C25 C26 H26 119.8 . . ?
C27 C26 C25 120.5(4) . . ?
C27 C26 H26 119.8 . . ?
C26 C27 H27 119.3 . . ?
C26 C27 C28 121.5(4) . . ?
C28 C27 H27 119.3 . . ?
C23 C28 C32 122.9(4) . . ?
C27 C28 C23 116.9(4) . . ?
C27 C28 C32 120.2(4) . . ?
C24 C29 H29 107.8 . . ?
C30 C29 C24 109.9(4) . . ?
C30 C29 H29 107.8 . . ?
C31 C29 C24 111.8(4) . . ?
C31 C29 H29 107.8 . . ?
C31 C29 C30 111.6(4) . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C28 C32 H32 108.1 . . ?
C28 C32 C33 112.1(4) . . ?
C28 C32 C34 111.1(3) . . ?
C33 C32 H32 108.1 . . ?
C34 C32 H32 108.1 . . ?
C34 C32 C33 109.2(4) . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C32 C34 H34A 109.5 . . ?
C32 C34 H34B 109.5 . . ?
C32 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C36A C35A C41A 116.9(14) . . ?
C40A C35A C36A 121.1(17) . . ?
C40A C35A C41A 121.6(18) . . ?
C35A C36A H36A 122.0 . . ?
C35A C36A C37A 116.0(14) . . ?
C37A C36A H36A 122.0 . . ?
C36A C37A H37A 119.0 . . ?
C38A C37A C36A 122.0(14) . . ?
C38A C37A H37A 119.0 . . ?
C37A C38A H38A 121.5 . . ?
C37A C38A C39A 117(2) . . ?
C39A C38A H38A 121.5 . . ?
C38A C39A H39A 118.1 . . ?
C40A C39A C38A 124(2) . . ?
C40A C39A H39A 118.1 . . ?
C35A C40A H40A 120.1 . . ?
C39A C40A C35A 119.7(16) . . ?
C39A C40A H40A 120.1 . . ?
C35A C41A H41A 109.5 . . ?
C35A C41A H41B 109.5 . . ?
C35A C41A H41C 109.5 . . ?
H41A C41A H41B 109.5 . . ?
H41A C41A H41C 109.5 . . ?
H41B C41A H41C 109.5 . . ?
C36B C35B C40B 122.5(19) . . ?
C36B C35B C41B 120.1(16) . . ?
C41B C35B C40B 117.0(15) . . ?
C35B C36B H36B 118.7 . . ?
C37B C36B C35B 123(2) . . ?
C37B C36B H36B 118.7 . . ?
C36B C37B H37B 121.3 . . ?
C36B C37B C38B 117.4(18) . . ?
C38B C37B H37B 121.3 . . ?
C37B C38B H38B 119.0 . . ?
C39B C38B C37B 122.0(18) . . ?
C39B C38B H38B 119.0 . . ?
C38B C39B H39B 118.6 . . ?
C38B C39B C40B 123(2) . . ?
C40B C39B H39B 118.6 . . ?
C35B C40B H40B 124.6 . . ?
C39B C40B C35B 111(2) . . ?
C39B C40B H40B 124.6 . . ?
C35B C41B H41D 109.5 . . ?
C35B C41B H41E 109.5 . . ?
C35B C41B H41F 109.5 . . ?
H41D C41B H41E 109.5 . . ?
H41D C41B H41F 109.5 . . ?
H41E C41B H41F 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
P1 C2 C3 P3 -1.2(5) . . . . ?
P1 C2 C3 N2 178.9(3) . . . . ?
P2 P1 C2 N1 -176.9(4) . . . . ?
P2 P1 C2 C3 0.8(4) . . . . ?
P2 P3 C3 N2 -179.3(4) . . . . ?
P2 P3 C3 C2 0.9(4) . . . . ?
N1 C1 C4 C5 32.5(6) . . . . ?
N1 C1 C4 C9 -148.1(4) . . . . ?
N1 C2 C3 P3 176.9(3) . . . . ?
N1 C2 C3 N2 -3.0(4) . . . . ?
N1 C11 C12 C13 -178.1(4) . . . . ?
N1 C11 C12 C17 4.8(6) . . . . ?
N1 C11 C16 C15 178.1(4) . . . . ?
N1 C11 C16 C20 -1.3(6) . . . . ?
N2 C1 C4 C5 -148.8(4) . . . . ?
N2 C1 C4 C9 30.6(7) . . . . ?
N2 C23 C24 C25 179.8(3) . . . . ?
N2 C23 C24 C29 1.0(5) . . . . ?
N2 C23 C28 C27 179.5(3) . . . . ?
N2 C23 C28 C32 0.1(6) . . . . ?
C1 N1 C2 P1 -179.3(3) . . . . ?
C1 N1 C2 C3 2.7(4) . . . . ?
C1 N1 C11 C12 73.1(5) . . . . ?
C1 N1 C11 C16 -106.8(5) . . . . ?
C1 N2 C3 P3 -177.6(3) . . . . ?
C1 N2 C3 C2 2.3(5) . . . . ?
C1 N2 C23 C24 73.7(5) . . . . ?
C1 N2 C23 C28 -107.1(5) . . . . ?
C1 C4 C5 C6 -179.8(4) . . . . ?
C1 C4 C9 C8 -179.4(5) . . . . ?
C2 N1 C1 N2 -1.4(4) . . . . ?
C2 N1 C1 C4 177.5(4) . . . . ?
C2 N1 C11 C12 -103.0(5) . . . . ?
C2 N1 C11 C16 77.0(5) . . . . ?
C3 N2 C1 N1 -0.6(4) . . . . ?
C3 N2 C1 C4 -179.5(4) . . . . ?
C3 N2 C23 C24 -96.7(5) . . . . ?
C3 N2 C23 C28 82.6(5) . . . . ?
C4 C5 C6 C7 -0.1(6) . . . . ?
C5 C4 C9 C8 0.0(7) . . . . ?
C5 C6 C7 C8 -1.5(7) . . . . ?
C5 C6 C7 C10 -178.5(4) . . . . ?
C6 C7 C8 C9 2.4(8) . . . . ?
C7 C8 C9 C4 -1.7(9) . . . . ?
C9 C4 C5 C6 0.9(6) . . . . ?
C10 C7 C8 C9 179.4(5) . . . . ?
C11 N1 C1 N2 -178.0(4) . . . . ?
C11 N1 C1 C4 0.9(7) . . . . ?
C11 N1 C2 P1 -2.6(6) . . . . ?
C11 N1 C2 C3 179.5(3) . . . . ?
C11 C12 C13 C14 -0.2(6) . . . . ?
C11 C12 C17 C18 -122.7(5) . . . . ?
C11 C12 C17 C19 112.9(5) . . . . ?
C11 C16 C20 C21 -139.0(4) . . . . ?
C11 C16 C20 C22 96.6(5) . . . . ?
C12 C11 C16 C15 -1.9(6) . . . . ?
C12 C11 C16 C20 178.7(4) . . . . ?
C12 C13 C14 C15 -1.4(7) . . . . ?
C13 C12 C17 C18 60.3(6) . . . . ?
C13 C12 C17 C19 -64.1(5) . . . . ?
C13 C14 C15 C16 1.4(7) . . . . ?
C14 C15 C16 C11 0.2(6) . . . . ?
C14 C15 C16 C20 179.6(4) . . . . ?
C15 C16 C20 C21 41.6(6) . . . . ?
C15 C16 C20 C22 -82.8(5) . . . . ?
C16 C11 C12 C13 1.9(6) . . . . ?
C16 C11 C12 C17 -175.2(4) . . . . ?
C17 C12 C13 C14 177.0(4) . . . . ?
C23 N2 C1 N1 -171.8(4) . . . . ?
C23 N2 C1 C4 9.2(7) . . . . ?
C23 N2 C3 P3 -5.8(6) . . . . ?
C23 N2 C3 C2 174.1(4) . . . . ?
C23 C24 C25 C26 0.6(6) . . . . ?
C23 C24 C29 C30 116.3(5) . . . . ?
C23 C24 C29 C31 -119.3(4) . . . . ?
C23 C28 C32 C33 118.1(5) . . . . ?
C23 C28 C32 C34 -119.3(4) . . . . ?
C24 C23 C28 C27 -1.3(6) . . . . ?
C24 C23 C28 C32 179.3(4) . . . . ?
C24 C25 C26 C27 -1.0(6) . . . . ?
C25 C24 C29 C30 -62.4(5) . . . . ?
C25 C24 C29 C31 62.0(5) . . . . ?
C25 C26 C27 C28 0.2(6) . . . . ?
C26 C27 C28 C23 0.9(6) . . . . ?
C26 C27 C28 C32 -179.6(4) . . . . ?
C27 C28 C32 C33 -61.3(5) . . . . ?
C27 C28 C32 C34 61.3(5) . . . . ?
C28 C23 C24 C25 0.6(6) . . . . ?
C28 C23 C24 C29 -178.2(4) . . . . ?
C29 C24 C25 C26 179.3(4) . . . . ?
C35A C36A C37A C38A 6(2) . . . . ?
C36A C35A C40A C39A 6(3) . . . . ?
C36A C37A C38A C39A -3(3) . . . . ?
C37A C38A C39A C40A 1(3) . . . . ?
C38A C39A C40A C35A -2(3) . . . . ?
C40A C35A C36A C37A -7(3) . . . . ?
C41A C35A C36A C37A -179.6(13) . . . . ?
C41A C35A C40A C39A 177.7(17) . . . . ?
C35B C36B C37B C38B 8(4) . . . . ?
C36B C35B C40B C39B 14(3) . . . . ?
C36B C37B C38B C39B -7(3) . . . . ?
C37B C38B C39B C40B 10(3) . . . . ?
C38B C39B C40B C35B -13(3) . . . . ?
C40B C35B C36B C37B -13(3) . . . . ?
C41B C35B C36B C37B 175(2) . . . . ?
C41B C35B C40B C39B -173.7(18) . . . . ?

_olex2_date_sample_data_collection 2018-10-22
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.189
_oxdiff_exptl_absorpt_empirical_full_min 0.847
####################################################################### 
# 
# 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_compound5a
_database_code_depnum_ccdc_archive 'CCDC 1939612'
loop_
_audit_author_name
_audit_author_address
'Hans Georg Stammler'
;University of Bielefeld
Germany
;
_audit_update_record             
;
2019-07-10 deposited with the CCDC.	2019-10-18 downloaded from the CCDC.
;


_audit_creation_date             2019-03-18
_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         'C37 H39 Fe N2 O4 P3, C7 H8'
_chemical_formula_sum            'C44 H47 Fe N2 O4 P3'
_chemical_formula_weight         816.59
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C44 H47 Fe N2 O4 P3'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   10.9413(2)
_cell_length_b                   23.5902(4)
_cell_length_c                   16.2953(3)
_cell_angle_alpha                90
_cell_angle_beta                 96.991(2)
_cell_angle_gamma                90
_cell_volume                     4174.67(13)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    42796
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      32.6560
_cell_measurement_theta_min      3.0440
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.520
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.515
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.39a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.299
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1712
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 1 0.0918
0 0 -1 0.0918
0 1 0 0.1333
0 -1 0 0.1333
1 0 0 0.1468
-1 1 0 0.1883
-4 -5 2 0.1741
1 -5 -5 0.1252
1 5 4 0.1164
-1 -5 -4 0.1164
0 5 -4 0.0946
0 -5 4 0.0946

_exptl_crystal_size_max          0.368
_exptl_crystal_size_mid          0.267
_exptl_crystal_size_min          0.184
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.0003 -0.0025 0.9994 0.0048 0.0432 -0.0058
-0.0003 0.0025 -0.9994 -0.0048 -0.0432 0.0058
-0.0000 0.9997 0.0011 0.0152 0.0018 0.0259
0.0000 -0.9997 -0.0011 -0.0152 -0.0018 -0.0259
0.9994 -0.0003 0.0001 -0.0545 0.0184 0.0309
-0.9994 1.0000 0.0010 0.0697 -0.0166 -0.0050
-3.9968 -5.0022 1.9927 0.1515 0.0041 -0.2644
0.9977 -4.9863 -5.0025 -0.1547 -0.2063 -0.0693
1.0007 4.9882 4.0033 0.0409 0.1999 0.1368
-1.0007 -4.9882 -4.0033 -0.0409 -0.1999 -0.1368
-0.0014 5.0083 -3.9920 0.0569 -0.1638 0.1526
0.0014 -5.0083 3.9920 -0.0569 0.1638 -0.1526

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0417
_diffrn_reflns_av_unetI/netI     0.0286
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            127619
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.838
_diffrn_reflns_theta_min         2.534
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -42.00  51.00   1.00    5.76    --  -17.14  57.00 150.00   93
  2  ω    -91.00 -39.00   1.00    5.76    --  -17.14 154.00 126.53   52
  3  ω    -88.00  13.00   1.00    5.76    --  -17.14 -77.00 150.00  101
  4  ω     -8.00  86.00   1.00    5.76    --   17.14  57.00 120.00   94
  5  ω    -54.00  38.00   1.00    5.76    --   17.14 -38.00-180.00   92
  6  ω    -51.00  42.00   1.00    5.76    --   17.14 -57.00 -60.00   93
  7  ω     -4.00  88.00   1.00    5.76    --   17.14  41.00 -96.00   92
  8  ω     -4.00  88.00   1.00    5.76    --   17.14  38.00 -30.00   92
  9  ω     -8.00  86.00   1.00    5.76    --   17.14  57.00  30.00   94
 10  ω      6.00  75.00   1.00    5.76    --   17.14-131.00 100.45   69
 11  ω    -75.00 -27.00   1.00    5.76    --  -17.14 131.00-156.20   48
 12  ω    -91.00 -61.00   1.00    5.76    --  -17.14 154.00  82.56   30
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0545427000
_diffrn_orient_matrix_UB_12      0.0152282000
_diffrn_orient_matrix_UB_13      0.0048768000
_diffrn_orient_matrix_UB_21      0.0183620000
_diffrn_orient_matrix_UB_22      0.0017222000
_diffrn_orient_matrix_UB_23      0.0431947000
_diffrn_orient_matrix_UB_31      0.0308984000
_diffrn_orient_matrix_UB_32      0.0258674000
_diffrn_orient_matrix_UB_33      -0.0057750000
_diffrn_oxdiff_digest_frames     
;
013276e1a369d73b85ee513372dafeaa30000273358
;
_diffrn_oxdiff_digest_hkl        
;
01f7f3ba0b4390b256e94d13cbb7f2d5fb7236
;
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                12232
_reflns_number_total             14823
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.01
_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 1.171.40.39a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.39a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.39a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.477
_refine_diff_density_min         -0.319
_refine_diff_density_rms         0.060
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     549
_refine_ls_number_reflns         14823
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0344
_refine_ls_restrained_S_all      1.043
_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)+(0.0284P)²+2.2181P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0756
_refine_ls_wR_factor_ref         0.0823
_refine_special_details          'Disorder of toluene over two sites (85:15).'
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C38-C39 \\sim C38A-C39A
 with sigma of 0.02
 C38-C43 \\sim C38A-C43A
 with sigma of 0.02
 C38-C44 \\sim C38A-C44A
 with sigma of 0.02
 C39-C40 \\sim C39A-C40A
 with sigma of 0.02
 C40-C41 \\sim C40A-C41A
 with sigma of 0.02
 C41-C42 \\sim C41A-C42A
 with sigma of 0.02
 C42-C43 \\sim C42A-C43A
 with sigma of 0.02
 C38-C40 \\sim C38A-C40A
 with sigma of 0.04
 C38-C42 \\sim C38A-C42A
 with sigma of 0.04
 C39-C41 \\sim C39A-C41A
 with sigma of 0.04
 C39-C43 \\sim C39A-C43A
 with sigma of 0.04
 C39-C44 \\sim C39A-C44A
 with sigma of 0.04
 C40-C42 \\sim C40A-C42A
 with sigma of 0.04
 C41-C43 \\sim C41A-C43A
 with sigma of 0.04
 C43-C44 \\sim C43A-C44A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C43) = Uanis(C43A)
Uanis(C39) = Uanis(C39A)
4. Others
 Sof(C43A)=Sof(H43A)=Sof(C38A)=Sof(C39A)=Sof(H39A)=Sof(C44A)=Sof(H44D)=
 Sof(H44E)=Sof(H44F)=Sof(C40A)=Sof(H40A)=Sof(C42A)=Sof(H42A)=Sof(C41A)=
 Sof(H41A)=1-FVAR(1)
 Sof(C38)=Sof(C39)=Sof(H39)=Sof(C40)=Sof(H40)=Sof(C41)=Sof(H41)=Sof(C42)=
 Sof(H42)=Sof(C43)=Sof(H43)=Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(H44C)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C10(H10), C13(H13), C22(H22), C25(H25)
5.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C18(H18), C19(H19), C20(H20), C29(H29), C30(H30),
 C31(H31), C32(H32), C33(H33), C39(H39), C40(H40), C41(H41), C42(H42), C43(H43),
  C43A(H43A), C39A(H39A), C40A(H40A), C42A(H42A), C41A(H41A)
5.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A,
 H27B,H27C), C44(H44A,H44B,H44C), C44A(H44D,H44E,H44F)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
Fe1 Fe -0.00983(2) 0.62255(2) 0.36878(2) 0.01416(4) Uani 1 1 d . . . . .
P1 P 0.27831(3) 0.53374(2) 0.35418(2) 0.01623(6) Uani 1 1 d . . . . .
P2 P 0.09104(3) 0.54875(2) 0.32259(2) 0.01533(6) Uani 1 1 d . . . . .
P3 P 0.01596(3) 0.48368(2) 0.24531(2) 0.01590(6) Uani 1 1 d . . . . .
O1 O 0.22749(8) 0.68242(4) 0.39279(7) 0.0297(2) Uani 1 1 d . . . . .
O2 O -0.16363(10) 0.62998(5) 0.20813(6) 0.0332(2) Uani 1 1 d . . . . .
O3 O -0.08425(10) 0.55061(5) 0.50224(7) 0.0331(2) Uani 1 1 d . . . . .
O4 O -0.14456(9) 0.71610(4) 0.43394(7) 0.0286(2) Uani 1 1 d . . . . .
N1 N 0.36174(8) 0.43253(4) 0.28384(6) 0.01396(17) Uani 1 1 d . . . . .
N2 N 0.19180(8) 0.39736(4) 0.21987(6) 0.01366(17) Uani 1 1 d . . . . .
C1 C 0.31341(10) 0.38789(5) 0.23909(7) 0.01396(19) Uani 1 1 d . . . . .
C2 C 0.26855(10) 0.47136(5) 0.29501(7) 0.01420(19) Uani 1 1 d . . . . .
C3 C 0.16038(10) 0.44961(5) 0.25261(7) 0.01400(19) Uani 1 1 d . . . . .
C4 C 0.48416(10) 0.43565(5) 0.32899(7) 0.0160(2) Uani 1 1 d . . . . .
C5 C 0.50566(11) 0.40431(5) 0.40226(7) 0.0182(2) Uani 1 1 d . . . . .
C6 C 0.62426(11) 0.40684(6) 0.44492(8) 0.0228(2) Uani 1 1 d . . . . .
H6 H 0.643269 0.385391 0.492652 0.027 Uiso 1 1 calc R . . . .
C7 C 0.71394(11) 0.44083(6) 0.41720(8) 0.0252(3) Uani 1 1 d . . . . .
H7 H 0.792315 0.442022 0.446547 0.030 Uiso 1 1 calc R . . . .
C8 C 0.68808(11) 0.47293(6) 0.34645(8) 0.0243(3) Uani 1 1 d . . . . .
H8 H 0.748889 0.496141 0.329383 0.029 Uiso 1 1 calc R . . . .
C9 C 0.57202(10) 0.47115(5) 0.30000(7) 0.0192(2) Uani 1 1 d . . . . .
C10 C 0.40601(12) 0.37160(6) 0.43908(8) 0.0230(2) Uani 1 1 d . . . . .
H10 H 0.328790 0.376190 0.402371 0.028 Uiso 1 1 calc R . . . .
C11 C 0.38789(14) 0.39662(7) 0.52376(9) 0.0305(3) Uani 1 1 d . . . . .
H11A H 0.462309 0.392177 0.560982 0.046 Uiso 1 1 calc GR . . . .
H11B H 0.321823 0.377145 0.545523 0.046 Uiso 1 1 calc GR . . . .
H11C H 0.368199 0.436172 0.517725 0.046 Uiso 1 1 calc GR . . . .
C12 C 0.43456(16) 0.30828(6) 0.44666(10) 0.0360(3) Uani 1 1 d . . . . .
H12A H 0.442420 0.293006 0.392944 0.054 Uiso 1 1 calc GR . . . .
H12B H 0.368935 0.289250 0.469565 0.054 Uiso 1 1 calc GR . . . .
H12C H 0.510248 0.302794 0.482219 0.054 Uiso 1 1 calc GR . . . .
C13 C 0.54627(12) 0.50765(6) 0.22338(8) 0.0237(2) Uani 1 1 d . . . . .
H13 H 0.464082 0.498074 0.196062 0.028 Uiso 1 1 calc R . . . .
C14 C 0.54729(13) 0.57084(6) 0.24579(9) 0.0282(3) Uani 1 1 d . . . . .
H14A H 0.484931 0.578207 0.281062 0.042 Uiso 1 1 calc GR . . . .
H14B H 0.531109 0.592984 0.196233 0.042 Uiso 1 1 calc GR . . . .
H14C H 0.626461 0.580849 0.274085 0.042 Uiso 1 1 calc GR . . . .
C15 C 0.63963(14) 0.49700(7) 0.16182(9) 0.0333(3) Uani 1 1 d . . . . .
H15A H 0.719241 0.510472 0.184912 0.050 Uiso 1 1 calc GR . . . .
H15B H 0.613910 0.516763 0.111153 0.050 Uiso 1 1 calc GR . . . .
H15C H 0.644051 0.457103 0.150929 0.050 Uiso 1 1 calc GR . . . .
C16 C 0.10074(9) 0.36198(5) 0.17278(7) 0.01372(19) Uani 1 1 d . . . . .
C17 C 0.02097(10) 0.33069(5) 0.21661(7) 0.0157(2) Uani 1 1 d . . . . .
C18 C -0.07468(10) 0.30177(5) 0.17002(8) 0.0191(2) Uani 1 1 d . . . . .
H18 H -0.129087 0.280296 0.196804 0.023 Uiso 1 1 calc R . . . .
C19 C -0.08998(11) 0.30451(5) 0.08447(8) 0.0214(2) Uani 1 1 d . . . . .
H19 H -0.155944 0.285926 0.054574 0.026 Uiso 1 1 calc R . . . .
C20 C -0.00812(11) 0.33459(5) 0.04329(7) 0.0200(2) Uani 1 1 d . . . . .
H20 H -0.018554 0.335236 -0.014198 0.024 Uiso 1 1 calc R . . . .
C21 C 0.09012(10) 0.36408(5) 0.08639(7) 0.0160(2) Uani 1 1 d . . . . .
C22 C 0.03413(11) 0.32691(5) 0.31055(7) 0.0202(2) Uani 1 1 d . . . . .
H22 H 0.105608 0.349678 0.332574 0.024 Uiso 1 1 calc R . . . .
C23 C -0.07920(15) 0.35102(6) 0.34462(9) 0.0308(3) Uani 1 1 d . . . . .
H23A H -0.088949 0.390204 0.329330 0.046 Uiso 1 1 calc GR . . . .
H23B H -0.068864 0.347765 0.403783 0.046 Uiso 1 1 calc GR . . . .
H23C H -0.150973 0.330214 0.322138 0.046 Uiso 1 1 calc GR . . . .
C24 C 0.05657(13) 0.26562(6) 0.34057(9) 0.0277(3) Uani 1 1 d . . . . .
H24A H -0.010308 0.242074 0.317146 0.042 Uiso 1 1 calc GR . . . .
H24B H 0.061817 0.264507 0.399787 0.042 Uiso 1 1 calc GR . . . .
H24C H 0.132216 0.251976 0.323535 0.042 Uiso 1 1 calc GR . . . .
C25 C 0.18023(11) 0.39546(5) 0.03903(7) 0.0201(2) Uani 1 1 d . . . . .
H25 H 0.235748 0.417341 0.078837 0.024 Uiso 1 1 calc R . . . .
C26 C 0.11352(14) 0.43694(7) -0.02318(9) 0.0319(3) Uani 1 1 d . . . . .
H26A H 0.059361 0.416333 -0.063355 0.048 Uiso 1 1 calc GR . . . .
H26B H 0.172840 0.457334 -0.050520 0.048 Uiso 1 1 calc GR . . . .
H26C H 0.066484 0.463190 0.005280 0.048 Uiso 1 1 calc GR . . . .
C27 C 0.25811(12) 0.35319(6) -0.00365(8) 0.0257(3) Uani 1 1 d . . . . .
H27A H 0.300837 0.328467 0.036970 0.039 Uiso 1 1 calc GR . . . .
H27B H 0.316790 0.373456 -0.031729 0.039 Uiso 1 1 calc GR . . . .
H27C H 0.205483 0.331167 -0.042944 0.039 Uiso 1 1 calc GR . . . .
C28 C 0.38199(10) 0.33835(5) 0.21512(7) 0.0161(2) Uani 1 1 d . . . . .
C29 C 0.33318(11) 0.28403(5) 0.21817(8) 0.0216(2) Uani 1 1 d . . . . .
H29 H 0.255983 0.278861 0.235408 0.026 Uiso 1 1 calc R . . . .
C30 C 0.39938(13) 0.23747(6) 0.19556(9) 0.0276(3) Uani 1 1 d . . . . .
H30 H 0.366772 0.201207 0.198238 0.033 Uiso 1 1 calc R . . . .
C31 C 0.51386(12) 0.24500(6) 0.16902(9) 0.0293(3) Uani 1 1 d . . . . .
H31 H 0.558155 0.213811 0.154015 0.035 Uiso 1 1 calc R . . . .
C32 C 0.56228(12) 0.29903(6) 0.16488(8) 0.0273(3) Uani 1 1 d . . . . .
H32 H 0.638698 0.304038 0.146412 0.033 Uiso 1 1 calc R . . . .
C33 C 0.49748(11) 0.34570(6) 0.18809(7) 0.0212(2) Uani 1 1 d . . . . .
H33 H 0.530790 0.381842 0.185690 0.025 Uiso 1 1 calc R . . . .
C34 C 0.13460(11) 0.65910(5) 0.38357(8) 0.0203(2) Uani 1 1 d . . . . .
C35 C -0.10326(11) 0.62641(5) 0.27030(8) 0.0208(2) Uani 1 1 d . . . . .
C36 C -0.05487(11) 0.57743(5) 0.44974(8) 0.0209(2) Uani 1 1 d . . . . .
C37 C -0.09071(11) 0.68023(5) 0.40792(8) 0.0190(2) Uani 1 1 d . . . . .
C38 C 0.69450(15) 0.16776(8) 0.39231(10) 0.0305(4) Uani 0.850(2) 1 d D . P A 1
C39 C 0.61270(17) 0.15524(10) 0.44915(11) 0.0283(4) Uani 0.850(2) 1 d D . P A 1
H39 H 0.566193 0.184200 0.468551 0.034 Uiso 0.850(2) 1 calc R . P A 1
C40 C 0.59966(16) 0.10046(8) 0.47712(10) 0.0303(4) Uani 0.850(2) 1 d D . P A 1
H40 H 0.544485 0.092791 0.514819 0.036 Uiso 0.850(2) 1 calc R . P A 1
C41 C 0.66904(17) 0.05696(8) 0.44882(11) 0.0335(4) Uani 0.850(2) 1 d D . P A 1
H41 H 0.661212 0.020118 0.467791 0.040 Uiso 0.850(2) 1 calc R . P A 1
C42 C 0.75004(17) 0.06891(9) 0.39208(12) 0.0360(4) Uani 0.850(2) 1 d D . P A 1
H42 H 0.795980 0.039902 0.372242 0.043 Uiso 0.850(2) 1 calc R . P A 1
C43 C 0.7628(6) 0.1241(2) 0.3647(3) 0.0343(5) Uani 0.850(2) 1 d D . P A 1
H43 H 0.818250 0.131816 0.327228 0.041 Uiso 0.850(2) 1 calc R . P A 1
C44 C 0.7101(2) 0.22748(10) 0.36378(14) 0.0458(5) Uani 0.850(2) 1 d D . P A 1
H44A H 0.631227 0.245745 0.354993 0.069 Uiso 0.850(2) 1 calc GR . P A 1
H44B H 0.746329 0.227109 0.312989 0.069 Uiso 0.850(2) 1 calc GR . P A 1
H44C H 0.762884 0.247808 0.405092 0.069 Uiso 0.850(2) 1 calc GR . P A 1
C43A C 0.760(4) 0.1304(12) 0.354(2) 0.0343(5) Uani 0.150(2) 1 d D . P A 2
H43A H 0.809467 0.110570 0.321744 0.041 Uiso 0.150(2) 1 calc R . P A 2
C38A C 0.7168(7) 0.1042(3) 0.4198(5) 0.0231(18) Uani 0.150(2) 1 d D . P A 2
C39A C 0.6289(10) 0.1319(5) 0.4627(7) 0.0283(4) Uani 0.150(2) 1 d D . P A 2
H39A H 0.595473 0.113478 0.505202 0.034 Uiso 0.150(2) 1 calc R . P A 2
C44A C 0.7561(11) 0.0461(4) 0.4466(8) 0.039(3) Uani 0.150(2) 1 d D . P A 2
H44D H 0.793969 0.027858 0.403469 0.058 Uiso 0.150(2) 1 calc GR . P A 2
H44E H 0.685521 0.024590 0.457924 0.058 Uiso 0.150(2) 1 calc GR . P A 2
H44F H 0.814050 0.048272 0.495679 0.058 Uiso 0.150(2) 1 calc GR . P A 2
C40A C 0.5927(9) 0.1875(5) 0.4405(6) 0.0272(19) Uani 0.150(2) 1 d D . P A 2
H40A H 0.534608 0.206067 0.467953 0.033 Uiso 0.150(2) 1 calc R . P A 2
C42A C 0.7299(9) 0.1868(4) 0.3360(6) 0.033(2) Uani 0.150(2) 1 d D . P A 2
H42A H 0.767747 0.205921 0.295942 0.039 Uiso 0.150(2) 1 calc R . P A 2
C41A C 0.6439(10) 0.2146(4) 0.3773(6) 0.030(2) Uani 0.150(2) 1 d D . P A 2
H41A H 0.620495 0.251450 0.362575 0.036 Uiso 0.150(2) 1 calc R . P A 2


_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
Fe1 P2 2.2400(3) . ?
Fe1 C34 1.7905(12) . ?
Fe1 C35 1.7970(13) . ?
Fe1 C36 1.8097(13) . ?
Fe1 C37 1.7830(12) . ?
P1 P2 2.0814(4) . ?
P1 C2 1.7556(11) . ?
P2 P3 2.0893(4) . ?
P3 C3 1.7637(11) . ?
O1 C34 1.1493(15) . ?
O2 C35 1.1431(16) . ?
O3 C36 1.1412(16) . ?
O4 C37 1.1418(15) . ?
N1 C1 1.3515(14) . ?
N1 C2 1.3990(14) . ?
N1 C4 1.4494(14) . ?
N2 C1 1.3480(13) . ?
N2 C3 1.4025(14) . ?
N2 C16 1.4464(14) . ?
C1 C28 1.4672(15) . ?
C2 C3 1.3937(15) . ?
C4 C5 1.3997(17) . ?
C4 C9 1.3996(16) . ?
C5 C6 1.3968(16) . ?
C5 C10 1.5177(17) . ?
C6 H6 0.9300 . ?
C6 C7 1.3847(19) . ?
C7 H7 0.9300 . ?
C7 C8 1.380(2) . ?
C8 H8 0.9300 . ?
C8 C9 1.3976(16) . ?
C9 C13 1.5146(18) . ?
C10 H10 0.9800 . ?
C10 C11 1.5358(19) . ?
C10 C12 1.528(2) . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13 0.9800 . ?
C13 C14 1.534(2) . ?
C13 C15 1.5371(18) . ?
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 1.4030(15) . ?
C16 C21 1.3991(15) . ?
C17 C18 1.3941(16) . ?
C17 C22 1.5227(16) . ?
C18 H18 0.9300 . ?
C18 C19 1.3851(17) . ?
C19 H19 0.9300 . ?
C19 C20 1.3791(18) . ?
C20 H20 0.9300 . ?
C20 C21 1.3960(16) . ?
C21 C25 1.5169(16) . ?
C22 H22 0.9800 . ?
C22 C23 1.5286(18) . ?
C22 C24 1.5366(19) . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25 0.9800 . ?
C25 C26 1.5289(18) . ?
C25 C27 1.5324(18) . ?
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 1.3914(17) . ?
C28 C33 1.3987(16) . ?
C29 H29 0.9300 . ?
C29 C30 1.3899(17) . ?
C30 H30 0.9300 . ?
C30 C31 1.385(2) . ?
C31 H31 0.9300 . ?
C31 C32 1.385(2) . ?
C32 H32 0.9300 . ?
C32 C33 1.3867(17) . ?
C33 H33 0.9300 . ?
C38 C39 1.396(2) . ?
C38 C43 1.378(4) . ?
C38 C44 1.500(3) . ?
C39 H39 0.9300 . ?
C39 C40 1.383(3) . ?
C40 H40 0.9300 . ?
C40 C41 1.388(2) . ?
C41 H41 0.9300 . ?
C41 C42 1.385(3) . ?
C42 H42 0.9300 . ?
C42 C43 1.390(5) . ?
C43 H43 0.9300 . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
C43A H43A 0.9300 . ?
C43A C38A 1.367(16) . ?
C43A C42A 1.394(19) . ?
C38A C39A 1.416(11) . ?
C38A C44A 1.486(11) . ?
C39A H39A 0.9300 . ?
C39A C40A 1.405(12) . ?
C44A H44D 0.9600 . ?
C44A H44E 0.9600 . ?
C44A H44F 0.9600 . ?
C40A H40A 0.9300 . ?
C40A C41A 1.386(11) . ?
C42A H42A 0.9300 . ?
C42A C41A 1.386(12) . ?
C41A H41A 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
C34 Fe1 P2 87.52(4) . . ?
C34 Fe1 C35 119.52(6) . . ?
C34 Fe1 C36 119.96(6) . . ?
C35 Fe1 P2 89.39(4) . . ?
C35 Fe1 C36 120.33(6) . . ?
C36 Fe1 P2 88.67(4) . . ?
C37 Fe1 P2 178.49(4) . . ?
C37 Fe1 C34 93.01(5) . . ?
C37 Fe1 C35 91.58(6) . . ?
C37 Fe1 C36 89.83(5) . . ?
C2 P1 P2 90.83(4) . . ?
P1 P2 Fe1 124.021(16) . . ?
P1 P2 P3 109.094(17) . . ?
P3 P2 Fe1 126.867(16) . . ?
C3 P3 P2 90.62(4) . . ?
C1 N1 C2 109.69(9) . . ?
C1 N1 C4 126.17(9) . . ?
C2 N1 C4 122.95(9) . . ?
C1 N2 C3 109.76(9) . . ?
C1 N2 C16 128.63(9) . . ?
C3 N2 C16 121.61(9) . . ?
N1 C1 C28 125.81(10) . . ?
N2 C1 N1 107.85(9) . . ?
N2 C1 C28 126.33(10) . . ?
N1 C2 P1 128.59(8) . . ?
C3 C2 P1 124.90(8) . . ?
C3 C2 N1 106.43(9) . . ?
N2 C3 P3 129.34(8) . . ?
C2 C3 P3 124.44(8) . . ?
C2 C3 N2 106.23(9) . . ?
C5 C4 N1 117.07(10) . . ?
C5 C4 C9 123.57(10) . . ?
C9 C4 N1 119.30(10) . . ?
C4 C5 C10 123.47(10) . . ?
C6 C5 C4 116.83(11) . . ?
C6 C5 C10 119.58(11) . . ?
C5 C6 H6 119.5 . . ?
C7 C6 C5 120.98(12) . . ?
C7 C6 H6 119.5 . . ?
C6 C7 H7 119.7 . . ?
C8 C7 C6 120.59(11) . . ?
C8 C7 H7 119.7 . . ?
C7 C8 H8 119.5 . . ?
C7 C8 C9 121.10(12) . . ?
C9 C8 H8 119.5 . . ?
C4 C9 C13 123.50(10) . . ?
C8 C9 C4 116.83(12) . . ?
C8 C9 C13 119.66(11) . . ?
C5 C10 H10 108.1 . . ?
C5 C10 C11 109.72(11) . . ?
C5 C10 C12 112.29(12) . . ?
C11 C10 H10 108.1 . . ?
C12 C10 H10 108.1 . . ?
C12 C10 C11 110.52(11) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C9 C13 H13 108.2 . . ?
C9 C13 C14 111.16(11) . . ?
C9 C13 C15 111.92(12) . . ?
C14 C13 H13 108.2 . . ?
C14 C13 C15 109.15(11) . . ?
C15 C13 H13 108.2 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C17 C16 N2 117.67(9) . . ?
C21 C16 N2 118.74(10) . . ?
C21 C16 C17 123.38(10) . . ?
C16 C17 C22 123.64(10) . . ?
C18 C17 C16 116.90(10) . . ?
C18 C17 C22 119.46(10) . . ?
C17 C18 H18 119.5 . . ?
C19 C18 C17 121.06(11) . . ?
C19 C18 H18 119.5 . . ?
C18 C19 H19 119.8 . . ?
C20 C19 C18 120.50(11) . . ?
C20 C19 H19 119.8 . . ?
C19 C20 H20 119.4 . . ?
C19 C20 C21 121.16(11) . . ?
C21 C20 H20 119.4 . . ?
C16 C21 C25 123.35(10) . . ?
C20 C21 C16 116.94(11) . . ?
C20 C21 C25 119.71(10) . . ?
C17 C22 H22 108.0 . . ?
C17 C22 C23 111.20(11) . . ?
C17 C22 C24 111.53(10) . . ?
C23 C22 H22 108.0 . . ?
C23 C22 C24 109.85(10) . . ?
C24 C22 H22 108.0 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C21 C25 H25 108.0 . . ?
C21 C25 C26 111.24(10) . . ?
C21 C25 C27 110.19(10) . . ?
C26 C25 H25 108.0 . . ?
C26 C25 C27 111.25(11) . . ?
C27 C25 H25 108.0 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C29 C28 C1 120.87(10) . . ?
C29 C28 C33 119.39(11) . . ?
C33 C28 C1 119.74(11) . . ?
C28 C29 H29 119.9 . . ?
C30 C29 C28 120.24(12) . . ?
C30 C29 H29 119.9 . . ?
C29 C30 H30 119.9 . . ?
C31 C30 C29 120.11(13) . . ?
C31 C30 H30 119.9 . . ?
C30 C31 H31 120.0 . . ?
C32 C31 C30 119.93(12) . . ?
C32 C31 H31 120.0 . . ?
C31 C32 H32 119.8 . . ?
C31 C32 C33 120.40(12) . . ?
C33 C32 H32 119.8 . . ?
C28 C33 H33 120.0 . . ?
C32 C33 C28 119.93(12) . . ?
C32 C33 H33 120.0 . . ?
O1 C34 Fe1 179.69(13) . . ?
O2 C35 Fe1 178.51(12) . . ?
O3 C36 Fe1 177.63(12) . . ?
O4 C37 Fe1 178.08(11) . . ?
C39 C38 C44 120.74(19) . . ?
C43 C38 C39 118.4(2) . . ?
C43 C38 C44 120.9(2) . . ?
C38 C39 H39 119.4 . . ?
C40 C39 C38 121.10(19) . . ?
C40 C39 H39 119.4 . . ?
C39 C40 H40 120.0 . . ?
C39 C40 C41 119.90(17) . . ?
C41 C40 H40 120.0 . . ?
C40 C41 H41 120.3 . . ?
C42 C41 C40 119.44(18) . . ?
C42 C41 H41 120.3 . . ?
C41 C42 H42 119.9 . . ?
C41 C42 C43 120.1(2) . . ?
C43 C42 H42 119.9 . . ?
C38 C43 C42 121.1(3) . . ?
C38 C43 H43 119.5 . . ?
C42 C43 H43 119.5 . . ?
C38 C44 H44A 109.5 . . ?
C38 C44 H44B 109.5 . . ?
C38 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C38A C43A H43A 119.8 . . ?
C38A C43A C42A 120.3(15) . . ?
C42A C43A H43A 119.8 . . ?
C43A C38A C39A 119.7(11) . . ?
C43A C38A C44A 122.2(11) . . ?
C39A C38A C44A 118.1(9) . . ?
C38A C39A H39A 120.3 . . ?
C40A C39A C38A 119.4(10) . . ?
C40A C39A H39A 120.3 . . ?
C38A C44A H44D 109.5 . . ?
C38A C44A H44E 109.5 . . ?
C38A C44A H44F 109.5 . . ?
H44D C44A H44E 109.5 . . ?
H44D C44A H44F 109.5 . . ?
H44E C44A H44F 109.5 . . ?
C39A C40A H40A 120.2 . . ?
C41A C40A C39A 119.6(9) . . ?
C41A C40A H40A 120.2 . . ?
C43A C42A H42A 119.9 . . ?
C41A C42A C43A 120.2(11) . . ?
C41A C42A H42A 119.9 . . ?
C40A C41A H41A 119.9 . . ?
C42A C41A C40A 120.2(9) . . ?
C42A C41A H41A 119.9 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
P1 C2 C3 P3 4.56(15) . . . . ?
P1 C2 C3 N2 -175.02(8) . . . . ?
P2 P1 C2 N1 -178.81(10) . . . . ?
P2 P1 C2 C3 -2.40(10) . . . . ?
P2 P3 C3 N2 176.08(10) . . . . ?
P2 P3 C3 C2 -3.40(10) . . . . ?
N1 C1 C28 C29 138.92(12) . . . . ?
N1 C1 C28 C33 -41.67(17) . . . . ?
N1 C2 C3 P3 -178.37(8) . . . . ?
N1 C2 C3 N2 2.05(12) . . . . ?
N1 C4 C5 C6 179.14(10) . . . . ?
N1 C4 C5 C10 -4.80(17) . . . . ?
N1 C4 C9 C8 179.35(10) . . . . ?
N1 C4 C9 C13 0.63(17) . . . . ?
N2 C1 C28 C29 -41.81(17) . . . . ?
N2 C1 C28 C33 137.60(12) . . . . ?
N2 C16 C17 C18 173.14(10) . . . . ?
N2 C16 C17 C22 -7.02(16) . . . . ?
N2 C16 C21 C20 -172.58(10) . . . . ?
N2 C16 C21 C25 8.55(16) . . . . ?
C1 N1 C2 P1 174.98(9) . . . . ?
C1 N1 C2 C3 -1.95(12) . . . . ?
C1 N1 C4 C5 -73.37(14) . . . . ?
C1 N1 C4 C9 109.50(13) . . . . ?
C1 N2 C3 P3 178.95(9) . . . . ?
C1 N2 C3 C2 -1.50(12) . . . . ?
C1 N2 C16 C17 103.57(13) . . . . ?
C1 N2 C16 C21 -81.45(15) . . . . ?
C1 C28 C29 C30 -179.77(12) . . . . ?
C1 C28 C33 C32 -179.59(11) . . . . ?
C2 N1 C1 N2 1.03(12) . . . . ?
C2 N1 C1 C28 -179.59(10) . . . . ?
C2 N1 C4 C5 92.83(13) . . . . ?
C2 N1 C4 C9 -84.30(14) . . . . ?
C3 N2 C1 N1 0.31(12) . . . . ?
C3 N2 C1 C28 -179.07(10) . . . . ?
C3 N2 C16 C17 -76.87(13) . . . . ?
C3 N2 C16 C21 98.11(12) . . . . ?
C4 N1 C1 N2 168.76(10) . . . . ?
C4 N1 C1 C28 -11.86(18) . . . . ?
C4 N1 C2 P1 6.78(16) . . . . ?
C4 N1 C2 C3 -170.15(10) . . . . ?
C4 C5 C6 C7 2.66(18) . . . . ?
C4 C5 C10 C11 -116.53(13) . . . . ?
C4 C5 C10 C12 120.14(13) . . . . ?
C4 C9 C13 C14 111.67(13) . . . . ?
C4 C9 C13 C15 -125.99(13) . . . . ?
C5 C4 C9 C8 2.42(17) . . . . ?
C5 C4 C9 C13 -176.30(11) . . . . ?
C5 C6 C7 C8 -0.17(19) . . . . ?
C6 C5 C10 C11 59.42(15) . . . . ?
C6 C5 C10 C12 -63.91(15) . . . . ?
C6 C7 C8 C9 -1.4(2) . . . . ?
C7 C8 C9 C4 0.29(18) . . . . ?
C7 C8 C9 C13 179.06(12) . . . . ?
C8 C9 C13 C14 -67.01(15) . . . . ?
C8 C9 C13 C15 55.32(16) . . . . ?
C9 C4 C5 C6 -3.86(17) . . . . ?
C9 C4 C5 C10 172.19(11) . . . . ?
C10 C5 C6 C7 -173.56(12) . . . . ?
C16 N2 C1 N1 179.90(10) . . . . ?
C16 N2 C1 C28 0.52(18) . . . . ?
C16 N2 C3 P3 -0.68(16) . . . . ?
C16 N2 C3 C2 178.87(10) . . . . ?
C16 C17 C18 C19 -0.55(17) . . . . ?
C16 C17 C22 C23 118.58(12) . . . . ?
C16 C17 C22 C24 -118.41(12) . . . . ?
C16 C21 C25 C26 -126.68(13) . . . . ?
C16 C21 C25 C27 109.45(12) . . . . ?
C17 C16 C21 C20 2.10(17) . . . . ?
C17 C16 C21 C25 -176.77(11) . . . . ?
C17 C18 C19 C20 2.10(19) . . . . ?
C18 C17 C22 C23 -61.58(15) . . . . ?
C18 C17 C22 C24 61.43(14) . . . . ?
C18 C19 C20 C21 -1.57(19) . . . . ?
C19 C20 C21 C16 -0.48(17) . . . . ?
C19 C20 C21 C25 178.43(11) . . . . ?
C20 C21 C25 C26 54.48(15) . . . . ?
C20 C21 C25 C27 -69.38(14) . . . . ?
C21 C16 C17 C18 -1.59(16) . . . . ?
C21 C16 C17 C22 178.25(11) . . . . ?
C22 C17 C18 C19 179.60(11) . . . . ?
C28 C29 C30 C31 -0.7(2) . . . . ?
C29 C28 C33 C32 -0.17(18) . . . . ?
C29 C30 C31 C32 -0.1(2) . . . . ?
C30 C31 C32 C33 0.8(2) . . . . ?
C31 C32 C33 C28 -0.62(19) . . . . ?
C33 C28 C29 C30 0.81(18) . . . . ?
C38 C39 C40 C41 0.3(3) . . . . ?
C39 C38 C43 C42 0.6(8) . . . . ?
C39 C40 C41 C42 -0.6(3) . . . . ?
C40 C41 C42 C43 0.9(4) . . . . ?
C41 C42 C43 C38 -0.9(8) . . . . ?
C43 C38 C39 C40 -0.3(4) . . . . ?
C44 C38 C39 C40 -178.61(17) . . . . ?
C44 C38 C43 C42 178.9(4) . . . . ?
C43A C38A C39A C40A -4(3) . . . . ?
C43A C42A C41A C40A 4(3) . . . . ?
C38A C43A C42A C41A -8(5) . . . . ?
C38A C39A C40A C41A -0.4(17) . . . . ?
C39A C40A C41A C42A 0.3(17) . . . . ?
C44A C38A C39A C40A 178.1(10) . . . . ?
C42A C43A C38A C39A 8(5) . . . . ?
C42A C43A C38A C44A -174(3) . . . . ?

_olex2_date_sample_data_collection 2019-03-18
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.108
_oxdiff_exptl_absorpt_empirical_full_min 0.881
####################################################################### 
# 
# 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_compound5b
_database_code_depnum_ccdc_archive 'CCDC 1939613'
loop_
_audit_author_name
_audit_author_address
'Hans Georg Stammler'
;University of Bielefeld
Germany
;
_audit_update_record             
;
2019-07-10 deposited with the CCDC.	2019-10-18 downloaded from the CCDC.
;



_audit_creation_date             2019-02-11
_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         'C38 H41 Fe N2 O4 P3, C7 H8'
_chemical_formula_sum            'C45 H49 Fe N2 O4 P3'
_chemical_formula_weight         830.62
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C44 H49 Fe N2 O3 P3'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   10.83254(14)
_cell_length_b                   24.9423(3)
_cell_length_c                   16.03521(18)
_cell_angle_alpha                90
_cell_angle_beta                 96.0125(11)
_cell_angle_gamma                90
_cell_volume                     4308.69(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    93941
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      32.6160
_cell_measurement_theta_min      2.9980
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.505
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.777
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.39a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1744
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -5 -2 0.0788
0 -5 3 0.0777
2 3 -5 0.0722
-2 -3 5 0.0722
0 0 1 0.0710
0 5 2 0.0788
0 0 -1 0.0710
-1 1 0 0.0850
0 5 -3 0.0777
-1 -1 0 0.0757
1 1 0 0.0757
1 -1 0 0.0850

_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.151
_exptl_crystal_size_min          0.142
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.0031 -4.9932 -2.0011 0.1162 -0.0049 0.1206
-0.0029 -4.9767 2.9934 0.1548 -0.0817 -0.0842
2.0053 2.9719 -4.9899 -0.1577 -0.0249 0.2055
-2.0053 -2.9719 4.9899 0.1577 0.0249 -0.2055
-0.0012 0.0033 0.9989 0.0077 -0.0154 -0.0410
-0.0031 4.9932 2.0011 -0.1162 0.0049 -0.1206
0.0012 -0.0033 -0.9989 -0.0077 0.0154 0.0410
-1.0000 0.9991 -0.0007 -0.0063 0.0687 -0.0197
0.0029 4.9767 -2.9934 -0.1548 0.0817 0.0842
-0.9997 -0.9956 -0.0020 0.0464 0.0544 -0.0042
0.9997 0.9956 0.0020 -0.0464 -0.0544 0.0042
1.0000 -0.9991 0.0007 0.0063 -0.0687 0.0197

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0435
_diffrn_reflns_av_unetI/netI     0.0200
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            261252
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.880
_diffrn_reflns_theta_min         2.526
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -72.00 -24.00   1.00   34.42    --  -17.14 126.00  80.50   48
  2  ω    -42.00  51.00   1.00   34.42    --  -17.14  57.00  60.00   93
  3  ω     -8.00  86.00   1.00   34.42    --   17.14  57.00 150.00   94
  4  ω    -51.00  42.00   1.00   34.42    --   17.14 -57.00 150.00   93
  5  ω     -4.00  88.00   1.00   34.42    --   17.14  38.00  90.00   92
  6  ω      6.00  75.00   1.00   34.42    --   17.14-131.00 -76.29   69
  7  ω     -8.00  86.00   1.00   34.42    --   17.14  57.00-150.00   94
  8  ω    -54.00  47.00   1.00   34.42    --   17.14 -77.00 -30.00  101
  9  ω    -13.00  88.00   1.00   34.42    --   17.14  77.00 -60.00  101
 10  ω    -76.00 -27.00   1.00   34.42    --  -17.14 132.00 125.75   49
 11  ω    -74.00 -27.00   1.00   34.42    --  -17.14 130.00 -14.47   47
 12  ω    -88.00  13.00   1.00   34.42    --  -17.14 -77.00 -90.00  101
 13  ω     -1.00  69.00   1.00   34.42    --   17.14-121.00 -15.47   70
 14  ω      6.00  76.00   1.00   34.42    --   17.14-132.00 104.16   70
 15  ω     34.00 102.00   1.00   34.42    --   17.14-178.00-120.00   68
 16  ω     -1.00  69.00   1.00   34.42    --   17.14-121.00  63.35   70
 17  ω   -102.00 -55.00   1.00   34.42    --  -17.14 178.00 -90.00   47
 18  ω    -86.00   8.00   1.00   34.42    --  -17.14 -57.00  60.00   94
 19  ω     -8.00  64.00   1.00   34.42    --   17.14-113.00  83.47   72
 20  ω     13.00  85.00   1.00   34.42    --   17.14-147.00 143.11   72
 21  ω     10.00  79.00   1.00   34.42    --   17.14-138.00  36.10   69
 22  ω    -11.00  62.00   1.00   34.42    --   17.14-110.00 -43.80   73
 23  ω      3.00  72.00   1.00   34.42    --   17.14-126.00-130.76   69
 24  ω    -88.00 -16.00   1.00   34.42    --  -17.14 -38.00  90.00   72
 25  ω    -20.00  56.00   1.00   34.42    --   17.14 -99.00-180.00   76
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0201123000
_diffrn_orient_matrix_UB_12      -0.0264147000
_diffrn_orient_matrix_UB_13      0.0077912000
_diffrn_orient_matrix_UB_21      -0.0615321000
_diffrn_orient_matrix_UB_22      0.0071467000
_diffrn_orient_matrix_UB_23      -0.0154857000
_diffrn_orient_matrix_UB_31      0.0119594000
_diffrn_orient_matrix_UB_32      -0.0077261000
_diffrn_orient_matrix_UB_33      -0.0409732000
_diffrn_oxdiff_digest_frames     
;
0184baab6d09e2b3f7627ce149193a7f9701984d1b3
;
_diffrn_oxdiff_digest_hkl        
;
01032c01b9d7f2128de70d05e56bc6919ba88a
;
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                13655
_reflns_number_total             15612
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.01
_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 1.171.40.39a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.39a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.39a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.545
_refine_diff_density_min         -0.408
_refine_diff_density_rms         0.057
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     506
_refine_ls_number_reflns         15612
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0311
_refine_ls_restrained_S_all      1.039
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0346P)²+2.2156P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0789
_refine_ls_wR_factor_ref         0.0827
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C10(H10), C13(H13), C22(H22), C25(H25)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C18(H18), C19(H19), C20(H20), C29(H29), C31(H31),
 C32(H32), C33(H33), C40(H40), C41(H41), C42(H42), C43(H43), C44(H44)
2.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A,
 H27B,H27C), C34(H34A,H34B,H34C), C45(H45A,H45B,H45C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
Fe1 Fe 1.01116(2) 0.61196(2) 0.13823(2) 0.01238(4) Uani 1 1 d . . . . .
P1 P 0.71648(2) 0.52924(2) 0.15198(2) 0.01392(5) Uani 1 1 d . . . . .
P2 P 0.90668(2) 0.54052(2) 0.17952(2) 0.01328(5) Uani 1 1 d . . . . .
P3 P 0.98039(2) 0.47451(2) 0.24814(2) 0.01426(5) Uani 1 1 d . . . . .
O1 O 0.77838(8) 0.67325(4) 0.11342(6) 0.02726(18) Uani 1 1 d . . . . .
O2 O 1.15222(10) 0.61356(5) 0.30482(6) 0.0357(2) Uani 1 1 d . . . . .
O3 O 1.08560(9) 0.54912(4) -0.00419(6) 0.03008(19) Uani 1 1 d . . . . .
O4 O 1.15723(9) 0.70162(4) 0.08372(6) 0.02950(19) Uani 1 1 d . . . . .
N1 N 0.62826(7) 0.43125(3) 0.21509(5) 0.01126(14) Uani 1 1 d . . . . .
N2 N 0.79889(7) 0.39347(3) 0.27115(5) 0.01143(14) Uani 1 1 d . . . . .
C1 C 0.67522(9) 0.38701(4) 0.25513(6) 0.01118(15) Uani 1 1 d . . . . .
C2 C 0.72426(9) 0.46734(4) 0.20445(6) 0.01152(15) Uani 1 1 d . . . . .
C3 C 0.83313(9) 0.44382(4) 0.24176(6) 0.01186(15) Uani 1 1 d . . . . .
C4 C 0.50478(9) 0.43610(4) 0.17177(6) 0.01245(16) Uani 1 1 d . . . . .
C5 C 0.48271(9) 0.41093(4) 0.09347(6) 0.01410(17) Uani 1 1 d . . . . .
C6 C 0.36293(10) 0.41475(5) 0.05255(7) 0.01886(19) Uani 1 1 d . . . . .
H6 H 0.343794 0.397309 0.001573 0.023 Uiso 1 1 calc R . . . .
C7 C 0.27195(10) 0.44415(5) 0.08666(7) 0.0211(2) Uani 1 1 d . . . . .
H7 H 0.192805 0.446490 0.058191 0.025 Uiso 1 1 calc R . . . .
C8 C 0.29805(10) 0.47001(5) 0.16272(7) 0.0199(2) Uani 1 1 d . . . . .
H8 H 0.236619 0.490305 0.184133 0.024 Uiso 1 1 calc R . . . .
C9 C 0.41516(9) 0.46617(4) 0.20795(6) 0.01468(17) Uani 1 1 d . . . . .
C10 C 0.58331(10) 0.38287(4) 0.05045(6) 0.01722(18) Uani 1 1 d . . . . .
H10 H 0.660625 0.384515 0.088022 0.021 Uiso 1 1 calc R . . . .
C11 C 0.60417(12) 0.41251(5) -0.03067(7) 0.0246(2) Uani 1 1 d . . . . .
H11A H 0.529853 0.410937 -0.068872 0.037 Uiso 1 1 calc GR . . . .
H11B H 0.671064 0.395882 -0.055857 0.037 Uiso 1 1 calc GR . . . .
H11C H 0.624652 0.449277 -0.018062 0.037 Uiso 1 1 calc GR . . . .
C12 C 0.55250(13) 0.32371(5) 0.03292(8) 0.0279(2) Uani 1 1 d . . . . .
H12A H 0.544765 0.305513 0.084871 0.042 Uiso 1 1 calc GR . . . .
H12B H 0.617744 0.307487 0.005510 0.042 Uiso 1 1 calc GR . . . .
H12C H 0.475697 0.321079 -0.002591 0.042 Uiso 1 1 calc GR . . . .
C13 C 0.44098(10) 0.49483(4) 0.29148(7) 0.01805(18) Uani 1 1 d . . . . .
H13 H 0.521281 0.482436 0.318448 0.022 Uiso 1 1 calc R . . . .
C14 C 0.44887(12) 0.55553(5) 0.27800(8) 0.0250(2) Uani 1 1 d . . . . .
H14A H 0.516211 0.563320 0.245472 0.037 Uiso 1 1 calc GR . . . .
H14B H 0.462843 0.573185 0.331345 0.037 Uiso 1 1 calc GR . . . .
H14C H 0.372492 0.568087 0.248725 0.037 Uiso 1 1 calc GR . . . .
C15 C 0.34163(12) 0.48322(5) 0.35086(8) 0.0251(2) Uani 1 1 d . . . . .
H15A H 0.264860 0.499838 0.329431 0.038 Uiso 1 1 calc GR . . . .
H15B H 0.368190 0.497371 0.405474 0.038 Uiso 1 1 calc GR . . . .
H15C H 0.329792 0.445191 0.354748 0.038 Uiso 1 1 calc GR . . . .
C16 C 0.88578(9) 0.35739(4) 0.31699(6) 0.01217(16) Uani 1 1 d . . . . .
C17 C 0.95864(9) 0.32395(4) 0.27175(6) 0.01521(17) Uani 1 1 d . . . . .
C18 C 1.04706(10) 0.29229(4) 0.31839(7) 0.0198(2) Uani 1 1 d . . . . .
H18 H 1.096893 0.269466 0.290569 0.024 Uiso 1 1 calc R . . . .
C19 C 1.06213(11) 0.29414(4) 0.40520(7) 0.0210(2) Uani 1 1 d . . . . .
H19 H 1.122297 0.273000 0.434915 0.025 Uiso 1 1 calc R . . . .
C20 C 0.98795(10) 0.32736(4) 0.44785(7) 0.01921(19) Uani 1 1 d . . . . .
H20 H 0.998336 0.328063 0.506155 0.023 Uiso 1 1 calc R . . . .
C21 C 0.89772(9) 0.35984(4) 0.40460(6) 0.01466(17) Uani 1 1 d . . . . .
C22 C 0.81792(11) 0.39584(5) 0.45316(6) 0.01969(19) Uani 1 1 d . . . . .
H22 H 0.765905 0.417724 0.412663 0.024 Uiso 1 1 calc R . . . .
C23 C 0.89901(12) 0.43375(5) 0.51061(7) 0.0252(2) Uani 1 1 d . . . . .
H23A H 0.951608 0.413143 0.550500 0.038 Uiso 1 1 calc GR . . . .
H23B H 0.846960 0.456766 0.539790 0.038 Uiso 1 1 calc GR . . . .
H23C H 0.949285 0.455104 0.477566 0.038 Uiso 1 1 calc GR . . . .
C24 C 0.73192(12) 0.36200(6) 0.50229(8) 0.0285(3) Uani 1 1 d . . . . .
H24A H 0.682369 0.338926 0.464317 0.043 Uiso 1 1 calc GR . . . .
H24B H 0.678659 0.385231 0.530116 0.043 Uiso 1 1 calc GR . . . .
H24C H 0.780923 0.340672 0.543169 0.043 Uiso 1 1 calc GR . . . .
C25 C 0.94710(11) 0.32154(5) 0.17632(7) 0.0219(2) Uani 1 1 d . . . . .
H25 H 0.877684 0.344585 0.154833 0.026 Uiso 1 1 calc R . . . .
C26 C 1.06498(14) 0.34309(5) 0.14318(9) 0.0316(3) Uani 1 1 d . . . . .
H26A H 1.079253 0.379296 0.162076 0.047 Uiso 1 1 calc GR . . . .
H26B H 1.055157 0.342319 0.082991 0.047 Uiso 1 1 calc GR . . . .
H26C H 1.134437 0.321157 0.163684 0.047 Uiso 1 1 calc GR . . . .
C27 C 0.92016(12) 0.26461(6) 0.14292(8) 0.0288(3) Uani 1 1 d . . . . .
H27A H 0.988402 0.241534 0.161676 0.043 Uiso 1 1 calc GR . . . .
H27B H 0.909436 0.265274 0.082741 0.043 Uiso 1 1 calc GR . . . .
H27C H 0.845783 0.251410 0.163466 0.043 Uiso 1 1 calc GR . . . .
C28 C 0.60072(9) 0.34140(4) 0.27805(6) 0.01273(16) Uani 1 1 d . . . . .
C29 C 0.63662(10) 0.28873(4) 0.26399(7) 0.01664(18) Uani 1 1 d . . . . .
H29 H 0.711145 0.282222 0.241800 0.020 Uiso 1 1 calc R . . . .
C30 C 0.56220(11) 0.24579(4) 0.28277(7) 0.0198(2) Uani 1 1 d . . . . .
C31 C 0.45224(11) 0.25628(5) 0.31744(7) 0.0216(2) Uani 1 1 d . . . . .
H31 H 0.402178 0.227900 0.330730 0.026 Uiso 1 1 calc R . . . .
C32 C 0.41617(10) 0.30844(5) 0.33249(7) 0.0210(2) Uani 1 1 d . . . . .
H32 H 0.342472 0.314828 0.355804 0.025 Uiso 1 1 calc R . . . .
C33 C 0.49004(10) 0.35112(4) 0.31276(7) 0.01698(18) Uani 1 1 d . . . . .
H33 H 0.465806 0.386119 0.322665 0.020 Uiso 1 1 calc R . . . .
C34 C 0.59683(13) 0.18913(5) 0.26328(10) 0.0309(3) Uani 1 1 d . . . . .
H34A H 0.534861 0.174214 0.222671 0.046 Uiso 1 1 calc GR . . . .
H34B H 0.601969 0.168070 0.313639 0.046 Uiso 1 1 calc GR . . . .
H34C H 0.675775 0.188928 0.241102 0.046 Uiso 1 1 calc GR . . . .
C35 C 0.86852(10) 0.64871(4) 0.12315(7) 0.01794(18) Uani 1 1 d . . . . .
C36 C 1.09713(11) 0.61231(5) 0.23999(7) 0.0205(2) Uani 1 1 d . . . . .
C37 C 1.05645(10) 0.57234(4) 0.05204(7) 0.01853(19) Uani 1 1 d . . . . .
C38 C 1.09908(10) 0.66709(4) 0.10532(7) 0.01856(19) Uani 1 1 d . . . . .
C39 C 0.28262(12) 0.38798(5) 0.59023(7) 0.0237(2) Uani 1 1 d . . . . .
C40 C 0.36142(13) 0.36117(5) 0.54109(8) 0.0278(2) Uani 1 1 d . . . . .
H40 H 0.400965 0.380260 0.501745 0.033 Uiso 1 1 calc R . . . .
C41 C 0.38200(14) 0.30640(6) 0.54980(8) 0.0304(3) Uani 1 1 d . . . . .
H41 H 0.434909 0.289119 0.516430 0.036 Uiso 1 1 calc R . . . .
C42 C 0.32376(13) 0.27753(6) 0.60816(8) 0.0306(3) Uani 1 1 d . . . . .
H42 H 0.336573 0.240788 0.613849 0.037 Uiso 1 1 calc R . . . .
C43 C 0.24633(13) 0.30389(6) 0.65792(8) 0.0311(3) Uani 1 1 d . . . . .
H43 H 0.207813 0.284783 0.697747 0.037 Uiso 1 1 calc R . . . .
C44 C 0.22567(12) 0.35838(6) 0.64899(8) 0.0278(2) Uani 1 1 d . . . . .
H44 H 0.172974 0.375479 0.682714 0.033 Uiso 1 1 calc R . . . .
C45 C 0.25935(15) 0.44704(6) 0.58024(10) 0.0360(3) Uani 1 1 d . . . . .
H45A H 0.194665 0.453011 0.535549 0.054 Uiso 1 1 calc GR . . . .
H45B H 0.333959 0.464526 0.567303 0.054 Uiso 1 1 calc GR . . . .
H45C H 0.234537 0.461378 0.631488 0.054 Uiso 1 1 calc GR . . . .


_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
Fe1 P2 2.2474(3) . ?
Fe1 C35 1.7911(11) . ?
Fe1 C36 1.7921(11) . ?
Fe1 C37 1.8080(11) . ?
Fe1 C38 1.7837(11) . ?
P1 P2 2.0805(4) . ?
P1 C2 1.7562(9) . ?
P2 P3 2.0917(4) . ?
P3 C3 1.7626(10) . ?
O1 C35 1.1491(14) . ?
O2 C36 1.1435(14) . ?
O3 C37 1.1436(14) . ?
O4 C38 1.1420(13) . ?
N1 C1 1.3492(12) . ?
N1 C2 1.3992(12) . ?
N1 C4 1.4463(12) . ?
N2 C1 1.3471(12) . ?
N2 C3 1.4049(12) . ?
N2 C16 1.4460(12) . ?
C1 C28 1.4638(13) . ?
C2 C3 1.3947(13) . ?
C4 C5 1.4018(13) . ?
C4 C9 1.3999(14) . ?
C5 C6 1.3946(14) . ?
C5 C10 1.5201(14) . ?
C6 H6 0.9300 . ?
C6 C7 1.3859(16) . ?
C7 H7 0.9300 . ?
C7 C8 1.3825(17) . ?
C8 H8 0.9300 . ?
C8 C9 1.3970(14) . ?
C9 C13 1.5181(15) . ?
C10 H10 0.9800 . ?
C10 C11 1.5334(15) . ?
C10 C12 1.5321(16) . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13 0.9800 . ?
C13 C14 1.5329(16) . ?
C13 C15 1.5374(16) . ?
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 1.4018(14) . ?
C16 C21 1.3986(13) . ?
C17 C18 1.3965(14) . ?
C17 C25 1.5234(15) . ?
C18 H18 0.9300 . ?
C18 C19 1.3853(16) . ?
C19 H19 0.9300 . ?
C19 C20 1.3837(16) . ?
C20 H20 0.9300 . ?
C20 C21 1.3966(14) . ?
C21 C22 1.5169(15) . ?
C22 H22 0.9800 . ?
C22 C23 1.5312(17) . ?
C22 C24 1.5346(17) . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25 0.9800 . ?
C25 C26 1.5310(18) . ?
C25 C27 1.5347(18) . ?
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 1.3950(14) . ?
C28 C33 1.3949(14) . ?
C29 H29 0.9300 . ?
C29 C30 1.3922(14) . ?
C30 C31 1.3911(17) . ?
C30 C34 1.5034(16) . ?
C31 H31 0.9300 . ?
C31 C32 1.3868(17) . ?
C32 H32 0.9300 . ?
C32 C33 1.3880(15) . ?
C33 H33 0.9300 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C39 C40 1.3920(17) . ?
C39 C44 1.3910(17) . ?
C39 C45 1.5004(19) . ?
C40 H40 0.9300 . ?
C40 C41 1.3888(19) . ?
C41 H41 0.9300 . ?
C41 C42 1.3840(19) . ?
C42 H42 0.9300 . ?
C42 C43 1.383(2) . ?
C43 H43 0.9300 . ?
C43 C44 1.382(2) . ?
C44 H44 0.9300 . ?
C45 H45A 0.9600 . ?
C45 H45B 0.9600 . ?
C45 H45C 0.9600 . ?

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
C35 Fe1 P2 89.52(3) . . ?
C35 Fe1 C36 118.62(5) . . ?
C35 Fe1 C37 118.41(5) . . ?
C36 Fe1 P2 88.01(4) . . ?
C36 Fe1 C37 122.81(5) . . ?
C37 Fe1 P2 88.70(3) . . ?
C38 Fe1 P2 177.85(4) . . ?
C38 Fe1 C35 92.60(5) . . ?
C38 Fe1 C36 91.32(5) . . ?
C38 Fe1 C37 89.95(5) . . ?
C2 P1 P2 91.17(3) . . ?
P1 P2 Fe1 124.244(14) . . ?
P1 P2 P3 108.677(15) . . ?
P3 P2 Fe1 127.068(14) . . ?
C3 P3 P2 91.03(3) . . ?
C1 N1 C2 109.65(8) . . ?
C1 N1 C4 125.49(8) . . ?
C2 N1 C4 123.33(8) . . ?
C1 N2 C3 109.59(8) . . ?
C1 N2 C16 127.15(8) . . ?
C3 N2 C16 123.10(8) . . ?
N1 C1 C28 124.39(8) . . ?
N2 C1 N1 108.10(8) . . ?
N2 C1 C28 127.49(8) . . ?
N1 C2 P1 128.69(7) . . ?
C3 C2 P1 124.84(7) . . ?
C3 C2 N1 106.44(8) . . ?
N2 C3 P3 129.64(7) . . ?
C2 C3 P3 124.18(7) . . ?
C2 C3 N2 106.19(8) . . ?
C5 C4 N1 117.07(8) . . ?
C9 C4 N1 119.50(8) . . ?
C9 C4 C5 123.41(9) . . ?
C4 C5 C10 123.34(9) . . ?
C6 C5 C4 116.99(9) . . ?
C6 C5 C10 119.60(9) . . ?
C5 C6 H6 119.5 . . ?
C7 C6 C5 121.03(10) . . ?
C7 C6 H6 119.5 . . ?
C6 C7 H7 119.8 . . ?
C8 C7 C6 120.45(10) . . ?
C8 C7 H7 119.8 . . ?
C7 C8 H8 119.4 . . ?
C7 C8 C9 121.11(10) . . ?
C9 C8 H8 119.4 . . ?
C4 C9 C13 123.11(9) . . ?
C8 C9 C4 116.93(9) . . ?
C8 C9 C13 119.95(9) . . ?
C5 C10 H10 108.0 . . ?
C5 C10 C11 109.83(9) . . ?
C5 C10 C12 111.96(9) . . ?
C11 C10 H10 108.0 . . ?
C12 C10 H10 108.0 . . ?
C12 C10 C11 110.94(9) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C9 C13 H13 108.3 . . ?
C9 C13 C14 110.39(9) . . ?
C9 C13 C15 112.42(9) . . ?
C14 C13 H13 108.3 . . ?
C14 C13 C15 109.05(9) . . ?
C15 C13 H13 108.3 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C17 C16 N2 118.62(8) . . ?
C21 C16 N2 118.05(8) . . ?
C21 C16 C17 123.23(9) . . ?
C16 C17 C25 123.50(9) . . ?
C18 C17 C16 116.81(9) . . ?
C18 C17 C25 119.68(9) . . ?
C17 C18 H18 119.3 . . ?
C19 C18 C17 121.42(10) . . ?
C19 C18 H18 119.3 . . ?
C18 C19 H19 119.9 . . ?
C20 C19 C18 120.22(10) . . ?
C20 C19 H19 119.9 . . ?
C19 C20 H20 119.5 . . ?
C19 C20 C21 120.95(10) . . ?
C21 C20 H20 119.5 . . ?
C16 C21 C22 122.93(9) . . ?
C20 C21 C16 117.37(9) . . ?
C20 C21 C22 119.69(9) . . ?
C21 C22 H22 108.0 . . ?
C21 C22 C23 110.65(9) . . ?
C21 C22 C24 110.31(10) . . ?
C23 C22 H22 108.0 . . ?
C23 C22 C24 111.82(9) . . ?
C24 C22 H22 108.0 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C17 C25 H25 108.0 . . ?
C17 C25 C26 110.56(10) . . ?
C17 C25 C27 112.31(10) . . ?
C26 C25 H25 108.0 . . ?
C26 C25 C27 109.80(10) . . ?
C27 C25 H25 108.0 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C29 C28 C1 121.39(9) . . ?
C33 C28 C1 118.98(9) . . ?
C33 C28 C29 119.61(9) . . ?
C28 C29 H29 119.6 . . ?
C30 C29 C28 120.79(10) . . ?
C30 C29 H29 119.6 . . ?
C29 C30 C34 121.02(11) . . ?
C31 C30 C29 118.76(10) . . ?
C31 C30 C34 120.17(10) . . ?
C30 C31 H31 119.5 . . ?
C32 C31 C30 120.98(10) . . ?
C32 C31 H31 119.5 . . ?
C31 C32 H32 120.0 . . ?
C31 C32 C33 120.01(10) . . ?
C33 C32 H32 120.0 . . ?
C28 C33 H33 120.1 . . ?
C32 C33 C28 119.85(10) . . ?
C32 C33 H33 120.1 . . ?
C30 C34 H34A 109.5 . . ?
C30 C34 H34B 109.5 . . ?
C30 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
O1 C35 Fe1 178.59(10) . . ?
O2 C36 Fe1 178.71(11) . . ?
O3 C37 Fe1 177.29(10) . . ?
O4 C38 Fe1 178.51(11) . . ?
C40 C39 C45 121.15(12) . . ?
C44 C39 C40 118.05(12) . . ?
C44 C39 C45 120.79(12) . . ?
C39 C40 H40 119.4 . . ?
C41 C40 C39 121.13(12) . . ?
C41 C40 H40 119.4 . . ?
C40 C41 H41 120.0 . . ?
C42 C41 C40 120.00(12) . . ?
C42 C41 H41 120.0 . . ?
C41 C42 H42 120.3 . . ?
C43 C42 C41 119.32(13) . . ?
C43 C42 H42 120.3 . . ?
C42 C43 H43 119.7 . . ?
C44 C43 C42 120.59(12) . . ?
C44 C43 H43 119.7 . . ?
C39 C44 H44 119.6 . . ?
C43 C44 C39 120.89(12) . . ?
C43 C44 H44 119.6 . . ?
C39 C45 H45A 109.5 . . ?
C39 C45 H45B 109.5 . . ?
C39 C45 H45C 109.5 . . ?
H45A C45 H45B 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
P1 C2 C3 P3 4.21(13) . . . . ?
P1 C2 C3 N2 -176.04(7) . . . . ?
P2 P1 C2 N1 -179.64(8) . . . . ?
P2 P1 C2 C3 -2.20(8) . . . . ?
P2 P3 C3 N2 177.13(9) . . . . ?
P2 P3 C3 C2 -3.18(8) . . . . ?
N1 C1 C28 C29 134.83(10) . . . . ?
N1 C1 C28 C33 -43.57(14) . . . . ?
N1 C2 C3 P3 -177.87(7) . . . . ?
N1 C2 C3 N2 1.88(10) . . . . ?
N1 C4 C5 C6 178.77(9) . . . . ?
N1 C4 C5 C10 -4.49(14) . . . . ?
N1 C4 C9 C8 179.19(9) . . . . ?
N1 C4 C9 C13 0.39(14) . . . . ?
N2 C1 C28 C29 -47.00(14) . . . . ?
N2 C1 C28 C33 134.60(10) . . . . ?
N2 C16 C17 C18 175.91(9) . . . . ?
N2 C16 C17 C25 -3.01(15) . . . . ?
N2 C16 C21 C20 -175.76(9) . . . . ?
N2 C16 C21 C22 4.13(14) . . . . ?
C1 N1 C2 P1 176.42(7) . . . . ?
C1 N1 C2 C3 -1.40(10) . . . . ?
C1 N1 C4 C5 -75.31(12) . . . . ?
C1 N1 C4 C9 106.26(11) . . . . ?
C1 N2 C3 P3 177.96(7) . . . . ?
C1 N2 C3 C2 -1.78(10) . . . . ?
C1 N2 C16 C17 101.83(11) . . . . ?
C1 N2 C16 C21 -81.68(12) . . . . ?
C1 C28 C29 C30 -177.22(9) . . . . ?
C1 C28 C33 C32 178.00(10) . . . . ?
C2 N1 C1 N2 0.30(10) . . . . ?
C2 N1 C1 C28 178.77(9) . . . . ?
C2 N1 C4 C5 89.08(11) . . . . ?
C2 N1 C4 C9 -89.35(11) . . . . ?
C3 N2 C1 N1 0.93(10) . . . . ?
C3 N2 C1 C28 -177.49(9) . . . . ?
C3 N2 C16 C17 -83.28(12) . . . . ?
C3 N2 C16 C21 93.20(11) . . . . ?
C4 N1 C1 N2 166.48(8) . . . . ?
C4 N1 C1 C28 -15.04(15) . . . . ?
C4 N1 C2 P1 9.87(14) . . . . ?
C4 N1 C2 C3 -167.94(8) . . . . ?
C4 C5 C6 C7 2.68(15) . . . . ?
C4 C5 C10 C11 -114.91(11) . . . . ?
C4 C5 C10 C12 121.38(11) . . . . ?
C4 C9 C13 C14 106.97(11) . . . . ?
C4 C9 C13 C15 -131.02(10) . . . . ?
C5 C4 C9 C8 0.86(15) . . . . ?
C5 C4 C9 C13 -177.93(9) . . . . ?
C5 C6 C7 C8 -0.57(17) . . . . ?
C6 C5 C10 C11 61.75(13) . . . . ?
C6 C5 C10 C12 -61.95(13) . . . . ?
C6 C7 C8 C9 -1.58(17) . . . . ?
C7 C8 C9 C4 1.42(15) . . . . ?
C7 C8 C9 C13 -179.75(10) . . . . ?
C8 C9 C13 C14 -71.79(12) . . . . ?
C8 C9 C13 C15 50.22(13) . . . . ?
C9 C4 C5 C6 -2.87(15) . . . . ?
C9 C4 C5 C10 173.87(9) . . . . ?
C10 C5 C6 C7 -174.19(10) . . . . ?
C16 N2 C1 N1 176.38(8) . . . . ?
C16 N2 C1 C28 -2.03(15) . . . . ?
C16 N2 C3 P3 2.28(14) . . . . ?
C16 N2 C3 C2 -177.45(8) . . . . ?
C16 C17 C18 C19 -0.29(16) . . . . ?
C16 C17 C25 C26 113.57(12) . . . . ?
C16 C17 C25 C27 -123.41(11) . . . . ?
C16 C21 C22 C23 -122.89(11) . . . . ?
C16 C21 C22 C24 112.86(11) . . . . ?
C17 C16 C21 C20 0.55(15) . . . . ?
C17 C16 C21 C22 -179.56(10) . . . . ?
C17 C18 C19 C20 0.76(18) . . . . ?
C18 C17 C25 C26 -65.33(13) . . . . ?
C18 C17 C25 C27 57.69(14) . . . . ?
C18 C19 C20 C21 -0.57(17) . . . . ?
C19 C20 C21 C16 -0.07(16) . . . . ?
C19 C20 C21 C22 -179.96(10) . . . . ?
C20 C21 C22 C23 56.99(13) . . . . ?
C20 C21 C22 C24 -67.26(13) . . . . ?
C21 C16 C17 C18 -0.38(15) . . . . ?
C21 C16 C17 C25 -179.30(10) . . . . ?
C25 C17 C18 C19 178.68(11) . . . . ?
C28 C29 C30 C31 -1.24(16) . . . . ?
C28 C29 C30 C34 176.54(11) . . . . ?
C29 C28 C33 C32 -0.43(15) . . . . ?
C29 C30 C31 C32 0.60(17) . . . . ?
C30 C31 C32 C33 0.12(17) . . . . ?
C31 C32 C33 C28 -0.20(17) . . . . ?
C33 C28 C29 C30 1.17(15) . . . . ?
C34 C30 C31 C32 -177.21(11) . . . . ?
C39 C40 C41 C42 0.0(2) . . . . ?
C40 C39 C44 C43 -0.33(19) . . . . ?
C40 C41 C42 C43 -0.7(2) . . . . ?
C41 C42 C43 C44 0.8(2) . . . . ?
C42 C43 C44 C39 -0.4(2) . . . . ?
C44 C39 C40 C41 0.5(2) . . . . ?
C45 C39 C40 C41 -179.38(13) . . . . ?
C45 C39 C44 C43 179.57(13) . . . . ?

_olex2_date_sample_data_collection 2019-02-08
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.251
_oxdiff_exptl_absorpt_empirical_full_min 0.893
####################################################################### 
# 
# 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_compound5d
_database_code_depnum_ccdc_archive 'CCDC 1939615'
loop_
_audit_author_name
_audit_author_address
'Hans Georg Stammler'
;University of Bielefeld
Germany
;
_audit_update_record             
;
2019-07-10 deposited with the CCDC.	2019-10-18 downloaded from the CCDC.
;




_audit_creation_date             2019-06-27
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
dennis.rottschaefer@uni-bielefeld.de
beate.neumann@uni-bielefeld.de
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C40 H44 N3 O5 P3 W, 1.5(C7 H8)'
_chemical_formula_sum            'C50.50 H56 N3 O5 P3 W'
_chemical_formula_weight         1061.74
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C34 H44 N3 O5 P3 W'
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'
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'
W W -5.4734 5.5774 '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                   12.0860(2)
_cell_length_b                   13.1486(2)
_cell_length_c                   16.9350(2)
_cell_angle_alpha                106.1610(10)
_cell_angle_beta                 98.4870(10)
_cell_angle_gamma                100.5390(10)
_cell_volume                     2484.47(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    58491
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.3490
_cell_measurement_theta_min      2.7300
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    5.599
_exptl_absorpt_correction_T_max  0.529
_exptl_absorpt_correction_T_min  0.116
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.54a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1078
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 1 0.0345
1 1 -1 0.0858
0 0 -1 0.0394
0 -1 -1 0.0755
-1 -1 1 0.0742
-1 1 0 0.0726
1 -1 0 0.0643

_exptl_crystal_size_max          0.181
_exptl_crystal_size_mid          0.137
_exptl_crystal_size_min          0.074
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.0001 0.0001 0.9996 0.0084 0.0964 0.0049
0.9995 0.9996 -0.9998 -0.0065 -0.0193 -0.1926
-0.0001 -0.0001 -0.9996 -0.0084 -0.0964 -0.0049
-0.0000 -1.0000 -0.9995 0.0690 -0.1471 0.0798
-0.9995 -0.9996 0.9998 0.0065 0.0193 0.1926
-0.9997 1.0000 0.0001 -0.1567 0.0244 0.0181
0.9997 -1.0000 -0.0001 0.1567 -0.0244 -0.0181

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0474
_diffrn_reflns_av_unetI/netI     0.0201
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            92149
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.490
_diffrn_reflns_theta_min         2.779
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -116.00  -5.00   1.00    2.00    --  -38.50 -19.00   0.00  111
  2  ω    -64.00  30.00   1.00    2.00    --  -38.50  57.00   0.00   94
  3  ω    -59.00  33.00   1.00    2.00    --  -38.50  38.00 120.00   92
  4  ω     22.00 114.00   1.00    2.00    --   42.89  38.00 -30.00   92
  5  ω     13.00 114.00   1.00    2.00    --   42.89  77.00  60.00  101
  6  ω     13.00 114.00   1.00    2.00    --   42.89  77.00 120.00  101
  7  ω     22.00 114.00   1.00    2.00    --   42.89  38.00 150.00   92
  8  ω      1.00  82.00   1.00    2.00    --   42.89 -99.00  90.00   81
  9  ω     18.00 111.00   1.00    2.00    --   42.89  57.00-150.00   93
 10  ω     13.00 114.00   1.00    2.00    --   42.89  77.00 -30.00  101
 11  ω     13.00 114.00   1.00    2.00    --   42.89  77.00-150.00  101
 12  ω     13.00 114.00   1.00    2.00    --   42.89  77.00 -90.00  101
 13  ω    -26.00  68.00   1.00    2.00    --   42.89 -57.00-180.00   94
 14  ω     41.00 118.00   1.00    8.00    --  111.00-125.00 -90.00   77
 15  ω     89.00 178.00   1.00    8.00    --  111.00  45.00 -60.00   89
 16  ω     85.00 178.00   1.00    8.00    --  111.00  61.00 -60.00   93
 17  ω     81.00 178.00   1.00    8.00    --  111.00  77.00 150.00   97
 18  ω     83.00 178.00   1.00    8.00    --  111.00  70.00  16.73   95
 19  ω     85.00 178.00   1.00    8.00    --  111.00  61.00-120.00   93
 20  ω     81.00 178.00   1.00    8.00    --  111.00  77.00  30.00   97
 21  ω     81.00 178.00   1.00    8.00    --  111.00  77.00-120.00   97
 22  ω     81.00 178.00   1.00    8.00    --  111.00  77.00  60.00   97
 23  ω     81.00 178.00   1.00    8.00    --  111.00  77.00 -60.00   97
 24  ω     81.00 178.00   1.00    8.00    --  111.00  77.00 -90.00   97
 25  ω     85.00 178.00   1.00    8.00    --  111.00  61.00  90.00   93
 26  ω     85.00 178.00   1.00    8.00    --  111.00  61.00-180.00   93
 27  ω     85.00 178.00   1.00    8.00    --  111.00  61.00 -90.00   93
 28  ω     81.00 178.00   1.00    8.00    --  111.00  77.00   0.00   97
 29  ω     85.00 178.00   1.00    8.00    --  111.00  61.00 120.00   93
 30  ω     94.00 178.00   1.00    8.00    --  111.00 125.00 -60.00   84
 31  ω     81.00 178.00   1.00    8.00    --  111.00  77.00 120.00   97
 32  ω     85.00 178.00   1.00    8.00    --  111.00  61.00-150.00   93
 33  ω     41.00 118.00   1.00    8.00    --  111.00-125.00 -60.00   77
 34  ω     31.00 110.00   1.00    8.00    --  111.00 -94.00  90.00   79
 35  ω     85.00 178.00   1.00    8.00    --  111.00  61.00   0.00   93
 36  ω     81.00 178.00   1.00    8.00    --  111.00  77.00-150.00   97
 37  ω     41.00 118.00   1.00    8.00    --  111.00-125.00  60.00   77
 38  ω     85.00 178.00   1.00    8.00    --  111.00  61.00  60.00   93
 39  ω     94.00 178.00   1.00    8.00    --  111.00 125.00 -30.00   84
 40  ω     89.00 178.00   1.00    8.00    --  111.00  45.00  30.00   89
 41  ω     89.00 178.00   1.00    8.00    --  111.00  45.00  60.00   89
 42  ω     81.00 178.00   1.00    8.00    --  111.00  77.00 -30.00   97
 43  ω     85.00 178.00   1.00    8.00    --  111.00  61.00 -30.00   93
 44  ω     85.00 178.00   1.00    8.00    --  111.00  61.00 150.00   93
 45  ω     81.00 178.00   1.00    8.00    --  111.00  77.00-180.00   97
 46  ω     41.00 118.00   1.00    8.00    --  111.00-125.00-180.00   77
 47  ω     81.00 178.00   1.00    8.00    --  111.00  77.00  90.00   97
 48  ω     89.00 178.00   1.00    8.00    --  111.00  45.00 150.00   89
 49  ω     40.00 141.00   1.00    8.00    --  111.00 -77.00 -60.00  101
 50  ω     41.00 118.00   1.00    8.00    --  111.00-125.00 -30.00   77
 51  ω     31.00 110.00   1.00    8.00    --  111.00 -94.00  60.00   79
 52  ω     88.00 178.00   1.00    8.00    --  111.00  47.00 110.31   90
 53  ω   -107.00 -13.00   1.00    2.00    --  -38.50 -57.00 -60.00   94
 54  ω     13.00 114.00   1.00    2.00    --   42.89  77.00  30.00  101
 55  ω     18.00 111.00   1.00    2.00    --   42.89  57.00-120.00   93
 56  ω     22.00 114.00   1.00    2.00    --   42.89  38.00   0.00   92
 57  ω     22.00 114.00   1.00    2.00    --   42.89  38.00  30.00   92
 58  ω     22.00 114.00   1.00    2.00    --   42.89  38.00  90.00   92
 59  ω     22.00 114.00   1.00    2.00    --   42.89  38.00 -90.00   92
 60  ω     18.00 111.00   1.00    2.00    --   42.89  57.00 -30.00   93
 61  ω     18.00 111.00   1.00    2.00    --   42.89  57.00  90.00   93
 62  ω     18.00 111.00   1.00    2.00    --   42.89  57.00 120.00   93
 63  ω     23.00  97.00   1.00    2.00    --   42.89-125.00 -60.00   74
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0793185000
_diffrn_orient_matrix_UB_12      -0.0774299000
_diffrn_orient_matrix_UB_13      0.0084192000
_diffrn_orient_matrix_UB_21      0.0263964000
_diffrn_orient_matrix_UB_22      0.0507515000
_diffrn_orient_matrix_UB_23      0.0963820000
_diffrn_orient_matrix_UB_31      -0.1029510000
_diffrn_orient_matrix_UB_32      -0.0847676000
_diffrn_orient_matrix_UB_33      0.0049677000
_diffrn_oxdiff_digest_frames     
;
01f812d98aa51174b5998ca4360e2754df05809a99c
;
_diffrn_oxdiff_digest_hkl        
;
01435365d267d9ddcd7bc7eac9a3e0977f7262
;
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9927
_reflns_number_total             10372
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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 1.171.40.54a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.54a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.54a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         3.385
_refine_diff_density_min         -1.106
_refine_diff_density_rms         0.108
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     664
_refine_ls_number_reflns         10372
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0403
_refine_ls_restrained_S_all      1.078
_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)+(0.0638P)²+4.7652P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1108
_refine_ls_wR_factor_ref         0.1120
_refine_special_details          
'Disorder of C29, C30, C32, C33, C34, and C35 over two sites (52:48). Disorder of a half toluene on an inversion center.'
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(C29B)=Sof(H29B)=Sof(C30B)=Sof(H30B)=Sof(C32B)=Sof(H32B)=Sof(C33B)=
 Sof(H33B)=Sof(C34B)=Sof(H34D)=Sof(H34E)=Sof(H34F)=Sof(C35B)=Sof(H35D)=
 Sof(H35E)=Sof(H35F)=1-FVAR(1)
 Sof(C29)=Sof(H29)=Sof(C30)=Sof(H30)=Sof(C32)=Sof(H32)=Sof(C33)=Sof(H33)=
 Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(H34C)=Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(H35C)=
 FVAR(1)
 Fixed Sof: C48(0.5) H48(0.5) C49(0.5) H49(0.5) C50(0.5) H50(0.5) C51(0.5)
 H51(0.5) C52(0.5) H52(0.5) C53(0.5) C54(0.5) H54A(0.5) H54B(0.5) H54C(0.5)
3.a Ternary CH refined with riding coordinates:
 C10(H10), C13(H13), C22(H22), C25(H25)
3.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C18(H18), C19(H19), C20(H20), C29(H29), C29B(H29B),
 C30(H30), C30B(H30B), C32(H32), C32B(H32B), C33(H33), C33B(H33B), C41(H41),
 C42(H42), C43(H43), C44(H44), C45(H45), C48(H48), C49(H49), C50(H50), C51(H51),
  C52(H52)
3.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A,
 H27B,H27C), C34(H34A,H34B,H34C), C34B(H34D,H34E,H34F), C35(H35A,H35B,H35C),
 C35B(H35D,H35E,H35F), C47(H47A,H47B,H47C), C54(H54A,H54B,H54C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
W1 W 0.83308(2) 0.86708(2) 0.81039(2) 0.03454(7) Uani 1 1 d . . . . .
P1 P 0.81907(8) 0.66677(7) 0.57539(5) 0.03061(18) Uani 1 1 d . . . . .
P2 P 0.79686(8) 0.81237(7) 0.65380(5) 0.02895(17) Uani 1 1 d . . . . .
P3 P 0.72986(7) 0.89568(7) 0.57655(5) 0.02902(17) Uani 1 1 d . . . . .
O1 O 0.7970(3) 0.6147(3) 0.7917(2) 0.0516(7) Uani 1 1 d . . . . .
O2 O 1.1000(3) 0.8739(3) 0.8252(2) 0.0577(9) Uani 1 1 d . . . . .
O3 O 0.8706(4) 0.9303(4) 1.0073(2) 0.0694(10) Uani 1 1 d . . . . .
O4 O 0.8770(6) 1.1138(3) 0.8120(4) 0.103(2) Uani 1 1 d . . . . .
O5 O 0.5662(3) 0.8567(3) 0.7964(2) 0.0498(7) Uani 1 1 d . . . . .
N1 N 0.7560(2) 0.6385(2) 0.40026(18) 0.0283(6) Uani 1 1 d . . . . .
N2 N 0.6986(2) 0.7858(2) 0.40015(17) 0.0261(5) Uani 1 1 d . . . . .
N3 N 0.6464(3) 0.5602(4) -0.0077(2) 0.0512(9) Uani 1 1 d . . . . .
C1 C 0.7140(3) 0.6916(3) 0.3488(2) 0.0279(6) Uani 1 1 d . . . . .
C2 C 0.7681(3) 0.6984(3) 0.4847(2) 0.0262(6) Uani 1 1 d . . . . .
C3 C 0.7309(3) 0.7922(3) 0.4848(2) 0.0253(6) Uani 1 1 d . . . . .
C4 C 0.7830(3) 0.5330(3) 0.3759(2) 0.0307(7) Uani 1 1 d . . . . .
C5 C 0.6957(3) 0.4416(3) 0.3643(3) 0.0361(8) Uani 1 1 d . . . . .
C6 C 0.7203(4) 0.3401(3) 0.3318(3) 0.0472(10) Uani 1 1 d . . . . .
H6 H 0.663747 0.276805 0.321169 0.057 Uiso 1 1 calc R . . . .
C7 C 0.8277(4) 0.3329(4) 0.3152(3) 0.0560(12) Uani 1 1 d . . . . .
H7 H 0.841692 0.264791 0.291710 0.067 Uiso 1 1 calc R . . . .
C8 C 0.9135(4) 0.4245(4) 0.3329(4) 0.0614(14) Uani 1 1 d . . . . .
H8 H 0.985918 0.417533 0.323232 0.074 Uiso 1 1 calc R . . . .
C9 C 0.8948(4) 0.5280(4) 0.3652(3) 0.0459(10) Uani 1 1 d . . . . .
C10 C 0.5789(3) 0.4509(3) 0.3835(4) 0.0504(11) Uani 1 1 d . . . . .
H10 H 0.587909 0.525195 0.420703 0.061 Uiso 1 1 calc R . . . .
C11 C 0.5374(4) 0.3735(4) 0.4308(4) 0.0635(14) Uani 1 1 d . . . . .
H11A H 0.521182 0.299672 0.394402 0.095 Uiso 1 1 calc GR . . . .
H11B H 0.468726 0.388444 0.448803 0.095 Uiso 1 1 calc GR . . . .
H11C H 0.596066 0.383433 0.478962 0.095 Uiso 1 1 calc GR . . . .
C12 C 0.4895(4) 0.4352(5) 0.3054(5) 0.087(2) Uani 1 1 d . . . . .
H12A H 0.513449 0.490215 0.280227 0.131 Uiso 1 1 calc GR . . . .
H12B H 0.416906 0.440846 0.320652 0.131 Uiso 1 1 calc GR . . . .
H12C H 0.481559 0.364486 0.266032 0.131 Uiso 1 1 calc GR . . . .
C13 C 0.9916(4) 0.6289(4) 0.3874(4) 0.0654(16) Uani 1 1 d . . . . .
H13 H 0.960616 0.691692 0.411686 0.079 Uiso 1 1 calc R . . . .
C14 C 1.0887(4) 0.6270(5) 0.4546(5) 0.083(2) Uani 1 1 d . . . . .
H14A H 1.058411 0.615930 0.501626 0.125 Uiso 1 1 calc GR . . . .
H14B H 1.144913 0.695198 0.472651 0.125 Uiso 1 1 calc GR . . . .
H14C H 1.124139 0.568837 0.431925 0.125 Uiso 1 1 calc GR . . . .
C15 C 1.0317(8) 0.6442(7) 0.3077(6) 0.121(4) Uani 1 1 d . . . . .
H15A H 1.063430 0.584266 0.282464 0.181 Uiso 1 1 calc GR . . . .
H15B H 1.089356 0.711060 0.323071 0.181 Uiso 1 1 calc GR . . . .
H15C H 0.967208 0.646621 0.268348 0.181 Uiso 1 1 calc GR . . . .
C16 C 0.6540(3) 0.8714(3) 0.3779(2) 0.0298(7) Uani 1 1 d . . . . .
C17 C 0.7321(4) 0.9613(4) 0.3735(3) 0.0459(10) Uani 1 1 d . . . . .
C18 C 0.6877(5) 1.0424(5) 0.3525(4) 0.0626(14) Uani 1 1 d . . . . .
H18 H 0.737321 1.102633 0.348078 0.075 Uiso 1 1 calc R . . . .
C19 C 0.5698(4) 1.0350(4) 0.3381(3) 0.0553(12) Uani 1 1 d . . . . .
H19 H 0.541049 1.089898 0.323702 0.066 Uiso 1 1 calc R . . . .
C20 C 0.4956(3) 0.9467(4) 0.3451(3) 0.0438(9) Uani 1 1 d . . . . .
H20 H 0.416920 0.942946 0.335464 0.053 Uiso 1 1 calc R . . . .
C21 C 0.5354(3) 0.8632(3) 0.3661(2) 0.0340(7) Uani 1 1 d . . . . .
C22 C 0.8612(4) 0.9701(5) 0.3885(5) 0.0685(17) Uani 1 1 d . . . . .
H22 H 0.876491 0.915693 0.415436 0.082 Uiso 1 1 calc R . . . .
C23 C 0.9272(4) 1.0808(5) 0.4481(5) 0.081(2) Uani 1 1 d . . . . .
H23A H 0.910510 1.136494 0.425000 0.122 Uiso 1 1 calc GR . . . .
H23B H 1.008265 1.084187 0.455888 0.122 Uiso 1 1 calc GR . . . .
H23C H 0.904692 1.091798 0.501365 0.122 Uiso 1 1 calc GR . . . .
C24 C 0.9011(7) 0.9415(8) 0.3037(7) 0.118(4) Uani 1 1 d . . . . .
H24A H 0.853615 0.873061 0.266830 0.178 Uiso 1 1 calc GR . . . .
H24B H 0.979817 0.936371 0.313507 0.178 Uiso 1 1 calc GR . . . .
H24C H 0.894388 0.997472 0.278199 0.178 Uiso 1 1 calc GR . . . .
C25 C 0.4526(3) 0.7686(4) 0.3750(4) 0.0562(13) Uani 1 1 d . . . . .
H25 H 0.497160 0.721002 0.393312 0.067 Uiso 1 1 calc R . . . .
C26 C 0.3853(5) 0.8096(6) 0.4422(5) 0.0786(18) Uani 1 1 d . . . . .
H26A H 0.335703 0.851066 0.422988 0.118 Uiso 1 1 calc GR . . . .
H26B H 0.438099 0.854965 0.493232 0.118 Uiso 1 1 calc GR . . . .
H26C H 0.339741 0.748609 0.452463 0.118 Uiso 1 1 calc GR . . . .
C27 C 0.3714(6) 0.7026(6) 0.2912(6) 0.105(3) Uani 1 1 d . . . . .
H27A H 0.323691 0.639632 0.297477 0.158 Uiso 1 1 calc GR . . . .
H27B H 0.415450 0.679936 0.249603 0.158 Uiso 1 1 calc GR . . . .
H27C H 0.323750 0.746735 0.273816 0.158 Uiso 1 1 calc GR . . . .
C28 C 0.6927(3) 0.6560(3) 0.2571(2) 0.0303(7) Uani 1 1 d . . . . .
C29 C 0.6791(11) 0.7348(8) 0.2124(5) 0.035(2) Uani 0.516(17) 1 d . . P A 1
H29 H 0.680840 0.806285 0.242441 0.042 Uiso 0.516(17) 1 calc R . P A 1
C29B C 0.6250(12) 0.6947(11) 0.2066(5) 0.037(3) Uani 0.484(17) 1 d . . P A 2
H29B H 0.587627 0.746597 0.232352 0.045 Uiso 0.484(17) 1 calc R . P A 2
C30 C 0.6637(11) 0.7038(8) 0.1260(5) 0.039(2) Uani 0.516(17) 1 d . . P A 1
H30 H 0.654837 0.754556 0.098163 0.047 Uiso 0.516(17) 1 calc R . P A 1
C30B C 0.6077(12) 0.6631(12) 0.1210(6) 0.044(3) Uani 0.484(17) 1 d . . P A 2
H30B H 0.557397 0.692067 0.091520 0.052 Uiso 0.484(17) 1 calc R . P A 2
C31 C 0.6610(3) 0.5912(4) 0.0775(2) 0.0410(9) Uani 1 1 d . . . . .
C32 C 0.6671(13) 0.5207(7) 0.1230(5) 0.042(2) Uani 0.516(17) 1 d . . P A 1
H32 H 0.661051 0.447851 0.094179 0.050 Uiso 0.516(17) 1 calc R . P A 1
C32B C 0.7320(12) 0.5414(10) 0.1259(5) 0.041(3) Uani 0.484(17) 1 d . . P A 2
H32B H 0.766294 0.487791 0.098496 0.049 Uiso 0.484(17) 1 calc R . P A 2
C33 C 0.6817(12) 0.5516(7) 0.2088(5) 0.039(2) Uani 0.516(17) 1 d . . P A 1
H33 H 0.684105 0.498614 0.235285 0.046 Uiso 0.516(17) 1 calc R . P A 1
C33B C 0.7479(12) 0.5735(9) 0.2114(5) 0.038(2) Uani 0.484(17) 1 d . . P A 2
H33B H 0.794798 0.542546 0.241662 0.046 Uiso 0.484(17) 1 calc R . P A 2
C34 C 0.6336(17) 0.6465(14) -0.0521(11) 0.060(4) Uani 0.516(17) 1 d . . P A 1
H34A H 0.573861 0.680909 -0.034696 0.090 Uiso 0.516(17) 1 calc GR . P A 1
H34B H 0.614077 0.611890 -0.111898 0.090 Uiso 0.516(17) 1 calc GR . P A 1
H34C H 0.704963 0.700298 -0.037377 0.090 Uiso 0.516(17) 1 calc GR . P A 1
C34B C 0.5934(17) 0.6121(17) -0.0563(11) 0.058(4) Uani 0.484(17) 1 d . . P A 2
H34D H 0.513069 0.600060 -0.054732 0.087 Uiso 0.484(17) 1 calc GR . P A 2
H34E H 0.601882 0.583932 -0.113198 0.087 Uiso 0.484(17) 1 calc GR . P A 2
H34F H 0.628011 0.688878 -0.034996 0.087 Uiso 0.484(17) 1 calc GR . P A 2
C35 C 0.7018(14) 0.4715(17) -0.0527(10) 0.062(4) Uani 0.516(17) 1 d . . P A 1
H35A H 0.783991 0.497490 -0.038028 0.093 Uiso 0.516(17) 1 calc GR . P A 1
H35B H 0.675991 0.453457 -0.112398 0.093 Uiso 0.516(17) 1 calc GR . P A 1
H35C H 0.680147 0.407929 -0.036004 0.093 Uiso 0.516(17) 1 calc GR . P A 1
C35B C 0.6509(16) 0.4572(13) -0.0543(10) 0.054(4) Uani 0.484(17) 1 d . . P A 2
H35D H 0.716051 0.437356 -0.028059 0.081 Uiso 0.484(17) 1 calc GR . P A 2
H35E H 0.658105 0.456610 -0.110084 0.081 Uiso 0.484(17) 1 calc GR . P A 2
H35F H 0.581622 0.405886 -0.057082 0.081 Uiso 0.484(17) 1 calc GR . P A 2
C36 C 0.8086(3) 0.7053(3) 0.7994(3) 0.0382(8) Uani 1 1 d . . . . .
C37 C 1.0050(4) 0.8728(3) 0.8190(3) 0.0451(9) Uani 1 1 d . . . . .
C38 C 0.8578(4) 0.9050(4) 0.9353(3) 0.0454(9) Uani 1 1 d . . . . .
C39 C 0.8618(5) 1.0260(4) 0.8125(3) 0.0618(14) Uani 1 1 d . . . . .
C40 C 0.6620(4) 0.8607(3) 0.8017(2) 0.0409(9) Uani 1 1 d . . . . .
C41 C 0.4167(8) 0.8657(5) 0.1004(4) 0.082(2) Uani 1 1 d . . . . .
H41 H 0.429312 0.886073 0.158735 0.098 Uiso 1 1 calc R . . . .
C42 C 0.3018(9) 0.8035(6) 0.0489(6) 0.102(3) Uani 1 1 d . . . . .
H42 H 0.238641 0.786747 0.072324 0.123 Uiso 1 1 calc R . . . .
C43 C 0.2957(6) 0.7711(6) -0.0400(5) 0.0811(18) Uani 1 1 d . . . . .
H43 H 0.227633 0.730478 -0.077791 0.097 Uiso 1 1 calc R . . . .
C44 C 0.3932(7) 0.8020(6) -0.0670(5) 0.090(2) Uani 1 1 d . . . . .
H44 H 0.390443 0.777557 -0.124501 0.108 Uiso 1 1 calc R . . . .
C45 C 0.4910(8) 0.8636(7) -0.0181(5) 0.095(2) Uani 1 1 d . . . . .
H45 H 0.552032 0.886477 -0.041584 0.114 Uiso 1 1 calc R . . . .
C46 C 0.5025(6) 0.8926(7) 0.0627(5) 0.0806(19) Uani 1 1 d . . . . .
C47 C 0.6175(7) 0.9659(7) 0.1207(5) 0.091(2) Uani 1 1 d . . . . .
H47A H 0.609730 1.039561 0.140910 0.136 Uiso 1 1 calc GR . . . .
H47B H 0.677682 0.963640 0.089440 0.136 Uiso 1 1 calc GR . . . .
H47C H 0.636368 0.940021 0.167453 0.136 Uiso 1 1 calc GR . . . .
C48 C 1.0265(14) 0.5254(16) -0.0618(8) 0.084(5) Uani 0.5 1 d . . P B -1
H48 H 1.024330 0.537645 -0.113503 0.100 Uiso 0.5 1 calc R . P B -1
C49 C 1.0372(15) 0.4267(15) -0.0573(10) 0.083(5) Uani 0.5 1 d . . P B -1
H49 H 1.040882 0.372094 -0.104830 0.100 Uiso 0.5 1 calc R . P B -1
C50 C 1.0426(14) 0.4090(13) 0.0189(10) 0.075(4) Uani 0.5 1 d . . P B -1
H50 H 1.050478 0.341910 0.023963 0.090 Uiso 0.5 1 calc R . P B -1
C51 C 1.0364(13) 0.4904(12) 0.0872(9) 0.065(3) Uani 0.5 1 d . . P B -1
H51 H 1.039316 0.477064 0.138550 0.078 Uiso 0.5 1 calc R . P B -1
C52 C 1.0259(12) 0.5917(13) 0.0835(8) 0.064(3) Uani 0.5 1 d . . P B -1
H52 H 1.023971 0.646238 0.131574 0.077 Uiso 0.5 1 calc R . P B -1
C53 C 1.0185(14) 0.6107(14) 0.0070(8) 0.075(4) Uani 0.5 1 d . . P B -1
C54 C 0.9837(13) 0.7050(11) -0.0034(8) 0.082(4) Uani 0.5 1 d . . P B -1
H54A H 1.009685 0.720907 -0.050560 0.123 Uiso 0.5 1 calc GR . P B -1
H54B H 1.016762 0.765897 0.046497 0.123 Uiso 0.5 1 calc GR . P B -1
H54C H 0.901297 0.691784 -0.013244 0.123 Uiso 0.5 1 calc GR . P B -1


_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
W1 P2 2.4942(9) . ?
W1 C36 2.044(4) . ?
W1 C37 2.047(5) . ?
W1 C38 1.996(4) . ?
W1 C39 2.044(5) . ?
W1 C40 2.036(5) . ?
P1 P2 2.0925(12) . ?
P1 C2 1.755(3) . ?
P2 P3 2.0921(12) . ?
P3 C3 1.761(3) . ?
O1 C36 1.142(5) . ?
O2 C37 1.135(6) . ?
O3 C38 1.151(6) . ?
O4 C39 1.138(7) . ?
O5 C40 1.138(6) . ?
N1 C1 1.357(5) . ?
N1 C2 1.399(4) . ?
N1 C4 1.446(4) . ?
N2 C1 1.363(4) . ?
N2 C3 1.403(4) . ?
N2 C16 1.448(4) . ?
N3 C31 1.359(5) . ?
N3 C34 1.543(19) . ?
N3 C34B 1.367(18) . ?
N3 C35 1.527(17) . ?
N3 C35B 1.381(16) . ?
C1 C28 1.461(5) . ?
C2 C3 1.388(4) . ?
C4 C5 1.393(5) . ?
C4 C9 1.400(5) . ?
C5 C6 1.398(5) . ?
C5 C10 1.513(5) . ?
C6 H6 0.9300 . ?
C6 C7 1.382(6) . ?
C7 H7 0.9300 . ?
C7 C8 1.366(7) . ?
C8 H8 0.9300 . ?
C8 C9 1.392(6) . ?
C9 C13 1.516(6) . ?
C10 H10 0.9800 . ?
C10 C11 1.522(7) . ?
C10 C12 1.517(8) . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13 0.9800 . ?
C13 C14 1.518(10) . ?
C13 C15 1.550(9) . ?
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 1.398(6) . ?
C16 C21 1.397(5) . ?
C17 C18 1.384(6) . ?
C17 C22 1.521(6) . ?
C18 H18 0.9300 . ?
C18 C19 1.390(7) . ?
C19 H19 0.9300 . ?
C19 C20 1.376(7) . ?
C20 H20 0.9300 . ?
C20 C21 1.388(6) . ?
C21 C25 1.505(6) . ?
C22 H22 0.9800 . ?
C22 C23 1.514(10) . ?
C22 C24 1.551(11) . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25 0.9800 . ?
C25 C26 1.530(8) . ?
C25 C27 1.523(8) . ?
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 1.461(9) . ?
C28 C29B 1.359(9) . ?
C28 C33 1.359(9) . ?
C28 C33B 1.473(9) . ?
C29 H29 0.9300 . ?
C29 C30 1.379(12) . ?
C29B H29B 0.9300 . ?
C29B C30B 1.364(13) . ?
C30 H30 0.9300 . ?
C30 C31 1.473(10) . ?
C30B H30B 0.9300 . ?
C30B C31 1.353(10) . ?
C31 C32 1.364(10) . ?
C31 C32B 1.461(10) . ?
C32 H32 0.9300 . ?
C32 C33 1.371(12) . ?
C32B H32B 0.9300 . ?
C32B C33B 1.363(12) . ?
C33 H33 0.9300 . ?
C33B H33B 0.9300 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C34B H34D 0.9600 . ?
C34B H34E 0.9600 . ?
C34B H34F 0.9600 . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C35B H35D 0.9600 . ?
C35B H35E 0.9600 . ?
C35B H35F 0.9600 . ?
C41 H41 0.9300 . ?
C41 C42 1.479(12) . ?
C41 C46 1.339(10) . ?
C42 H42 0.9300 . ?
C42 C43 1.432(11) . ?
C43 H43 0.9300 . ?
C43 C44 1.360(10) . ?
C44 H44 0.9300 . ?
C44 C45 1.315(11) . ?
C45 H45 0.9300 . ?
C45 C46 1.293(10) . ?
C46 C47 1.551(11) . ?
C47 H47A 0.9600 . ?
C47 H47B 0.9600 . ?
C47 H47C 0.9600 . ?
C48 H48 0.9300 . ?
C48 C49 1.35(3) . ?
C48 C53 1.40(2) . ?
C49 H49 0.9300 . ?
C49 C50 1.37(2) . ?
C50 H50 0.9300 . ?
C50 C51 1.363(19) . ?
C51 H51 0.9300 . ?
C51 C52 1.379(19) . ?
C52 H52 0.9300 . ?
C52 C53 1.379(19) . ?
C53 C54 1.43(2) . ?
C54 H54A 0.9600 . ?
C54 H54B 0.9600 . ?
C54 H54C 0.9600 . ?

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
C36 W1 P2 87.65(11) . . ?
C36 W1 C37 87.75(17) . . ?
C37 W1 P2 91.86(12) . . ?
C38 W1 P2 177.65(13) . . ?
C38 W1 C36 90.30(18) . . ?
C38 W1 C37 89.22(17) . . ?
C38 W1 C39 93.8(2) . . ?
C38 W1 C40 90.80(17) . . ?
C39 W1 P2 88.28(15) . . ?
C39 W1 C36 175.42(17) . . ?
C39 W1 C37 90.3(2) . . ?
C40 W1 P2 88.11(11) . . ?
C40 W1 C36 92.02(16) . . ?
C40 W1 C37 179.76(16) . . ?
C40 W1 C39 90.0(2) . . ?
C2 P1 P2 91.83(11) . . ?
P1 P2 W1 125.13(5) . . ?
P3 P2 W1 127.30(4) . . ?
P3 P2 P1 107.46(5) . . ?
C3 P3 P2 91.93(11) . . ?
C1 N1 C2 110.9(3) . . ?
C1 N1 C4 127.4(3) . . ?
C2 N1 C4 121.7(3) . . ?
C1 N2 C3 110.4(3) . . ?
C1 N2 C16 129.1(3) . . ?
C3 N2 C16 120.5(3) . . ?
C31 N3 C34 118.3(8) . . ?
C31 N3 C34B 123.3(9) . . ?
C31 N3 C35 119.9(8) . . ?
C31 N3 C35B 122.1(8) . . ?
C34B N3 C35B 111.9(12) . . ?
C35 N3 C34 114.3(11) . . ?
N1 C1 N2 106.1(3) . . ?
N1 C1 C28 126.7(3) . . ?
N2 C1 C28 127.1(3) . . ?
N1 C2 P1 129.1(2) . . ?
C3 C2 P1 124.7(3) . . ?
C3 C2 N1 106.2(3) . . ?
N2 C3 P3 129.5(2) . . ?
C2 C3 P3 124.0(3) . . ?
C2 C3 N2 106.4(3) . . ?
C5 C4 N1 117.8(3) . . ?
C5 C4 C9 123.6(3) . . ?
C9 C4 N1 118.5(3) . . ?
C4 C5 C6 116.6(4) . . ?
C4 C5 C10 122.0(3) . . ?
C6 C5 C10 121.5(4) . . ?
C5 C6 H6 119.6 . . ?
C7 C6 C5 120.8(4) . . ?
C7 C6 H6 119.6 . . ?
C6 C7 H7 119.6 . . ?
C8 C7 C6 120.8(4) . . ?
C8 C7 H7 119.6 . . ?
C7 C8 H8 119.3 . . ?
C7 C8 C9 121.4(4) . . ?
C9 C8 H8 119.3 . . ?
C4 C9 C13 122.6(4) . . ?
C8 C9 C4 116.5(4) . . ?
C8 C9 C13 120.9(4) . . ?
C5 C10 H10 107.2 . . ?
C5 C10 C11 111.6(4) . . ?
C5 C10 C12 112.5(5) . . ?
C11 C10 H10 107.2 . . ?
C12 C10 H10 107.2 . . ?
C12 C10 C11 110.9(4) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C9 C13 H13 107.1 . . ?
C9 C13 C14 110.6(5) . . ?
C9 C13 C15 111.2(5) . . ?
C14 C13 H13 107.1 . . ?
C14 C13 C15 113.3(6) . . ?
C15 C13 H13 107.1 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C17 C16 N2 118.5(3) . . ?
C21 C16 N2 118.5(3) . . ?
C21 C16 C17 122.9(3) . . ?
C16 C17 C22 122.3(3) . . ?
C18 C17 C16 117.5(4) . . ?
C18 C17 C22 120.2(4) . . ?
C17 C18 H18 119.6 . . ?
C17 C18 C19 120.8(5) . . ?
C19 C18 H18 119.6 . . ?
C18 C19 H19 119.9 . . ?
C20 C19 C18 120.1(4) . . ?
C20 C19 H19 119.9 . . ?
C19 C20 H20 119.3 . . ?
C19 C20 C21 121.5(4) . . ?
C21 C20 H20 119.3 . . ?
C16 C21 C25 122.5(3) . . ?
C20 C21 C16 117.1(4) . . ?
C20 C21 C25 120.4(4) . . ?
C17 C22 H22 107.4 . . ?
C17 C22 C24 110.5(6) . . ?
C23 C22 C17 111.4(5) . . ?
C23 C22 H22 107.4 . . ?
C23 C22 C24 112.6(5) . . ?
C24 C22 H22 107.4 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C21 C25 H25 108.3 . . ?
C21 C25 C26 110.0(4) . . ?
C21 C25 C27 111.1(6) . . ?
C26 C25 H25 108.3 . . ?
C27 C25 H25 108.3 . . ?
C27 C25 C26 110.9(5) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C1 C28 C33B 120.7(4) . . ?
C29 C28 C1 119.5(4) . . ?
C29B C28 C1 125.1(5) . . ?
C29B C28 C33B 114.2(5) . . ?
C33 C28 C1 124.0(5) . . ?
C33 C28 C29 116.6(5) . . ?
C28 C29 H29 119.8 . . ?
C30 C29 C28 120.3(7) . . ?
C30 C29 H29 119.8 . . ?
C28 C29B H29B 117.6 . . ?
C28 C29B C30B 124.9(7) . . ?
C30B C29B H29B 117.6 . . ?
C29 C30 H30 119.7 . . ?
C29 C30 C31 120.6(7) . . ?
C31 C30 H30 119.7 . . ?
C29B C30B H30B 118.8 . . ?
C31 C30B C29B 122.4(7) . . ?
C31 C30B H30B 118.8 . . ?
N3 C31 C30 120.9(5) . . ?
N3 C31 C32 123.4(5) . . ?
N3 C31 C32B 120.0(5) . . ?
C30B C31 N3 123.2(5) . . ?
C30B C31 C32B 116.8(6) . . ?
C32 C31 C30 115.6(6) . . ?
C31 C32 H32 118.2 . . ?
C31 C32 C33 123.5(7) . . ?
C33 C32 H32 118.2 . . ?
C31 C32B H32B 120.0 . . ?
C33B C32B C31 119.9(7) . . ?
C33B C32B H32B 120.0 . . ?
C28 C33 C32 123.1(7) . . ?
C28 C33 H33 118.5 . . ?
C32 C33 H33 118.5 . . ?
C28 C33B H33B 119.1 . . ?
C32B C33B C28 121.7(7) . . ?
C32B C33B H33B 119.1 . . ?
N3 C34 H34A 109.5 . . ?
N3 C34 H34B 109.5 . . ?
N3 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
N3 C34B H34D 109.5 . . ?
N3 C34B H34E 109.5 . . ?
N3 C34B H34F 109.5 . . ?
H34D C34B H34E 109.5 . . ?
H34D C34B H34F 109.5 . . ?
H34E C34B H34F 109.5 . . ?
N3 C35 H35A 109.5 . . ?
N3 C35 H35B 109.5 . . ?
N3 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
N3 C35B H35D 109.5 . . ?
N3 C35B H35E 109.5 . . ?
N3 C35B H35F 109.5 . . ?
H35D C35B H35E 109.5 . . ?
H35D C35B H35F 109.5 . . ?
H35E C35B H35F 109.5 . . ?
O1 C36 W1 178.0(4) . . ?
O2 C37 W1 178.0(4) . . ?
O3 C38 W1 177.4(5) . . ?
O4 C39 W1 178.7(6) . . ?
O5 C40 W1 179.6(4) . . ?
C42 C41 H41 120.1 . . ?
C46 C41 H41 120.1 . . ?
C46 C41 C42 119.8(7) . . ?
C41 C42 H42 122.7 . . ?
C43 C42 C41 114.5(7) . . ?
C43 C42 H42 122.7 . . ?
C42 C43 H43 121.3 . . ?
C44 C43 C42 117.5(7) . . ?
C44 C43 H43 121.3 . . ?
C43 C44 H44 117.5 . . ?
C45 C44 C43 125.0(8) . . ?
C45 C44 H44 117.5 . . ?
C44 C45 H45 120.0 . . ?
C46 C45 C44 120.0(9) . . ?
C46 C45 H45 120.0 . . ?
C41 C46 C47 116.9(7) . . ?
C45 C46 C41 122.8(8) . . ?
C45 C46 C47 120.2(7) . . ?
C46 C47 H47A 109.5 . . ?
C46 C47 H47B 109.5 . . ?
C46 C47 H47C 109.5 . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C49 C48 H48 118.1 . . ?
C49 C48 C53 123.7(14) . . ?
C53 C48 H48 118.1 . . ?
C48 C49 H49 120.8 . . ?
C48 C49 C50 118.3(14) . . ?
C50 C49 H49 120.8 . . ?
C49 C50 H50 120.3 . . ?
C51 C50 C49 119.5(16) . . ?
C51 C50 H50 120.3 . . ?
C50 C51 H51 118.7 . . ?
C50 C51 C52 122.7(14) . . ?
C52 C51 H51 118.7 . . ?
C51 C52 H52 120.6 . . ?
C53 C52 C51 118.7(13) . . ?
C53 C52 H52 120.6 . . ?
C48 C53 C54 121.8(14) . . ?
C52 C53 C48 117.0(16) . . ?
C52 C53 C54 120.2(14) . . ?
C53 C54 H54A 109.5 . . ?
C53 C54 H54B 109.5 . . ?
C53 C54 H54C 109.5 . . ?
H54A C54 H54B 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
P1 C2 C3 P3 0.4(4) . . . . ?
P1 C2 C3 N2 179.6(2) . . . . ?
P2 P1 C2 N1 179.4(3) . . . . ?
P2 P1 C2 C3 -0.7(3) . . . . ?
P2 P3 C3 N2 -178.8(3) . . . . ?
P2 P3 C3 C2 0.1(3) . . . . ?
N1 C1 C28 C29 -162.6(6) . . . . ?
N1 C1 C28 C29B 162.4(9) . . . . ?
N1 C1 C28 C33 19.1(9) . . . . ?
N1 C1 C28 C33B -18.9(8) . . . . ?
N1 C2 C3 P3 -179.6(2) . . . . ?
N1 C2 C3 N2 -0.5(3) . . . . ?
N1 C4 C5 C6 173.1(4) . . . . ?
N1 C4 C5 C10 -5.3(6) . . . . ?
N1 C4 C9 C8 -173.2(4) . . . . ?
N1 C4 C9 C13 6.9(7) . . . . ?
N2 C1 C28 C29 15.6(7) . . . . ?
N2 C1 C28 C29B -19.4(10) . . . . ?
N2 C1 C28 C33 -162.7(8) . . . . ?
N2 C1 C28 C33B 159.3(7) . . . . ?
N2 C16 C17 C18 -179.7(4) . . . . ?
N2 C16 C17 C22 1.9(7) . . . . ?
N2 C16 C21 C20 179.8(3) . . . . ?
N2 C16 C21 C25 -0.4(5) . . . . ?
N3 C31 C32 C33 -179.9(8) . . . . ?
N3 C31 C32B C33B 179.1(9) . . . . ?
C1 N1 C2 P1 -179.6(3) . . . . ?
C1 N1 C2 C3 0.4(4) . . . . ?
C1 N1 C4 C5 -89.0(4) . . . . ?
C1 N1 C4 C9 90.9(5) . . . . ?
C1 N2 C3 P3 179.4(2) . . . . ?
C1 N2 C3 C2 0.3(4) . . . . ?
C1 N2 C16 C17 -94.0(5) . . . . ?
C1 N2 C16 C21 89.1(4) . . . . ?
C1 C28 C29 C30 177.3(7) . . . . ?
C1 C28 C29B C30B 178.3(10) . . . . ?
C1 C28 C33 C32 -176.8(8) . . . . ?
C1 C28 C33B C32B -178.0(9) . . . . ?
C2 N1 C1 N2 -0.2(4) . . . . ?
C2 N1 C1 C28 178.3(3) . . . . ?
C2 N1 C4 C5 88.9(4) . . . . ?
C2 N1 C4 C9 -91.1(4) . . . . ?
C3 N2 C1 N1 -0.1(4) . . . . ?
C3 N2 C1 C28 -178.6(3) . . . . ?
C3 N2 C16 C17 87.2(4) . . . . ?
C3 N2 C16 C21 -89.6(4) . . . . ?
C4 N1 C1 N2 177.9(3) . . . . ?
C4 N1 C1 C28 -3.6(5) . . . . ?
C4 N1 C2 P1 2.2(5) . . . . ?
C4 N1 C2 C3 -177.8(3) . . . . ?
C4 C5 C6 C7 2.2(7) . . . . ?
C4 C5 C10 C11 -135.8(4) . . . . ?
C4 C5 C10 C12 98.8(5) . . . . ?
C4 C9 C13 C14 119.4(5) . . . . ?
C4 C9 C13 C15 -113.7(6) . . . . ?
C5 C4 C9 C8 6.8(7) . . . . ?
C5 C4 C9 C13 -173.1(5) . . . . ?
C5 C6 C7 C8 2.3(8) . . . . ?
C6 C5 C10 C11 45.9(6) . . . . ?
C6 C5 C10 C12 -79.6(5) . . . . ?
C6 C7 C8 C9 -2.4(9) . . . . ?
C7 C8 C9 C4 -2.0(8) . . . . ?
C7 C8 C9 C13 177.9(6) . . . . ?
C8 C9 C13 C14 -60.5(7) . . . . ?
C8 C9 C13 C15 66.4(8) . . . . ?
C9 C4 C5 C6 -6.8(6) . . . . ?
C9 C4 C5 C10 174.7(4) . . . . ?
C10 C5 C6 C7 -179.4(5) . . . . ?
C16 N2 C1 N1 -178.9(3) . . . . ?
C16 N2 C1 C28 2.6(5) . . . . ?
C16 N2 C3 P3 -1.6(4) . . . . ?
C16 N2 C3 C2 179.3(3) . . . . ?
C16 C17 C18 C19 1.1(9) . . . . ?
C16 C17 C22 C23 -132.5(5) . . . . ?
C16 C17 C22 C24 101.6(6) . . . . ?
C16 C21 C25 C26 121.8(5) . . . . ?
C16 C21 C25 C27 -115.0(5) . . . . ?
C17 C16 C21 C20 3.1(6) . . . . ?
C17 C16 C21 C25 -177.1(4) . . . . ?
C17 C18 C19 C20 0.4(9) . . . . ?
C18 C17 C22 C23 49.1(7) . . . . ?
C18 C17 C22 C24 -76.8(7) . . . . ?
C18 C19 C20 C21 -0.3(8) . . . . ?
C19 C20 C21 C16 -1.4(6) . . . . ?
C19 C20 C21 C25 178.8(4) . . . . ?
C20 C21 C25 C26 -58.4(6) . . . . ?
C20 C21 C25 C27 64.8(6) . . . . ?
C21 C16 C17 C18 -3.0(7) . . . . ?
C21 C16 C17 C22 178.6(5) . . . . ?
C22 C17 C18 C19 179.6(6) . . . . ?
C28 C29 C30 C31 -0.2(14) . . . . ?
C28 C29B C30B C31 -2(2) . . . . ?
C29 C28 C33 C32 4.8(13) . . . . ?
C29 C30 C31 N3 -179.7(8) . . . . ?
C29 C30 C31 C32 4.1(13) . . . . ?
C29B C28 C33B C32B 0.8(14) . . . . ?
C29B C30B C31 N3 -178.8(10) . . . . ?
C29B C30B C31 C32B 4.7(16) . . . . ?
C30 C31 C32 C33 -3.8(14) . . . . ?
C30B C31 C32B C33B -4.3(15) . . . . ?
C31 C32 C33 C28 -0.7(17) . . . . ?
C31 C32B C33B C28 1.6(16) . . . . ?
C33 C28 C29 C30 -4.2(12) . . . . ?
C33B C28 C29B C30B -0.5(15) . . . . ?
C34 N3 C31 C30 0.5(10) . . . . ?
C34 N3 C31 C32 176.4(10) . . . . ?
C34B N3 C31 C30B 12.0(13) . . . . ?
C34B N3 C31 C32B -171.7(11) . . . . ?
C35 N3 C31 C30 148.7(12) . . . . ?
C35 N3 C31 C32 -35.4(14) . . . . ?
C35B N3 C31 C30B -147.8(15) . . . . ?
C35B N3 C31 C32B 28.6(14) . . . . ?
C41 C42 C43 C44 -1.2(10) . . . . ?
C42 C41 C46 C45 -2.2(11) . . . . ?
C42 C41 C46 C47 175.1(6) . . . . ?
C42 C43 C44 C45 -3.5(13) . . . . ?
C43 C44 C45 C46 5.5(14) . . . . ?
C44 C45 C46 C41 -2.5(13) . . . . ?
C44 C45 C46 C47 -179.6(7) . . . . ?
C46 C41 C42 C43 3.9(10) . . . . ?
C48 C49 C50 C51 0(3) . . . . ?
C49 C48 C53 C52 2(3) . . . . ?
C49 C48 C53 C54 -166.8(17) . . . . ?
C49 C50 C51 C52 -1(3) . . . . ?
C50 C51 C52 C53 2(3) . . . . ?
C51 C52 C53 C48 -2(2) . . . . ?
C51 C52 C53 C54 166.8(15) . . . . ?
C53 C48 C49 C50 -1(3) . . . . ?

_olex2_date_sample_data_collection 2019-05-21
_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 1.494
_oxdiff_exptl_absorpt_empirical_full_min 0.612
####################################################################### 
# 
# 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_compound4b
_database_code_depnum_ccdc_archive 'CCDC 1939610'
loop_
_audit_author_name
_audit_author_address
'Hans Georg Stammler'
;University of Bielefeld
Germany
;
_audit_update_record             
;
2019-07-10 deposited with the CCDC.	2019-10-18 downloaded from the CCDC.
;



_audit_creation_date             2019-04-08
_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         'C34 H41 N2 P3'
_chemical_formula_sum            'C34 H41 N2 P3'
_chemical_formula_weight         570.60
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C34 H41 N2 P3'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   10.8550(3)
_cell_length_b                   15.5962(3)
_cell_length_c                   19.1059(4)
_cell_angle_alpha                90
_cell_angle_beta                 102.358(2)
_cell_angle_gamma                90
_cell_volume                     3159.62(13)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    27571
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      32.6240
_cell_measurement_theta_min      3.4780
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.213
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.532
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.47a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.200
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1216
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 1 0 0.0537
0 -1 0 0.0537
1 -3 5 0.1090
-1 3 -5 0.1090
-5 0 2 0.1416
5 0 -2 0.1416
0 0 1 0.1069
0 0 -1 0.1069
1 5 4 0.0787

_exptl_crystal_size_max          0.286
_exptl_crystal_size_mid          0.214
_exptl_crystal_size_min          0.107
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.0033 0.9995 0.0103 -0.0377 0.0024 0.0253
-0.0033 -0.9995 -0.0103 0.0377 -0.0024 -0.0253
0.9832 -3.0443 4.9732 -0.0021 -0.0839 -0.2398
-0.9832 3.0443 -4.9732 0.0021 0.0839 0.2398
-5.0029 0.0401 1.9965 0.0007 0.3257 -0.0289
5.0029 -0.0401 -1.9965 -0.0007 -0.3257 0.0289
-0.0014 -0.0070 1.0006 -0.0213 -0.0022 -0.0314
0.0014 0.0070 -1.0006 0.0213 0.0022 0.0314
1.0111 4.9588 4.0547 -0.2822 -0.0628 -0.0058

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0394
_diffrn_reflns_av_unetI/netI     0.0210
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            70658
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.824
_diffrn_reflns_theta_min         2.612
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -38.00  54.00   1.00    5.50    --  -17.14  38.00 120.00   92
  2  ω    -76.00 -27.00   1.00    5.50    --  -17.14 132.00 101.29   49
  3  ω    -13.00  88.00   1.00    5.50    --   17.14  77.00-150.00  101
  4  ω     -8.00  86.00   1.00    5.50    --   17.14  57.00   0.00   94
  5  ω    -54.00  38.00   1.00    5.50    --   17.14 -38.00 -60.00   92
  6  ω     -8.00  86.00   1.00    5.50    --   17.14  57.00 120.00   94
  7  ω    -54.00  47.00   1.00    5.50    --   17.14 -77.00-150.00  101
  8  ω    -32.00  53.00   1.00    5.50    --   17.14 -90.00 -83.29   85
  9  ω    -11.00  62.00   1.00    5.50    --   17.14-110.00  65.63   73
 10  ω    -91.00 -39.00   1.00    5.50    --  -17.14 154.00-144.14   52
 11  ω    -91.00 -39.00   1.00    5.50    --  -17.14 154.00 135.98   52
 12  ω    -84.00 -34.00   1.00    5.50    --  -17.14 146.00 -80.12   50
 13  ω     35.00 101.00   1.00    5.50    --   17.14 178.00 120.00   66
 14  ω    -13.00  88.00   1.00    5.50    --   17.14  77.00-120.00  101
 15  ω     34.00 102.00   1.00    5.50    --   17.14-178.00 -90.00   68
 16  ω      2.00  71.00   1.00    5.50    --   17.14-125.00 160.51   69
 17  ω     35.00 101.00   1.00    5.50    --   17.14 178.00-180.00   66
 18  ω     -2.00  68.00   1.00    5.50    --   17.14-120.00 125.51   70
 19  ω    -20.00   5.00   1.00    5.50    --   17.14 -99.00  30.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0090364000
_diffrn_orient_matrix_UB_12      -0.0374407000
_diffrn_orient_matrix_UB_13      -0.0215650000
_diffrn_orient_matrix_UB_21      -0.0659637000
_diffrn_orient_matrix_UB_22      0.0026133000
_diffrn_orient_matrix_UB_23      -0.0022327000
_diffrn_orient_matrix_UB_31      -0.0064682000
_diffrn_orient_matrix_UB_32      0.0256821000
_diffrn_orient_matrix_UB_33      -0.0312164000
_diffrn_oxdiff_digest_frames     
;
014a6c2231e60673a3ba0a2b5582dd226001962acb7
;
_diffrn_oxdiff_digest_hkl        
;
01dce08475e98abda01380f1a78eca99c2b341
;
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4716
_reflns_number_total             5715
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.01
_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 1.171.40.47a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.47a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.47a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.610
_refine_diff_density_min         -0.264
_refine_diff_density_rms         0.049
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     234
_refine_ls_number_reflns         5715
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0521
_refine_ls_R_factor_gt           0.0388
_refine_ls_restrained_S_all      1.070
_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)+(0.0412P)²+2.3832P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0970
_refine_ls_wR_factor_ref         0.1052
_refine_special_details          
'Disorder of the tolyl-ligand on a twofold axis (50:50). Influenced disorder of methylgroups C10 and C14 with the same occupation.'
_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. Others
 Fixed Sof: H9A(0.5) H9B(0.5) C10(0.5) H10A(0.5) H10B(0.5) H10C(0.5) C10B(0.5)
 H10D(0.5) H10E(0.5) H10F(0.5) H12(0.5) H12A(0.5) C14(0.5) H14A(0.5) H14B(0.5)
 H14C(0.5) C14B(0.5) H14D(0.5) H14E(0.5) H14F(0.5) C15(0.5) C16(0.5) H16(0.5)
 C17(0.5) C18(0.5) H18(0.5) C19(0.5) H19(0.5) C20(0.5) H20(0.5) C21(0.5)
 H21A(0.5) H21B(0.5) H21C(0.5)
3.a Ternary CH refined with riding coordinates:
 C9(H9A), C9(H9B), C12(H12), C12(H12A)
3.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C16(H16), C18(H18), C19(H19), C20(H20)
3.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C10B(H10D,H10E,H10F), C11(H11A,H11B,H11C), C13(H13A,H13B,
 H13C), C14(H14A,H14B,H14C), C14B(H14D,H14E,H14F), C21(H21A,H21B,H21C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
P1 P 0.44278(3) 0.60189(2) 0.66249(2) 0.02286(8) Uani 1 1 d . . . . .
P2 P 0.500000 0.68516(2) 0.750000 0.02432(9) Uani 1 2 d S T P . .
N1 N 0.45656(10) 0.42124(6) 0.69291(5) 0.0267(2) Uani 1 1 d . . . . .
C1 C 0.500000 0.37063(10) 0.750000 0.0324(4) Uani 1 2 d S T P . .
C2 C 0.47407(10) 0.50779(6) 0.71324(5) 0.02115(19) Uani 1 1 d . . . . .
C3 C 0.40956(13) 0.39264(7) 0.61994(5) 0.0281(2) Uani 1 1 d . . . . .
C4 C 0.49747(14) 0.36378(7) 0.58110(6) 0.0318(3) Uani 1 1 d . . . . .
C5 C 0.44942(17) 0.33704(8) 0.51054(6) 0.0403(3) Uani 1 1 d . . . . .
H5 H 0.504548 0.316619 0.483246 0.048 Uiso 1 1 calc R . . . .
C6 C 0.32262(17) 0.34037(8) 0.48085(6) 0.0450(4) Uani 1 1 d . . . . .
H6 H 0.293037 0.321751 0.434023 0.054 Uiso 1 1 calc R . . . .
C7 C 0.23848(16) 0.37112(9) 0.51984(7) 0.0408(3) Uani 1 1 d . . . . .
H7 H 0.153073 0.373997 0.498637 0.049 Uiso 1 1 calc R . . . .
C8 C 0.28034(14) 0.39800(7) 0.59090(6) 0.0323(3) Uani 1 1 d . . . . .
C9 C 0.63833(15) 0.36456(9) 0.60991(7) 0.0399(3) Uani 1 1 d . . . . .
H9A H 0.648881 0.373769 0.661589 0.048 Uiso 0.5 1 calc R . . A 1
H9B H 0.658546 0.384451 0.659707 0.048 Uiso 0.5 1 calc R . . B 2
C10 C 0.7085(5) 0.4440(3) 0.5821(3) 0.0440(10) Uani 0.5 1 d . . . C 1
H10A H 0.698629 0.440373 0.531044 0.066 Uiso 0.5 1 calc GR . . C 1
H10B H 0.796561 0.442572 0.604395 0.066 Uiso 0.5 1 calc GR . . C 1
H10C H 0.672279 0.496678 0.594219 0.066 Uiso 0.5 1 calc GR . . C 1
C10B C 0.6881(6) 0.4252(4) 0.5625(3) 0.0389(9) Uani 0.5 1 d . . . C 2
H10D H 0.667810 0.404340 0.514072 0.058 Uiso 0.5 1 calc GR . . C 2
H10E H 0.778009 0.429610 0.578133 0.058 Uiso 0.5 1 calc GR . . C 2
H10F H 0.650626 0.480576 0.564602 0.058 Uiso 0.5 1 calc GR . . C 2
C11 C 0.6993(2) 0.27753(11) 0.60290(10) 0.0634(5) Uani 1 1 d . . . . .
H11A H 0.658087 0.234256 0.625343 0.095 Uiso 1 1 calc GR . . . .
H11B H 0.787026 0.279780 0.625829 0.095 Uiso 1 1 calc GR . . . .
H11C H 0.691047 0.263889 0.553110 0.095 Uiso 1 1 calc GR . . . .
C12 C 0.18446(14) 0.43208(10) 0.63141(8) 0.0412(3) Uani 1 1 d . . . . .
H12 H 0.234095 0.449627 0.678277 0.049 Uiso 0.5 1 calc R . . D 1
H12A H 0.223704 0.441456 0.681989 0.049 Uiso 0.5 1 calc R . . E 2
C13 C 0.12277(14) 0.51432(10) 0.59732(8) 0.0433(3) Uani 1 1 d . . . . .
H13A H 0.186088 0.557633 0.598708 0.065 Uiso 1 1 calc GR . . . .
H13B H 0.061640 0.533794 0.623370 0.065 Uiso 1 1 calc GR . . . .
H13C H 0.081800 0.503246 0.548456 0.065 Uiso 1 1 calc GR . . . .
C14 C 0.1037(3) 0.3586(3) 0.6470(3) 0.0529(10) Uani 0.5 1 d . . . F 1
H14A H 0.053460 0.337298 0.602877 0.079 Uiso 0.5 1 calc GR . . F 1
H14B H 0.049353 0.378270 0.677269 0.079 Uiso 0.5 1 calc GR . . F 1
H14C H 0.156818 0.313516 0.670809 0.079 Uiso 0.5 1 calc GR . . F 1
C14B C 0.0615(3) 0.3716(3) 0.6237(2) 0.0479(9) Uani 0.5 1 d . . . F 2
H14D H 0.017161 0.370389 0.574500 0.072 Uiso 0.5 1 calc GR . . F 2
H14E H 0.007168 0.394027 0.652843 0.072 Uiso 0.5 1 calc GR . . F 2
H14F H 0.087224 0.314570 0.639094 0.072 Uiso 0.5 1 calc GR . . F 2
C15 C 0.52997(16) 0.27621(12) 0.75315(12) 0.0180(4) Uani 0.5 1 d . . . G -1
C16 C 0.4245(2) 0.22440(13) 0.73027(10) 0.0197(3) Uani 0.5 1 d . . . G -1
H16 H 0.346182 0.249468 0.712957 0.024 Uiso 0.5 1 calc R . . G -1
C17 C 0.4353(2) 0.13506(18) 0.73308(13) 0.0218(5) Uani 0.5 1 d . . . G -1
C18 C 0.5547(3) 0.10013(18) 0.75892(14) 0.0236(5) Uani 0.5 1 d . . . G -1
H18 H 0.563407 0.040841 0.761832 0.028 Uiso 0.5 1 calc R . . G -1
C19 C 0.6611(2) 0.15112(14) 0.78044(11) 0.0240(4) Uani 0.5 1 d . . . G -1
H19 H 0.739912 0.126136 0.796500 0.029 Uiso 0.5 1 calc R . . G -1
C20 C 0.6486(2) 0.23973(14) 0.77773(11) 0.0223(4) Uani 0.5 1 d . . . G -1
H20 H 0.719016 0.274555 0.792219 0.027 Uiso 0.5 1 calc R . . G -1
C21 C 0.3222(2) 0.07861(15) 0.70971(14) 0.0323(5) Uani 0.5 1 d . . . G -1
H21A H 0.257282 0.095596 0.733946 0.049 Uiso 0.5 1 calc GR . . G -1
H21B H 0.345328 0.020078 0.721315 0.049 Uiso 0.5 1 calc GR . . G -1
H21C H 0.291719 0.084003 0.658902 0.049 Uiso 0.5 1 calc GR . . G -1


_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
P1 P2 2.1032(4) . ?
P1 C2 1.7516(10) . ?
N1 C1 1.3472(13) . ?
N1 C2 1.4063(13) . ?
N1 C3 1.4485(13) . ?
C1 C15 1.507(2) . ?
C2 C2 1.3971(19) 2_656 ?
C3 C4 1.4025(17) . ?
C3 C8 1.3961(19) . ?
C4 C5 1.4010(17) . ?
C4 C9 1.510(2) . ?
C5 H5 0.9300 . ?
C5 C6 1.373(2) . ?
C6 H6 0.9300 . ?
C6 C7 1.382(2) . ?
C7 H7 0.9300 . ?
C7 C8 1.4006(17) . ?
C8 C12 1.520(2) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 C10 1.603(6) . ?
C9 C10B 1.489(7) . ?
C9 C11 1.528(2) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C10B H10D 0.9600 . ?
C10B H10E 0.9600 . ?
C10B H10F 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 H12 0.9800 . ?
C12 H12A 0.9800 . ?
C12 C13 1.527(2) . ?
C12 C14 1.511(4) . ?
C12 C14B 1.614(4) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C14B H14D 0.9600 . ?
C14B H14E 0.9600 . ?
C14B H14F 0.9600 . ?
C15 C16 1.393(3) . ?
C15 C20 1.394(3) . ?
C16 H16 0.9300 . ?
C16 C17 1.398(3) . ?
C17 C18 1.396(3) . ?
C17 C21 1.498(3) . ?
C18 H18 0.9300 . ?
C18 C19 1.390(3) . ?
C19 H19 0.9300 . ?
C19 C20 1.388(3) . ?
C20 H20 0.9300 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?

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 P1 P2 95.05(3) . . ?
P1 P2 P1 103.73(2) 2_656 . ?
C1 N1 C2 109.61(9) . . ?
C1 N1 C3 126.09(10) . . ?
C2 N1 C3 124.08(9) . . ?
N1 C1 N1 108.27(13) . 2_656 ?
N1 C1 C15 129.81(11) . . ?
N1 C1 C15 120.34(10) 2_656 . ?
N1 C2 P1 130.74(7) . . ?
C2 C2 P1 123.04(3) 2_656 . ?
C2 C2 N1 106.21(5) 2_656 . ?
C4 C3 N1 117.95(12) . . ?
C8 C3 N1 118.75(11) . . ?
C8 C3 C4 123.26(10) . . ?
C3 C4 C9 123.72(11) . . ?
C5 C4 C3 116.70(13) . . ?
C5 C4 C9 119.50(12) . . ?
C4 C5 H5 119.3 . . ?
C6 C5 C4 121.34(13) . . ?
C6 C5 H5 119.3 . . ?
C5 C6 H6 119.7 . . ?
C5 C6 C7 120.68(12) . . ?
C7 C6 H6 119.7 . . ?
C6 C7 H7 119.6 . . ?
C6 C7 C8 120.77(15) . . ?
C8 C7 H7 119.6 . . ?
C3 C8 C7 117.21(12) . . ?
C3 C8 C12 123.91(11) . . ?
C7 C8 C12 118.88(13) . . ?
C4 C9 H9A 105.0 . . ?
C4 C9 H9B 110.8 . . ?
C4 C9 C10 113.6(2) . . ?
C4 C9 C11 112.62(14) . . ?
C10 C9 H9A 105.0 . . ?
C10B C9 C4 104.7(2) . . ?
C10B C9 H9B 110.8 . . ?
C10B C9 C11 106.9(3) . . ?
C11 C9 H9A 105.0 . . ?
C11 C9 H9B 110.8 . . ?
C11 C9 C10 114.3(3) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C10B H10D 109.5 . . ?
C9 C10B H10E 109.5 . . ?
C9 C10B H10F 109.5 . . ?
H10D C10B H10E 109.5 . . ?
H10D C10B H10F 109.5 . . ?
H10E C10B H10F 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C8 C12 H12 105.1 . . ?
C8 C12 H12A 110.7 . . ?
C8 C12 C13 111.24(11) . . ?
C8 C12 C14B 113.1(2) . . ?
C13 C12 H12 105.1 . . ?
C13 C12 H12A 110.7 . . ?
C13 C12 C14B 99.97(18) . . ?
C14 C12 C8 109.0(2) . . ?
C14 C12 H12 105.1 . . ?
C14 C12 C13 120.08(19) . . ?
C14B C12 H12A 110.7 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C12 C14B H14D 109.5 . . ?
C12 C14B H14E 109.5 . . ?
C12 C14B H14F 109.5 . . ?
H14D C14B H14E 109.5 . . ?
H14D C14B H14F 109.5 . . ?
H14E C14B H14F 109.5 . . ?
C16 C15 C1 113.49(15) . . ?
C16 C15 C20 120.5(2) . . ?
C20 C15 C1 126.04(16) . . ?
C15 C16 H16 119.7 . . ?
C15 C16 C17 120.6(2) . . ?
C17 C16 H16 119.7 . . ?
C16 C17 C21 121.2(2) . . ?
C18 C17 C16 117.8(2) . . ?
C18 C17 C21 121.04(18) . . ?
C17 C18 H18 118.9 . . ?
C19 C18 C17 122.1(2) . . ?
C19 C18 H18 118.9 . . ?
C18 C19 H19 120.3 . . ?
C20 C19 C18 119.3(2) . . ?
C20 C19 H19 120.3 . . ?
C15 C20 H20 120.2 . . ?
C19 C20 C15 119.6(2) . . ?
C19 C20 H20 120.2 . . ?
C17 C21 H21A 109.5 . . ?
C17 C21 H21B 109.5 . . ?
C17 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?

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
P2 P1 C2 N1 178.08(10) . . . . ?
P2 P1 C2 C2 -2.48(13) . . . 2_656 ?
N1 C1 C15 C16 -65.6(2) . . . . ?
N1 C1 C15 C16 130.53(15) 2_656 . . . ?
N1 C1 C15 C20 116.1(2) . . . . ?
N1 C1 C15 C20 -47.8(2) 2_656 . . . ?
N1 C3 C4 C5 -179.60(10) . . . . ?
N1 C3 C4 C9 -2.81(16) . . . . ?
N1 C3 C8 C7 178.97(10) . . . . ?
N1 C3 C8 C12 -0.18(17) . . . . ?
C1 N1 C2 P1 177.09(7) . . . . ?
C1 N1 C2 C2 -2.42(14) . . . 2_656 ?
C1 N1 C3 C4 -74.10(14) . . . . ?
C1 N1 C3 C8 108.21(12) . . . . ?
C1 C15 C16 C17 -176.95(18) . . . . ?
C1 C15 C20 C19 177.17(18) . . . . ?
C2 N1 C1 N1 0.93(5) . . . 2_656 ?
C2 N1 C1 C15 -164.44(11) . . . . ?
C2 N1 C3 C4 99.80(13) . . . . ?
C2 N1 C3 C8 -77.89(14) . . . . ?
C3 N1 C1 N1 175.57(13) . . . 2_656 ?
C3 N1 C1 C15 10.19(17) . . . . ?
C3 N1 C2 P1 2.32(18) . . . . ?
C3 N1 C2 C2 -177.19(12) . . . 2_656 ?
C3 C4 C5 C6 0.99(17) . . . . ?
C3 C4 C9 C10 -99.8(2) . . . . ?
C3 C4 C9 C10B -116.1(2) . . . . ?
C3 C4 C9 C11 128.15(13) . . . . ?
C3 C8 C12 C13 115.20(14) . . . . ?
C3 C8 C12 C14 -110.2(2) . . . . ?
C3 C8 C12 C14B -133.25(18) . . . . ?
C4 C3 C8 C7 1.40(17) . . . . ?
C4 C3 C8 C12 -177.74(11) . . . . ?
C4 C5 C6 C7 0.58(19) . . . . ?
C5 C4 C9 C10 76.9(3) . . . . ?
C5 C4 C9 C10B 60.6(2) . . . . ?
C5 C4 C9 C11 -55.15(16) . . . . ?
C5 C6 C7 C8 -1.2(2) . . . . ?
C6 C7 C8 C3 0.27(18) . . . . ?
C6 C7 C8 C12 179.46(12) . . . . ?
C7 C8 C12 C13 -63.93(15) . . . . ?
C7 C8 C12 C14 70.7(2) . . . . ?
C7 C8 C12 C14B 47.6(2) . . . . ?
C8 C3 C4 C5 -2.02(16) . . . . ?
C8 C3 C4 C9 174.77(11) . . . . ?
C9 C4 C5 C6 -175.93(11) . . . . ?
C15 C16 C17 C18 -0.5(3) . . . . ?
C15 C16 C17 C21 179.0(2) . . . . ?
C16 C15 C20 C19 -1.0(3) . . . . ?
C16 C17 C18 C19 -0.9(3) . . . . ?
C17 C18 C19 C20 1.4(3) . . . . ?
C18 C19 C20 C15 -0.4(3) . . . . ?
C20 C15 C16 C17 1.5(3) . . . . ?
C21 C17 C18 C19 179.5(3) . . . . ?

_olex2_date_sample_data_collection 2019-04-05
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.108
_oxdiff_exptl_absorpt_empirical_full_min 0.892
####################################################################### 
# 
# 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_compound5c
_database_code_depnum_ccdc_archive 'CCDC 1939614'
loop_
_audit_author_name
_audit_author_address
'Hans Georg Stammler'
;University of Bielefeld
Germany
;
_audit_update_record             
;
2019-07-10 deposited with the CCDC.	2019-10-18 downloaded from the CCDC.
;



_audit_creation_date             2019-04-05
_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         'C38 H39 Mo N2 O5 P3'
_chemical_formula_sum            'C38 H39 Mo N2 O5 P3'
_chemical_formula_weight         792.56
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C38 H39 Mo N2 O5 P3'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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 -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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                   12.68020(10)
_cell_length_b                   13.72590(10)
_cell_length_c                   23.0210(2)
_cell_angle_alpha                93.5620(10)
_cell_angle_beta                 101.0270(10)
_cell_angle_gamma                98.0390(10)
_cell_volume                     3877.80(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    105202
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      32.6150
_cell_measurement_theta_min      3.0660
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.505
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.463
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.47a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.358
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1632
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-2 1 5 0.0813
2 -1 -5 0.0813
-1 4 -5 0.0965
1 -4 5 0.0965
5 3 3 0.0705
-1 0 -5 0.1035
-4 -3 5 0.0674
2 -5 3 0.0714
-1 -5 -4 0.1164
1 5 -2 0.0973
-5 -3 -1 0.0852

_exptl_crystal_size_max          0.196
_exptl_crystal_size_mid          0.167
_exptl_crystal_size_min          0.163
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-1.9908 0.9941 5.0075 -0.0593 -0.1062 -0.1354
1.9908 -0.9941 -5.0075 0.0593 0.1062 0.1354
-0.9941 4.0034 -4.9882 -0.0917 -0.1334 0.1993
0.9941 -4.0034 4.9882 0.0917 0.1334 -0.1993
5.0041 2.9785 2.9881 0.3268 -0.1929 0.0145
-1.0035 0.0107 -4.9956 -0.1075 0.0627 0.1278
-3.9979 -2.9942 5.0068 -0.1890 0.0937 -0.2240
1.9888 -5.0004 2.9835 0.1244 0.2049 -0.1542
-1.0143 -4.9820 -4.0049 -0.1171 0.2957 0.0111
1.0087 4.9921 -1.9938 0.0565 -0.2227 0.1525
-5.0022 -2.9819 -0.9885 -0.3066 0.1686 -0.0690

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0347
_diffrn_reflns_av_unetI/netI     0.0216
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            240247
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.846
_diffrn_reflns_theta_min         2.607
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -88.00  13.00   1.00   10.00    --  -17.14 -77.00 120.00  101
  2  ω    -75.00 -27.00   1.00   10.00    --  -17.14 131.00  91.94   48
  3  ω     -8.00  86.00   1.00   10.00    --   17.14  57.00 -60.00   94
  4  ω    -51.00  42.00   1.00   10.00    --   17.14 -57.00  30.00   93
  5  ω    -51.00  42.00   1.00   10.00    --   17.14 -57.00 150.00   93
  6  ω     -8.00  86.00   1.00   10.00    --   17.14  57.00  60.00   94
  7  ω     -8.00  86.00   1.00   10.00    --   17.14  57.00-180.00   94
  8  ω    -51.00  42.00   1.00   10.00    --   17.14 -57.00-120.00   93
  9  ω     17.00  91.00   1.00   10.00    --   17.14-154.00  19.71   74
 10  ω    -76.00 -27.00   1.00   10.00    --  -17.14 132.00  -0.72   49
 11  ω    -75.00 -27.00   1.00   10.00    --  -17.14 131.00 -56.72   48
 12  ω    -72.00 -24.00   1.00   10.00    --  -17.14 126.00 178.71   48
 13  ω    -76.00 -27.00   1.00   10.00    --  -17.14 132.00  30.84   49
 14  ω     17.00  91.00   1.00   10.00    --   17.14-154.00 117.32   74
 15  ω     18.00  92.00   1.00   10.00    --   17.14-156.00 -31.31   74
 16  ω      3.00  72.00   1.00   10.00    --   17.14-126.00-157.63   69
 17  ω     35.00 101.00   1.00   10.00    --   17.14 178.00-180.00   66
 18  ω   -102.00 -55.00   1.00   10.00    --  -17.14 178.00  30.00   47
 19  ω    -20.00  56.00   1.00   10.00    --   17.14 -99.00 -90.00   76
 20  ω    -54.00  38.00   1.00   10.00    --   17.14 -38.00-150.00   92
 21  ω    -13.00  88.00   1.00   10.00    --   17.14  77.00 150.00  101
 22  ω     -4.00  88.00   1.00   10.00    --   17.14  38.00   0.00   92
 23  ω    -51.00  42.00   1.00   10.00    --   17.14 -57.00-180.00   93
 24  ω    -68.00   5.00   1.00   10.00    --   17.14   0.00-180.00   73
 25  ω      6.00  76.00   1.00   10.00    --   17.14-132.00-107.65   70
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0570247000
_diffrn_orient_matrix_UB_12      0.0038089000
_diffrn_orient_matrix_UB_13      0.0100663000
_diffrn_orient_matrix_UB_21      -0.0020164000
_diffrn_orient_matrix_UB_22      -0.0490919000
_diffrn_orient_matrix_UB_23      -0.0122560000
_diffrn_orient_matrix_UB_31      0.0084727000
_diffrn_orient_matrix_UB_32      0.0179479000
_diffrn_orient_matrix_UB_33      -0.0272422000
_diffrn_oxdiff_digest_frames     
;
01ee8ab338ebed4b1acc0e3be826262166019852c52
;
_diffrn_oxdiff_digest_hkl        
;
018c117ea63cae84997943726e38057fe48e71
;
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                24041
_reflns_number_total             27490
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.01
_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 1.171.40.47a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.47a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.47a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.644
_refine_diff_density_min         -0.581
_refine_diff_density_rms         0.062
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     899
_refine_ls_number_reflns         27490
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0356
_refine_ls_R_factor_gt           0.0279
_refine_ls_restrained_S_all      1.055
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0213P)²+2.4112P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0619
_refine_ls_wR_factor_ref         0.0652
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C10(H10), C13(H13), C22(H22), C25(H25), C48(H48), C51(H51), C60(H60), C63(H63)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C18(H18), C19(H19), C20(H20), C29(H29), C30(H30),
 C31(H31), C32(H32), C33(H33), C44(H44), C45(H45), C46(H46), C56(H56), C57(H57),
  C58(H58), C67(H67), C68(H68), C69(H69), C70(H70), C71(H71)
2.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A,
 H27B,H27C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C), C52(H52A,H52B,H52C),
 C53(H53A,H53B,H53C), C61(H61A,H61B,H61C), C62(H62A,H62B,H62C), C64(H64A,H64B,
 H64C), C65(H65A,H65B,H65C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
Mo1 Mo 0.18643(2) 0.29841(2) 0.21741(2) 0.01505(2) Uani 1 1 d . . . . .
Mo2 Mo 0.73712(2) 1.17269(2) 0.27633(2) 0.01544(2) Uani 1 1 d . . . . .
P1 P 0.36956(3) 0.49810(2) 0.12609(2) 0.01658(6) Uani 1 1 d . . . . .
P2 P 0.24231(3) 0.45005(2) 0.16840(2) 0.01681(6) Uani 1 1 d . . . . .
P3 P 0.15094(3) 0.56469(2) 0.17083(2) 0.01758(6) Uani 1 1 d . . . . .
P4 P 0.89613(2) 0.93948(2) 0.32974(2) 0.01449(5) Uani 1 1 d . . . . .
P5 P 0.76519(3) 1.01754(2) 0.32595(2) 0.01571(5) Uani 1 1 d . . . . .
P6 P 0.64982(3) 0.93594(2) 0.36557(2) 0.01673(6) Uani 1 1 d . . . . .
O1 O 0.42749(10) 0.25615(9) 0.26513(7) 0.0485(3) Uani 1 1 d . . . . .
O2 O 0.21554(10) 0.44266(9) 0.33472(5) 0.0375(3) Uani 1 1 d . . . . .
O3 O -0.05751(8) 0.33599(8) 0.17507(5) 0.0291(2) Uani 1 1 d . . . . .
O4 O 0.17729(14) 0.15402(11) 0.10183(5) 0.0567(4) Uani 1 1 d . . . . .
O5 O 0.07986(9) 0.12385(7) 0.27944(5) 0.0286(2) Uani 1 1 d . . . . .
O6 O 0.97057(9) 1.29653(8) 0.33174(5) 0.0288(2) Uani 1 1 d . . . . .
O7 O 0.84019(11) 1.09449(9) 0.16966(5) 0.0406(3) Uani 1 1 d . . . . .
O8 O 0.50972(12) 1.05873(13) 0.20456(7) 0.0635(4) Uani 1 1 d . . . . .
O9 O 0.63840(10) 1.24225(9) 0.38634(5) 0.0380(3) Uani 1 1 d . . . . .
O10 O 0.67736(11) 1.36554(8) 0.21967(5) 0.0360(3) Uani 1 1 d . . . . .
N1 N 0.37262(8) 0.69606(7) 0.09091(4) 0.01376(17) Uani 1 1 d . . . . .
N2 N 0.22612(8) 0.73517(7) 0.11661(4) 0.01475(17) Uani 1 1 d . . . . .
N3 N 0.87274(7) 0.76012(7) 0.38573(4) 0.01169(16) Uani 1 1 d . . . . .
N4 N 0.71732(8) 0.76042(7) 0.41393(4) 0.01301(16) Uani 1 1 d . . . . .
C1 C 0.30949(9) 0.76742(8) 0.09063(5) 0.01499(19) Uani 1 1 d . . . . .
C2 C 0.32785(9) 0.61440(8) 0.11698(5) 0.01337(19) Uani 1 1 d . . . . .
C3 C 0.23527(9) 0.64071(8) 0.13440(5) 0.01406(19) Uani 1 1 d . . . . .
C4 C 0.46511(9) 0.69623(8) 0.06267(5) 0.01415(19) Uani 1 1 d . . . . .
C5 C 0.44552(9) 0.67971(8) 0.00058(5) 0.01435(19) Uani 1 1 d . . . . .
C6 C 0.53597(10) 0.67754(9) -0.02540(5) 0.0177(2) Uani 1 1 d . . . . .
H6 H 0.526198 0.667109 -0.066516 0.021 Uiso 1 1 calc R . . . .
C7 C 0.63989(10) 0.69063(9) 0.00888(6) 0.0199(2) Uani 1 1 d . . . . .
H7 H 0.699121 0.688700 -0.009320 0.024 Uiso 1 1 calc R . . . .
C8 C 0.65640(10) 0.70656(10) 0.07006(6) 0.0220(2) Uani 1 1 d . . . . .
H8 H 0.726846 0.715539 0.092505 0.026 Uiso 1 1 calc R . . . .
C9 C 0.56934(10) 0.70942(10) 0.09870(5) 0.0196(2) Uani 1 1 d . . . . .
C10 C 0.33306(10) 0.66421(9) -0.03876(5) 0.0185(2) Uani 1 1 d . . . . .
H10 H 0.279743 0.665470 -0.013115 0.022 Uiso 1 1 calc R . . . .
C11 C 0.30937(13) 0.56348(10) -0.07505(6) 0.0285(3) Uani 1 1 d . . . . .
H11A H 0.359714 0.561258 -0.101217 0.043 Uiso 1 1 calc GR . . . .
H11B H 0.236477 0.553722 -0.098029 0.043 Uiso 1 1 calc GR . . . .
H11C H 0.317062 0.512297 -0.048662 0.043 Uiso 1 1 calc GR . . . .
C12 C 0.32087(11) 0.74786(11) -0.07967(6) 0.0253(3) Uani 1 1 d . . . . .
H12A H 0.333550 0.810063 -0.056013 0.038 Uiso 1 1 calc GR . . . .
H12B H 0.248655 0.737655 -0.103510 0.038 Uiso 1 1 calc GR . . . .
H12C H 0.372771 0.748176 -0.105060 0.038 Uiso 1 1 calc GR . . . .
C13 C 0.59095(11) 0.72561(14) 0.16618(6) 0.0338(4) Uani 1 1 d . . . . .
H13 H 0.521553 0.729807 0.178239 0.041 Uiso 1 1 calc R . . . .
C14 C 0.63779(13) 0.63848(16) 0.19422(7) 0.0415(4) Uani 1 1 d . . . . .
H14A H 0.585893 0.579252 0.182593 0.062 Uiso 1 1 calc GR . . . .
H14B H 0.653207 0.651046 0.236721 0.062 Uiso 1 1 calc GR . . . .
H14C H 0.703634 0.630555 0.180923 0.062 Uiso 1 1 calc GR . . . .
C15 C 0.66810(14) 0.82219(16) 0.18926(8) 0.0482(5) Uani 1 1 d . . . . .
H15A H 0.737729 0.818363 0.179419 0.072 Uiso 1 1 calc GR . . . .
H15B H 0.676375 0.832427 0.231621 0.072 Uiso 1 1 calc GR . . . .
H15C H 0.638532 0.876293 0.171191 0.072 Uiso 1 1 calc GR . . . .
C16 C 0.13619(9) 0.78726(8) 0.12172(5) 0.0160(2) Uani 1 1 d . . . . .
C17 C 0.03823(10) 0.75653(9) 0.08087(5) 0.0181(2) Uani 1 1 d . . . . .
C18 C -0.04542(10) 0.81164(10) 0.08364(6) 0.0227(2) Uani 1 1 d . . . . .
H18 H -0.111415 0.794527 0.056876 0.027 Uiso 1 1 calc R . . . .
C19 C -0.03157(11) 0.89145(10) 0.12566(7) 0.0257(3) Uani 1 1 d . . . . .
H19 H -0.088059 0.927711 0.126488 0.031 Uiso 1 1 calc R . . . .
C20 C 0.06524(11) 0.91788(9) 0.16642(6) 0.0233(2) Uani 1 1 d . . . . .
H20 H 0.072175 0.970673 0.194935 0.028 Uiso 1 1 calc R . . . .
C21 C 0.15284(10) 0.86675(9) 0.16555(6) 0.0180(2) Uani 1 1 d . . . . .
C22 C 0.02029(11) 0.66786(10) 0.03491(6) 0.0222(2) Uani 1 1 d . . . . .
H22 H 0.086617 0.637524 0.040789 0.027 Uiso 1 1 calc R . . . .
C23 C -0.07327(12) 0.59088(11) 0.04417(8) 0.0309(3) Uani 1 1 d . . . . .
H23A H -0.057545 0.571247 0.083818 0.046 Uiso 1 1 calc GR . . . .
H23B H -0.081590 0.534242 0.016101 0.046 Uiso 1 1 calc GR . . . .
H23C H -0.139364 0.618891 0.038385 0.046 Uiso 1 1 calc GR . . . .
C24 C -0.00195(18) 0.69669(14) -0.02869(7) 0.0450(4) Uani 1 1 d . . . . .
H24A H -0.064767 0.729445 -0.034917 0.068 Uiso 1 1 calc GR . . . .
H24B H -0.014915 0.638408 -0.055921 0.068 Uiso 1 1 calc GR . . . .
H24C H 0.059836 0.740386 -0.035265 0.068 Uiso 1 1 calc GR . . . .
C25 C 0.25905(11) 0.89405(9) 0.21088(6) 0.0208(2) Uani 1 1 d . . . . .
H25 H 0.318600 0.883581 0.190792 0.025 Uiso 1 1 calc R . . . .
C26 C 0.26271(17) 0.82742(14) 0.26170(8) 0.0477(5) Uani 1 1 d . . . . .
H26A H 0.206291 0.837666 0.282855 0.072 Uiso 1 1 calc GR . . . .
H26B H 0.332164 0.843110 0.288321 0.072 Uiso 1 1 calc GR . . . .
H26C H 0.251974 0.759578 0.245885 0.072 Uiso 1 1 calc GR . . . .
C27 C 0.28015(16) 1.00094(12) 0.23727(10) 0.0490(5) Uani 1 1 d . . . . .
H27A H 0.278228 1.043928 0.205869 0.074 Uiso 1 1 calc GR . . . .
H27B H 0.350341 1.014322 0.263302 0.074 Uiso 1 1 calc GR . . . .
H27C H 0.225200 1.012085 0.259307 0.074 Uiso 1 1 calc GR . . . .
C28 C 0.32911(11) 0.86444(9) 0.06793(6) 0.0206(2) Uani 1 1 d . . . . .
C29 C 0.24502(13) 0.90314(11) 0.03362(8) 0.0328(3) Uani 1 1 d . . . . .
H29 H 0.175174 0.867287 0.024248 0.039 Uiso 1 1 calc R . . . .
C30 C 0.26607(18) 0.99587(13) 0.01342(9) 0.0477(5) Uani 1 1 d . . . . .
H30 H 0.210114 1.021894 -0.009730 0.057 Uiso 1 1 calc R . . . .
C31 C 0.3693(2) 1.04940(12) 0.02749(10) 0.0530(6) Uani 1 1 d . . . . .
H31 H 0.382816 1.111252 0.013687 0.064 Uiso 1 1 calc R . . . .
C32 C 0.45225(18) 1.01157(12) 0.06189(9) 0.0474(5) Uani 1 1 d . . . . .
H32 H 0.521645 1.048280 0.071596 0.057 Uiso 1 1 calc R . . . .
C33 C 0.43310(13) 0.91892(11) 0.08221(7) 0.0307(3) Uani 1 1 d . . . . .
H33 H 0.489550 0.893394 0.105279 0.037 Uiso 1 1 calc R . . . .
C34 C 0.34239(12) 0.27207(10) 0.24738(7) 0.0271(3) Uani 1 1 d . . . . .
C35 C 0.20305(11) 0.39065(10) 0.29260(6) 0.0223(2) Uani 1 1 d . . . . .
C36 C 0.17916(14) 0.20617(11) 0.14244(6) 0.0299(3) Uani 1 1 d . . . . .
C37 C 0.03012(11) 0.32337(9) 0.18933(5) 0.0198(2) Uani 1 1 d . . . . .
C38 C 0.12241(11) 0.18649(9) 0.25742(6) 0.0203(2) Uani 1 1 d . . . . .
C39 C 0.80268(9) 0.71127(8) 0.41509(5) 0.01246(18) Uani 1 1 d . . . . .
C40 C 0.83282(9) 0.84481(8) 0.36547(5) 0.01239(18) Uani 1 1 d . . . . .
C41 C 0.73227(9) 0.84422(8) 0.38227(5) 0.01342(19) Uani 1 1 d . . . . .
C42 C 0.98291(9) 0.74200(8) 0.38581(5) 0.01242(18) Uani 1 1 d . . . . .
C43 C 1.00452(9) 0.68665(8) 0.33736(5) 0.01472(19) Uani 1 1 d . . . . .
C44 C 1.11197(10) 0.67119(9) 0.34032(5) 0.0190(2) Uani 1 1 d . . . . .
H44 H 1.128944 0.633036 0.309586 0.023 Uiso 1 1 calc R . . . .
C45 C 1.19360(10) 0.71149(10) 0.38804(6) 0.0205(2) Uani 1 1 d . . . . .
H45 H 1.264522 0.700143 0.389086 0.025 Uiso 1 1 calc R . . . .
C46 C 1.17023(10) 0.76871(9) 0.43432(5) 0.0183(2) Uani 1 1 d . . . . .
H46 H 1.226063 0.796636 0.465733 0.022 Uiso 1 1 calc R . . . .
C47 C 1.06377(9) 0.78502(8) 0.43441(5) 0.01463(19) Uani 1 1 d . . . . .
C48 C 0.91958(10) 0.64858(9) 0.28184(5) 0.0172(2) Uani 1 1 d . . . . .
H48 H 0.847758 0.655215 0.290051 0.021 Uiso 1 1 calc R . . . .
C49 C 0.93953(11) 0.71276(10) 0.23151(5) 0.0206(2) Uani 1 1 d . . . . .
H49A H 0.931845 0.779667 0.242417 0.031 Uiso 1 1 calc GR . . . .
H49B H 0.887507 0.687873 0.195818 0.031 Uiso 1 1 calc GR . . . .
H49C H 1.011688 0.710862 0.224828 0.031 Uiso 1 1 calc GR . . . .
C50 C 0.91982(12) 0.53971(10) 0.26208(6) 0.0247(3) Uani 1 1 d . . . . .
H50A H 0.985782 0.533356 0.248516 0.037 Uiso 1 1 calc GR . . . .
H50B H 0.858533 0.516920 0.230359 0.037 Uiso 1 1 calc GR . . . .
H50C H 0.915297 0.500792 0.295005 0.037 Uiso 1 1 calc GR . . . .
C51 C 1.03998(10) 0.84660(8) 0.48592(5) 0.0164(2) Uani 1 1 d . . . . .
H51 H 0.964094 0.857318 0.475619 0.020 Uiso 1 1 calc R . . . .
C52 C 1.11239(11) 0.94775(9) 0.49664(6) 0.0235(2) Uani 1 1 d . . . . .
H52A H 1.187331 0.938991 0.506422 0.035 Uiso 1 1 calc GR . . . .
H52B H 1.094886 0.985883 0.528893 0.035 Uiso 1 1 calc GR . . . .
H52C H 1.100346 0.981783 0.461343 0.035 Uiso 1 1 calc GR . . . .
C53 C 1.05414(11) 0.79375(10) 0.54297(5) 0.0220(2) Uani 1 1 d . . . . .
H53A H 1.008449 0.730499 0.535919 0.033 Uiso 1 1 calc GR . . . .
H53B H 1.034133 0.832873 0.573963 0.033 Uiso 1 1 calc GR . . . .
H53C H 1.128712 0.784767 0.554764 0.033 Uiso 1 1 calc GR . . . .
C54 C 0.62358(9) 0.72535(9) 0.43874(5) 0.01491(19) Uani 1 1 d . . . . .
C55 C 0.61482(10) 0.76833(9) 0.49423(5) 0.0189(2) Uani 1 1 d . . . . .
C56 C 0.52895(11) 0.72617(11) 0.51894(6) 0.0257(3) Uani 1 1 d . . . . .
H56 H 0.520981 0.752663 0.555737 0.031 Uiso 1 1 calc R . . . .
C57 C 0.45563(11) 0.64615(12) 0.49006(6) 0.0288(3) Uani 1 1 d . . . . .
H57 H 0.400101 0.618368 0.507901 0.035 Uiso 1 1 calc R . . . .
C58 C 0.46434(11) 0.60692(11) 0.43453(6) 0.0252(3) Uani 1 1 d . . . . .
H58 H 0.413553 0.553777 0.415085 0.030 Uiso 1 1 calc R . . . .
C59 C 0.54836(10) 0.64610(9) 0.40737(5) 0.0183(2) Uani 1 1 d . . . . .
C60 C 0.69112(11) 0.85822(10) 0.52731(6) 0.0221(2) Uani 1 1 d . . . . .
H60 H 0.746948 0.876951 0.504208 0.027 Uiso 1 1 calc R . . . .
C61 C 0.62835(14) 0.94509(11) 0.53245(7) 0.0316(3) Uani 1 1 d . . . . .
H61A H 0.597073 0.960635 0.493408 0.047 Uiso 1 1 calc GR . . . .
H61B H 0.677137 1.001636 0.553317 0.047 Uiso 1 1 calc GR . . . .
H61C H 0.571549 0.927370 0.553827 0.047 Uiso 1 1 calc GR . . . .
C62 C 0.74828(14) 0.83895(12) 0.58952(6) 0.0325(3) Uani 1 1 d . . . . .
H62A H 0.694926 0.821431 0.613110 0.049 Uiso 1 1 calc GR . . . .
H62B H 0.796421 0.897534 0.608043 0.049 Uiso 1 1 calc GR . . . .
H62C H 0.789291 0.785810 0.586375 0.049 Uiso 1 1 calc GR . . . .
C63 C 0.55114(11) 0.60506(10) 0.34493(6) 0.0239(3) Uani 1 1 d . . . . .
H63 H 0.620401 0.633752 0.335494 0.029 Uiso 1 1 calc R . . . .
C64 C 0.45909(13) 0.63835(15) 0.30085(7) 0.0373(4) Uani 1 1 d . . . . .
H64A H 0.390419 0.613694 0.310421 0.056 Uiso 1 1 calc GR . . . .
H64B H 0.460496 0.612960 0.261239 0.056 Uiso 1 1 calc GR . . . .
H64C H 0.468763 0.709218 0.303298 0.056 Uiso 1 1 calc GR . . . .
C65 C 0.54389(15) 0.49290(12) 0.33893(9) 0.0410(4) Uani 1 1 d . . . . .
H65A H 0.600758 0.473867 0.367833 0.061 Uiso 1 1 calc GR . . . .
H65B H 0.551812 0.471267 0.299753 0.061 Uiso 1 1 calc GR . . . .
H65C H 0.474536 0.462977 0.345446 0.061 Uiso 1 1 calc GR . . . .
C66 C 0.81682(9) 0.61858(8) 0.44176(5) 0.01407(19) Uani 1 1 d . . . . .
C67 C 0.80709(11) 0.60703(9) 0.50030(5) 0.0207(2) Uani 1 1 d . . . . .
H67 H 0.787585 0.657627 0.522828 0.025 Uiso 1 1 calc R . . . .
C68 C 0.82649(13) 0.52017(10) 0.52486(6) 0.0276(3) Uani 1 1 d . . . . .
H68 H 0.820342 0.512587 0.563991 0.033 Uiso 1 1 calc R . . . .
C69 C 0.85500(14) 0.44460(10) 0.49139(7) 0.0315(3) Uani 1 1 d . . . . .
H69 H 0.869466 0.386897 0.508344 0.038 Uiso 1 1 calc R . . . .
C70 C 0.86204(15) 0.45455(10) 0.43288(7) 0.0325(3) Uani 1 1 d . . . . .
H70 H 0.879861 0.403116 0.410242 0.039 Uiso 1 1 calc R . . . .
C71 C 0.84251(12) 0.54133(9) 0.40789(6) 0.0227(2) Uani 1 1 d . . . . .
H71 H 0.846624 0.547811 0.368377 0.027 Uiso 1 1 calc R . . . .
C72 C 0.88766(11) 1.24943(9) 0.31382(5) 0.0204(2) Uani 1 1 d . . . . .
C73 C 0.80339(13) 1.12293(10) 0.20766(6) 0.0255(3) Uani 1 1 d . . . . .
C74 C 0.58987(13) 1.09963(12) 0.23168(7) 0.0328(3) Uani 1 1 d . . . . .
C75 C 0.67304(11) 1.21716(10) 0.34692(6) 0.0221(2) Uani 1 1 d . . . . .
C76 C 0.70125(12) 1.29497(10) 0.23927(6) 0.0238(3) 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
Mo1 P2 2.5083(3) . ?
Mo1 C34 2.0559(14) . ?
Mo1 C35 2.0390(13) . ?
Mo1 C36 2.0556(14) . ?
Mo1 C37 2.0473(13) . ?
Mo1 C38 1.9952(13) . ?
Mo2 P5 2.5150(3) . ?
Mo2 C72 2.0476(14) . ?
Mo2 C73 2.0508(13) . ?
Mo2 C74 2.0402(16) . ?
Mo2 C75 2.0480(13) . ?
Mo2 C76 1.9988(13) . ?
P1 P2 2.0907(4) . ?
P1 C2 1.7627(11) . ?
P2 P3 2.0846(4) . ?
P3 C3 1.7536(11) . ?
P4 P5 2.0895(4) . ?
P4 C40 1.7615(11) . ?
P5 P6 2.0991(4) . ?
P6 C41 1.7608(11) . ?
O1 C34 1.1347(18) . ?
O2 C35 1.1395(16) . ?
O3 C37 1.1374(16) . ?
O4 C36 1.1359(18) . ?
O5 C38 1.1472(16) . ?
O6 C72 1.1420(17) . ?
O7 C73 1.1403(17) . ?
O8 C74 1.137(2) . ?
O9 C75 1.1363(16) . ?
O10 C76 1.1478(16) . ?
N1 C1 1.3485(14) . ?
N1 C2 1.4052(14) . ?
N1 C4 1.4454(14) . ?
N2 C1 1.3472(14) . ?
N2 C3 1.3972(14) . ?
N2 C16 1.4471(14) . ?
N3 C39 1.3473(14) . ?
N3 C40 1.4024(13) . ?
N3 C42 1.4523(14) . ?
N4 C39 1.3501(14) . ?
N4 C41 1.4094(14) . ?
N4 C54 1.4507(14) . ?
C1 C28 1.4671(16) . ?
C2 C3 1.3964(15) . ?
C4 C5 1.4014(15) . ?
C4 C9 1.4009(16) . ?
C5 C6 1.3943(16) . ?
C5 C10 1.5153(16) . ?
C6 H6 0.9300 . ?
C6 C7 1.3821(17) . ?
C7 H7 0.9300 . ?
C7 C8 1.3825(18) . ?
C8 H8 0.9300 . ?
C8 C9 1.3935(17) . ?
C9 C13 1.5215(18) . ?
C10 H10 0.9800 . ?
C10 C11 1.5311(18) . ?
C10 C12 1.5355(18) . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13 0.9800 . ?
C13 C14 1.532(3) . ?
C13 C15 1.532(2) . ?
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 1.4008(17) . ?
C16 C21 1.4039(17) . ?
C17 C18 1.3948(17) . ?
C17 C22 1.5242(18) . ?
C18 H18 0.9300 . ?
C18 C19 1.384(2) . ?
C19 H19 0.9300 . ?
C19 C20 1.383(2) . ?
C20 H20 0.9300 . ?
C20 C21 1.3969(17) . ?
C21 C25 1.5218(18) . ?
C22 H22 0.9800 . ?
C22 C23 1.531(2) . ?
C22 C24 1.525(2) . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25 0.9800 . ?
C25 C26 1.527(2) . ?
C25 C27 1.520(2) . ?
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 1.390(2) . ?
C28 C33 1.391(2) . ?
C29 H29 0.9300 . ?
C29 C30 1.390(2) . ?
C30 H30 0.9300 . ?
C30 C31 1.377(3) . ?
C31 H31 0.9300 . ?
C31 C32 1.374(3) . ?
C32 H32 0.9300 . ?
C32 C33 1.388(2) . ?
C33 H33 0.9300 . ?
C39 C66 1.4651(15) . ?
C40 C41 1.4005(15) . ?
C42 C43 1.4023(15) . ?
C42 C47 1.4005(16) . ?
C43 C44 1.3976(16) . ?
C43 C48 1.5164(16) . ?
C44 H44 0.9300 . ?
C44 C45 1.3834(18) . ?
C45 H45 0.9300 . ?
C45 C46 1.3862(18) . ?
C46 H46 0.9300 . ?
C46 C47 1.3993(16) . ?
C47 C51 1.5149(16) . ?
C48 H48 0.9800 . ?
C48 C49 1.5361(17) . ?
C48 C50 1.5353(17) . ?
C49 H49A 0.9600 . ?
C49 H49B 0.9600 . ?
C49 H49C 0.9600 . ?
C50 H50A 0.9600 . ?
C50 H50B 0.9600 . ?
C50 H50C 0.9600 . ?
C51 H51 0.9800 . ?
C51 C52 1.5316(17) . ?
C51 C53 1.5324(16) . ?
C52 H52A 0.9600 . ?
C52 H52B 0.9600 . ?
C52 H52C 0.9600 . ?
C53 H53A 0.9600 . ?
C53 H53B 0.9600 . ?
C53 H53C 0.9600 . ?
C54 C55 1.4039(16) . ?
C54 C59 1.4012(17) . ?
C55 C56 1.3948(17) . ?
C55 C60 1.5186(18) . ?
C56 H56 0.9300 . ?
C56 C57 1.378(2) . ?
C57 H57 0.9300 . ?
C57 C58 1.386(2) . ?
C58 H58 0.9300 . ?
C58 C59 1.3969(17) . ?
C59 C63 1.5197(17) . ?
C60 H60 0.9800 . ?
C60 C61 1.5340(19) . ?
C60 C62 1.5329(19) . ?
C61 H61A 0.9600 . ?
C61 H61B 0.9600 . ?
C61 H61C 0.9600 . ?
C62 H62A 0.9600 . ?
C62 H62B 0.9600 . ?
C62 H62C 0.9600 . ?
C63 H63 0.9800 . ?
C63 C64 1.534(2) . ?
C63 C65 1.525(2) . ?
C64 H64A 0.9600 . ?
C64 H64B 0.9600 . ?
C64 H64C 0.9600 . ?
C65 H65A 0.9600 . ?
C65 H65B 0.9600 . ?
C65 H65C 0.9600 . ?
C66 C67 1.3931(16) . ?
C66 C71 1.3890(16) . ?
C67 H67 0.9300 . ?
C67 C68 1.3835(17) . ?
C68 H68 0.9300 . ?
C68 C69 1.3829(19) . ?
C69 H69 0.9300 . ?
C69 C70 1.381(2) . ?
C70 H70 0.9300 . ?
C70 C71 1.3873(18) . ?
C71 H71 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
C34 Mo1 P2 95.02(4) . . ?
C35 Mo1 P2 86.41(4) . . ?
C35 Mo1 C34 88.42(6) . . ?
C35 Mo1 C36 176.74(6) . . ?
C35 Mo1 C37 90.90(5) . . ?
C36 Mo1 P2 92.81(4) . . ?
C36 Mo1 C34 88.50(6) . . ?
C37 Mo1 P2 86.11(4) . . ?
C37 Mo1 C34 178.64(6) . . ?
C37 Mo1 C36 92.20(6) . . ?
C38 Mo1 P2 171.54(4) . . ?
C38 Mo1 C34 92.59(5) . . ?
C38 Mo1 C35 90.11(5) . . ?
C38 Mo1 C36 91.08(6) . . ?
C38 Mo1 C37 86.24(5) . . ?
C72 Mo2 P5 95.55(3) . . ?
C72 Mo2 C73 87.85(6) . . ?
C72 Mo2 C75 92.01(5) . . ?
C73 Mo2 P5 90.05(4) . . ?
C74 Mo2 P5 87.72(5) . . ?
C74 Mo2 C72 174.80(6) . . ?
C74 Mo2 C73 88.10(6) . . ?
C74 Mo2 C75 92.18(6) . . ?
C75 Mo2 P5 87.40(4) . . ?
C75 Mo2 C73 177.42(5) . . ?
C76 Mo2 P5 174.58(4) . . ?
C76 Mo2 C72 88.12(5) . . ?
C76 Mo2 C73 94.09(5) . . ?
C76 Mo2 C74 88.91(6) . . ?
C76 Mo2 C75 88.48(5) . . ?
C2 P1 P2 92.54(4) . . ?
P1 P2 Mo1 135.377(16) . . ?
P3 P2 Mo1 117.545(16) . . ?
P3 P2 P1 107.000(18) . . ?
C3 P3 P2 92.68(4) . . ?
C40 P4 P5 91.97(4) . . ?
P4 P5 Mo2 128.053(16) . . ?
P4 P5 P6 107.333(17) . . ?
P6 P5 Mo2 124.424(16) . . ?
C41 P6 P5 92.49(4) . . ?
C1 N1 C2 109.76(9) . . ?
C1 N1 C4 126.20(10) . . ?
C2 N1 C4 123.64(9) . . ?
C1 N2 C3 109.90(9) . . ?
C1 N2 C16 125.26(10) . . ?
C3 N2 C16 124.71(9) . . ?
C39 N3 C40 109.48(9) . . ?
C39 N3 C42 125.73(9) . . ?
C40 N3 C42 123.51(9) . . ?
C39 N4 C41 109.30(9) . . ?
C39 N4 C54 123.24(9) . . ?
C41 N4 C54 127.34(9) . . ?
N1 C1 C28 126.48(10) . . ?
N2 C1 N1 107.88(10) . . ?
N2 C1 C28 125.61(10) . . ?
N1 C2 P1 130.45(8) . . ?
C3 C2 P1 123.55(8) . . ?
C3 C2 N1 105.97(9) . . ?
N2 C3 P3 129.38(8) . . ?
C2 C3 P3 124.16(8) . . ?
C2 C3 N2 106.46(9) . . ?
C5 C4 N1 118.14(10) . . ?
C9 C4 N1 118.51(10) . . ?
C9 C4 C5 123.31(10) . . ?
C4 C5 C10 123.75(10) . . ?
C6 C5 C4 116.97(10) . . ?
C6 C5 C10 119.28(10) . . ?
C5 C6 H6 119.4 . . ?
C7 C6 C5 121.13(11) . . ?
C7 C6 H6 119.4 . . ?
C6 C7 H7 119.8 . . ?
C6 C7 C8 120.44(11) . . ?
C8 C7 H7 119.8 . . ?
C7 C8 H8 119.4 . . ?
C7 C8 C9 121.17(11) . . ?
C9 C8 H8 119.4 . . ?
C4 C9 C13 123.54(11) . . ?
C8 C9 C4 116.97(11) . . ?
C8 C9 C13 119.48(11) . . ?
C5 C10 H10 108.1 . . ?
C5 C10 C11 110.85(11) . . ?
C5 C10 C12 110.69(10) . . ?
C11 C10 H10 108.1 . . ?
C11 C10 C12 110.83(11) . . ?
C12 C10 H10 108.1 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C9 C13 H13 108.2 . . ?
C9 C13 C14 110.69(13) . . ?
C9 C13 C15 111.46(14) . . ?
C14 C13 H13 108.2 . . ?
C14 C13 C15 109.99(13) . . ?
C15 C13 H13 108.2 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C17 C16 N2 117.28(10) . . ?
C17 C16 C21 124.06(11) . . ?
C21 C16 N2 118.63(11) . . ?
C16 C17 C22 123.38(11) . . ?
C18 C17 C16 116.70(12) . . ?
C18 C17 C22 119.93(12) . . ?
C17 C18 H18 119.5 . . ?
C19 C18 C17 120.92(12) . . ?
C19 C18 H18 119.5 . . ?
C18 C19 H19 119.6 . . ?
C20 C19 C18 120.77(12) . . ?
C20 C19 H19 119.6 . . ?
C19 C20 H20 119.4 . . ?
C19 C20 C21 121.23(12) . . ?
C21 C20 H20 119.4 . . ?
C16 C21 C25 122.04(10) . . ?
C20 C21 C16 116.28(12) . . ?
C20 C21 C25 121.66(11) . . ?
C17 C22 H22 108.0 . . ?
C17 C22 C23 110.33(11) . . ?
C17 C22 C24 112.53(12) . . ?
C23 C22 H22 108.0 . . ?
C24 C22 H22 108.0 . . ?
C24 C22 C23 109.88(13) . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C21 C25 H25 107.8 . . ?
C21 C25 C26 110.98(11) . . ?
C26 C25 H25 107.8 . . ?
C27 C25 C21 113.83(11) . . ?
C27 C25 H25 107.8 . . ?
C27 C25 C26 108.37(14) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C29 C28 C1 120.95(12) . . ?
C29 C28 C33 119.89(13) . . ?
C33 C28 C1 119.15(12) . . ?
C28 C29 H29 120.2 . . ?
C28 C29 C30 119.51(16) . . ?
C30 C29 H29 120.2 . . ?
C29 C30 H30 119.8 . . ?
C31 C30 C29 120.40(18) . . ?
C31 C30 H30 119.8 . . ?
C30 C31 H31 119.9 . . ?
C32 C31 C30 120.12(15) . . ?
C32 C31 H31 119.9 . . ?
C31 C32 H32 119.8 . . ?
C31 C32 C33 120.39(18) . . ?
C33 C32 H32 119.8 . . ?
C28 C33 H33 120.2 . . ?
C32 C33 C28 119.68(17) . . ?
C32 C33 H33 120.2 . . ?
O1 C34 Mo1 178.10(15) . . ?
O2 C35 Mo1 178.00(12) . . ?
O4 C36 Mo1 178.16(14) . . ?
O3 C37 Mo1 178.06(12) . . ?
O5 C38 Mo1 176.04(12) . . ?
N3 C39 N4 108.58(9) . . ?
N3 C39 C66 124.85(10) . . ?
N4 C39 C66 126.55(10) . . ?
N3 C40 P4 128.51(8) . . ?
C41 C40 P4 124.90(8) . . ?
C41 C40 N3 106.50(9) . . ?
N4 C41 P6 130.68(8) . . ?
C40 C41 P6 123.20(8) . . ?
C40 C41 N4 106.10(9) . . ?
C43 C42 N3 119.68(10) . . ?
C47 C42 N3 117.08(9) . . ?
C47 C42 C43 123.20(10) . . ?
C42 C43 C48 123.50(10) . . ?
C44 C43 C42 116.92(11) . . ?
C44 C43 C48 119.50(10) . . ?
C43 C44 H44 119.3 . . ?
C45 C44 C43 121.33(11) . . ?
C45 C44 H44 119.3 . . ?
C44 C45 H45 119.8 . . ?
C44 C45 C46 120.33(11) . . ?
C46 C45 H45 119.8 . . ?
C45 C46 H46 119.6 . . ?
C45 C46 C47 120.90(11) . . ?
C47 C46 H46 119.6 . . ?
C42 C47 C51 122.82(10) . . ?
C46 C47 C42 117.25(10) . . ?
C46 C47 C51 119.93(10) . . ?
C43 C48 H48 108.4 . . ?
C43 C48 C49 108.91(10) . . ?
C43 C48 C50 112.95(10) . . ?
C49 C48 H48 108.4 . . ?
C50 C48 H48 108.4 . . ?
C50 C48 C49 109.73(10) . . ?
C48 C49 H49A 109.5 . . ?
C48 C49 H49B 109.5 . . ?
C48 C49 H49C 109.5 . . ?
H49A C49 H49B 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C48 C50 H50A 109.5 . . ?
C48 C50 H50B 109.5 . . ?
C48 C50 H50C 109.5 . . ?
H50A C50 H50B 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C47 C51 H51 108.0 . . ?
C47 C51 C52 110.97(10) . . ?
C47 C51 C53 111.68(9) . . ?
C52 C51 H51 108.0 . . ?
C52 C51 C53 109.96(10) . . ?
C53 C51 H51 108.0 . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52B 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C51 C53 H53A 109.5 . . ?
C51 C53 H53B 109.5 . . ?
C51 C53 H53C 109.5 . . ?
H53A C53 H53B 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C55 C54 N4 119.02(10) . . ?
C59 C54 N4 118.09(10) . . ?
C59 C54 C55 122.80(11) . . ?
C54 C55 C60 123.82(11) . . ?
C56 C55 C54 117.04(12) . . ?
C56 C55 C60 119.12(11) . . ?
C55 C56 H56 119.2 . . ?
C57 C56 C55 121.51(12) . . ?
C57 C56 H56 119.2 . . ?
C56 C57 H57 119.9 . . ?
C56 C57 C58 120.26(12) . . ?
C58 C57 H57 119.9 . . ?
C57 C58 H58 119.5 . . ?
C57 C58 C59 120.91(13) . . ?
C59 C58 H58 119.5 . . ?
C54 C59 C63 123.25(11) . . ?
C58 C59 C54 117.41(11) . . ?
C58 C59 C63 119.27(11) . . ?
C55 C60 H60 108.2 . . ?
C55 C60 C61 109.97(12) . . ?
C55 C60 C62 112.97(12) . . ?
C61 C60 H60 108.2 . . ?
C62 C60 H60 108.2 . . ?
C62 C60 C61 109.27(11) . . ?
C60 C61 H61A 109.5 . . ?
C60 C61 H61B 109.5 . . ?
C60 C61 H61C 109.5 . . ?
H61A C61 H61B 109.5 . . ?
H61A C61 H61C 109.5 . . ?
H61B C61 H61C 109.5 . . ?
C60 C62 H62A 109.5 . . ?
C60 C62 H62B 109.5 . . ?
C60 C62 H62C 109.5 . . ?
H62A C62 H62B 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
C59 C63 H63 108.0 . . ?
C59 C63 C64 108.95(11) . . ?
C59 C63 C65 112.74(12) . . ?
C64 C63 H63 108.0 . . ?
C65 C63 H63 108.0 . . ?
C65 C63 C64 111.12(13) . . ?
C63 C64 H64A 109.5 . . ?
C63 C64 H64B 109.5 . . ?
C63 C64 H64C 109.5 . . ?
H64A C64 H64B 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
C63 C65 H65A 109.5 . . ?
C63 C65 H65B 109.5 . . ?
C63 C65 H65C 109.5 . . ?
H65A C65 H65B 109.5 . . ?
H65A C65 H65C 109.5 . . ?
H65B C65 H65C 109.5 . . ?
C67 C66 C39 121.61(10) . . ?
C71 C66 C39 118.80(10) . . ?
C71 C66 C67 119.58(11) . . ?
C66 C67 H67 120.1 . . ?
C68 C67 C66 119.90(11) . . ?
C68 C67 H67 120.1 . . ?
C67 C68 H68 119.9 . . ?
C69 C68 C67 120.21(12) . . ?
C69 C68 H68 119.9 . . ?
C68 C69 H69 119.9 . . ?
C70 C69 C68 120.20(12) . . ?
C70 C69 H69 119.9 . . ?
C69 C70 H70 120.0 . . ?
C69 C70 C71 119.94(12) . . ?
C71 C70 H70 120.0 . . ?
C66 C71 H71 119.9 . . ?
C70 C71 C66 120.13(12) . . ?
C70 C71 H71 119.9 . . ?
O6 C72 Mo2 175.30(11) . . ?
O7 C73 Mo2 179.42(12) . . ?
O8 C74 Mo2 176.91(16) . . ?
O9 C75 Mo2 179.37(14) . . ?
O10 C76 Mo2 176.87(12) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
P1 C2 C3 P3 3.13(15) . . . . ?
P1 C2 C3 N2 -176.39(8) . . . . ?
P2 P1 C2 N1 179.93(10) . . . . ?
P2 P1 C2 C3 -2.36(10) . . . . ?
P2 P3 C3 N2 177.72(10) . . . . ?
P2 P3 C3 C2 -1.69(10) . . . . ?
P4 C40 C41 P6 4.16(15) . . . . ?
P4 C40 C41 N4 -174.74(8) . . . . ?
P5 P4 C40 N3 -178.25(9) . . . . ?
P5 P4 C40 C41 -2.32(10) . . . . ?
P5 P6 C41 N4 175.55(10) . . . . ?
P5 P6 C41 C40 -3.05(10) . . . . ?
N1 C1 C28 C29 136.51(14) . . . . ?
N1 C1 C28 C33 -44.89(18) . . . . ?
N1 C2 C3 P3 -178.68(8) . . . . ?
N1 C2 C3 N2 1.80(12) . . . . ?
N1 C4 C5 C6 -178.28(10) . . . . ?
N1 C4 C5 C10 1.59(17) . . . . ?
N1 C4 C9 C8 178.34(11) . . . . ?
N1 C4 C9 C13 -1.22(19) . . . . ?
N2 C1 C28 C29 -45.56(19) . . . . ?
N2 C1 C28 C33 133.04(13) . . . . ?
N2 C16 C17 C18 -175.70(10) . . . . ?
N2 C16 C17 C22 4.26(17) . . . . ?
N2 C16 C21 C20 176.56(10) . . . . ?
N2 C16 C21 C25 -5.23(17) . . . . ?
N3 C39 C66 C67 129.88(13) . . . . ?
N3 C39 C66 C71 -48.93(17) . . . . ?
N3 C40 C41 P6 -179.16(8) . . . . ?
N3 C40 C41 N4 1.95(12) . . . . ?
N3 C42 C43 C44 -179.54(10) . . . . ?
N3 C42 C43 C48 3.83(16) . . . . ?
N3 C42 C47 C46 -179.26(9) . . . . ?
N3 C42 C47 C51 1.08(15) . . . . ?
N4 C39 C66 C67 -52.29(17) . . . . ?
N4 C39 C66 C71 128.91(13) . . . . ?
N4 C54 C55 C56 -174.10(11) . . . . ?
N4 C54 C55 C60 7.42(17) . . . . ?
N4 C54 C59 C58 173.90(11) . . . . ?
N4 C54 C59 C63 -9.16(17) . . . . ?
C1 N1 C2 P1 176.26(9) . . . . ?
C1 N1 C2 C3 -1.76(12) . . . . ?
C1 N1 C4 C5 -73.20(15) . . . . ?
C1 N1 C4 C9 109.00(14) . . . . ?
C1 N2 C3 P3 179.24(9) . . . . ?
C1 N2 C3 C2 -1.27(13) . . . . ?
C1 N2 C16 C17 100.13(14) . . . . ?
C1 N2 C16 C21 -77.89(15) . . . . ?
C1 C28 C29 C30 179.19(14) . . . . ?
C1 C28 C33 C32 -178.85(13) . . . . ?
C2 N1 C1 N2 0.99(13) . . . . ?
C2 N1 C1 C28 179.22(11) . . . . ?
C2 N1 C4 C5 98.86(13) . . . . ?
C2 N1 C4 C9 -78.94(14) . . . . ?
C3 N2 C1 N1 0.19(13) . . . . ?
C3 N2 C1 C28 -178.06(11) . . . . ?
C3 N2 C16 C17 -75.30(15) . . . . ?
C3 N2 C16 C21 106.69(13) . . . . ?
C4 N1 C1 N2 173.97(10) . . . . ?
C4 N1 C1 C28 -7.80(19) . . . . ?
C4 N1 C2 P1 3.06(17) . . . . ?
C4 N1 C2 C3 -174.96(10) . . . . ?
C4 C5 C6 C7 0.35(17) . . . . ?
C4 C5 C10 C11 -120.42(12) . . . . ?
C4 C5 C10 C12 116.18(13) . . . . ?
C4 C9 C13 C14 114.28(14) . . . . ?
C4 C9 C13 C15 -122.96(15) . . . . ?
C5 C4 C9 C8 0.66(19) . . . . ?
C5 C4 C9 C13 -178.90(13) . . . . ?
C5 C6 C7 C8 -0.21(19) . . . . ?
C6 C5 C10 C11 59.44(14) . . . . ?
C6 C5 C10 C12 -63.96(14) . . . . ?
C6 C7 C8 C9 0.3(2) . . . . ?
C7 C8 C9 C4 -0.5(2) . . . . ?
C7 C8 C9 C13 179.08(14) . . . . ?
C8 C9 C13 C14 -65.28(18) . . . . ?
C8 C9 C13 C15 57.49(19) . . . . ?
C9 C4 C5 C6 -0.59(17) . . . . ?
C9 C4 C5 C10 179.28(11) . . . . ?
C10 C5 C6 C7 -179.53(11) . . . . ?
C16 N2 C1 N1 -175.82(10) . . . . ?
C16 N2 C1 C28 5.94(19) . . . . ?
C16 N2 C3 P3 -4.73(17) . . . . ?
C16 N2 C3 C2 174.75(10) . . . . ?
C16 C17 C18 C19 -1.13(18) . . . . ?
C16 C17 C22 C23 119.89(13) . . . . ?
C16 C17 C22 C24 -117.00(15) . . . . ?
C16 C21 C25 C26 -80.74(16) . . . . ?
C16 C21 C25 C27 156.69(14) . . . . ?
C17 C16 C21 C20 -1.31(18) . . . . ?
C17 C16 C21 C25 176.90(11) . . . . ?
C17 C18 C19 C20 -0.7(2) . . . . ?
C18 C17 C22 C23 -60.16(15) . . . . ?
C18 C17 C22 C24 62.96(17) . . . . ?
C18 C19 C20 C21 1.7(2) . . . . ?
C19 C20 C21 C16 -0.67(18) . . . . ?
C19 C20 C21 C25 -178.89(12) . . . . ?
C20 C21 C25 C26 97.37(16) . . . . ?
C20 C21 C25 C27 -25.20(19) . . . . ?
C21 C16 C17 C18 2.20(18) . . . . ?
C21 C16 C17 C22 -177.84(11) . . . . ?
C22 C17 C18 C19 178.90(12) . . . . ?
C28 C29 C30 C31 -0.4(3) . . . . ?
C29 C28 C33 C32 -0.2(2) . . . . ?
C29 C30 C31 C32 -0.3(3) . . . . ?
C30 C31 C32 C33 0.6(3) . . . . ?
C31 C32 C33 C28 -0.4(3) . . . . ?
C33 C28 C29 C30 0.6(2) . . . . ?
C39 N3 C40 P4 174.70(8) . . . . ?
C39 N3 C40 C41 -1.82(12) . . . . ?
C39 N3 C42 C43 100.81(13) . . . . ?
C39 N3 C42 C47 -81.57(13) . . . . ?
C39 N4 C41 P6 179.76(9) . . . . ?
C39 N4 C41 C40 -1.45(12) . . . . ?
C39 N4 C54 C55 102.13(13) . . . . ?
C39 N4 C54 C59 -74.59(14) . . . . ?
C39 C66 C67 C68 -176.69(13) . . . . ?
C39 C66 C71 C70 176.60(13) . . . . ?
C40 N3 C39 N4 0.93(12) . . . . ?
C40 N3 C39 C66 179.09(10) . . . . ?
C40 N3 C42 C43 -93.52(13) . . . . ?
C40 N3 C42 C47 84.09(13) . . . . ?
C41 N4 C39 N3 0.34(12) . . . . ?
C41 N4 C39 C66 -177.78(10) . . . . ?
C41 N4 C54 C55 -82.30(14) . . . . ?
C41 N4 C54 C59 100.99(13) . . . . ?
C42 N3 C39 N4 168.28(10) . . . . ?
C42 N3 C39 C66 -13.56(17) . . . . ?
C42 N3 C40 P4 7.02(15) . . . . ?
C42 N3 C40 C41 -169.51(9) . . . . ?
C42 C43 C44 C45 -2.05(17) . . . . ?
C42 C43 C48 C49 104.35(12) . . . . ?
C42 C43 C48 C50 -133.47(11) . . . . ?
C42 C47 C51 C52 -126.28(12) . . . . ?
C42 C47 C51 C53 110.65(12) . . . . ?
C43 C42 C47 C46 -1.74(16) . . . . ?
C43 C42 C47 C51 178.60(10) . . . . ?
C43 C44 C45 C46 -0.08(19) . . . . ?
C44 C43 C48 C49 -72.20(13) . . . . ?
C44 C43 C48 C50 49.98(14) . . . . ?
C44 C45 C46 C47 1.44(18) . . . . ?
C45 C46 C47 C42 -0.55(17) . . . . ?
C45 C46 C47 C51 179.12(11) . . . . ?
C46 C47 C51 C52 54.07(14) . . . . ?
C46 C47 C51 C53 -69.00(14) . . . . ?
C47 C42 C43 C44 3.00(16) . . . . ?
C47 C42 C43 C48 -173.63(10) . . . . ?
C48 C43 C44 C45 174.73(11) . . . . ?
C54 N4 C39 N3 176.61(10) . . . . ?
C54 N4 C39 C66 -1.51(17) . . . . ?
C54 N4 C41 P6 3.69(17) . . . . ?
C54 N4 C41 C40 -177.53(10) . . . . ?
C54 C55 C56 C57 -0.3(2) . . . . ?
C54 C55 C60 C61 115.18(13) . . . . ?
C54 C55 C60 C62 -122.45(13) . . . . ?
C54 C59 C63 C64 -105.52(14) . . . . ?
C54 C59 C63 C65 130.64(14) . . . . ?
C55 C54 C59 C58 -2.68(18) . . . . ?
C55 C54 C59 C63 174.26(12) . . . . ?
C55 C56 C57 C58 -1.6(2) . . . . ?
C56 C55 C60 C61 -63.27(16) . . . . ?
C56 C55 C60 C62 59.10(16) . . . . ?
C56 C57 C58 C59 1.3(2) . . . . ?
C57 C58 C59 C54 0.7(2) . . . . ?
C57 C58 C59 C63 -176.33(13) . . . . ?
C58 C59 C63 C64 71.36(16) . . . . ?
C58 C59 C63 C65 -52.48(17) . . . . ?
C59 C54 C55 C56 2.45(18) . . . . ?
C59 C54 C55 C60 -176.03(12) . . . . ?
C60 C55 C56 C57 178.27(13) . . . . ?
C66 C67 C68 C69 -0.3(2) . . . . ?
C67 C66 C71 C70 -2.2(2) . . . . ?
C67 C68 C69 C70 -1.4(3) . . . . ?
C68 C69 C70 C71 1.2(3) . . . . ?
C69 C70 C71 C66 0.6(2) . . . . ?
C71 C66 C67 C68 2.1(2) . . . . ?

_olex2_date_sample_data_collection 2019-04-04
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.070
_oxdiff_exptl_absorpt_empirical_full_min 0.940
