# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2021

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

data_q1_21dtk5_0m
_database_code_depnum_ccdc_archive 'CCDC 1989000'
loop_
_audit_author_name
_audit_author_address
'DV Kama'
;University of the Free State
South Africa
;
_audit_update_record             
;
2021-10-05 deposited with the CCDC.	2021-10-20 downloaded from the CCDC.
;
_audit_creation_date             2021-10-05
_audit_creation_method           
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C32 H35 N P2'
_chemical_formula_sum            'C32 H35 N P2'
_chemical_formula_weight         495.55
_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'
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      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                   11.4833(12)
_cell_length_b                   12.0246(13)
_cell_length_c                   12.2349(13)
_cell_angle_alpha                64.285(5)
_cell_angle_beta                 81.986(5)
_cell_angle_gamma                68.172(5)
_cell_volume                     1412.5(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9830
_cell_measurement_temperature    106(2)
_cell_measurement_theta_max      28.38
_cell_measurement_theta_min      2.69
_shelx_estimated_absorpt_T_max   0.980
_shelx_estimated_absorpt_T_min   0.950
_exptl_absorpt_coefficient_mu    0.174
_exptl_absorpt_correction_T_max  0.7426
_exptl_absorpt_correction_T_min  0.7018
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.0869 before and 0.0785 after correction.
The Ratio of minimum to maximum transmission is 0.9451.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.165
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Cuboid
_exptl_crystal_F_000             528
_exptl_crystal_size_max          0.296
_exptl_crystal_size_mid          0.259
_exptl_crystal_size_min          0.118
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0627
_diffrn_reflns_av_unetI/netI     0.0320
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.991
_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       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            59293
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.486
_diffrn_reflns_theta_min         2.624
_diffrn_ambient_temperature      106.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6213
_reflns_number_total             7095
_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       'SAINT V8.40B (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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    ?
_refine_diff_density_max         0.309
_refine_diff_density_min         -0.285
_refine_diff_density_rms         0.049
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     324
_refine_ls_number_reflns         7095
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0442
_refine_ls_R_factor_gt           0.0380
_refine_ls_restrained_S_all      1.045
_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)+(0.0458P)²+0.5522P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0998
_refine_ls_wR_factor_ref         0.1038
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C4(H4A,H4B), C3(H3A,H3B)
2.b Aromatic/amide H refined with riding coordinates:
 C26(H26), C22(H22), C42(H42), C12(H12), C32(H32), C23(H23), C25(H25),
 C16(H16), C43(H43), C13(H13), C33(H33), C46(H46), C15(H15), C45(H45), C36(H36),
  C35(H35)
2.c Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C47(H47A,H47B,H47C), C37(H37A,H37B,H37C), C17(H17A,H17B,
 H17C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_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 0.66309(3) 0.86133(3) 0.13254(3) 0.02302(8) Uani 1 1 d . . . . .
P2 P 0.76633(3) 0.58016(3) 0.30513(3) 0.02294(8) Uani 1 1 d . . . . .
N1 N 0.64087(10) 0.72364(10) 0.24590(10) 0.0240(2) Uani 1 1 d . . . . .
C21 C 0.75113(12) 0.80390(12) 0.01881(11) 0.0229(2) Uani 1 1 d . . . . .
C11 C 0.78064(12) 0.88476(12) 0.19769(12) 0.0251(2) Uani 1 1 d . . . . .
C26 C 0.87970(12) 0.73364(13) 0.02511(12) 0.0276(3) Uani 1 1 d . . . . .
H26 H 0.929263 0.716490 0.090470 0.033 Uiso 1 1 calc R . . . .
C1 C 0.50968(12) 0.72872(13) 0.26616(12) 0.0259(3) Uani 1 1 d . . . . .
C22 C 0.68174(12) 0.82795(13) -0.07882(12) 0.0271(3) Uani 1 1 d . . . . .
H22 H 0.594188 0.876328 -0.085563 0.033 Uiso 1 1 calc R . . . .
C41 C 0.76047(12) 0.52553(12) 0.46981(11) 0.0238(2) Uani 1 1 d . . . . .
C42 C 0.87257(12) 0.43849(14) 0.53450(12) 0.0295(3) Uani 1 1 d . . . . .
H42 H 0.944645 0.408470 0.492285 0.035 Uiso 1 1 calc R . . . .
C31 C 0.71327(12) 0.46494(12) 0.28344(12) 0.0257(3) Uani 1 1 d . . . . .
C12 C 0.85137(13) 0.95985(14) 0.12113(12) 0.0303(3) Uani 1 1 d . . . . .
H12 H 0.847345 0.985749 0.036122 0.036 Uiso 1 1 calc R . . . .
C32 C 0.71580(13) 0.34307(13) 0.37323(13) 0.0302(3) Uani 1 1 d . . . . .
H32 H 0.742230 0.317128 0.453575 0.036 Uiso 1 1 calc R . . . .
C24 C 0.86642(13) 0.71207(13) -0.16016(12) 0.0284(3) Uani 1 1 d . . . . .
C23 C 0.73877(13) 0.78216(14) -0.16659(12) 0.0297(3) Uani 1 1 d . . . . .
H23 H 0.689407 0.799202 -0.232053 0.036 Uiso 1 1 calc R . . . .
C25 C 0.93602(13) 0.68850(14) -0.06295(13) 0.0309(3) Uani 1 1 d . . . . .
H25 H 1.023665 0.640661 -0.056781 0.037 Uiso 1 1 calc R . . . .
C2 C 0.41444(12) 0.83267(13) 0.30635(13) 0.0304(3) Uani 1 1 d . . . . .
H2A H 0.432062 0.915477 0.276725 0.036 Uiso 1 1 calc R . . . .
H2B H 0.399594 0.798929 0.394635 0.036 Uiso 1 1 calc R . . . .
C16 C 0.78843(14) 0.84971(13) 0.32164(12) 0.0310(3) Uani 1 1 d . . . . .
H16 H 0.740988 0.799219 0.376013 0.037 Uiso 1 1 calc R . . . .
C44 C 0.77839(13) 0.43846(15) 0.72324(12) 0.0314(3) Uani 1 1 d . . . . .
C43 C 0.88101(13) 0.39477(16) 0.65943(13) 0.0345(3) Uani 1 1 d . . . . .
H43 H 0.958138 0.334163 0.701556 0.041 Uiso 1 1 calc R . . . .
C13 C 0.92729(14) 0.99731(15) 0.16676(14) 0.0350(3) Uani 1 1 d . . . . .
H13 H 0.974750 1.047938 0.112610 0.042 Uiso 1 1 calc R . . . .
C33 C 0.68000(14) 0.25870(14) 0.34658(14) 0.0352(3) Uani 1 1 d . . . . .
H33 H 0.684092 0.175236 0.409006 0.042 Uiso 1 1 calc R . . . .
C14 C 0.93511(15) 0.96196(15) 0.29059(14) 0.0350(3) Uani 1 1 d . . . . .
C46 C 0.65770(14) 0.56777(15) 0.53517(13) 0.0372(3) Uani 1 1 d . . . . .
H46 H 0.579857 0.627021 0.493811 0.045 Uiso 1 1 calc R . . . .
C34 C 0.63854(13) 0.29354(15) 0.23120(15) 0.0342(3) Uani 1 1 d . . . . .
C4 C 0.41975(14) 0.77948(16) 0.15882(14) 0.0364(3) Uani 1 1 d . . . . .
H4A H 0.439056 0.845451 0.082541 0.044 Uiso 1 1 calc R . . . .
H4B H 0.408640 0.708789 0.144907 0.044 Uiso 1 1 calc R . . . .
C15 C 0.86445(16) 0.88753(15) 0.36663(13) 0.0363(3) Uani 1 1 d . . . . .
H15 H 0.868402 0.861948 0.451588 0.044 Uiso 1 1 calc R . . . .
C45 C 0.66703(14) 0.52483(16) 0.65964(13) 0.0380(3) Uani 1 1 d . . . . .
H45 H 0.595427 0.555377 0.702087 0.046 Uiso 1 1 calc R . . . .
C3 C 0.31362(13) 0.83956(16) 0.23050(15) 0.0383(3) Uani 1 1 d . . . . .
H3A H 0.258228 0.930336 0.181030 0.046 Uiso 1 1 calc R . . . .
H3B H 0.264044 0.782746 0.277819 0.046 Uiso 1 1 calc R . . . .
C36 C 0.67522(16) 0.49787(15) 0.16644(13) 0.0363(3) Uani 1 1 d . . . . .
H36 H 0.675244 0.579142 0.102650 0.044 Uiso 1 1 calc R . . . .
C35 C 0.63757(16) 0.41437(16) 0.14187(14) 0.0393(3) Uani 1 1 d . . . . .
H35 H 0.610336 0.440416 0.061769 0.047 Uiso 1 1 calc R . . . .
C27 C 0.92894(16) 0.66434(17) -0.25619(15) 0.0398(3) Uani 1 1 d . . . . .
H27A H 0.864756 0.672964 -0.307297 0.060 Uiso 1 1 calc GR . . . .
H27B H 0.982969 0.571712 -0.217343 0.060 Uiso 1 1 calc GR . . . .
H27C H 0.979762 0.717295 -0.306396 0.060 Uiso 1 1 calc GR . . . .
C47 C 0.78729(16) 0.3931(2) 0.85862(14) 0.0478(4) Uani 1 1 d . . . . .
H47A H 0.833789 0.298134 0.896479 0.072 Uiso 1 1 calc GR . . . .
H47B H 0.702698 0.411928 0.891177 0.072 Uiso 1 1 calc GR . . . .
H47C H 0.831166 0.439795 0.876184 0.072 Uiso 1 1 calc GR . . . .
C37 C 0.59384(17) 0.20608(19) 0.2027(2) 0.0501(4) Uani 1 1 d . . . . .
H37A H 0.515893 0.259020 0.153700 0.075 Uiso 1 1 calc GR . . . .
H37B H 0.578498 0.138299 0.278460 0.075 Uiso 1 1 calc GR . . . .
H37C H 0.658000 0.163927 0.157309 0.075 Uiso 1 1 calc GR . . . .
C17 C 1.01568(18) 1.0045(2) 0.34068(18) 0.0497(4) Uani 1 1 d . . . . .
H17A H 0.961839 1.070420 0.370055 0.074 Uiso 1 1 calc GR . . . .
H17B H 1.068804 1.042744 0.276617 0.074 Uiso 1 1 calc GR . . . .
H17C H 1.068743 0.928005 0.407909 0.074 Uiso 1 1 calc GR . . . .
H1 H 0.5091(15) 0.6451(16) 0.3236(14) 0.027(4) Uiso 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
P1 N1 1.7183(11) . ?
P1 C21 1.8324(13) . ?
P1 C11 1.8205(14) . ?
P2 N1 1.7132(11) . ?
P2 C41 1.8281(13) . ?
P2 C31 1.8312(14) . ?
N1 C1 1.4749(16) . ?
C21 C26 1.3954(17) . ?
C21 C22 1.3928(18) . ?
C11 C12 1.3971(18) . ?
C11 C16 1.3931(18) . ?
C26 H26 0.9500 . ?
C26 C25 1.3877(18) . ?
C1 C2 1.5385(18) . ?
C1 C4 1.542(2) . ?
C1 H1 0.946(16) . ?
C22 H22 0.9500 . ?
C22 C23 1.3907(19) . ?
C41 C42 1.3937(18) . ?
C41 C46 1.3906(18) . ?
C42 H42 0.9500 . ?
C42 C43 1.3887(19) . ?
C31 C32 1.3912(18) . ?
C31 C36 1.397(2) . ?
C12 H12 0.9500 . ?
C12 C13 1.386(2) . ?
C32 H32 0.9500 . ?
C32 C33 1.392(2) . ?
C24 C23 1.3860(19) . ?
C24 C25 1.392(2) . ?
C24 C27 1.5062(19) . ?
C23 H23 0.9500 . ?
C25 H25 0.9500 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C3 1.539(2) . ?
C16 H16 0.9500 . ?
C16 C15 1.385(2) . ?
C44 C43 1.383(2) . ?
C44 C45 1.381(2) . ?
C44 C47 1.508(2) . ?
C43 H43 0.9500 . ?
C13 H13 0.9500 . ?
C13 C14 1.391(2) . ?
C33 H33 0.9500 . ?
C33 C34 1.386(2) . ?
C14 C15 1.390(2) . ?
C14 C17 1.509(2) . ?
C46 H46 0.9500 . ?
C46 C45 1.385(2) . ?
C34 C35 1.385(2) . ?
C34 C37 1.504(2) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C4 C3 1.541(2) . ?
C15 H15 0.9500 . ?
C45 H45 0.9500 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C36 H36 0.9500 . ?
C36 C35 1.381(2) . ?
C35 H35 0.9500 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 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
N1 P1 C21 104.20(5) . . ?
N1 P1 C11 103.56(6) . . ?
C11 P1 C21 102.79(6) . . ?
N1 P2 C41 106.14(6) . . ?
N1 P2 C31 101.35(6) . . ?
C41 P2 C31 102.14(6) . . ?
P2 N1 P1 119.84(6) . . ?
C1 N1 P1 115.91(8) . . ?
C1 N1 P2 122.72(8) . . ?
C26 C21 P1 125.46(10) . . ?
C22 C21 P1 116.53(9) . . ?
C22 C21 C26 117.94(12) . . ?
C12 C11 P1 119.55(10) . . ?
C16 C11 P1 122.00(10) . . ?
C16 C11 C12 117.54(12) . . ?
C21 C26 H26 119.6 . . ?
C25 C26 C21 120.79(12) . . ?
C25 C26 H26 119.6 . . ?
N1 C1 C2 119.79(11) . . ?
N1 C1 C4 121.05(11) . . ?
N1 C1 H1 108.8(10) . . ?
C2 C1 C4 88.41(11) . . ?
C2 C1 H1 107.5(10) . . ?
C4 C1 H1 109.5(10) . . ?
C21 C22 H22 119.5 . . ?
C23 C22 C21 120.95(12) . . ?
C23 C22 H22 119.5 . . ?
C42 C41 P2 116.10(10) . . ?
C46 C41 P2 126.43(10) . . ?
C46 C41 C42 117.36(12) . . ?
C41 C42 H42 119.3 . . ?
C43 C42 C41 121.31(12) . . ?
C43 C42 H42 119.3 . . ?
C32 C31 P2 124.75(11) . . ?
C32 C31 C36 117.49(13) . . ?
C36 C31 P2 117.62(10) . . ?
C11 C12 H12 119.4 . . ?
C13 C12 C11 121.30(13) . . ?
C13 C12 H12 119.4 . . ?
C31 C32 H32 119.6 . . ?
C31 C32 C33 120.70(13) . . ?
C33 C32 H32 119.6 . . ?
C23 C24 C25 118.02(12) . . ?
C23 C24 C27 121.27(13) . . ?
C25 C24 C27 120.71(13) . . ?
C22 C23 H23 119.4 . . ?
C24 C23 C22 121.11(13) . . ?
C24 C23 H23 119.4 . . ?
C26 C25 C24 121.19(12) . . ?
C26 C25 H25 119.4 . . ?
C24 C25 H25 119.4 . . ?
C1 C2 H2A 114.0 . . ?
C1 C2 H2B 114.0 . . ?
C1 C2 C3 88.02(11) . . ?
H2A C2 H2B 111.2 . . ?
C3 C2 H2A 114.0 . . ?
C3 C2 H2B 114.0 . . ?
C11 C16 H16 119.6 . . ?
C15 C16 C11 120.86(13) . . ?
C15 C16 H16 119.6 . . ?
C43 C44 C47 121.09(14) . . ?
C45 C44 C43 118.22(13) . . ?
C45 C44 C47 120.69(14) . . ?
C42 C43 H43 119.6 . . ?
C44 C43 C42 120.75(13) . . ?
C44 C43 H43 119.6 . . ?
C12 C13 H13 119.5 . . ?
C12 C13 C14 121.04(13) . . ?
C14 C13 H13 119.5 . . ?
C32 C33 H33 119.2 . . ?
C34 C33 C32 121.60(14) . . ?
C34 C33 H33 119.2 . . ?
C13 C14 C17 121.34(14) . . ?
C15 C14 C13 117.60(14) . . ?
C15 C14 C17 121.05(14) . . ?
C41 C46 H46 119.5 . . ?
C45 C46 C41 121.06(13) . . ?
C45 C46 H46 119.5 . . ?
C33 C34 C37 122.10(15) . . ?
C35 C34 C33 117.42(13) . . ?
C35 C34 C37 120.47(15) . . ?
C1 C4 H4A 114.0 . . ?
C1 C4 H4B 114.0 . . ?
H4A C4 H4B 111.2 . . ?
C3 C4 C1 87.86(11) . . ?
C3 C4 H4A 114.0 . . ?
C3 C4 H4B 114.0 . . ?
C16 C15 C14 121.65(13) . . ?
C16 C15 H15 119.2 . . ?
C14 C15 H15 119.2 . . ?
C44 C45 C46 121.29(13) . . ?
C44 C45 H45 119.4 . . ?
C46 C45 H45 119.4 . . ?
C2 C3 C4 88.43(10) . . ?
C2 C3 H3A 113.9 . . ?
C2 C3 H3B 113.9 . . ?
C4 C3 H3A 113.9 . . ?
C4 C3 H3B 113.9 . . ?
H3A C3 H3B 111.1 . . ?
C31 C36 H36 119.4 . . ?
C35 C36 C31 121.16(14) . . ?
C35 C36 H36 119.4 . . ?
C34 C35 H35 119.2 . . ?
C36 C35 C34 121.58(14) . . ?
C36 C35 H35 119.2 . . ?
C24 C27 H27A 109.5 . . ?
C24 C27 H27B 109.5 . . ?
C24 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C44 C47 H47A 109.5 . . ?
C44 C47 H47B 109.5 . . ?
C44 C47 H47C 109.5 . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C34 C37 H37A 109.5 . . ?
C34 C37 H37B 109.5 . . ?
C34 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C14 C17 H17A 109.5 . . ?
C14 C17 H17B 109.5 . . ?
C14 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 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 N1 C1 C2 -62.36(14) . . . . ?
P1 N1 C1 C4 45.55(15) . . . . ?
P1 C21 C26 C25 176.45(11) . . . . ?
P1 C21 C22 C23 -176.57(10) . . . . ?
P1 C11 C12 C13 169.78(11) . . . . ?
P1 C11 C16 C15 -169.47(11) . . . . ?
P2 N1 C1 C2 131.84(11) . . . . ?
P2 N1 C1 C4 -120.26(12) . . . . ?
P2 C41 C42 C43 177.13(11) . . . . ?
P2 C41 C46 C45 -176.08(13) . . . . ?
P2 C31 C32 C33 -176.37(11) . . . . ?
P2 C31 C36 C35 178.02(12) . . . . ?
N1 P1 C21 C26 -79.02(12) . . . . ?
N1 P1 C21 C22 97.93(10) . . . . ?
N1 P1 C11 C12 159.60(10) . . . . ?
N1 P1 C11 C16 -31.61(12) . . . . ?
N1 P2 C41 C42 -159.00(10) . . . . ?
N1 P2 C41 C46 17.22(14) . . . . ?
N1 P2 C31 C32 -130.06(12) . . . . ?
N1 P2 C31 C36 54.36(12) . . . . ?
N1 C1 C2 C3 145.58(12) . . . . ?
N1 C1 C4 C3 -144.50(12) . . . . ?
C21 P1 N1 P2 51.28(9) . . . . ?
C21 P1 N1 C1 -114.97(10) . . . . ?
C21 P1 C11 C12 51.33(12) . . . . ?
C21 P1 C11 C16 -139.88(11) . . . . ?
C21 C26 C25 C24 0.2(2) . . . . ?
C21 C22 C23 C24 -0.5(2) . . . . ?
C11 P1 N1 P2 -55.93(8) . . . . ?
C11 P1 N1 C1 137.83(9) . . . . ?
C11 P1 C21 C26 28.76(12) . . . . ?
C11 P1 C21 C22 -154.29(10) . . . . ?
C11 C12 C13 C14 -0.4(2) . . . . ?
C11 C16 C15 C14 0.3(2) . . . . ?
C26 C21 C22 C23 0.62(19) . . . . ?
C1 C2 C3 C4 -20.24(10) . . . . ?
C1 C4 C3 C2 20.19(10) . . . . ?
C22 C21 C26 C25 -0.47(19) . . . . ?
C41 P2 N1 P1 128.83(7) . . . . ?
C41 P2 N1 C1 -65.90(11) . . . . ?
C41 P2 C31 C32 -20.60(13) . . . . ?
C41 P2 C31 C36 163.82(11) . . . . ?
C41 C42 C43 C44 -1.2(2) . . . . ?
C41 C46 C45 C44 -0.2(3) . . . . ?
C42 C41 C46 C45 0.1(2) . . . . ?
C31 P2 N1 P1 -124.83(7) . . . . ?
C31 P2 N1 C1 40.44(11) . . . . ?
C31 P2 C41 C42 95.23(11) . . . . ?
C31 P2 C41 C46 -88.56(14) . . . . ?
C31 C32 C33 C34 -1.2(2) . . . . ?
C31 C36 C35 C34 -1.5(2) . . . . ?
C12 C11 C16 C15 -0.5(2) . . . . ?
C12 C13 C14 C15 0.2(2) . . . . ?
C12 C13 C14 C17 -178.85(15) . . . . ?
C32 C31 C36 C35 2.1(2) . . . . ?
C32 C33 C34 C35 1.9(2) . . . . ?
C32 C33 C34 C37 -177.03(14) . . . . ?
C23 C24 C25 C26 0.0(2) . . . . ?
C25 C24 C23 C22 0.1(2) . . . . ?
C2 C1 C4 C3 -20.21(11) . . . . ?
C16 C11 C12 C13 0.5(2) . . . . ?
C43 C44 C45 C46 -0.4(2) . . . . ?
C13 C14 C15 C16 -0.2(2) . . . . ?
C33 C34 C35 C36 -0.6(2) . . . . ?
C46 C41 C42 C43 0.6(2) . . . . ?
C4 C1 C2 C3 20.22(10) . . . . ?
C45 C44 C43 C42 1.1(2) . . . . ?
C36 C31 C32 C33 -0.8(2) . . . . ?
C27 C24 C23 C22 -178.93(13) . . . . ?
C27 C24 C25 C26 179.08(14) . . . . ?
C47 C44 C43 C42 -179.05(15) . . . . ?
C47 C44 C45 C46 179.70(16) . . . . ?
C37 C34 C35 C36 178.39(15) . . . . ?
C17 C14 C15 C16 178.88(15) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_15dtk1_0m
_database_code_depnum_ccdc_archive 'CCDC 1558628'
loop_
_audit_author_name
_audit_author_address
'DV Kama'
;University of the Free State
South Africa
;
_audit_update_record             
;
2021-10-12 deposited with the CCDC.	2021-10-20 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT910_15dtk1_0m           
;
PROBLEM:  Test for missing reflections below Theta-Min 
RESPONSE: 7 reflections that are below Theta (min) value have been omitted
 from the refinement. The FCF reflections are caused
 by partial obscurity of the beam stop and due to overflow
 reflections which are not automatically excluded
 by the Bruker APEX II software. Sufficient unique
 reflections were obtained (6933) to yield
 a fully refined structure with 80.0 % data completeness.
;

# end Validation Reply Form_audit_creation_date               2021-10-12
_audit_creation_method           
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C37 H39 Br N O3 P2 Re'
_chemical_formula_sum            'C37 H39 Br N O3 P2 Re'
_chemical_formula_weight         873.74
_chemical_absolute_configuration ?
_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'
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'
Re Re -1.0185 7.2310 '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           1
_space_group_name_H-M_alt        'P 1'
_space_group_name_Hall           'P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'

_cell_length_a                   9.7040(17)
_cell_length_b                   9.8836(17)
_cell_length_c                   10.5780(19)
_cell_angle_alpha                92.787(6)
_cell_angle_beta                 111.417(6)
_cell_angle_gamma                104.512(6)
_cell_volume                     903.2(3)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    9853
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      2.35
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    4.593
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4892
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.1848 before and 0.0697 after correction.
The Ratio of minimum to maximum transmission is 0.6560.
The λ/2 correction factor is 0.00150.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.606
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Cuboid
_exptl_crystal_F_000             432
_exptl_crystal_size_max          0.236
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.093
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0452
_diffrn_reflns_av_unetI/netI     0.0546
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            15530
_diffrn_reflns_point_group_measured_fraction_full 0.844
_diffrn_reflns_point_group_measured_fraction_max 0.797
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         28.000
_diffrn_reflns_theta_min         3.230
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.598
_reflns_Friedel_fraction_full    0.691
_reflns_Friedel_fraction_max     0.597
_reflns_number_gt                6928
_reflns_number_total             6933
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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    'ShelXD (Sheldrick, 2008)'
_refine_diff_density_max         1.663
_refine_diff_density_min         -0.737
_refine_diff_density_rms         0.095
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.516(7)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     420
_refine_ls_number_reflns         6933
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0240
_refine_ls_R_factor_gt           0.0239
_refine_ls_restrained_S_all      1.015
_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)] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0515
_refine_ls_wR_factor_ref         0.0515
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.484(7)
 0.516(7)
2. 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
3. Others
 Fixed Sof: Br3(0.15) Br1(0.85)
4.a Ternary CH refined with riding coordinates:
 C1(H1)
4.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B)
4.c Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C15(H15), C16(H16), C22(H22), C23(H23), C25(H25),
 C26(H26), C32(H32), C33(H33), C35(H35), C36(H36), C42(H42), C43(H43), C45(H45),
  C46(H46)
4.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C27(H27A,H27B,H27C), C37(H37A,H37B,H37C), C47(H47A,H47B,
 H47C)
;
_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
C1 C 0.2219(6) -0.0778(6) -0.2816(5) 0.0196(11) Uani 1 1 d . . . . .
H1 H 0.275177 0.004741 -0.311022 0.024 Uiso 1 1 calc R . . . .
C2 C 0.0792(8) -0.1593(7) -0.4083(6) 0.0247(14) Uani 1 1 d . . . . .
H2A H 0.017176 -0.236549 -0.381400 0.030 Uiso 1 1 calc R . . . .
H2B H 0.016805 -0.096827 -0.445756 0.030 Uiso 1 1 calc R . . . .
C3 C 0.1241(8) -0.2183(7) -0.5183(6) 0.0374(16) Uani 1 1 d . . . . .
H3A H 0.031557 -0.273900 -0.594656 0.045 Uiso 1 1 calc R . . . .
H3B H 0.176392 -0.140740 -0.552369 0.045 Uiso 1 1 calc R . . . .
C4 C 0.2286(10) -0.3093(8) -0.4620(7) 0.050(2) Uani 1 1 d . . . . .
H4A H 0.255121 -0.346274 -0.533866 0.060 Uiso 1 1 calc R . . . .
H4B H 0.175367 -0.388801 -0.430593 0.060 Uiso 1 1 calc R . . . .
C5 C 0.3755(9) -0.2231(9) -0.3427(7) 0.0444(18) Uani 1 1 d . . . . .
H5A H 0.430722 -0.145750 -0.374956 0.053 Uiso 1 1 calc R . . . .
H5B H 0.442256 -0.282494 -0.306997 0.053 Uiso 1 1 calc R . . . .
C6 C 0.3355(7) -0.1640(7) -0.2285(6) 0.0267(12) Uani 1 1 d . . . . .
H6A H 0.290866 -0.241649 -0.189549 0.032 Uiso 1 1 calc R . . . .
H6B H 0.429460 -0.104592 -0.156012 0.032 Uiso 1 1 calc R . . . .
C7 C 0.0558(7) 0.2864(6) 0.0900(6) 0.0209(11) Uani 1 1 d . . . . .
C8 C -0.0012(7) 0.0169(6) 0.1778(6) 0.0231(12) Uani 1 1 d . . . . .
C9 C 0.2774(11) 0.1528(9) 0.1678(9) 0.0240(17) Uani 1 1 d . . . A 1
C11 C 0.0531(6) 0.1766(5) -0.3187(5) 0.0183(10) Uani 1 1 d . . . . .
C12 C -0.1062(6) 0.1133(6) -0.3830(5) 0.0215(11) Uani 1 1 d . . . . .
H12 H -0.156813 0.051779 -0.339560 0.026 Uiso 1 1 calc R . . . .
C13 C -0.1889(7) 0.1416(6) -0.5108(6) 0.0247(12) Uani 1 1 d . . . . .
H13 H -0.295056 0.099193 -0.552087 0.030 Uiso 1 1 calc R . . . .
C14 C -0.1168(7) 0.2319(6) -0.5787(6) 0.0237(12) Uani 1 1 d . . . . .
C15 C 0.0414(8) 0.2917(7) -0.5174(7) 0.0279(15) Uani 1 1 d . . . . .
H15 H 0.091723 0.349977 -0.563303 0.033 Uiso 1 1 calc R . . . .
C16 C 0.1271(7) 0.2658(6) -0.3871(6) 0.0255(12) Uani 1 1 d . . . . .
H16 H 0.233278 0.308115 -0.346321 0.031 Uiso 1 1 calc R . . . .
C17 C -0.2082(8) 0.2622(8) -0.7185(7) 0.0352(15) Uani 1 1 d . . . . .
H17A H -0.205234 0.198814 -0.788580 0.053 Uiso 1 1 calc GR . . . .
H17B H -0.163899 0.358051 -0.726743 0.053 Uiso 1 1 calc GR . . . .
H17C H -0.313425 0.248888 -0.729004 0.053 Uiso 1 1 calc GR . . . .
C21 C 0.3431(6) 0.2744(5) -0.0931(5) 0.0185(10) Uani 1 1 d . . . . .
C22 C 0.3474(7) 0.4118(6) -0.0505(6) 0.0264(12) Uani 1 1 d . . . . .
H22 H 0.256667 0.430752 -0.055069 0.032 Uiso 1 1 calc R . . . .
C23 C 0.4841(7) 0.5199(6) -0.0016(6) 0.0306(14) Uani 1 1 d . . . . .
H23 H 0.483174 0.610913 0.024125 0.037 Uiso 1 1 calc R . . . .
C24 C 0.6231(6) 0.4959(6) 0.0101(5) 0.0248(12) Uani 1 1 d . . . . .
C25 C 0.6188(6) 0.3593(6) -0.0334(6) 0.0241(12) Uani 1 1 d . . . . .
H25 H 0.709876 0.340855 -0.028338 0.029 Uiso 1 1 calc R . . . .
C26 C 0.4810(6) 0.2491(6) -0.0845(5) 0.0194(11) Uani 1 1 d . . . . .
H26 H 0.481226 0.158604 -0.112827 0.023 Uiso 1 1 calc R . . . .
C27 C 0.7747(8) 0.6130(7) 0.0723(7) 0.0388(16) Uani 1 1 d . . . . .
H27A H 0.757221 0.701429 0.048157 0.058 Uiso 1 1 calc GR . . . .
H27B H 0.847100 0.592714 0.037507 0.058 Uiso 1 1 calc GR . . . .
H27C H 0.815614 0.619000 0.170485 0.058 Uiso 1 1 calc GR . . . .
C31 C 0.2738(6) -0.1603(6) 0.0668(5) 0.0181(10) Uani 1 1 d . . . . .
C32 C 0.4265(6) -0.0832(6) 0.0992(5) 0.0202(11) Uani 1 1 d . . . . .
H32 H 0.448651 -0.007220 0.054253 0.024 Uiso 1 1 calc R . . . .
C33 C 0.5472(7) -0.1194(6) 0.1991(6) 0.0241(12) Uani 1 1 d . . . . .
H33 H 0.649121 -0.068519 0.218508 0.029 Uiso 1 1 calc R . . . .
C34 C 0.5164(7) -0.2301(6) 0.2691(5) 0.0251(12) Uani 1 1 d . . . . .
C35 C 0.3634(7) -0.3051(6) 0.2394(5) 0.0261(12) Uani 1 1 d . . . . .
H35 H 0.341791 -0.379124 0.286631 0.031 Uiso 1 1 calc R . . . .
C36 C 0.2418(7) -0.2706(6) 0.1395(6) 0.0244(12) Uani 1 1 d . . . . .
H36 H 0.139972 -0.320639 0.121288 0.029 Uiso 1 1 calc R . . . .
C37 C 0.6473(8) -0.2716(8) 0.3746(7) 0.0405(17) Uani 1 1 d . . . . .
H37A H 0.744477 -0.211680 0.379990 0.061 Uiso 1 1 calc GR . . . .
H37B H 0.639434 -0.368365 0.347927 0.061 Uiso 1 1 calc GR . . . .
H37C H 0.640801 -0.261080 0.462826 0.061 Uiso 1 1 calc GR . . . .
C41 C -0.0273(6) -0.2760(5) -0.1514(5) 0.0173(10) Uani 1 1 d . . . . .
C42 C 0.0070(7) -0.4032(6) -0.1631(6) 0.0250(12) Uani 1 1 d . . . . .
H42 H 0.108576 -0.405721 -0.120436 0.030 Uiso 1 1 calc R . . . .
C43 C -0.1068(7) -0.5260(6) -0.2369(6) 0.0275(13) Uani 1 1 d . . . . .
H43 H -0.080109 -0.609525 -0.242620 0.033 Uiso 1 1 calc R . . . .
C44 C -0.2594(6) -0.5276(6) -0.3024(6) 0.0230(11) Uani 1 1 d . . . . .
C45 C -0.2938(6) -0.4006(6) -0.2924(6) 0.0244(12) Uani 1 1 d . . . . .
H45 H -0.395444 -0.398581 -0.336416 0.029 Uiso 1 1 calc R . . . .
C46 C -0.1806(6) -0.2762(6) -0.2186(5) 0.0227(12) Uani 1 1 d . . . . .
H46 H -0.207292 -0.192613 -0.213944 0.027 Uiso 1 1 calc R . . . .
C47 C -0.3851(7) -0.6625(6) -0.3815(7) 0.0346(15) Uani 1 1 d . . . . .
H47A H -0.483909 -0.651881 -0.391101 0.052 Uiso 1 1 calc GR . . . .
H47B H -0.367142 -0.739891 -0.332629 0.052 Uiso 1 1 calc GR . . . .
H47C H -0.383783 -0.681285 -0.470898 0.052 Uiso 1 1 calc GR . . . .
N1 N 0.1811(5) -0.0223(4) -0.1694(4) 0.0154(9) Uani 1 1 d . . . . .
O1 O 0.0534(6) 0.3976(5) 0.1230(5) 0.0357(11) Uani 1 1 d . . . . .
O2 O -0.0424(6) -0.0324(5) 0.2587(5) 0.0362(11) Uani 1 1 d . . . . .
Br3 Br 0.3369(10) 0.1857(9) 0.2222(9) 0.0286(16) Uani 0.15 1 d . . P A 1
P1 P 0.15822(16) 0.14090(15) -0.14767(15) 0.0157(3) Uani 1 1 d . . . . .
P2 P 0.11542(16) -0.10907(15) -0.05699(14) 0.0149(3) Uani 1 1 d . . . . .
Br1 Br -0.23675(10) 0.04605(8) -0.10843(9) 0.02419(17) Uani 0.85 1 d . . P A 2
Re1 Re 0.06330(2) 0.09681(2) 0.03690(2) 0.01562(5) Uani 1 1 d . . . . .
O3 O 0.4002(9) 0.1897(12) 0.2489(10) 0.051(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
C1 H1 0.9800 . ?
C1 C2 1.531(8) . ?
C1 C6 1.524(7) . ?
C1 N1 1.502(7) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C3 1.522(9) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.504(10) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 C5 1.524(11) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C6 1.529(9) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 O1 1.145(7) . ?
C7 Re1 1.956(6) . ?
C8 O2 1.150(7) . ?
C8 Re1 1.945(6) . ?
C9 Br3 0.644(8) . ?
C9 Re1 1.947(9) . ?
C9 O3 1.138(10) . ?
C11 C12 1.396(8) . ?
C11 C16 1.394(8) . ?
C11 P1 1.826(5) . ?
C12 H12 0.9300 . ?
C12 C13 1.381(7) . ?
C13 H13 0.9300 . ?
C13 C14 1.385(9) . ?
C14 C15 1.381(9) . ?
C14 C17 1.510(7) . ?
C15 H15 0.9300 . ?
C15 C16 1.400(8) . ?
C16 H16 0.9300 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C21 C22 1.395(7) . ?
C21 C26 1.394(8) . ?
C21 P1 1.810(5) . ?
C22 H22 0.9300 . ?
C22 C23 1.380(8) . ?
C23 H23 0.9300 . ?
C23 C24 1.390(9) . ?
C24 C25 1.390(8) . ?
C24 C27 1.517(8) . ?
C25 H25 0.9300 . ?
C25 C26 1.397(8) . ?
C26 H26 0.9300 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C31 C32 1.390(8) . ?
C31 C36 1.401(8) . ?
C31 P2 1.821(5) . ?
C32 H32 0.9300 . ?
C32 C33 1.400(7) . ?
C33 H33 0.9300 . ?
C33 C34 1.383(8) . ?
C34 C35 1.392(9) . ?
C34 C37 1.516(8) . ?
C35 H35 0.9300 . ?
C35 C36 1.397(7) . ?
C36 H36 0.9300 . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?
C41 C42 1.390(7) . ?
C41 C46 1.394(7) . ?
C41 P2 1.823(5) . ?
C42 H42 0.9300 . ?
C42 C43 1.381(8) . ?
C43 H43 0.9300 . ?
C43 C44 1.383(8) . ?
C44 C45 1.386(8) . ?
C44 C47 1.516(7) . ?
C45 H45 0.9300 . ?
C45 C46 1.390(7) . ?
C46 H46 0.9300 . ?
C47 H47A 0.9600 . ?
C47 H47B 0.9600 . ?
C47 H47C 0.9600 . ?
N1 P1 1.698(4) . ?
N1 P2 1.713(5) . ?
Br3 Re1 2.554(9) . ?
Br3 O3 0.565(9) . ?
P1 P2 2.684(2) . ?
P1 Re1 2.4586(16) . ?
P2 Re1 2.4635(15) . ?
Br1 Re1 2.6489(10) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 H1 106.8 . . ?
C6 C1 H1 106.8 . . ?
C6 C1 C2 112.1(5) . . ?
N1 C1 H1 106.8 . . ?
N1 C1 C2 112.6(5) . . ?
N1 C1 C6 111.4(4) . . ?
C1 C2 H2A 109.3 . . ?
C1 C2 H2B 109.3 . . ?
H2A C2 H2B 108.0 . . ?
C3 C2 C1 111.4(6) . . ?
C3 C2 H2A 109.3 . . ?
C3 C2 H2B 109.3 . . ?
C2 C3 H3A 109.4 . . ?
C2 C3 H3B 109.4 . . ?
H3A C3 H3B 108.0 . . ?
C4 C3 C2 111.1(5) . . ?
C4 C3 H3A 109.4 . . ?
C4 C3 H3B 109.4 . . ?
C3 C4 H4A 109.6 . . ?
C3 C4 H4B 109.6 . . ?
C3 C4 C5 110.1(6) . . ?
H4A C4 H4B 108.2 . . ?
C5 C4 H4A 109.6 . . ?
C5 C4 H4B 109.6 . . ?
C4 C5 H5A 109.6 . . ?
C4 C5 H5B 109.6 . . ?
C4 C5 C6 110.3(6) . . ?
H5A C5 H5B 108.1 . . ?
C6 C5 H5A 109.6 . . ?
C6 C5 H5B 109.6 . . ?
C1 C6 C5 111.7(5) . . ?
C1 C6 H6A 109.3 . . ?
C1 C6 H6B 109.3 . . ?
C5 C6 H6A 109.3 . . ?
C5 C6 H6B 109.3 . . ?
H6A C6 H6B 107.9 . . ?
O1 C7 Re1 178.9(6) . . ?
O2 C8 Re1 178.4(6) . . ?
Br3 C9 Re1 157.8(15) . . ?
Br3 C9 O3 18.5(13) . . ?
O3 C9 Re1 176.2(10) . . ?
C12 C11 P1 119.3(4) . . ?
C16 C11 C12 118.8(5) . . ?
C16 C11 P1 121.9(4) . . ?
C11 C12 H12 119.8 . . ?
C13 C12 C11 120.3(5) . . ?
C13 C12 H12 119.8 . . ?
C12 C13 H13 119.4 . . ?
C12 C13 C14 121.3(5) . . ?
C14 C13 H13 119.4 . . ?
C13 C14 C17 120.9(5) . . ?
C15 C14 C13 118.7(5) . . ?
C15 C14 C17 120.4(6) . . ?
C14 C15 H15 119.6 . . ?
C14 C15 C16 120.9(6) . . ?
C16 C15 H15 119.6 . . ?
C11 C16 C15 119.9(6) . . ?
C11 C16 H16 120.0 . . ?
C15 C16 H16 120.0 . . ?
C14 C17 H17A 109.5 . . ?
C14 C17 H17B 109.5 . . ?
C14 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C22 C21 P1 116.6(4) . . ?
C26 C21 C22 118.2(5) . . ?
C26 C21 P1 125.1(4) . . ?
C21 C22 H22 119.5 . . ?
C23 C22 C21 121.1(6) . . ?
C23 C22 H22 119.5 . . ?
C22 C23 H23 119.3 . . ?
C22 C23 C24 121.5(5) . . ?
C24 C23 H23 119.3 . . ?
C23 C24 C25 117.5(5) . . ?
C23 C24 C27 121.3(6) . . ?
C25 C24 C27 121.1(6) . . ?
C24 C25 H25 119.2 . . ?
C24 C25 C26 121.6(5) . . ?
C26 C25 H25 119.2 . . ?
C21 C26 C25 120.1(5) . . ?
C21 C26 H26 119.9 . . ?
C25 C26 H26 119.9 . . ?
C24 C27 H27A 109.5 . . ?
C24 C27 H27B 109.5 . . ?
C24 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C32 C31 C36 119.2(5) . . ?
C32 C31 P2 120.8(4) . . ?
C36 C31 P2 119.7(4) . . ?
C31 C32 H32 119.8 . . ?
C31 C32 C33 120.4(5) . . ?
C33 C32 H32 119.8 . . ?
C32 C33 H33 119.7 . . ?
C34 C33 C32 120.6(5) . . ?
C34 C33 H33 119.7 . . ?
C33 C34 C35 119.1(5) . . ?
C33 C34 C37 120.5(6) . . ?
C35 C34 C37 120.3(6) . . ?
C34 C35 H35 119.5 . . ?
C34 C35 C36 120.9(5) . . ?
C36 C35 H35 119.5 . . ?
C31 C36 H36 120.1 . . ?
C35 C36 C31 119.7(5) . . ?
C35 C36 H36 120.1 . . ?
C34 C37 H37A 109.5 . . ?
C34 C37 H37B 109.5 . . ?
C34 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C42 C41 C46 117.6(5) . . ?
C42 C41 P2 124.3(4) . . ?
C46 C41 P2 118.2(4) . . ?
C41 C42 H42 119.3 . . ?
C43 C42 C41 121.4(5) . . ?
C43 C42 H42 119.3 . . ?
C42 C43 H43 119.3 . . ?
C42 C43 C44 121.4(5) . . ?
C44 C43 H43 119.3 . . ?
C43 C44 C45 117.4(5) . . ?
C43 C44 C47 121.6(5) . . ?
C45 C44 C47 120.9(5) . . ?
C44 C45 H45 119.1 . . ?
C44 C45 C46 121.8(5) . . ?
C46 C45 H45 119.1 . . ?
C41 C46 H46 119.8 . . ?
C45 C46 C41 120.4(5) . . ?
C45 C46 H46 119.8 . . ?
C44 C47 H47A 109.5 . . ?
C44 C47 H47B 109.5 . . ?
C44 C47 H47C 109.5 . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C1 N1 P1 125.1(4) . . ?
C1 N1 P2 130.2(4) . . ?
P1 N1 P2 103.8(2) . . ?
C9 Br3 Re1 16.8(12) . . ?
O3 Br3 C9 140(3) . . ?
O3 Br3 Re1 157(2) . . ?
C11 P1 P2 126.72(18) . . ?
C11 P1 Re1 127.44(19) . . ?
C21 P1 C11 102.7(2) . . ?
C21 P1 P2 124.28(17) . . ?
C21 P1 Re1 113.82(18) . . ?
N1 P1 C11 106.7(2) . . ?
N1 P1 C21 109.9(2) . . ?
N1 P1 P2 38.31(16) . . ?
N1 P1 Re1 95.31(16) . . ?
Re1 P1 P2 57.04(5) . . ?
C31 P2 C41 104.6(2) . . ?
C31 P2 P1 122.23(19) . . ?
C31 P2 Re1 113.31(17) . . ?
C41 P2 P1 127.15(17) . . ?
C41 P2 Re1 126.25(18) . . ?
N1 P2 C31 108.3(2) . . ?
N1 P2 C41 108.1(2) . . ?
N1 P2 P1 37.92(14) . . ?
N1 P2 Re1 94.73(15) . . ?
Re1 P2 P1 56.87(5) . . ?
C7 Re1 Br3 82.8(2) . . ?
C7 Re1 P1 100.14(19) . . ?
C7 Re1 P2 165.50(19) . . ?
C7 Re1 Br1 84.73(17) . . ?
C8 Re1 C7 94.0(3) . . ?
C8 Re1 C9 89.7(3) . . ?
C8 Re1 Br3 87.2(3) . . ?
C8 Re1 P1 165.66(18) . . ?
C8 Re1 P2 99.64(18) . . ?
C8 Re1 Br1 84.61(17) . . ?
C9 Re1 C7 87.5(3) . . ?
C9 Re1 Br3 5.5(4) . . ?
C9 Re1 P1 88.4(3) . . ?
C9 Re1 P2 87.6(3) . . ?
P1 Re1 Br3 92.0(2) . . ?
P1 Re1 P2 66.09(5) . . ?
P1 Re1 Br1 99.18(4) . . ?
P2 Re1 Br3 92.84(19) . . ?
P2 Re1 Br1 101.44(4) . . ?
Br3 O3 C9 21.2(15) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 55.8(8) . . . . ?
C1 N1 P1 C11 41.2(5) . . . . ?
C1 N1 P1 C21 -69.4(4) . . . . ?
C1 N1 P1 P2 170.1(5) . . . . ?
C1 N1 P1 Re1 172.9(4) . . . . ?
C1 N1 P2 C31 71.4(5) . . . . ?
C1 N1 P2 C41 -41.5(5) . . . . ?
C1 N1 P2 P1 -169.3(6) . . . . ?
C1 N1 P2 Re1 -172.1(4) . . . . ?
C2 C1 C6 C5 51.8(7) . . . . ?
C2 C1 N1 P1 -92.6(5) . . . . ?
C2 C1 N1 P2 74.7(6) . . . . ?
C2 C3 C4 C5 -59.7(8) . . . . ?
C3 C4 C5 C6 59.3(8) . . . . ?
C4 C5 C6 C1 -55.4(8) . . . . ?
C6 C1 C2 C3 -51.6(7) . . . . ?
C6 C1 N1 P1 140.5(4) . . . . ?
C6 C1 N1 P2 -52.2(6) . . . . ?
C11 C12 C13 C14 0.5(9) . . . . ?
C12 C11 C16 C15 0.7(9) . . . . ?
C12 C11 P1 C21 -167.0(4) . . . . ?
C12 C11 P1 N1 77.5(5) . . . . ?
C12 C11 P1 P2 40.4(5) . . . . ?
C12 C11 P1 Re1 -33.1(5) . . . . ?
C12 C13 C14 C15 1.3(9) . . . . ?
C12 C13 C14 C17 180.0(6) . . . . ?
C13 C14 C15 C16 -2.2(10) . . . . ?
C14 C15 C16 C11 1.1(10) . . . . ?
C16 C11 C12 C13 -1.5(8) . . . . ?
C16 C11 P1 C21 12.9(5) . . . . ?
C16 C11 P1 N1 -102.7(5) . . . . ?
C16 C11 P1 P2 -139.7(4) . . . . ?
C16 C11 P1 Re1 146.7(4) . . . . ?
C17 C14 C15 C16 179.2(6) . . . . ?
C21 C22 C23 C24 -1.5(9) . . . . ?
C22 C21 C26 C25 0.5(8) . . . . ?
C22 C21 P1 C11 76.4(5) . . . . ?
C22 C21 P1 N1 -170.4(4) . . . . ?
C22 C21 P1 P2 -130.1(4) . . . . ?
C22 C21 P1 Re1 -64.9(4) . . . . ?
C22 C23 C24 C25 1.9(9) . . . . ?
C22 C23 C24 C27 -176.1(6) . . . . ?
C23 C24 C25 C26 -1.2(8) . . . . ?
C24 C25 C26 C21 0.1(8) . . . . ?
C26 C21 C22 C23 0.2(8) . . . . ?
C26 C21 P1 C11 -106.8(5) . . . . ?
C26 C21 P1 N1 6.4(5) . . . . ?
C26 C21 P1 P2 46.7(5) . . . . ?
C26 C21 P1 Re1 112.0(4) . . . . ?
C27 C24 C25 C26 176.8(5) . . . . ?
C31 C32 C33 C34 -1.5(9) . . . . ?
C32 C31 C36 C35 -2.5(8) . . . . ?
C32 C31 P2 C41 142.4(5) . . . . ?
C32 C31 P2 N1 27.2(5) . . . . ?
C32 C31 P2 P1 -12.1(5) . . . . ?
C32 C31 P2 Re1 -76.5(5) . . . . ?
C32 C33 C34 C35 -0.2(9) . . . . ?
C32 C33 C34 C37 178.4(6) . . . . ?
C33 C34 C35 C36 0.5(9) . . . . ?
C34 C35 C36 C31 0.8(9) . . . . ?
C36 C31 C32 C33 2.8(8) . . . . ?
C36 C31 P2 C41 -43.4(5) . . . . ?
C36 C31 P2 N1 -158.6(4) . . . . ?
C36 C31 P2 P1 162.1(4) . . . . ?
C36 C31 P2 Re1 97.7(4) . . . . ?
C37 C34 C35 C36 -178.1(5) . . . . ?
C41 C42 C43 C44 0.1(10) . . . . ?
C42 C41 C46 C45 0.9(8) . . . . ?
C42 C41 P2 C31 -23.3(5) . . . . ?
C42 C41 P2 N1 92.1(5) . . . . ?
C42 C41 P2 P1 129.6(4) . . . . ?
C42 C41 P2 Re1 -157.6(4) . . . . ?
C42 C43 C44 C45 0.7(9) . . . . ?
C42 C43 C44 C47 -179.0(6) . . . . ?
C43 C44 C45 C46 -0.7(9) . . . . ?
C44 C45 C46 C41 -0.1(9) . . . . ?
C46 C41 C42 C43 -0.9(9) . . . . ?
C46 C41 P2 C31 158.0(4) . . . . ?
C46 C41 P2 N1 -86.7(5) . . . . ?
C46 C41 P2 P1 -49.2(5) . . . . ?
C46 C41 P2 Re1 23.6(5) . . . . ?
C47 C44 C45 C46 179.0(6) . . . . ?
N1 C1 C2 C3 -178.2(5) . . . . ?
N1 C1 C6 C5 179.0(5) . . . . ?
P1 C11 C12 C13 178.3(4) . . . . ?
P1 C11 C16 C15 -179.1(5) . . . . ?
P1 C21 C22 C23 177.3(5) . . . . ?
P1 C21 C26 C25 -176.3(4) . . . . ?
P1 N1 P2 C31 -119.3(2) . . . . ?
P1 N1 P2 C41 127.9(2) . . . . ?
P1 N1 P2 Re1 -2.8(2) . . . . ?
P2 C31 C32 C33 177.0(4) . . . . ?
P2 C31 C36 C35 -176.8(4) . . . . ?
P2 C41 C42 C43 -179.7(5) . . . . ?
P2 C41 C46 C45 179.8(4) . . . . ?
P2 N1 P1 C11 -128.9(2) . . . . ?
P2 N1 P1 C21 120.5(2) . . . . ?
P2 N1 P1 Re1 2.8(2) . . . . ?
Re1 C9 Br3 O3 179(3) . . . . ?
Re1 Br3 O3 C9 1(2) . . . . ?
O3 C9 Br3 Re1 -179(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.484(7)
2 0.516(7)


####################################################################### 
# 
# 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_tdk150615
_database_code_depnum_ccdc_archive 'CCDC 1558629'
loop_
_audit_author_name
_audit_author_address
'DV Kama'
;University of the Free State
South Africa
;
_audit_update_record             
;
2021-10-12 deposited with the CCDC.	2021-10-20 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT910_tdk150615           
;
PROBLEM: Test for missing reflections below Theta-Min ,
RESPONSE: 6 reflections that are below Theta (min) value have been omitted
 from the refinement. The FCF reflections are caused
 by partial obscurity of the beam stop and due to overflow
 reflections which are not automatically excluded
 by the Bruker APEX II software. Sufficient unique
 reflections were obtained (8599) to yield
 a fully refined structure with 96.0 % data completeness.
;

# end Validation Reply Form
_audit_creation_date             2021-10-12
_audit_creation_method           
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C37 H39 Cl N O3 P2 Tc'
_chemical_formula_sum            'C37 H39 Cl N O3 P2 Tc'
_chemical_formula_weight         741.08
_chemical_absolute_configuration ?
_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'
Cl Cl 0.1484 0.1585 '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'
Tc Tc -1.4390 0.7593 '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           1
_space_group_name_H-M_alt        'P 1'
_space_group_name_Hall           'P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'

_cell_length_a                   9.6184(3)
_cell_length_b                   9.8959(4)
_cell_length_c                   10.6919(4)
_cell_angle_alpha                92.434(3)
_cell_angle_beta                 111.683(3)
_cell_angle_gamma                104.288(3)
_cell_volume                     906.27(6)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    6867
_cell_measurement_temperature    182.9(6)
_cell_measurement_theta_max      29.0160
_cell_measurement_theta_min      3.0180
_shelx_estimated_absorpt_T_max   0.944
_shelx_estimated_absorpt_T_min   0.879
_exptl_absorpt_coefficient_mu    0.594
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71362
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.358
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       cube
_exptl_crystal_F_000             382
_exptl_crystal_size_max          0.222
_exptl_crystal_size_mid          0.119
_exptl_crystal_size_min          0.099
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0387
_diffrn_reflns_av_unetI/netI     0.0651
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            15248
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.000
_diffrn_reflns_theta_min         3.021
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      182.9(6)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4498
_diffrn_detector_type            Ruby
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
'#__ type_ start__ end____ width___ exp.time_ 1 omega 10.00 64.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 16.1514 57.0000 -90.0000 54 #__ type_ start__ end____ width___ exp.time_ 2 omega 13.00 89.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 16.1514 57.0000 -30.0000 76 #__ type_ start__ end____ width___ exp.time_ 3 omega 1.00 63.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 16.1514 57.0000 -150.0000 62 #__ type_ start__ end____ width___ exp.time_ 4 omega -25.00 23.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 16.1514 -48.0000 -19.0000 48 #__ type_ start__ end____ width___ exp.time_ 5 omega -12.00 89.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 16.1514 60.0000 104.2145 101 #__ type_ start__ end____ width___ exp.time_ 6 omega 53.00 79.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 16.1514 38.0000 30.0000 26 #__ type_ start__ end____ width___ exp.time_ 7 omega -38.00 48.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 18.0000 -58.0000 52.5966 86 #__ type_ start__ end____ width___ exp.time_ 8 omega -39.00 48.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 18.0000 -59.0000 -138.5858 87 #__ type_ start__ end____ width___ exp.time_ 9 omega -54.00 45.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 18.0000 -57.0000 -34.2645 99 #__ type_ start__ end____ width___ exp.time_ 10 omega -28.00 9.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 18.0000 -60.0000 143.0809 37'
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Ruby'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0253209000
_diffrn_orient_matrix_UB_12      -0.0631475000
_diffrn_orient_matrix_UB_13      0.0243561000
_diffrn_orient_matrix_UB_21      -0.0343061000
_diffrn_orient_matrix_UB_22      0.0352275000
_diffrn_orient_matrix_UB_23      0.0346041000
_diffrn_orient_matrix_UB_31      -0.0709241000
_diffrn_orient_matrix_UB_32      -0.0191637000
_diffrn_orient_matrix_UB_33      -0.0585064000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.922
_reflns_Friedel_fraction_full    0.948
_reflns_Friedel_fraction_max     0.920
_reflns_number_gt                7693
_reflns_number_total             8390
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
'CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01)'
_computing_data_collection       
'CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01)'
_computing_data_reduction        
'CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01)'
_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    ?
_refine_diff_density_max         1.044
_refine_diff_density_min         -0.879
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.38(4)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     399
_refine_ls_number_reflns         8390
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0521
_refine_ls_R_factor_gt           0.0459
_refine_ls_restrained_S_all      1.026
_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)+(0.0522P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0992
_refine_ls_wR_factor_ref         0.1035
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.62(4)
 0.38(4)
2. 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
3. Uiso/Uaniso restraints and constraints
Uanis(C6) = Uanis(C3)
Uanis(C1) = Uanis(C4)
4.a Ternary CH refined with riding coordinates:
 C1(H1)
4.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B)
4.c Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C15(H15), C16(H16), C22(H22), C23(H23), C25(H25),
 C26(H26), C32(H32), C33(H33), C35(H35), C36(H36), C42(H42), C43(H43), C45(H45),
  C46(H46)
4.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C27(H27A,H27B,H27C), C37(H37A,H37B,H37C), C47(H47A,H47B,
 H47C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C -0.0312(9) 0.9105(9) 0.7836(7) 0.0557(14) Uani 1 1 d . . . . .
H1 H -0.081828 0.826898 0.813307 0.067 Uiso 1 1 calc R . . . .
C2 C -0.1537(9) 0.9889(9) 0.7302(8) 0.0560(19) Uani 1 1 d . . . . .
H2A H -0.245181 0.928150 0.656690 0.067 Uiso 1 1 calc R . . . .
H2B H -0.112804 1.071165 0.694589 0.067 Uiso 1 1 calc R . . . .
C3 C -0.1991(9) 1.0348(10) 0.8451(7) 0.0646(17) Uani 1 1 d . . . . .
H3A H -0.273363 1.088852 0.811725 0.077 Uiso 1 1 calc R . . . .
H3B H -0.248331 0.952118 0.875215 0.077 Uiso 1 1 calc R . . . .
C4 C -0.0552(9) 1.1239(8) 0.9640(7) 0.0557(14) Uani 1 1 d . . . . .
H4A H -0.009689 1.208878 0.934560 0.067 Uiso 1 1 calc R . . . .
H4B H -0.085604 1.151745 1.035952 0.067 Uiso 1 1 calc R . . . .
C5 C 0.0605(10) 1.0480(10) 1.0169(7) 0.068(2) Uani 1 1 d . . . . .
H5A H 0.019143 0.970138 1.057213 0.081 Uiso 1 1 calc R . . . .
H5B H 0.152515 1.110652 1.088417 0.081 Uiso 1 1 calc R . . . .
C6 C 0.1080(10) 0.9906(10) 0.9095(8) 0.0646(17) Uani 1 1 d . . . . .
H6A H 0.170937 1.068307 0.884091 0.077 Uiso 1 1 calc R . . . .
H6B H 0.171552 0.928480 0.947745 0.077 Uiso 1 1 calc R . . . .
C7 C 0.2002(8) 0.8202(7) 0.3339(7) 0.0391(14) Uani 1 1 d . . . . .
C8 C 0.1392(7) 0.5491(7) 0.4193(7) 0.0393(14) Uani 1 1 d . . . . .
C9 C -0.0822(8) 0.6833(7) 0.3383(6) 0.0372(14) Uani 1 1 d . . . . .
C11 C 0.2217(6) 1.1078(6) 0.6595(6) 0.0317(12) Uani 1 1 d . . . . .
C12 C 0.3775(6) 1.1097(7) 0.7216(6) 0.0372(13) Uani 1 1 d . . . . .
H12 H 0.406227 1.027593 0.714151 0.045 Uiso 1 1 calc R . . . .
C13 C 0.4896(7) 1.2328(7) 0.7941(6) 0.0417(14) Uani 1 1 d . . . . .
H13 H 0.592874 1.231394 0.834713 0.050 Uiso 1 1 calc R . . . .
C14 C 0.4545(7) 1.3577(7) 0.8088(6) 0.0403(14) Uani 1 1 d . . . . .
C15 C 0.3013(8) 1.3559(7) 0.7498(7) 0.0494(17) Uani 1 1 d . . . . .
H15 H 0.273776 1.438591 0.757969 0.059 Uiso 1 1 calc R . . . .
C16 C 0.1857(7) 1.2324(6) 0.6778(6) 0.0417(14) Uani 1 1 d . . . . .
H16 H 0.082021 1.233629 0.641155 0.050 Uiso 1 1 calc R . . . .
C17 C 0.5825(8) 1.4915(7) 0.8878(8) 0.058(2) Uani 1 1 d . . . . .
H17A H 0.570309 1.567623 0.835683 0.087 Uiso 1 1 calc GR . . . .
H17B H 0.682511 1.476979 0.904475 0.087 Uiso 1 1 calc GR . . . .
H17C H 0.575419 1.514494 0.972943 0.087 Uiso 1 1 calc GR . . . .
C21 C -0.0784(6) 0.9988(6) 0.4429(5) 0.0284(11) Uani 1 1 d . . . . .
C22 C -0.0480(7) 1.1088(7) 0.3712(6) 0.0394(14) Uani 1 1 d . . . . .
H22 H 0.054789 1.158990 0.390659 0.047 Uiso 1 1 calc R . . . .
C23 C -0.1677(8) 1.1451(7) 0.2714(6) 0.0442(15) Uani 1 1 d . . . . .
H23 H -0.144047 1.220520 0.226571 0.053 Uiso 1 1 calc R . . . .
C24 C -0.3229(7) 1.0702(7) 0.2374(6) 0.0405(14) Uani 1 1 d . . . . .
C25 C -0.3531(7) 0.9592(7) 0.3049(6) 0.0435(15) Uani 1 1 d . . . . .
H25 H -0.456168 0.907575 0.282497 0.052 Uiso 1 1 calc R . . . .
C26 C -0.2338(7) 0.9206(7) 0.4069(6) 0.0365(13) Uani 1 1 d . . . . .
H26 H -0.257936 0.843930 0.450071 0.044 Uiso 1 1 calc R . . . .
C27 C -0.4517(9) 1.1101(10) 0.1295(8) 0.069(2) Uani 1 1 d . . . . .
H27A H -0.549935 1.044446 0.115503 0.103 Uiso 1 1 calc GR . . . .
H27B H -0.435618 1.108189 0.046110 0.103 Uiso 1 1 calc GR . . . .
H27C H -0.452103 1.203352 0.157856 0.103 Uiso 1 1 calc GR . . . .
C31 C -0.1543(6) 0.5599(6) 0.5958(5) 0.0299(11) Uani 1 1 d . . . . .
C32 C -0.2925(7) 0.5854(7) 0.5863(6) 0.0360(13) Uani 1 1 d . . . . .
H32 H -0.292607 0.675769 0.613929 0.043 Uiso 1 1 calc R . . . .
C33 C -0.4304(7) 0.4781(7) 0.5361(7) 0.0433(15) Uani 1 1 d . . . . .
H33 H -0.522190 0.496677 0.531415 0.052 Uiso 1 1 calc R . . . .
C34 C -0.4337(7) 0.3432(8) 0.4927(6) 0.0431(16) Uani 1 1 d . . . . .
C35 C -0.2939(8) 0.3164(7) 0.5049(7) 0.0512(18) Uani 1 1 d . . . . .
H35 H -0.293414 0.225467 0.479634 0.061 Uiso 1 1 calc R . . . .
C36 C -0.1550(8) 0.4249(7) 0.5545(7) 0.0448(15) Uani 1 1 d . . . . .
H36 H -0.062640 0.406838 0.560024 0.054 Uiso 1 1 calc R . . . .
C37 C -0.5864(9) 0.2262(9) 0.4301(8) 0.068(2) Uani 1 1 d . . . . .
H37A H -0.641171 0.237130 0.337517 0.102 Uiso 1 1 calc GR . . . .
H37B H -0.649385 0.231107 0.480980 0.102 Uiso 1 1 calc GR . . . .
H37C H -0.564853 0.136385 0.432329 0.102 Uiso 1 1 calc GR . . . .
C41 C 0.1388(6) 0.6549(6) 0.8214(6) 0.0333(12) Uani 1 1 d . . . . .
C42 C 0.0667(7) 0.5649(7) 0.8894(6) 0.0426(14) Uani 1 1 d . . . . .
H42 H -0.040325 0.522999 0.848055 0.051 Uiso 1 1 calc R . . . .
C43 C 0.1500(8) 0.5348(8) 1.0184(7) 0.0521(19) Uani 1 1 d . . . . .
H43 H 0.100264 0.472872 1.061941 0.063 Uiso 1 1 calc R . . . .
C44 C 0.3124(8) 0.6020(7) 1.0802(7) 0.0458(16) Uani 1 1 d . . . . .
C45 C 0.3813(7) 0.6907(7) 1.0136(6) 0.0424(15) Uani 1 1 d . . . . .
H45 H 0.488153 0.733629 1.054942 0.051 Uiso 1 1 calc R . . . .
C46 C 0.2985(7) 0.7199(7) 0.8862(6) 0.0368(13) Uani 1 1 d . . . . .
H46 H 0.349389 0.782602 0.843997 0.044 Uiso 1 1 calc R . . . .
C47 C 0.4029(10) 0.5677(10) 1.2171(8) 0.065(2) Uani 1 1 d . . . . .
H47A H 0.511810 0.593337 1.233646 0.097 Uiso 1 1 calc GR . . . .
H47B H 0.367149 0.468444 1.218519 0.097 Uiso 1 1 calc GR . . . .
H47C H 0.387387 0.619412 1.286485 0.097 Uiso 1 1 calc GR . . . .
N1 N 0.0104(5) 0.8550(5) 0.6746(5) 0.0283(10) Uani 1 1 d . . . . .
O1 O 0.2409(6) 0.8663(6) 0.2553(5) 0.0631(14) Uani 1 1 d . . . . .
O2 O 0.1417(6) 0.4418(5) 0.3864(6) 0.0587(14) Uani 1 1 d . . . . .
O3 O -0.1981(6) 0.6488(6) 0.2585(5) 0.0608(14) Uani 1 1 d . . . . .
P1 P 0.07849(16) 0.94423(16) 0.56488(14) 0.0281(3) Uani 1 1 d . . . . .
P2 P 0.03337(15) 0.69262(15) 0.65225(14) 0.0272(3) Uani 1 1 d . . . . .
Cl1 Cl 0.41611(19) 0.78511(19) 0.61812(19) 0.0459(4) Uani 1 1 d . . . . .
Tc1 Tc 0.13088(2) 0.73816(2) 0.47177(2) 0.03042(13) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 H1 0.9800 . ?
C1 C2 1.519(10) . ?
C1 C6 1.512(10) . ?
C1 N1 1.490(8) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C3 1.534(9) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.520(10) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 C5 1.452(11) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C6 1.520(10) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 O1 1.120(8) . ?
C7 Tc1 1.959(7) . ?
C8 O2 1.113(8) . ?
C8 Tc1 1.960(7) . ?
C9 O3 1.082(8) . ?
C9 Tc1 1.938(7) . ?
C11 C12 1.392(8) . ?
C11 C16 1.385(8) . ?
C11 P1 1.809(6) . ?
C12 H12 0.9300 . ?
C12 C13 1.378(8) . ?
C13 H13 0.9300 . ?
C13 C14 1.376(9) . ?
C14 C15 1.368(9) . ?
C14 C17 1.522(8) . ?
C15 H15 0.9300 . ?
C15 C16 1.393(8) . ?
C16 H16 0.9300 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C21 C22 1.392(8) . ?
C21 C26 1.399(8) . ?
C21 P1 1.811(5) . ?
C22 H22 0.9300 . ?
C22 C23 1.386(9) . ?
C23 H23 0.9300 . ?
C23 C24 1.393(9) . ?
C24 C25 1.370(9) . ?
C24 C27 1.499(9) . ?
C25 H25 0.9300 . ?
C25 C26 1.407(8) . ?
C26 H26 0.9300 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C31 C32 1.381(8) . ?
C31 C36 1.387(8) . ?
C31 P2 1.818(5) . ?
C32 H32 0.9300 . ?
C32 C33 1.381(8) . ?
C33 H33 0.9300 . ?
C33 C34 1.383(10) . ?
C34 C35 1.395(10) . ?
C34 C37 1.521(8) . ?
C35 H35 0.9300 . ?
C35 C36 1.392(9) . ?
C36 H36 0.9300 . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?
C41 C42 1.387(9) . ?
C41 C46 1.394(8) . ?
C41 P2 1.824(6) . ?
C42 H42 0.9300 . ?
C42 C43 1.404(9) . ?
C43 H43 0.9300 . ?
C43 C44 1.416(9) . ?
C44 C45 1.353(10) . ?
C44 C47 1.504(10) . ?
C45 H45 0.9300 . ?
C45 C46 1.386(8) . ?
C46 H46 0.9300 . ?
C47 H47A 0.9600 . ?
C47 H47B 0.9600 . ?
C47 H47C 0.9600 . ?
N1 P1 1.719(5) . ?
N1 P2 1.694(5) . ?
P1 P2 2.688(2) . ?
P1 Tc1 2.4717(15) . ?
P2 Tc1 2.4513(15) . ?
Cl1 Tc1 2.5155(17) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 H1 105.3 . . ?
C6 C1 H1 105.3 . . ?
C6 C1 C2 113.5(6) . . ?
N1 C1 H1 105.3 . . ?
N1 C1 C2 112.5(6) . . ?
N1 C1 C6 114.0(6) . . ?
C1 C2 H2A 109.7 . . ?
C1 C2 H2B 109.7 . . ?
C1 C2 C3 109.9(6) . . ?
H2A C2 H2B 108.2 . . ?
C3 C2 H2A 109.7 . . ?
C3 C2 H2B 109.7 . . ?
C2 C3 H3A 109.6 . . ?
C2 C3 H3B 109.6 . . ?
H3A C3 H3B 108.1 . . ?
C4 C3 C2 110.2(6) . . ?
C4 C3 H3A 109.6 . . ?
C4 C3 H3B 109.6 . . ?
C3 C4 H4A 109.3 . . ?
C3 C4 H4B 109.3 . . ?
H4A C4 H4B 107.9 . . ?
C5 C4 C3 111.8(7) . . ?
C5 C4 H4A 109.3 . . ?
C5 C4 H4B 109.3 . . ?
C4 C5 H5A 108.9 . . ?
C4 C5 H5B 108.9 . . ?
C4 C5 C6 113.5(7) . . ?
H5A C5 H5B 107.7 . . ?
C6 C5 H5A 108.9 . . ?
C6 C5 H5B 108.9 . . ?
C1 C6 C5 112.3(7) . . ?
C1 C6 H6A 109.1 . . ?
C1 C6 H6B 109.1 . . ?
C5 C6 H6A 109.1 . . ?
C5 C6 H6B 109.1 . . ?
H6A C6 H6B 107.9 . . ?
O1 C7 Tc1 179.2(6) . . ?
O2 C8 Tc1 178.3(7) . . ?
O3 C9 Tc1 175.5(6) . . ?
C12 C11 P1 118.9(4) . . ?
C16 C11 C12 117.1(5) . . ?
C16 C11 P1 124.0(4) . . ?
C11 C12 H12 119.8 . . ?
C13 C12 C11 120.3(6) . . ?
C13 C12 H12 119.8 . . ?
C12 C13 H13 118.7 . . ?
C14 C13 C12 122.6(6) . . ?
C14 C13 H13 118.7 . . ?
C13 C14 C17 120.8(6) . . ?
C15 C14 C13 117.3(6) . . ?
C15 C14 C17 121.9(6) . . ?
C14 C15 H15 119.4 . . ?
C14 C15 C16 121.1(6) . . ?
C16 C15 H15 119.4 . . ?
C11 C16 C15 121.4(6) . . ?
C11 C16 H16 119.3 . . ?
C15 C16 H16 119.3 . . ?
C14 C17 H17A 109.5 . . ?
C14 C17 H17B 109.5 . . ?
C14 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C22 C21 C26 118.0(5) . . ?
C22 C21 P1 121.2(4) . . ?
C26 C21 P1 120.4(5) . . ?
C21 C22 H22 119.3 . . ?
C23 C22 C21 121.4(6) . . ?
C23 C22 H22 119.3 . . ?
C22 C23 H23 119.6 . . ?
C22 C23 C24 120.8(6) . . ?
C24 C23 H23 119.6 . . ?
C23 C24 C27 120.6(7) . . ?
C25 C24 C23 117.9(5) . . ?
C25 C24 C27 121.5(6) . . ?
C24 C25 H25 118.9 . . ?
C24 C25 C26 122.3(6) . . ?
C26 C25 H25 118.9 . . ?
C21 C26 C25 119.4(6) . . ?
C21 C26 H26 120.3 . . ?
C25 C26 H26 120.3 . . ?
C24 C27 H27A 109.5 . . ?
C24 C27 H27B 109.5 . . ?
C24 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C32 C31 C36 119.4(5) . . ?
C32 C31 P2 125.2(4) . . ?
C36 C31 P2 115.4(4) . . ?
C31 C32 H32 119.7 . . ?
C33 C32 C31 120.6(6) . . ?
C33 C32 H32 119.7 . . ?
C32 C33 H33 119.6 . . ?
C32 C33 C34 120.9(6) . . ?
C34 C33 H33 119.6 . . ?
C33 C34 C35 118.7(5) . . ?
C33 C34 C37 121.2(6) . . ?
C35 C34 C37 120.1(7) . . ?
C34 C35 H35 119.8 . . ?
C36 C35 C34 120.4(7) . . ?
C36 C35 H35 119.8 . . ?
C31 C36 C35 120.0(6) . . ?
C31 C36 H36 120.0 . . ?
C35 C36 H36 120.0 . . ?
C34 C37 H37A 109.5 . . ?
C34 C37 H37B 109.5 . . ?
C34 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C42 C41 C46 118.3(5) . . ?
C42 C41 P2 122.9(4) . . ?
C46 C41 P2 118.8(5) . . ?
C41 C42 H42 118.9 . . ?
C41 C42 C43 122.2(6) . . ?
C43 C42 H42 118.9 . . ?
C42 C43 H43 121.1 . . ?
C42 C43 C44 117.7(7) . . ?
C44 C43 H43 121.1 . . ?
C43 C44 C47 118.0(7) . . ?
C45 C44 C43 119.6(6) . . ?
C45 C44 C47 122.4(6) . . ?
C44 C45 H45 118.8 . . ?
C44 C45 C46 122.4(6) . . ?
C46 C45 H45 118.8 . . ?
C41 C46 H46 120.1 . . ?
C45 C46 C41 119.8(6) . . ?
C45 C46 H46 120.1 . . ?
C44 C47 H47A 109.5 . . ?
C44 C47 H47B 109.5 . . ?
C44 C47 H47C 109.5 . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C1 N1 P1 129.2(5) . . ?
C1 N1 P2 126.0(5) . . ?
P2 N1 P1 103.9(3) . . ?
C11 P1 C21 104.3(3) . . ?
C11 P1 P2 127.1(2) . . ?
C11 P1 Tc1 126.33(18) . . ?
C21 P1 P2 122.6(2) . . ?
C21 P1 Tc1 113.60(18) . . ?
N1 P1 C11 108.3(2) . . ?
N1 P1 C21 108.7(2) . . ?
N1 P1 P2 37.71(16) . . ?
N1 P1 Tc1 94.21(17) . . ?
Tc1 P1 P2 56.55(5) . . ?
C31 P2 C41 103.0(3) . . ?
C31 P2 P1 124.31(19) . . ?
C31 P2 Tc1 113.68(18) . . ?
C41 P2 P1 126.38(19) . . ?
C41 P2 Tc1 127.2(2) . . ?
N1 P2 C31 109.9(2) . . ?
N1 P2 C41 106.5(2) . . ?
N1 P2 P1 38.37(17) . . ?
N1 P2 Tc1 95.59(18) . . ?
Tc1 P2 P1 57.27(5) . . ?
C7 Tc1 C8 93.9(3) . . ?
C7 Tc1 P1 99.6(2) . . ?
C7 Tc1 P2 165.8(2) . . ?
C7 Tc1 Cl1 85.9(2) . . ?
C8 Tc1 P1 165.7(2) . . ?
C8 Tc1 P2 100.2(2) . . ?
C8 Tc1 Cl1 85.48(19) . . ?
C9 Tc1 C7 89.3(3) . . ?
C9 Tc1 C8 86.9(3) . . ?
C9 Tc1 P1 88.77(18) . . ?
C9 Tc1 P2 89.47(19) . . ?
C9 Tc1 Cl1 170.63(17) . . ?
P1 Tc1 Cl1 99.94(5) . . ?
P2 Tc1 P1 66.18(5) . . ?
P2 Tc1 Cl1 97.19(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
C1 C2 C3 C4 56.4(10) . . . . ?
C1 N1 P1 C11 41.8(6) . . . . ?
C1 N1 P1 C21 -71.0(5) . . . . ?
C1 N1 P1 P2 169.4(6) . . . . ?
C1 N1 P1 Tc1 172.3(5) . . . . ?
C1 N1 P2 C31 69.5(5) . . . . ?
C1 N1 P2 C41 -41.3(5) . . . . ?
C1 N1 P2 P1 -169.8(6) . . . . ?
C1 N1 P2 Tc1 -172.8(5) . . . . ?
C2 C1 C6 C5 48.3(11) . . . . ?
C2 C1 N1 P1 56.5(8) . . . . ?
C2 C1 N1 P2 -136.3(6) . . . . ?
C2 C3 C4 C5 -58.7(10) . . . . ?
C3 C4 C5 C6 55.0(11) . . . . ?
C4 C5 C6 C1 -49.4(12) . . . . ?
C6 C1 C2 C3 -52.4(10) . . . . ?
C6 C1 N1 P1 -74.5(8) . . . . ?
C6 C1 N1 P2 92.7(8) . . . . ?
C11 C12 C13 C14 0.0(10) . . . . ?
C12 C11 C16 C15 2.9(10) . . . . ?
C12 C11 P1 C21 -154.6(5) . . . . ?
C12 C11 P1 N1 89.8(5) . . . . ?
C12 C11 P1 P2 52.4(6) . . . . ?
C12 C11 P1 Tc1 -20.1(6) . . . . ?
C12 C13 C14 C15 1.0(10) . . . . ?
C12 C13 C14 C17 -178.9(7) . . . . ?
C13 C14 C15 C16 0.0(10) . . . . ?
C14 C15 C16 C11 -2.0(11) . . . . ?
C16 C11 C12 C13 -1.9(9) . . . . ?
C16 C11 P1 C21 27.3(6) . . . . ?
C16 C11 P1 N1 -88.4(6) . . . . ?
C16 C11 P1 P2 -125.8(5) . . . . ?
C16 C11 P1 Tc1 161.8(4) . . . . ?
C17 C14 C15 C16 179.9(7) . . . . ?
C21 C22 C23 C24 -1.5(10) . . . . ?
C22 C21 C26 C25 -2.7(9) . . . . ?
C22 C21 P1 C11 43.6(5) . . . . ?
C22 C21 P1 N1 159.0(5) . . . . ?
C22 C21 P1 P2 -161.8(4) . . . . ?
C22 C21 P1 Tc1 -97.6(5) . . . . ?
C22 C23 C24 C25 -0.4(10) . . . . ?
C22 C23 C24 C27 179.9(6) . . . . ?
C23 C24 C25 C26 0.7(10) . . . . ?
C24 C25 C26 C21 0.9(10) . . . . ?
C26 C21 C22 C23 3.1(9) . . . . ?
C26 C21 P1 C11 -143.8(5) . . . . ?
C26 C21 P1 N1 -28.4(5) . . . . ?
C26 C21 P1 P2 10.8(6) . . . . ?
C26 C21 P1 Tc1 75.0(5) . . . . ?
C27 C24 C25 C26 -179.6(6) . . . . ?
C31 C32 C33 C34 -0.8(9) . . . . ?
C32 C31 C36 C35 -0.4(9) . . . . ?
C32 C31 P2 C41 106.8(5) . . . . ?
C32 C31 P2 N1 -6.3(6) . . . . ?
C32 C31 P2 P1 -46.6(6) . . . . ?
C32 C31 P2 Tc1 -112.1(5) . . . . ?
C32 C33 C34 C35 2.1(9) . . . . ?
C32 C33 C34 C37 -176.6(6) . . . . ?
C33 C34 C35 C36 -2.6(10) . . . . ?
C34 C35 C36 C31 1.8(10) . . . . ?
C36 C31 C32 C33 -0.1(9) . . . . ?
C36 C31 P2 C41 -76.1(5) . . . . ?
C36 C31 P2 N1 170.8(4) . . . . ?
C36 C31 P2 P1 130.5(4) . . . . ?
C36 C31 P2 Tc1 65.1(5) . . . . ?
C37 C34 C35 C36 176.1(6) . . . . ?
C41 C42 C43 C44 1.2(11) . . . . ?
C42 C41 C46 C45 1.6(9) . . . . ?
C42 C41 P2 C31 -12.2(6) . . . . ?
C42 C41 P2 N1 103.4(5) . . . . ?
C42 C41 P2 P1 140.5(5) . . . . ?
C42 C41 P2 Tc1 -146.0(5) . . . . ?
C42 C43 C44 C45 -0.5(11) . . . . ?
C42 C43 C44 C47 -178.6(7) . . . . ?
C43 C44 C45 C46 0.5(10) . . . . ?
C44 C45 C46 C41 -1.1(10) . . . . ?
C46 C41 C42 C43 -1.7(10) . . . . ?
C46 C41 P2 C31 168.3(5) . . . . ?
C46 C41 P2 N1 -76.2(5) . . . . ?
C46 C41 P2 P1 -39.1(6) . . . . ?
C46 C41 P2 Tc1 34.4(6) . . . . ?
C47 C44 C45 C46 178.5(7) . . . . ?
N1 C1 C2 C3 176.3(7) . . . . ?
N1 C1 C6 C5 178.8(8) . . . . ?
P1 C11 C12 C13 179.8(5) . . . . ?
P1 C11 C16 C15 -178.9(5) . . . . ?
P1 C21 C22 C23 175.8(5) . . . . ?
P1 C21 C26 C25 -175.5(4) . . . . ?
P1 N1 P2 C31 -120.6(3) . . . . ?
P1 N1 P2 C41 128.5(3) . . . . ?
P1 N1 P2 Tc1 -2.9(2) . . . . ?
P2 C31 C32 C33 177.0(5) . . . . ?
P2 C31 C36 C35 -177.7(5) . . . . ?
P2 C41 C42 C43 178.7(6) . . . . ?
P2 C41 C46 C45 -178.8(5) . . . . ?
P2 N1 P1 C11 -127.7(3) . . . . ?
P2 N1 P1 C21 119.6(3) . . . . ?
P2 N1 P1 Tc1 2.9(2) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.62(4)
2 0.38(4)


####################################################################### 
# 
# 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_17dtk17_0m
_database_code_depnum_ccdc_archive 'CCDC 1989002'
loop_
_audit_author_name
_audit_author_address
'DV Kama'
;University of the Free State
South Africa
;
_audit_update_record             
;
2021-10-12 deposited with the CCDC.	2021-10-20 downloaded from the CCDC.
;
_audit_creation_date             2021-10-12
_audit_creation_method           
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C34 H39 N O0.2 P2'
_chemical_formula_sum            'C34 H39 N O0.20 P2'
_chemical_formula_weight         526.80
_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'
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                   10.145(5)
_cell_length_b                   12.466(5)
_cell_length_c                   13.495(5)
_cell_angle_alpha                75.985(5)
_cell_angle_beta                 69.761(5)
_cell_angle_gamma                67.446(5)
_cell_volume                     1467.0(11)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3873
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.512
_cell_measurement_theta_min      3.999
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.172
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6940
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.0831 before and 0.0716 after correction.
The Ratio of minimum to maximum transmission is 0.9307.
The λ/2 correction factor is 0.00150.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.193
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Cuboid
_exptl_crystal_F_000             563
_exptl_crystal_size_max          0.399
_exptl_crystal_size_mid          0.164
_exptl_crystal_size_min          0.154
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0782
_diffrn_reflns_av_unetI/netI     0.0943
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            28068
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         28.502
_diffrn_reflns_theta_min         4.535
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4738
_reflns_number_total             7324
_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       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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    'ShelXD (Sheldrick, 2008)'
_refine_diff_density_max         0.306
_refine_diff_density_min         -0.350
_refine_diff_density_rms         0.065
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     347
_refine_ls_number_reflns         7324
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0971
_refine_ls_R_factor_gt           0.0536
_refine_ls_restrained_S_all      1.034
_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)+(0.0505P)²+0.1665P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1150
_refine_ls_wR_factor_ref         0.1332
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: O1(0.2)
3.a Ternary CH refined with riding coordinates:
 C1(H1)
3.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B)
3.c Aromatic/amide H refined with riding coordinates:
 C46(H46), C45(H45), C43(H43), C42(H42), C36(H36), C35(H35), C33(H33),
 C32(H32), C16(H16), C15(H15), C13(H13), C12(H12), C26(H26), C25(H25), C23(H23),
  C22(H22)
3.d Idealised Me refined as rotating group:
 C47(H47A,H47B,H47C), C37(H37A,H37B,H37C), C17(H17A,H17B,H17C), C27(H27A,H27B,
 H27C)
;
_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
C1 C 0.3488(2) 0.35437(17) 0.67732(15) 0.0201(4) Uani 1 1 d . . . . .
H1 H 0.426875 0.388800 0.662416 0.024 Uiso 1 1 calc R . . . .
C2 C 0.2012(2) 0.45394(19) 0.69906(17) 0.0279(5) Uani 1 1 d . . . . .
H2A H 0.189159 0.488071 0.760350 0.033 Uiso 1 1 calc R . . . .
H2B H 0.120372 0.423196 0.715755 0.033 Uiso 1 1 calc R . . . .
C3 C 0.1929(3) 0.5486(2) 0.60344(18) 0.0351(6) Uani 1 1 d . . . . .
H3A H 0.095193 0.607919 0.618131 0.042 Uiso 1 1 calc R . . . .
H3B H 0.265998 0.585938 0.592084 0.042 Uiso 1 1 calc R . . . .
C4 C 0.2216(3) 0.4981(2) 0.50294(19) 0.0405(6) Uani 1 1 d . . . . .
H4A H 0.142127 0.468864 0.510967 0.049 Uiso 1 1 calc R . . . .
H4B H 0.222607 0.559234 0.442747 0.049 Uiso 1 1 calc R . . . .
C5 C 0.3685(3) 0.4000(2) 0.48221(17) 0.0300(5) Uani 1 1 d . . . . .
H5A H 0.448543 0.431057 0.467518 0.036 Uiso 1 1 calc R . . . .
H5B H 0.382778 0.366601 0.419884 0.036 Uiso 1 1 calc R . . . .
C6 C 0.3754(2) 0.30426(19) 0.57705(16) 0.0261(5) Uani 1 1 d . . . . .
H6A H 0.300519 0.268724 0.588378 0.031 Uiso 1 1 calc R . . . .
H6B H 0.472139 0.243878 0.562097 0.031 Uiso 1 1 calc R . . . .
C41 C 0.4279(2) 0.40440(18) 0.87138(15) 0.0200(4) Uani 1 1 d . . . . .
C46 C 0.3398(2) 0.43226(18) 0.97298(16) 0.0221(5) Uani 1 1 d . . . . .
H46 H 0.311363 0.374311 1.024350 0.027 Uiso 1 1 calc R . . . .
C45 C 0.2939(2) 0.54402(19) 0.99902(17) 0.0243(5) Uani 1 1 d . . . . .
H45 H 0.235337 0.559783 1.067529 0.029 Uiso 1 1 calc R . . . .
C44 C 0.3336(2) 0.63316(18) 0.92494(16) 0.0214(5) Uani 1 1 d . . . . .
C43 C 0.4220(2) 0.60581(18) 0.82380(16) 0.0237(5) Uani 1 1 d . . . . .
H43 H 0.450417 0.664013 0.772744 0.028 Uiso 1 1 calc R . . . .
C42 C 0.4689(2) 0.49399(18) 0.79720(16) 0.0225(5) Uani 1 1 d . . . . .
H42 H 0.528563 0.478269 0.728896 0.027 Uiso 1 1 calc R . . . .
C47 C 0.2858(2) 0.75514(18) 0.95245(17) 0.0269(5) Uani 1 1 d . . . . .
H47A H 0.189597 0.772472 1.003718 0.040 Uiso 1 1 calc GR . . . .
H47B H 0.280872 0.810363 0.889305 0.040 Uiso 1 1 calc GR . . . .
H47C H 0.356535 0.760330 0.981875 0.040 Uiso 1 1 calc GR . . . .
C31 C 0.6583(2) 0.23027(18) 0.74883(16) 0.0221(5) Uani 1 1 d . . . . .
C36 C 0.7650(2) 0.26843(19) 0.75914(16) 0.0254(5) Uani 1 1 d . . . . .
H36 H 0.739259 0.314823 0.811918 0.030 Uiso 1 1 calc R . . . .
C35 C 0.9085(2) 0.2383(2) 0.69200(17) 0.0278(5) Uani 1 1 d . . . . .
H35 H 0.977994 0.263859 0.701129 0.033 Uiso 1 1 calc R . . . .
C34 C 0.9505(2) 0.17120(19) 0.61205(17) 0.0266(5) Uani 1 1 d . . . . .
C33 C 0.8452(2) 0.1327(2) 0.60141(17) 0.0286(5) Uani 1 1 d . . . . .
H33 H 0.871142 0.087385 0.547760 0.034 Uiso 1 1 calc R . . . .
C32 C 0.7025(2) 0.16065(19) 0.66921(16) 0.0253(5) Uani 1 1 d . . . . .
H32 H 0.634682 0.132276 0.661423 0.030 Uiso 1 1 calc R . . . .
C37 C 1.1068(2) 0.1392(2) 0.53833(19) 0.0395(6) Uani 1 1 d . . . . .
H37A H 1.164126 0.062175 0.563039 0.059 Uiso 1 1 calc GR . . . .
H37B H 1.151868 0.194643 0.537303 0.059 Uiso 1 1 calc GR . . . .
H37C H 1.103713 0.140277 0.467771 0.059 Uiso 1 1 calc GR . . . .
C11 C 0.4102(2) 0.02632(18) 0.78819(15) 0.0205(4) Uani 1 1 d . . . . .
C16 C 0.5021(2) -0.02953(18) 0.85517(16) 0.0236(5) Uani 1 1 d . . . . .
H16 H 0.486473 0.004312 0.914329 0.028 Uiso 1 1 calc R . . . .
C15 C 0.6154(2) -0.13384(18) 0.83503(16) 0.0238(5) Uani 1 1 d . . . . .
H15 H 0.675222 -0.169153 0.880704 0.029 Uiso 1 1 calc R . . . .
C14 C 0.6419(2) -0.18743(18) 0.74751(16) 0.0232(5) Uani 1 1 d . . . . .
C13 C 0.5517(2) -0.13177(19) 0.68055(16) 0.0246(5) Uani 1 1 d . . . . .
H13 H 0.568246 -0.165371 0.621016 0.029 Uiso 1 1 calc R . . . .
C12 C 0.4372(2) -0.02689(18) 0.70063(16) 0.0235(5) Uani 1 1 d . . . . .
H12 H 0.377572 0.008358 0.654794 0.028 Uiso 1 1 calc R . . . .
C17 C 0.7613(2) -0.3041(2) 0.72958(18) 0.0318(5) Uani 1 1 d . . . . .
H17A H 0.844268 -0.307975 0.750859 0.048 Uiso 1 1 calc GR . . . .
H17B H 0.793286 -0.313317 0.655470 0.048 Uiso 1 1 calc GR . . . .
H17C H 0.722757 -0.365416 0.770964 0.048 Uiso 1 1 calc GR . . . .
C21 C 0.1786(2) 0.16609(18) 0.94444(16) 0.0228(5) Uani 1 1 d . . . . .
C26 C 0.1659(2) 0.06217(19) 1.01004(17) 0.0304(5) Uani 1 1 d . . . . .
H26 H 0.214795 -0.008753 0.982164 0.036 Uiso 1 1 calc R . . . .
C25 C 0.0821(2) 0.0637(2) 1.11505(18) 0.0313(5) Uani 1 1 d . . . . .
H25 H 0.075335 -0.006420 1.156676 0.038 Uiso 1 1 calc R . . . .
C24 C 0.0078(2) 0.1670(2) 1.15995(17) 0.0271(5) Uani 1 1 d . . . . .
C23 C 0.0203(2) 0.26993(19) 1.09518(17) 0.0257(5) Uani 1 1 d . . . . .
H23 H -0.028602 0.340544 1.123585 0.031 Uiso 1 1 calc R . . . .
C22 C 0.1035(2) 0.27002(18) 0.98961(16) 0.0221(5) Uani 1 1 d . . . . .
H22 H 0.109362 0.340422 0.948273 0.027 Uiso 1 1 calc R . . . .
C27 C -0.0847(3) 0.1672(2) 1.27455(18) 0.0400(6) Uani 1 1 d . . . . .
H27A H -0.138982 0.113778 1.291028 0.060 Uiso 1 1 calc GR . . . .
H27B H -0.153246 0.244645 1.285806 0.060 Uiso 1 1 calc GR . . . .
H27C H -0.020737 0.143326 1.319869 0.060 Uiso 1 1 calc GR . . . .
N1 N 0.36175(18) 0.26541(14) 0.77205(12) 0.0193(4) Uani 1 1 d . . . . .
P2 P 0.47510(6) 0.25389(5) 0.84668(4) 0.02022(14) Uani 1 1 d . . . . .
P1 P 0.26561(6) 0.16965(5) 0.80166(4) 0.02302(15) Uani 1 1 d . . . . .
O1 O 0.1758(10) 0.1853(9) 0.7495(7) 0.055(3) Uani 0.2 1 d . . 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
C1 H1 0.9800 . ?
C1 C2 1.522(3) . ?
C1 C6 1.524(3) . ?
C1 N1 1.483(2) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C3 1.525(3) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.523(3) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 C5 1.508(3) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C6 1.525(3) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C41 C46 1.394(3) . ?
C41 C42 1.396(3) . ?
C41 P2 1.834(2) . ?
C46 H46 0.9300 . ?
C46 C45 1.381(3) . ?
C45 H45 0.9300 . ?
C45 C44 1.387(3) . ?
C44 C43 1.388(3) . ?
C44 C47 1.506(3) . ?
C43 H43 0.9300 . ?
C43 C42 1.383(3) . ?
C42 H42 0.9300 . ?
C47 H47A 0.9600 . ?
C47 H47B 0.9600 . ?
C47 H47C 0.9600 . ?
C31 C36 1.396(3) . ?
C31 C32 1.389(3) . ?
C31 P2 1.832(2) . ?
C36 H36 0.9300 . ?
C36 C35 1.384(3) . ?
C35 H35 0.9300 . ?
C35 C34 1.375(3) . ?
C34 C33 1.387(3) . ?
C34 C37 1.509(3) . ?
C33 H33 0.9300 . ?
C33 C32 1.380(3) . ?
C32 H32 0.9300 . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?
C11 C16 1.397(3) . ?
C11 C12 1.388(3) . ?
C11 P1 1.828(2) . ?
C16 H16 0.9300 . ?
C16 C15 1.376(3) . ?
C15 H15 0.9300 . ?
C15 C14 1.392(3) . ?
C14 C13 1.384(3) . ?
C14 C17 1.502(3) . ?
C13 H13 0.9300 . ?
C13 C12 1.386(3) . ?
C12 H12 0.9300 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C21 C26 1.404(3) . ?
C21 C22 1.391(3) . ?
C21 P1 1.818(2) . ?
C26 H26 0.9300 . ?
C26 C25 1.378(3) . ?
C25 H25 0.9300 . ?
C25 C24 1.383(3) . ?
C24 C23 1.390(3) . ?
C24 C27 1.506(3) . ?
C23 H23 0.9300 . ?
C23 C22 1.382(3) . ?
C22 H22 0.9300 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
N1 P2 1.7209(18) . ?
N1 P1 1.7113(16) . ?
P1 O1 1.267(8) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 H1 106.7 . . ?
C2 C1 C6 110.47(17) . . ?
C6 C1 H1 106.7 . . ?
N1 C1 H1 106.7 . . ?
N1 C1 C2 111.90(16) . . ?
N1 C1 C6 114.03(16) . . ?
C1 C2 H2A 109.3 . . ?
C1 C2 H2B 109.3 . . ?
C1 C2 C3 111.48(17) . . ?
H2A C2 H2B 108.0 . . ?
C3 C2 H2A 109.3 . . ?
C3 C2 H2B 109.3 . . ?
C2 C3 H3A 109.3 . . ?
C2 C3 H3B 109.3 . . ?
H3A C3 H3B 108.0 . . ?
C4 C3 C2 111.52(19) . . ?
C4 C3 H3A 109.3 . . ?
C4 C3 H3B 109.3 . . ?
C3 C4 H4A 109.6 . . ?
C3 C4 H4B 109.6 . . ?
H4A C4 H4B 108.1 . . ?
C5 C4 C3 110.5(2) . . ?
C5 C4 H4A 109.6 . . ?
C5 C4 H4B 109.6 . . ?
C4 C5 H5A 109.3 . . ?
C4 C5 H5B 109.3 . . ?
C4 C5 C6 111.56(18) . . ?
H5A C5 H5B 108.0 . . ?
C6 C5 H5A 109.3 . . ?
C6 C5 H5B 109.3 . . ?
C1 C6 C5 110.75(17) . . ?
C1 C6 H6A 109.5 . . ?
C1 C6 H6B 109.5 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 108.1 . . ?
C46 C41 C42 117.22(19) . . ?
C46 C41 P2 116.74(14) . . ?
C42 C41 P2 126.02(15) . . ?
C41 C46 H46 119.3 . . ?
C45 C46 C41 121.46(18) . . ?
C45 C46 H46 119.3 . . ?
C46 C45 H45 119.4 . . ?
C46 C45 C44 121.24(19) . . ?
C44 C45 H45 119.4 . . ?
C45 C44 C43 117.58(19) . . ?
C45 C44 C47 121.86(19) . . ?
C43 C44 C47 120.55(18) . . ?
C44 C43 H43 119.2 . . ?
C42 C43 C44 121.53(18) . . ?
C42 C43 H43 119.2 . . ?
C41 C42 H42 119.5 . . ?
C43 C42 C41 120.97(19) . . ?
C43 C42 H42 119.5 . . ?
C44 C47 H47A 109.5 . . ?
C44 C47 H47B 109.5 . . ?
C44 C47 H47C 109.5 . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C36 C31 P2 121.55(16) . . ?
C32 C31 C36 117.28(19) . . ?
C32 C31 P2 120.68(15) . . ?
C31 C36 H36 119.5 . . ?
C35 C36 C31 121.0(2) . . ?
C35 C36 H36 119.5 . . ?
C36 C35 H35 119.4 . . ?
C34 C35 C36 121.29(19) . . ?
C34 C35 H35 119.4 . . ?
C35 C34 C33 118.07(19) . . ?
C35 C34 C37 121.23(19) . . ?
C33 C34 C37 120.7(2) . . ?
C34 C33 H33 119.5 . . ?
C32 C33 C34 121.0(2) . . ?
C32 C33 H33 119.5 . . ?
C31 C32 H32 119.3 . . ?
C33 C32 C31 121.33(19) . . ?
C33 C32 H32 119.3 . . ?
C34 C37 H37A 109.5 . . ?
C34 C37 H37B 109.5 . . ?
C34 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C16 C11 P1 124.79(16) . . ?
C12 C11 C16 117.7(2) . . ?
C12 C11 P1 117.31(16) . . ?
C11 C16 H16 119.5 . . ?
C15 C16 C11 121.1(2) . . ?
C15 C16 H16 119.5 . . ?
C16 C15 H15 119.4 . . ?
C16 C15 C14 121.2(2) . . ?
C14 C15 H15 119.4 . . ?
C15 C14 C17 120.5(2) . . ?
C13 C14 C15 117.9(2) . . ?
C13 C14 C17 121.6(2) . . ?
C14 C13 H13 119.4 . . ?
C14 C13 C12 121.2(2) . . ?
C12 C13 H13 119.4 . . ?
C11 C12 H12 119.5 . . ?
C13 C12 C11 120.9(2) . . ?
C13 C12 H12 119.5 . . ?
C14 C17 H17A 109.5 . . ?
C14 C17 H17B 109.5 . . ?
C14 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C26 C21 P1 121.85(16) . . ?
C22 C21 C26 117.44(19) . . ?
C22 C21 P1 120.09(16) . . ?
C21 C26 H26 119.5 . . ?
C25 C26 C21 121.0(2) . . ?
C25 C26 H26 119.5 . . ?
C26 C25 H25 119.3 . . ?
C26 C25 C24 121.5(2) . . ?
C24 C25 H25 119.3 . . ?
C25 C24 C23 117.6(2) . . ?
C25 C24 C27 120.8(2) . . ?
C23 C24 C27 121.6(2) . . ?
C24 C23 H23 119.2 . . ?
C22 C23 C24 121.7(2) . . ?
C22 C23 H23 119.2 . . ?
C21 C22 H22 119.6 . . ?
C23 C22 C21 120.80(19) . . ?
C23 C22 H22 119.6 . . ?
C24 C27 H27A 109.5 . . ?
C24 C27 H27B 109.5 . . ?
C24 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C1 N1 P2 121.69(12) . . ?
C1 N1 P1 117.49(12) . . ?
P1 N1 P2 120.76(10) . . ?
C31 P2 C41 101.71(9) . . ?
N1 P2 C41 104.33(9) . . ?
N1 P2 C31 103.08(9) . . ?
C21 P1 C11 103.65(10) . . ?
N1 P1 C11 104.25(9) . . ?
N1 P1 C21 104.34(8) . . ?
O1 P1 C11 110.9(5) . . ?
O1 P1 C21 113.1(4) . . ?
O1 P1 N1 119.1(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 55.1(2) . . . . ?
C1 N1 P2 C41 48.76(16) . . . . ?
C1 N1 P2 C31 -57.16(16) . . . . ?
C1 N1 P1 C11 116.94(15) . . . . ?
C1 N1 P1 C21 -134.62(15) . . . . ?
C1 N1 P1 O1 -7.3(6) . . . . ?
C2 C1 C6 C5 56.1(2) . . . . ?
C2 C1 N1 P2 -106.14(18) . . . . ?
C2 C1 N1 P1 76.63(19) . . . . ?
C2 C3 C4 C5 -55.2(3) . . . . ?
C3 C4 C5 C6 56.4(2) . . . . ?
C4 C5 C6 C1 -57.3(2) . . . . ?
C6 C1 C2 C3 -55.3(2) . . . . ?
C6 C1 N1 P2 127.57(16) . . . . ?
C6 C1 N1 P1 -49.7(2) . . . . ?
C41 C46 C45 C44 0.1(3) . . . . ?
C46 C41 C42 C43 -0.7(3) . . . . ?
C46 C41 P2 C31 -148.83(16) . . . . ?
C46 C41 P2 N1 104.22(17) . . . . ?
C46 C45 C44 C43 -0.4(3) . . . . ?
C46 C45 C44 C47 -179.33(19) . . . . ?
C45 C44 C43 C42 0.2(3) . . . . ?
C44 C43 C42 C41 0.4(3) . . . . ?
C42 C41 C46 C45 0.5(3) . . . . ?
C42 C41 P2 C31 32.9(2) . . . . ?
C42 C41 P2 N1 -74.07(19) . . . . ?
C47 C44 C43 C42 179.12(19) . . . . ?
C31 C36 C35 C34 0.9(3) . . . . ?
C36 C31 C32 C33 -1.5(3) . . . . ?
C36 C31 P2 C41 42.02(19) . . . . ?
C36 C31 P2 N1 149.93(17) . . . . ?
C36 C35 C34 C33 -1.0(3) . . . . ?
C36 C35 C34 C37 179.5(2) . . . . ?
C35 C34 C33 C32 -0.1(3) . . . . ?
C34 C33 C32 C31 1.5(3) . . . . ?
C32 C31 C36 C35 0.4(3) . . . . ?
C32 C31 P2 C41 -146.27(18) . . . . ?
C32 C31 P2 N1 -38.35(19) . . . . ?
C37 C34 C33 C32 179.3(2) . . . . ?
C11 C16 C15 C14 -0.2(3) . . . . ?
C16 C11 C12 C13 -0.1(3) . . . . ?
C16 C11 P1 C21 -41.30(18) . . . . ?
C16 C11 P1 N1 67.65(17) . . . . ?
C16 C11 P1 O1 -163.0(5) . . . . ?
C16 C15 C14 C13 0.7(3) . . . . ?
C16 C15 C14 C17 -177.09(17) . . . . ?
C15 C14 C13 C12 -0.9(3) . . . . ?
C14 C13 C12 C11 0.6(3) . . . . ?
C12 C11 C16 C15 -0.1(3) . . . . ?
C12 C11 P1 C21 143.38(15) . . . . ?
C12 C11 P1 N1 -107.67(15) . . . . ?
C12 C11 P1 O1 21.7(5) . . . . ?
C17 C14 C13 C12 176.87(18) . . . . ?
C21 C26 C25 C24 -0.2(4) . . . . ?
C26 C21 C22 C23 0.2(3) . . . . ?
C26 C21 P1 C11 -33.1(2) . . . . ?
C26 C21 P1 N1 -141.97(18) . . . . ?
C26 C21 P1 O1 87.1(5) . . . . ?
C26 C25 C24 C23 0.1(3) . . . . ?
C26 C25 C24 C27 179.3(2) . . . . ?
C25 C24 C23 C22 0.1(3) . . . . ?
C24 C23 C22 C21 -0.2(3) . . . . ?
C22 C21 C26 C25 0.0(3) . . . . ?
C22 C21 P1 C11 156.18(16) . . . . ?
C22 C21 P1 N1 47.30(18) . . . . ?
C22 C21 P1 O1 -83.6(5) . . . . ?
C27 C24 C23 C22 -179.1(2) . . . . ?
N1 C1 C2 C3 176.48(17) . . . . ?
N1 C1 C6 C5 -176.88(17) . . . . ?
P2 C41 C46 C45 -177.92(16) . . . . ?
P2 C41 C42 C43 177.54(16) . . . . ?
P2 C31 C36 C35 172.36(16) . . . . ?
P2 C31 C32 C33 -173.59(17) . . . . ?
P2 N1 P1 C11 -60.32(13) . . . . ?
P2 N1 P1 C21 48.12(13) . . . . ?
P2 N1 P1 O1 175.5(5) . . . . ?
P1 C11 C16 C15 -175.38(14) . . . . ?
P1 C11 C12 C13 175.54(14) . . . . ?
P1 C21 C26 C25 -170.98(17) . . . . ?
P1 C21 C22 C23 171.34(15) . . . . ?
P1 N1 P2 C41 -134.10(11) . . . . ?
P1 N1 P2 C31 119.98(11) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
