# Electronic Supplementary Material (ESI) for ChemComm.
# 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_dal193
_audit_block_doi                 10.5517/ccdc.csd.cc24r7nt
_database_code_depnum_ccdc_archive 'CCDC 1988546'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1021/acs.inorgchem.0c01353 2020
loop_
_audit_author_name
_audit_author_address
'Dale C. Swenson'
;University of Iowa
United States of America
;
_audit_update_record             
;
2020-03-05 deposited with the CCDC.	2021-08-18 downloaded from the CCDC.
;
_audit_creation_date             2019-08-08
_audit_creation_method           
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C20 H18 Cl2 N2 Ru S2, C3 H6 O'
_chemical_formula_sum            'C23 H24 Cl2 N2 O Ru S2'
_chemical_formula_weight         580.53
_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'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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                   9.5459(14)
_cell_length_b                   11.7033(17)
_cell_length_c                   12.1756(17)
_cell_angle_alpha                70.756(5)
_cell_angle_beta                 84.677(5)
_cell_angle_gamma                67.243(5)
_cell_volume                     1183.3(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4790
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.26
_cell_measurement_theta_min      2.31
_shelx_estimated_absorpt_T_max   0.979
_shelx_estimated_absorpt_T_min   0.881
_exptl_absorpt_coefficient_mu    1.084
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6840
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.0544 before and 0.0481 after correction.
The Ratio of minimum to maximum transmission is 0.9176.
The λ/2 correction factor is 0.00150.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark blue'
_exptl_crystal_density_diffrn    1.629
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       lath-like
_exptl_crystal_F_000             588
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0531
_diffrn_reflns_av_unetI/netI     0.0702
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13689
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.363
_diffrn_reflns_theta_min         2.415
_diffrn_ambient_temperature      150.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Nonius Kappa Apex II'
_diffrn_measurement_method       'CCD Phi and Omega Scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3504
_reflns_number_total             4816
_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       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.827
_refine_diff_density_min         -1.012
_refine_diff_density_rms         0.118
_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     284
_refine_ls_number_reflns         4816
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0747
_refine_ls_R_factor_gt           0.0453
_refine_ls_restrained_S_all      1.027
_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)+(0.0371P)²+2.0629P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0926
_refine_ls_wR_factor_ref         0.1042
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C22(H22), C25(H25), C23(H23), C3(H3), C24(H24), C6(H6), C5(H5), C15(H15),
 C12(H12), C4(H4), C14(H14), C13(H13)
2.b Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C17(H17A,H17B,H17C), C1A(H1AA,H1AB,H1AC), C3A(H3AA,H3AB,
 H3AC)
;
_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
Ru1 Ru 0.50794(4) 0.31108(4) 0.75546(3) 0.01937(12) Uani 1 1 d . . . . .
Cl1 Cl 0.31570(12) 0.51305(10) 0.75753(10) 0.0242(3) Uani 1 1 d . . . . .
S2 S 0.33127(14) 0.29792(11) 0.63984(10) 0.0239(3) Uani 1 1 d . . . . .
Cl2 Cl 0.70127(14) 0.11521(11) 0.73910(10) 0.0292(3) Uani 1 1 d . . . . .
S1 S 0.63041(14) 0.44357(12) 0.62987(12) 0.0322(3) Uani 1 1 d . . . . .
N2 N 0.4159(4) 0.2193(3) 0.8892(3) 0.0192(8) Uani 1 1 d . . . . .
N1 N 0.6143(4) 0.3189(3) 0.8821(3) 0.0223(9) Uani 1 1 d . . . . .
C21 C 0.3227(5) 0.1562(4) 0.8715(4) 0.0177(9) Uani 1 1 d . . . . .
C26 C 0.2689(5) 0.1906(4) 0.7572(4) 0.0199(10) Uani 1 1 d . . . . .
C2 C 0.4359(5) 0.2374(4) 0.9905(4) 0.0195(10) Uani 1 1 d . . . . .
C22 C 0.2848(5) 0.0618(4) 0.9589(4) 0.0223(10) Uani 1 1 d . . . . .
H22 H 0.3282 0.0306 1.0354 0.027 Uiso 1 1 calc R . . . .
C25 C 0.1659(5) 0.1430(5) 0.7342(5) 0.0286(12) Uani 1 1 d . . . . .
H25 H 0.1265 0.1698 0.6570 0.034 Uiso 1 1 calc R . . . .
C16 C 0.7521(5) 0.4296(5) 0.7412(5) 0.0316(12) Uani 1 1 d . . . . .
C23 C 0.1840(5) 0.0136(4) 0.9344(5) 0.0284(12) Uani 1 1 d . . . . .
H23 H 0.1581 -0.0500 0.9947 0.034 Uiso 1 1 calc R . . . .
C27 C 0.4170(7) 0.1930(5) 0.5514(5) 0.0401(14) Uani 1 1 d . . . . .
H27A H 0.4693 0.2351 0.4876 0.060 Uiso 1 1 calc GR . . . .
H27B H 0.3378 0.1779 0.5192 0.060 Uiso 1 1 calc GR . . . .
H27C H 0.4904 0.1092 0.5993 0.060 Uiso 1 1 calc GR . . . .
C1 C 0.5468(5) 0.2961(4) 0.9852(4) 0.0223(10) Uani 1 1 d . . . . .
C3 C 0.3593(6) 0.2103(5) 1.0954(4) 0.0277(11) Uani 1 1 d . . . . .
H3 H 0.2868 0.1716 1.1011 0.033 Uiso 1 1 calc R . . . .
C24 C 0.1206(6) 0.0566(5) 0.8235(5) 0.0348(13) Uani 1 1 d . . . . .
H24 H 0.0466 0.0272 0.8087 0.042 Uiso 1 1 calc R . . . .
C6 C 0.5682(5) 0.3286(5) 1.0828(4) 0.0280(11) Uani 1 1 d . . . . .
H6 H 0.6355 0.3720 1.0790 0.034 Uiso 1 1 calc R . . . .
C11 C 0.7372(5) 0.3630(4) 0.8578(5) 0.0290(12) Uani 1 1 d . . . . .
C5 C 0.4937(6) 0.2983(5) 1.1819(5) 0.0343(13) Uani 1 1 d . . . . .
H5 H 0.5127 0.3172 1.2479 0.041 Uiso 1 1 calc R . . . .
C17 C 0.7738(6) 0.3604(5) 0.5446(5) 0.0433(15) Uani 1 1 d . . . . .
H17A H 0.8356 0.2725 0.5944 0.065 Uiso 1 1 calc GR . . . .
H17B H 0.8390 0.4098 0.5121 0.065 Uiso 1 1 calc GR . . . .
H17C H 0.7244 0.3539 0.4811 0.065 Uiso 1 1 calc GR . . . .
C15 C 0.8647(6) 0.4823(5) 0.7096(6) 0.0446(16) Uani 1 1 d . . . . .
H15 H 0.8710 0.5310 0.6309 0.054 Uiso 1 1 calc R . . . .
C12 C 0.8461(6) 0.3391(5) 0.9399(5) 0.0364(13) Uani 1 1 d . . . . .
H12 H 0.8428 0.2885 1.0184 0.044 Uiso 1 1 calc R . . . .
C4 C 0.3886(6) 0.2391(5) 1.1882(5) 0.0368(13) Uani 1 1 d . . . . .
H4 H 0.3373 0.2190 1.2583 0.044 Uiso 1 1 calc R . . . .
O1A O 1.0607(7) 0.1988(6) 0.4359(5) 0.0961(18) Uani 1 1 d . . . . .
C14 C 0.9663(6) 0.4629(6) 0.7938(7) 0.058(2) Uani 1 1 d . . . . .
H14 H 1.0411 0.5004 0.7735 0.069 Uiso 1 1 calc R . . . .
C13 C 0.9593(6) 0.3891(6) 0.9071(7) 0.0504(18) Uani 1 1 d . . . . .
H13 H 1.0331 0.3721 0.9637 0.060 Uiso 1 1 calc R . . . .
C2A C 0.9875(10) 0.1772(8) 0.3711(7) 0.073(2) Uani 1 1 d . . . . .
C1A C 1.0094(9) 0.2088(7) 0.2483(6) 0.078(2) Uani 1 1 d . . . . .
H1AA H 1.0731 0.2608 0.2263 0.117 Uiso 1 1 calc GR . . . .
H1AB H 0.9106 0.2593 0.2062 0.117 Uiso 1 1 calc GR . . . .
H1AC H 1.0594 0.1280 0.2285 0.117 Uiso 1 1 calc GR . . . .
C3A C 0.8619(11) 0.1239(9) 0.4150(8) 0.103(3) Uani 1 1 d . . . . .
H3AA H 0.9006 0.0308 0.4228 0.155 Uiso 1 1 calc GR . . . .
H3AB H 0.7747 0.1717 0.3594 0.155 Uiso 1 1 calc GR . . . .
H3AC H 0.8303 0.1352 0.4909 0.155 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ru1 Cl1 2.3729(12) . ?
Ru1 S2 2.3736(12) . ?
Ru1 Cl2 2.3791(13) . ?
Ru1 S1 2.3700(13) . ?
Ru1 N2 1.972(4) . ?
Ru1 N1 1.967(4) . ?
S2 C26 1.793(5) . ?
S2 C27 1.808(5) . ?
S1 C16 1.792(5) . ?
S1 C17 1.808(6) . ?
N2 C21 1.425(5) . ?
N2 C2 1.360(5) . ?
N1 C1 1.351(6) . ?
N1 C11 1.426(6) . ?
C21 C26 1.402(6) . ?
C21 C22 1.395(6) . ?
C26 C25 1.391(6) . ?
C2 C1 1.456(6) . ?
C2 C3 1.416(6) . ?
C22 C23 1.385(6) . ?
C25 C24 1.385(7) . ?
C16 C11 1.401(7) . ?
C16 C15 1.401(7) . ?
C23 C24 1.382(7) . ?
C1 C6 1.414(6) . ?
C3 C4 1.360(7) . ?
C6 C5 1.357(7) . ?
C11 C12 1.393(7) . ?
C5 C4 1.407(7) . ?
C15 C14 1.379(9) . ?
C12 C13 1.387(7) . ?
O1A C2A 1.243(8) . ?
C14 C13 1.377(9) . ?
C2A C1A 1.433(10) . ?
C2A C3A 1.533(11) . ?

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
Cl1 Ru1 S2 85.92(4) . . ?
Cl1 Ru1 Cl2 176.00(5) . . ?
S2 Ru1 Cl2 92.33(5) . . ?
S1 Ru1 Cl1 84.55(4) . . ?
S1 Ru1 S2 107.53(5) . . ?
S1 Ru1 Cl2 92.56(5) . . ?
N2 Ru1 Cl1 89.34(11) . . ?
N2 Ru1 S2 85.29(11) . . ?
N2 Ru1 Cl2 94.10(11) . . ?
N2 Ru1 S1 165.30(11) . . ?
N1 Ru1 Cl1 87.58(11) . . ?
N1 Ru1 S2 165.01(12) . . ?
N1 Ru1 Cl2 94.94(11) . . ?
N1 Ru1 S1 85.25(12) . . ?
N1 Ru1 N2 81.13(15) . . ?
C26 S2 Ru1 95.47(15) . . ?
C26 S2 C27 100.0(2) . . ?
C27 S2 Ru1 114.3(2) . . ?
C16 S1 Ru1 95.56(16) . . ?
C16 S1 C17 98.9(3) . . ?
C17 S1 Ru1 113.55(19) . . ?
C21 N2 Ru1 120.1(3) . . ?
C2 N2 Ru1 113.5(3) . . ?
C2 N2 C21 126.0(4) . . ?
C1 N1 Ru1 113.5(3) . . ?
C1 N1 C11 125.5(4) . . ?
C11 N1 Ru1 120.4(3) . . ?
C26 C21 N2 116.9(4) . . ?
C22 C21 N2 124.7(4) . . ?
C22 C21 C26 118.4(4) . . ?
C21 C26 S2 120.0(3) . . ?
C25 C26 S2 119.5(4) . . ?
C25 C26 C21 120.5(4) . . ?
N2 C2 C1 113.9(4) . . ?
N2 C2 C3 128.0(4) . . ?
C3 C2 C1 118.1(4) . . ?
C23 C22 C21 120.1(4) . . ?
C24 C25 C26 120.1(5) . . ?
C11 C16 S1 120.0(4) . . ?
C11 C16 C15 120.8(5) . . ?
C15 C16 S1 119.2(4) . . ?
C24 C23 C22 121.0(5) . . ?
N1 C1 C2 114.2(4) . . ?
N1 C1 C6 127.0(4) . . ?
C6 C1 C2 118.7(4) . . ?
C4 C3 C2 120.7(5) . . ?
C23 C24 C25 119.4(4) . . ?
C5 C6 C1 120.6(5) . . ?
C16 C11 N1 116.6(4) . . ?
C12 C11 N1 125.0(5) . . ?
C12 C11 C16 118.3(5) . . ?
C6 C5 C4 120.8(5) . . ?
C14 C15 C16 119.4(6) . . ?
C13 C12 C11 120.2(6) . . ?
C3 C4 C5 121.0(5) . . ?
C13 C14 C15 120.0(6) . . ?
C14 C13 C12 121.0(6) . . ?
O1A C2A C1A 121.4(8) . . ?
O1A C2A C3A 122.7(7) . . ?
C1A C2A C3A 115.7(7) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Acetone and DiethylEther'
####################################################################### 
# 
# 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_aj1010
_database_code_depnum_ccdc_archive 'CCDC 1985944'
loop_
_audit_author_name
_audit_author_address
'HEMANT RAWAT'
;TATA INSTITUTE OF FUNDAMENTAL RESEARCH HYDERABAD
India
;
_audit_update_record             
;
2020-02-24 deposited with the CCDC.	2021-08-18 downloaded from the CCDC.
;
_audit_creation_date             2019-12-04
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C31 H37 N2 O P'
_chemical_formula_sum            'C31 H37 N2 O P'
_chemical_formula_weight         484.59
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H N O '
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      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 1 21 1'
_space_group_name_Hall           'P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   8.0570(6)
_cell_length_b                   14.0475(13)
_cell_length_c                   12.2644(9)
_cell_angle_alpha                90
_cell_angle_beta                 95.457(6)
_cell_angle_gamma                90
_cell_volume                     1381.80(19)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5593
_cell_measurement_temperature    298.16(10)
_cell_measurement_theta_max      27.1700
_cell_measurement_theta_min      2.8910
_shelx_estimated_absorpt_T_max   0.977
_shelx_estimated_absorpt_T_min   0.959
_exptl_absorpt_coefficient_mu    0.125
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.39367
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.29d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.165
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             520
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.19
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1035
_diffrn_reflns_av_unetI/netI     0.0980
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.882
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            15907
_diffrn_reflns_point_group_measured_fraction_full 0.907
_diffrn_reflns_point_group_measured_fraction_max 0.759
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.958
_diffrn_reflns_theta_min         2.900
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      298.16(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.882
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -43.00 -18.00   0.50   17.00    --    7.20 -43.00  24.00   50
  2  ω    -28.00  -1.00   0.50   17.00    --    7.20  43.00 176.00   54
  3  ω     -6.00  19.00   0.50   17.00    --   -7.60  43.00 176.00   50
  4  ω    -82.00 -11.00   0.50   17.00    --    7.20 -57.00 150.00  142
  5  ω     50.00  92.00   0.50   17.00    --    7.20  77.00   0.00   84
  6  ω     11.00  37.00   0.50   17.00    --    7.20 -57.00 150.00   52
  7  ω    -74.00  32.00   0.50   17.00    --   -7.60 -77.00-180.00  212
  8  ω    -30.00  33.00   0.50   17.00    --   -7.60 -82.00   0.00  126
  9  ω    -63.00 -38.00   0.50   17.00    --   -7.60 -82.00   0.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0184985000
_diffrn_orient_matrix_UB_12      0.0049700000
_diffrn_orient_matrix_UB_13      -0.0574421000
_diffrn_orient_matrix_UB_21      -0.0739723000
_diffrn_orient_matrix_UB_22      -0.0269395000
_diffrn_orient_matrix_UB_23      0.0027114000
_diffrn_orient_matrix_UB_31      -0.0447578000
_diffrn_orient_matrix_UB_32      0.0424017000
_diffrn_orient_matrix_UB_33      0.0084236000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.656
_reflns_Friedel_fraction_full    0.807
_reflns_Friedel_fraction_max     0.626
_reflns_number_gt                4143
_reflns_number_total             5547
_reflns_odcompleteness_completeness 99.63
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.524
_refine_diff_density_min         -0.201
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details 
;
 Flack x determined using 1371 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.04(12)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         5547
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0876
_refine_ls_R_factor_gt           0.0681
_refine_ls_restrained_S_all      1.055
_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)+(0.1084P)²+0.0463P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1850
_refine_ls_wR_factor_ref         0.1970
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C12(H12), C10(H10), C16(H16), C25(H25), C11(H11), C27(H27), C18(H18)
2.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C20(H20A,H20B,H20C), C4(H4A,H4B,H4C), C22(H22A,H22B,H22C),
 C7(H7A,H7B,H7C), C29(H29A,H29B,H29C), C6(H6A,H6B,H6C), C30(H30A,H30B,H30C),
 C31(H31A,H31B,H31C), C21(H21A,H21B,H21C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.49640(12) 0.47995(9) 0.38089(8) 0.0469(3) Uani 1 1 d . . . . .
O1 O 0.4033(4) 0.5725(3) 0.3961(3) 0.0639(10) Uani 1 1 d . . . . .
N2 N 0.5700(4) 0.4816(3) 0.6199(3) 0.0457(8) Uani 1 1 d . . . . .
N1 N 0.6782(4) 0.3626(3) 0.5430(3) 0.0453(8) Uani 1 1 d . . . . .
C1 C 0.5961(5) 0.4454(3) 0.5213(3) 0.0414(9) Uani 1 1 d . . . . .
C13 C 0.8466(6) 0.5413(4) 0.3695(4) 0.0511(11) Uani 1 1 d . . . . .
C14 C 0.8619(6) 0.5905(4) 0.4779(5) 0.0547(12) Uani 1 1 d . . . . .
C8 C 0.6967(5) 0.5044(3) 0.3180(4) 0.0485(11) Uani 1 1 d . . . . .
C3 C 0.7105(6) 0.3488(4) 0.6555(4) 0.0510(11) Uani 1 1 d . . . . .
C5 C 0.8026(8) 0.2643(4) 0.7011(5) 0.0704(16) Uani 1 1 d . . . . .
H5A H 0.745068 0.207560 0.675434 0.106 Uiso 1 1 calc GR . . . .
H5B H 0.809293 0.266393 0.779615 0.106 Uiso 1 1 calc GR . . . .
H5C H 0.912973 0.264243 0.677762 0.106 Uiso 1 1 calc GR . . . .
C12 C 0.9902(6) 0.5398(4) 0.3146(5) 0.0629(14) Uani 1 1 d . . . . .
H12 H 1.089884 0.561312 0.350694 0.076 Uiso 1 1 calc R . . . .
C2 C 0.6419(6) 0.4239(4) 0.7034(4) 0.0525(11) Uani 1 1 d . . . . .
C15 C 0.7894(7) 0.6806(4) 0.4862(6) 0.0676(16) Uani 1 1 d . . . . .
C23 C 0.5382(7) 0.4484(5) 0.1377(4) 0.0670(17) Uani 1 1 d . . . . .
C20 C 1.0605(7) 0.4608(4) 0.5586(5) 0.0675(14) Uani 1 1 d . . . . .
H20A H 1.001566 0.419252 0.506211 0.101 Uiso 1 1 calc GR . . . .
H20B H 1.074043 0.430048 0.628804 0.101 Uiso 1 1 calc GR . . . .
H20C H 1.168081 0.475353 0.535361 0.101 Uiso 1 1 calc GR . . . .
C9 C 0.6945(5) 0.4755(5) 0.2074(4) 0.0586(12) Uani 1 1 d . . . . .
C28 C 0.5043(7) 0.3540(6) 0.1082(4) 0.0737(18) Uani 1 1 d . . . . .
C10 C 0.8385(7) 0.4790(6) 0.1539(5) 0.0803(17) Uani 1 1 d . . . . .
H10 H 0.834138 0.462005 0.080357 0.096 Uiso 1 1 calc R . . . .
C4 C 0.7186(7) 0.2945(4) 0.4595(5) 0.0659(14) Uani 1 1 d . . . . .
H4A H 0.641224 0.301762 0.395474 0.099 Uiso 1 1 calc GR . . . .
H4B H 0.711319 0.230965 0.487385 0.099 Uiso 1 1 calc GR . . . .
H4C H 0.829763 0.306083 0.440597 0.099 Uiso 1 1 calc GR . . . .
C22 C 0.6953(8) 0.7278(5) 0.3925(7) 0.088(2) Uani 1 1 d . . . . .
H22A H 0.760293 0.727351 0.330812 0.132 Uiso 1 1 calc GR . . . .
H22B H 0.671792 0.792345 0.411580 0.132 Uiso 1 1 calc GR . . . .
H22C H 0.592491 0.694419 0.373936 0.132 Uiso 1 1 calc GR . . . .
C19 C 0.9627(6) 0.5517(4) 0.5673(5) 0.0597(13) Uani 1 1 d . . . . .
C7 C 0.4856(7) 0.5711(4) 0.6386(5) 0.0650(14) Uani 1 1 d . . . . .
H7A H 0.564767 0.616068 0.671639 0.098 Uiso 1 1 calc GR . . . .
H7B H 0.399901 0.560261 0.686412 0.098 Uiso 1 1 calc GR . . . .
H7C H 0.436657 0.595772 0.569937 0.098 Uiso 1 1 calc GR . . . .
C16 C 0.8101(8) 0.7264(5) 0.5879(8) 0.094(3) Uani 1 1 d . . . . .
H16 H 0.761490 0.785900 0.594360 0.112 Uiso 1 1 calc R . . . .
C25 C 0.2995(8) 0.4950(9) 0.0161(5) 0.103(3) Uani 1 1 d . . . . .
H25 H 0.231388 0.542940 -0.015520 0.124 Uiso 1 1 calc R . . . .
C24 C 0.4338(8) 0.5214(6) 0.0909(4) 0.0775(19) Uani 1 1 d . . . . .
C11 C 0.9892(7) 0.5075(5) 0.2086(5) 0.085(2) Uani 1 1 d . . . . .
H11 H 1.087211 0.504786 0.174420 0.102 Uiso 1 1 calc R . . . .
C29 C 0.6067(12) 0.2760(7) 0.1563(7) 0.107(3) Uani 1 1 d . . . . .
H29A H 0.705690 0.270294 0.118888 0.161 Uiso 1 1 calc GR . . . .
H29B H 0.544644 0.217693 0.149036 0.161 Uiso 1 1 calc GR . . . .
H29C H 0.637190 0.288919 0.232408 0.161 Uiso 1 1 calc GR . . . .
C26 C 0.2628(9) 0.4038(10) -0.0129(5) 0.109(3) Uani 1 1 d . . . . .
C27 C 0.3669(9) 0.3339(7) 0.0345(5) 0.095(3) Uani 1 1 d . . . . .
H27 H 0.343985 0.270648 0.016161 0.114 Uiso 1 1 calc R . . . .
C18 C 0.9765(7) 0.6008(5) 0.6652(5) 0.0764(18) Uani 1 1 d . . . . .
H18 H 1.040740 0.574577 0.724674 0.092 Uiso 1 1 calc R . . . .
C17 C 0.8985(8) 0.6881(6) 0.6789(7) 0.093(3) Uani 1 1 d . . . . .
C6 C 0.6367(8) 0.4473(6) 0.8213(4) 0.0798(18) Uani 1 1 d . . . . .
H6A H 0.686019 0.508709 0.836086 0.120 Uiso 1 1 calc GR . . . .
H6B H 0.697765 0.400116 0.865266 0.120 Uiso 1 1 calc GR . . . .
H6C H 0.522992 0.448150 0.838588 0.120 Uiso 1 1 calc GR . . . .
C30 C 0.1153(11) 0.3773(13) -0.0927(7) 0.170(6) Uani 1 1 d . . . . .
H30A H 0.017725 0.409992 -0.073275 0.254 Uiso 1 1 calc GR . . . .
H30B H 0.097253 0.309822 -0.089985 0.254 Uiso 1 1 calc GR . . . .
H30C H 0.137408 0.395240 -0.165433 0.254 Uiso 1 1 calc GR . . . .
C31 C 0.4687(13) 0.6227(7) 0.1224(7) 0.113(3) Uani 1 1 d . . . . .
H31A H 0.460885 0.630396 0.199567 0.169 Uiso 1 1 calc GR . . . .
H31B H 0.388770 0.663370 0.082420 0.169 Uiso 1 1 calc GR . . . .
H31C H 0.578924 0.639504 0.105595 0.169 Uiso 1 1 calc GR . . . .
C21 C 0.9087(11) 0.7398(9) 0.7842(9) 0.147(5) Uani 1 1 d . . . . .
H21A H 0.953704 0.802163 0.774785 0.220 Uiso 1 1 calc GR . . . .
H21B H 0.979719 0.705487 0.837956 0.220 Uiso 1 1 calc GR . . . .
H21C H 0.799205 0.745208 0.808429 0.220 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1 O1 1.522(4) . ?
P1 C1 1.892(4) . ?
P1 C8 1.885(4) . ?
N2 C1 1.347(5) . ?
N2 C2 1.388(6) . ?
N2 C7 1.457(7) . ?
N1 C1 1.352(6) . ?
N1 C3 1.393(6) . ?
N1 C4 1.460(6) . ?
C13 C14 1.494(7) . ?
C13 C8 1.408(7) . ?
C13 C12 1.393(7) . ?
C14 C15 1.401(8) . ?
C14 C19 1.411(8) . ?
C8 C9 1.415(7) . ?
C3 C5 1.481(8) . ?
C3 C2 1.351(7) . ?
C12 C11 1.376(9) . ?
C2 C6 1.488(7) . ?
C15 C22 1.473(10) . ?
C15 C16 1.399(10) . ?
C23 C9 1.502(7) . ?
C23 C28 1.395(10) . ?
C23 C24 1.413(9) . ?
C20 C19 1.509(8) . ?
C9 C10 1.387(7) . ?
C28 C29 1.461(12) . ?
C28 C27 1.391(9) . ?
C10 C11 1.389(9) . ?
C19 C18 1.380(8) . ?
C16 C17 1.375(13) . ?
C25 C24 1.400(10) . ?
C25 C26 1.354(15) . ?
C24 C31 1.495(12) . ?
C26 C27 1.383(13) . ?
C26 C30 1.512(10) . ?
C18 C17 1.395(11) . ?
C17 C21 1.477(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
O1 P1 C1 106.2(2) . . ?
O1 P1 C8 110.2(2) . . ?
C8 P1 C1 96.50(18) . . ?
C1 N2 C2 110.6(4) . . ?
C1 N2 C7 125.5(4) . . ?
C2 N2 C7 123.8(4) . . ?
C1 N1 C3 110.9(4) . . ?
C1 N1 C4 124.2(4) . . ?
C3 N1 C4 124.8(4) . . ?
N2 C1 P1 129.1(3) . . ?
N2 C1 N1 105.2(4) . . ?
N1 C1 P1 123.9(3) . . ?
C8 C13 C14 124.3(4) . . ?
C12 C13 C14 115.8(4) . . ?
C12 C13 C8 119.6(5) . . ?
C15 C14 C13 118.9(5) . . ?
C15 C14 C19 120.4(5) . . ?
C19 C14 C13 120.4(4) . . ?
C13 C8 P1 128.0(3) . . ?
C13 C8 C9 117.9(4) . . ?
C9 C8 P1 114.0(3) . . ?
N1 C3 C5 121.7(5) . . ?
C2 C3 N1 106.1(4) . . ?
C2 C3 C5 132.2(5) . . ?
C11 C12 C13 122.1(5) . . ?
N2 C2 C6 122.6(5) . . ?
C3 C2 N2 107.1(4) . . ?
C3 C2 C6 130.2(5) . . ?
C14 C15 C22 122.4(6) . . ?
C16 C15 C14 117.7(7) . . ?
C16 C15 C22 119.9(6) . . ?
C28 C23 C9 121.4(6) . . ?
C28 C23 C24 119.3(6) . . ?
C24 C23 C9 118.9(6) . . ?
C8 C9 C23 123.4(4) . . ?
C10 C9 C8 120.6(5) . . ?
C10 C9 C23 115.7(4) . . ?
C23 C28 C29 121.3(5) . . ?
C27 C28 C23 119.1(7) . . ?
C27 C28 C29 119.6(8) . . ?
C9 C10 C11 120.9(5) . . ?
C14 C19 C20 122.6(5) . . ?
C18 C19 C14 118.3(6) . . ?
C18 C19 C20 119.0(6) . . ?
C17 C16 C15 123.5(7) . . ?
C26 C25 C24 123.9(8) . . ?
C23 C24 C31 119.7(6) . . ?
C25 C24 C23 117.9(8) . . ?
C25 C24 C31 122.4(8) . . ?
C12 C11 C10 118.6(5) . . ?
C25 C26 C27 116.9(7) . . ?
C25 C26 C30 122.8(11) . . ?
C27 C26 C30 120.3(12) . . ?
C26 C27 C28 122.8(9) . . ?
C19 C18 C17 123.0(7) . . ?
C16 C17 C18 116.7(6) . . ?
C16 C17 C21 119.9(8) . . ?
C18 C17 C21 123.3(9) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.118
_oxdiff_exptl_absorpt_empirical_full_min 0.305
####################################################################### 
# 
# 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_AJ1003
_database_code_depnum_ccdc_archive 'CCDC 2082008'
_audit_update_record             
;
2021-08-04 deposited with the CCDC.	2021-08-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C31 H37 N2 O2 P'
_chemical_formula_sum            'C31 H37 N2 O2 P'
_chemical_formula_weight         500.59

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   14.0017(10)
_cell_length_b                   14.1141(8)
_cell_length_c                   14.6959(11)
_cell_angle_alpha                90
_cell_angle_beta                 109.903(8)
_cell_angle_gamma                90
_cell_volume                     2730.8(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3702
_cell_measurement_theta_min      3.0910
_cell_measurement_theta_max      26.6930

_exptl_crystal_description       platelet
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.218
_exptl_crystal_F_000             1072
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.140
_exptl_absorpt_coefficient_mu    0.131
_shelx_estimated_absorpt_T_min   0.968
_shelx_estimated_absorpt_T_max   0.982
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.71348
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.29d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            18615
_diffrn_reflns_av_unetI/netI     0.0722
_diffrn_reflns_av_R_equivalents  0.0580
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.474
_diffrn_reflns_theta_max         29.021
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.822
_diffrn_measured_fraction_theta_full 0.966
_diffrn_reflns_Laue_measured_fraction_max 0.822
_diffrn_reflns_Laue_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.822
_diffrn_reflns_point_group_measured_fraction_full 0.966
_reflns_number_total             5983
_reflns_number_gt                3776
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_structure_solution    'ShelXT-2018 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'CIFTAB (Sheldrick, 2015)'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0697P)²+0.5832P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5983
_refine_ls_number_parameters     335
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1066
_refine_ls_R_factor_gt           0.0609
_refine_ls_wR_factor_ref         0.1558
_refine_ls_wR_factor_gt          0.1371
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_restrained_S_all      1.015
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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 0.52548(4) 0.72458(4) 0.44640(4) 0.04074(18) Uani 1 1 d . . . . .
O1 O 0.59244(12) 0.64089(12) 0.46368(12) 0.0553(4) Uani 1 1 d . . . . .
O2 O 0.55871(12) 0.81356(12) 0.50064(11) 0.0548(4) Uani 1 1 d . . . . .
N1 N 0.36347(13) 0.59987(12) 0.44258(12) 0.0408(4) Uani 1 1 d . . . . .
N2 N 0.36871(13) 0.72009(12) 0.53400(13) 0.0410(4) Uani 1 1 d . . . . .
C1 C 0.41365(16) 0.68127(15) 0.47500(15) 0.0380(5) Uani 1 1 d . . . . .
C2 C 0.28852(16) 0.66410(17) 0.53578(16) 0.0453(5) Uani 1 1 d . . . . .
C3 C 0.28541(16) 0.58812(16) 0.47919(16) 0.0429(5) Uani 1 1 d . . . . .
C4 C 0.38721(18) 0.53066(16) 0.37895(17) 0.0505(6) Uani 1 1 d . . . . .
H4A H 0.334032 0.530700 0.317002 0.076 Uiso 1 1 calc R U . . .
H4B H 0.392761 0.468696 0.407221 0.076 Uiso 1 1 calc R U . . .
H4C H 0.450371 0.547285 0.370961 0.076 Uiso 1 1 calc R U . . .
C5 C 0.21674(18) 0.50491(18) 0.45513(19) 0.0566(6) Uani 1 1 d . . . . .
H5A H 0.186062 0.499693 0.386130 0.085 Uiso 1 1 calc R U . . .
H5B H 0.164697 0.512611 0.483408 0.085 Uiso 1 1 calc R U . . .
H5C H 0.254980 0.448538 0.480273 0.085 Uiso 1 1 calc R U . . .
C6 C 0.2212(2) 0.6911(2) 0.5911(2) 0.0660(7) Uani 1 1 d . . . . .
H6A H 0.260229 0.693622 0.658851 0.099 Uiso 1 1 calc R U . . .
H6B H 0.168103 0.644954 0.580153 0.099 Uiso 1 1 calc R U . . .
H6C H 0.191845 0.752169 0.569854 0.099 Uiso 1 1 calc R U . . .
C7 C 0.39868(19) 0.80710(18) 0.59001(18) 0.0562(6) Uani 1 1 d . . . . .
H7A H 0.425269 0.791991 0.657707 0.084 Uiso 1 1 calc R U . . .
H7B H 0.340617 0.847694 0.577655 0.084 Uiso 1 1 calc R U . . .
H7C H 0.449884 0.838906 0.571548 0.084 Uiso 1 1 calc R U . . .
C8 C 0.47098(16) 0.74562(15) 0.31489(15) 0.0395(5) Uani 1 1 d . . . . .
C9 C 0.37378(17) 0.78651(15) 0.26953(16) 0.0425(5) Uani 1 1 d . . . . .
C10 C 0.3324(2) 0.78799(17) 0.16939(18) 0.0555(6) Uani 1 1 d . . . . .
H10 H 0.267185 0.811801 0.139918 0.067 Uiso 1 1 calc R U . . .
C11 C 0.3851(2) 0.7553(2) 0.11323(19) 0.0657(7) Uani 1 1 d . . . . .
H11 H 0.355231 0.754808 0.046199 0.079 Uiso 1 1 calc R U . . .
C12 C 0.4832(2) 0.72306(19) 0.15639(19) 0.0610(7) Uani 1 1 d . . . . .
H12 H 0.520761 0.704901 0.117880 0.073 Uiso 1 1 calc R U . . .
C13 C 0.52685(17) 0.71722(16) 0.25649(16) 0.0456(5) Uani 1 1 d . . . . .
C14 C 0.63687(18) 0.6874(2) 0.29392(16) 0.0522(6) Uani 1 1 d . . . . .
C15 C 0.6647(2) 0.5933(2) 0.28482(19) 0.0612(7) Uani 1 1 d . . . . .
C16 C 0.7674(2) 0.5719(3) 0.3109(2) 0.0763(9) Uani 1 1 d . . . . .
H16 H 0.786084 0.509441 0.305595 0.092 Uiso 1 1 calc R U . . .
C17 C 0.8425(2) 0.6387(3) 0.3441(2) 0.0836(10) Uani 1 1 d . . . . .
C18 C 0.8139(2) 0.7303(3) 0.3521(2) 0.0778(10) Uani 1 1 d . . . . .
H18 H 0.863733 0.776501 0.374649 0.093 Uiso 1 1 calc R U . . .
C19 C 0.7118(2) 0.7563(2) 0.32735(18) 0.0608(7) Uani 1 1 d . . . . .
C20 C 0.6847(3) 0.8576(2) 0.3373(2) 0.0839(10) Uani 1 1 d . . . . .
H20A H 0.629768 0.876444 0.280429 0.126 Uiso 1 1 calc R U . . .
H20B H 0.742613 0.897178 0.344653 0.126 Uiso 1 1 calc R U . . .
H20C H 0.664247 0.864177 0.393034 0.126 Uiso 1 1 calc R U . . .
C21 C 0.9534(2) 0.6106(4) 0.3745(3) 0.1323(17) Uani 1 1 d . . . . .
H21A H 0.966817 0.582564 0.320491 0.198 Uiso 1 1 calc R U . . .
H21B H 0.968555 0.565635 0.426472 0.198 Uiso 1 1 calc R U . . .
H21C H 0.995215 0.665773 0.395625 0.198 Uiso 1 1 calc R U . . .
C22 C 0.5882(2) 0.5151(2) 0.2541(2) 0.0810(9) Uani 1 1 d . . . . .
H22A H 0.584539 0.482738 0.310283 0.121 Uiso 1 1 calc R U . . .
H22B H 0.608147 0.471167 0.213976 0.121 Uiso 1 1 calc R U . . .
H22C H 0.522839 0.541131 0.218305 0.121 Uiso 1 1 calc R U . . .
C23 C 0.31206(17) 0.83367(15) 0.32223(16) 0.0456(6) Uani 1 1 d . . . . .
C24 C 0.34012(19) 0.92392(17) 0.36332(18) 0.0537(6) Uani 1 1 d . . . . .
C25 C 0.2795(2) 0.96850(19) 0.4078(2) 0.0680(8) Uani 1 1 d . . . . .
H25 H 0.298441 1.027996 0.435182 0.082 Uiso 1 1 calc R U . . .
C26 C 0.1919(2) 0.9276(2) 0.4129(2) 0.0704(8) Uani 1 1 d . . . . .
C27 C 0.16216(19) 0.8423(2) 0.3664(2) 0.0642(7) Uani 1 1 d . . . . .
H27 H 0.101857 0.815045 0.366953 0.077 Uiso 1 1 calc R U . . .
C28 C 0.21888(17) 0.79489(17) 0.31861(18) 0.0500(6) Uani 1 1 d . . . . .
C29 C 0.17789(19) 0.70506(17) 0.2645(2) 0.0574(7) Uani 1 1 d . . . . .
H29A H 0.142153 0.719562 0.197719 0.086 Uiso 1 1 calc R U . . .
H29B H 0.132263 0.675479 0.292022 0.086 Uiso 1 1 calc R U . . .
H29C H 0.233069 0.662756 0.269270 0.086 Uiso 1 1 calc R U . . .
C30 C 0.1324(3) 0.9730(3) 0.4703(3) 0.1032(12) Uani 1 1 d . . . . .
H30A H 0.063653 0.950423 0.446829 0.155 Uiso 1 1 calc R U . . .
H30B H 0.132836 1.040599 0.463132 0.155 Uiso 1 1 calc R U . . .
H30C H 0.163073 0.956770 0.537467 0.155 Uiso 1 1 calc R U . . .
C31 C 0.4326(2) 0.97397(17) 0.3581(2) 0.0695(8) Uani 1 1 d . . . . .
H31A H 0.492489 0.943173 0.400227 0.104 Uiso 1 1 calc R U . . .
H31B H 0.431816 1.038704 0.377883 0.104 Uiso 1 1 calc R U . . .
H31C H 0.432757 0.972074 0.292844 0.104 Uiso 1 1 calc R U . . .


_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 O2 1.4753(17) . ?
P1 O1 1.4754(16) . ?
P1 C8 1.844(2) . ?
P1 C1 1.858(2) . ?
N1 C1 1.346(3) . ?
N1 C3 1.383(3) . ?
N1 C4 1.467(3) . ?
N2 C1 1.349(3) . ?
N2 C2 1.380(3) . ?
N2 C7 1.458(3) . ?
C2 C3 1.349(3) . ?
C2 C6 1.488(3) . ?
C3 C5 1.482(3) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 C13 1.402(3) . ?
C8 C9 1.418(3) . ?
C9 C10 1.386(3) . ?
C9 C23 1.499(3) . ?
C10 C11 1.362(4) . ?
C10 H10 0.9300 . ?
C11 C12 1.379(4) . ?
C11 H11 0.9300 . ?
C12 C13 1.390(3) . ?
C12 H12 0.9300 . ?
C13 C14 1.509(3) . ?
C14 C19 1.391(4) . ?
C14 C15 1.404(4) . ?
C15 C16 1.389(4) . ?
C15 C22 1.497(4) . ?
C16 C17 1.372(5) . ?
C16 H16 0.9300 . ?
C17 C18 1.371(5) . ?
C17 C21 1.516(4) . ?
C18 C19 1.399(4) . ?
C18 H18 0.9300 . ?
C19 C20 1.499(4) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 C28 1.399(3) . ?
C23 C24 1.407(3) . ?
C24 C25 1.387(4) . ?
C24 C31 1.500(4) . ?
C25 C26 1.379(4) . ?
C25 H25 0.9300 . ?
C26 C27 1.377(4) . ?
C26 C30 1.516(4) . ?
C27 C28 1.397(4) . ?
C27 H27 0.9300 . ?
C28 C29 1.503(3) . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 P1 O1 121.57(10) . . ?
O2 P1 C8 111.78(10) . . ?
O1 P1 C8 108.74(10) . . ?
O2 P1 C1 107.04(10) . . ?
O1 P1 C1 103.46(9) . . ?
C8 P1 C1 102.13(9) . . ?
C1 N1 C3 110.55(17) . . ?
C1 N1 C4 126.14(18) . . ?
C3 N1 C4 123.29(18) . . ?
C1 N2 C2 109.88(18) . . ?
C1 N2 C7 126.68(18) . . ?
C2 N2 C7 123.44(18) . . ?
N1 C1 N2 105.82(17) . . ?
N1 C1 P1 125.40(15) . . ?
N2 C1 P1 128.71(16) . . ?
C3 C2 N2 107.41(19) . . ?
C3 C2 C6 130.3(2) . . ?
N2 C2 C6 122.3(2) . . ?
C2 C3 N1 106.30(19) . . ?
C2 C3 C5 131.2(2) . . ?
N1 C3 C5 122.5(2) . . ?
N1 C4 H4A 109.5 . . ?
N1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C2 C6 H6A 109.5 . . ?
C2 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C2 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N2 C7 H7A 109.5 . . ?
N2 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
N2 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C13 C8 C9 118.3(2) . . ?
C13 C8 P1 118.51(16) . . ?
C9 C8 P1 123.13(17) . . ?
C10 C9 C8 119.5(2) . . ?
C10 C9 C23 115.8(2) . . ?
C8 C9 C23 124.6(2) . . ?
C11 C10 C9 121.4(2) . . ?
C11 C10 H10 119.3 . . ?
C9 C10 H10 119.3 . . ?
C10 C11 C12 119.6(2) . . ?
C10 C11 H11 120.2 . . ?
C12 C11 H11 120.2 . . ?
C11 C12 C13 121.1(2) . . ?
C11 C12 H12 119.5 . . ?
C13 C12 H12 119.5 . . ?
C12 C13 C8 119.7(2) . . ?
C12 C13 C14 115.4(2) . . ?
C8 C13 C14 124.7(2) . . ?
C19 C14 C15 119.6(2) . . ?
C19 C14 C13 119.2(2) . . ?
C15 C14 C13 120.7(2) . . ?
C16 C15 C14 118.4(3) . . ?
C16 C15 C22 119.3(3) . . ?
C14 C15 C22 122.2(2) . . ?
C17 C16 C15 122.9(3) . . ?
C17 C16 H16 118.5 . . ?
C15 C16 H16 118.5 . . ?
C18 C17 C16 117.9(3) . . ?
C18 C17 C21 121.5(4) . . ?
C16 C17 C21 120.6(4) . . ?
C17 C18 C19 121.9(3) . . ?
C17 C18 H18 119.1 . . ?
C19 C18 H18 119.1 . . ?
C14 C19 C18 119.3(3) . . ?
C14 C19 C20 121.0(3) . . ?
C18 C19 C20 119.7(3) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C17 C21 H21A 109.5 . . ?
C17 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C17 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C15 C22 H22A 109.5 . . ?
C15 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C15 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C28 C23 C24 119.4(2) . . ?
C28 C23 C9 120.1(2) . . ?
C24 C23 C9 119.9(2) . . ?
C25 C24 C23 119.1(2) . . ?
C25 C24 C31 119.2(2) . . ?
C23 C24 C31 121.6(2) . . ?
C26 C25 C24 122.3(3) . . ?
C26 C25 H25 118.9 . . ?
C24 C25 H25 118.9 . . ?
C27 C26 C25 117.6(3) . . ?
C27 C26 C30 121.0(3) . . ?
C25 C26 C30 121.4(3) . . ?
C26 C27 C28 122.7(3) . . ?
C26 C27 H27 118.7 . . ?
C28 C27 H27 118.7 . . ?
C27 C28 C23 118.4(2) . . ?
C27 C28 C29 119.3(2) . . ?
C23 C28 C29 122.2(2) . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C26 C30 H30A 109.5 . . ?
C26 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C26 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C24 C31 H31A 109.5 . . ?
C24 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C24 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?

_refine_diff_density_max         0.295
_refine_diff_density_min         -0.266
_refine_diff_density_rms         0.043



####################################################################### 
# 
# 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_DD1155B
_database_code_depnum_ccdc_archive 'CCDC 1985948'
loop_
_audit_author_name
_audit_author_address
'HEMANT RAWAT'
;TATA INSTITUTE OF FUNDAMENTAL RESEARCH HYDERABAD
India
;
_audit_update_record             
;
2020-02-24 deposited with the CCDC.	2021-08-18 downloaded from the CCDC.
;
_audit_creation_date             2020-02-24
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C110 H124 K4 N4 O4 P4,3(C6 H6)'
_chemical_formula_sum            'C128 H142 K4 N4 O4 P4'
_chemical_formula_weight         2080.73
_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'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   13.406(3)
_cell_length_b                   14.783(3)
_cell_length_c                   30.449(6)
_cell_angle_alpha                99.67(3)
_cell_angle_beta                 102.51(3)
_cell_angle_gamma                96.47(3)
_cell_volume                     5737(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    64584
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      59.3
_cell_measurement_theta_min      6.1
_shelx_estimated_absorpt_T_max   0.931
_shelx_estimated_absorpt_T_min   0.904
_exptl_absorpt_coefficient_mu    0.265
_exptl_absorpt_correction_T_max  0.9439
_exptl_absorpt_correction_T_min  0.5670
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'face indexed'
_exptl_absorpt_special_details   
;
programs X-Red32 and X-Shape by STOE & Cie GmbH 2010
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.204
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2212
_exptl_crystal_size_max          0.389
_exptl_crystal_size_mid          0.333
_exptl_crystal_size_min          0.272
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0781
_diffrn_reflns_av_unetI/netI     0.0914
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            48722
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.051
_diffrn_ambient_temperature      170.15
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'STOE IPDS2T'
_diffrn_measurement_method       ω
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                12940
_reflns_number_total             23376
_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       'X-Area (Stoe & Cie, 2010).'
_computing_data_collection       'X-Area (Stoe & Cie, 2010).'
_computing_data_reduction        'X-Area (Stoe & Cie, 2010).'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT-2018 (Sheldrick, 2015)'
_refine_diff_density_max         0.684
_refine_diff_density_min         -0.454
_refine_diff_density_rms         0.068
_refine_ls_extinction_coef       0.0056(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1306
_refine_ls_number_reflns         23376
_refine_ls_number_restraints     96
_refine_ls_R_factor_all          0.1286
_refine_ls_R_factor_gt           0.0656
_refine_ls_restrained_S_all      1.029
_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)+(0.1010P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1632
_refine_ls_wR_factor_ref         0.1940
_refine_special_details          ?
_olex2_refinement_description    
;
1. Others
 Fixed Uiso: H4A(0.12) H4B(0.12) H4C(0.12) H5A(0.1) H5B(0.1) H5C(0.1)
 H6A(0.158) H6B(0.158) H6C(0.158) H7A(0.168) H7B(0.168) H7C(0.168) H10(0.052)
 H11(0.055) H12(0.053) H16(0.058) H18(0.056) H20A(0.082) H20B(0.082)
 H20C(0.082) H21A(0.101) H21B(0.101) H21C(0.101) H22A(0.076) H22B(0.076)
 H22C(0.076) H25(0.063) H27(0.06) H29A(0.076) H29B(0.076) H29C(0.076)
 H30A(0.075) H30B(0.075) H30C(0.075) H31A(0.114) H31B(0.114) H31C(0.114)
 H35A(0.097) H35B(0.097) H35C(0.097) H36A(0.11) H36B(0.11) H36C(0.11)
 H37A(0.138) H37B(0.138) H37C(0.138) H38A(0.123) H38B(0.123) H38C(0.123)
 H41(0.058) H42(0.067) H43(0.061) H47(0.07) H49(0.069) H51A(0.094) H51B(0.094)
 H51C(0.094) H52A(0.09) H52B(0.09) H52C(0.09) H53A(0.12) H53B(0.12) H53C(0.12)
 H56(0.055) H58(0.06) H60A(0.074) H60B(0.074) H60C(0.074) H61A(0.093)
 H61B(0.093) H61C(0.093) H62A(0.08) H62B(0.08) H62C(0.08) H65(0.05) H66(0.054)
 H67(0.048) H71(0.048) H73(0.052) H75A(0.064) H75B(0.064) H75C(0.064)
 H76A(0.081) H76B(0.081) H76C(0.081) H77A(0.074) H77B(0.074) H77C(0.074)
 H80(0.052) H82(0.05) H84A(0.069) H84B(0.069) H84C(0.069) H85A(0.095)
 H85B(0.095) H85C(0.095) H86A(0.065) H86B(0.065) H86C(0.065) H89(0.05)
 H90(0.053) H91(0.051) H95(0.058) H97(0.056) H99A(0.07) H99B(0.07) H99C(0.07)
 H10A(0.103) H10B(0.103) H10C(0.103) H10D(0.071) H10E(0.071) H10F(0.071)
 H104(0.051) H106(0.048) H10G(0.084) H10H(0.084) H10I(0.084) H10J(0.082)
 H10K(0.082) H10L(0.082) H11A(0.073) H11B(0.073) H11C(0.073) H111(0.181)
 H112(0.196) H113(0.216) H114(0.233) H115(0.206) H116(0.184) H117(0.136)
 H118(0.13) H119(0.123) H120(0.134) H121(0.135) H122(0.134) H123(0.27)
 H124(0.266) H125(0.289) H126(0.31) H127(0.308) H128(0.289)
 Fixed X: H4A(0.86742) H4B(0.94866) H4C(0.828869) H5A(0.780656) H5B(0.892379)
 H5C(0.81405) H6A(1.070426) H6B(0.965997) H6C(1.046499) H7A(1.097054)
 H7B(1.099202) H7C(1.018898) H10(0.263043) H11(0.236661) H12(0.328584)
 H16(0.413928) H18(0.255427) H20A(0.497024) H20B(0.427838) H20C(0.529723)
 H21A(0.258261) H21B(0.298679) H21C(0.378535) H22A(0.213904) H22B(0.221491)
 H22C(0.314249) H25(0.409633) H27(0.598486) H29A(0.619462) H29B(0.607072)
 H29C(0.515183) H30A(0.302932) H30B(0.286391) H30C(0.373632) H31A(0.496465)
 H31B(0.532698) H31C(0.61329) H35A(0.769403) H35B(0.726214) H35C(0.683157)
 H36A(0.434734) H36B(0.361777) H36C(0.445881) H37A(0.465034) H37B(0.371906)
 H37C(0.445936) H38A(0.592962) H38B(0.705207) H38C(0.625991) H41(0.722094)
 H42(0.751542) H43(0.772183) H47(0.882071) H49(0.582031) H51A(0.915121)
 H51B(0.969736) H51C(0.904405) H52A(0.480765) H52B(0.538551) H52C(0.506572)
 H53A(0.801235) H53B(0.678361) H53C(0.727152) H56(0.702839) H58(0.977978)
 H60A(0.608262) H60B(0.57269) H60C(0.563065) H61A(0.927978) H61B(0.827323)
 H61C(0.928878) H62A(1.022237) H62B(0.947669) H62C(0.93333) H65(0.535585)
 H66(0.63805) H67(0.782494) H71(0.895284) H73(1.105561) H75A(0.722287)
 H75B(0.708467) H75C(0.680552) H76A(1.158591) H76B(1.070112) H76C(1.110843)
 H77A(1.069736) H77B(0.957314) H77C(0.979439) H80(0.353436) H82(0.422812)
 H84A(0.4393) H84B(0.518614) H84C(0.559183) H85A(0.279191) H85B(0.27773)
 H85C(0.215538) H86A(0.584728) H86B(0.571724) H86C(0.663989) H89(1.19163)
 H90(1.200866) H91(1.060289) H95(1.098447) H97(1.096421) H99A(1.085129)
 H99B(1.097008) H99C(0.984694) H10A(1.10314) H10B(1.075305) H10C(1.192129)
 H10D(1.071814) H10E(0.996141) H10F(1.118634) H104(0.830261) H106(0.71692)
 H10G(1.03105) H10H(0.958081) H10I(0.937393) H10J(0.721295) H10K(0.656594)
 H10L(0.627653) H11A(0.890459) H11B(0.809512) H11C(0.768896) H111(1.320803)
 H112(1.362449) H113(1.369369) H114(1.334641) H115(1.292993) H116(1.286074)
 H117(0.07974) H118(0.068464) H119(0.109269) H120(0.162911) H121(0.177086)
 H122(0.12661) H123(0.694757) H124(0.873332) H125(0.975829) H126(0.899752)
 H127(0.721177) H128(0.618678)
 Fixed Y: H4A(0.60713) H4B(0.553617) H4C(0.533625) H5A(0.729536) H5B(0.785217)
 H5C(0.833613) H6A(0.905064) H6B(0.926437) H6C(0.878019) H7A(0.809572)
 H7B(0.700092) H7C(0.74387) H10(0.168995) H11(0.30981) H12(0.446866) H16(-
 0.081621) H18(0.014425) H20A(0.011417) H20B(0.08609) H20C(0.11887) H21A(-
 0.149045) H21B(-0.191559) H21C(-0.155351) H22A(0.210841) H22B(0.165057)
 H22C(0.24067) H25(0.631579) H27(0.682436) H29A(0.57115) H29B(0.466843)
 H29C(0.500712) H30A(0.490615) H30B(0.419835) H30C(0.410826) H31A(0.811185)
 H31B(0.776717) H31C(0.794042) H35A(0.190774) H35B(0.285875) H35C(0.221923)
 H36A(0.114729) H36B(0.148173) H36C(0.222403) H37A(-0.078751) H37B(-0.02082)
 H37C(-0.036146) H38A(-0.046638) H38B(0.014422) H38C(0.039424) H41(0.151289)
 H42(0.019249) H43(0.024144) H47(0.491755) H49(0.421685) H51A(0.291211)
 H51B(0.395116) H51C(0.372609) H52A(0.294315) H52B(0.209156) H52C(0.276646)
 H53A(0.575884) H53B(0.554258) H53C(0.612593) H56(0.043758) H58(0.193183)
 H60A(0.010718) H60B(0.012814) H60C(0.098911) H61A(0.147516) H61B(0.071085)
 H61C(0.042772) H62A(0.246282) H62B(0.210693) H62C(0.303886) H65(0.650576)
 H66(0.779987) H67(0.850565) H71(0.963828) H73(0.906798) H75A(0.898008)
 H75B(0.790177) H75C(0.864297) H76A(0.985614) H76B(1.028379) H76C(1.070433)
 H77A(0.794798) H77B(0.792239) H77C(0.710844) H80(0.52851) H82(0.352048)
 H84A(0.679418) H84B(0.720636) H84C(0.670146) H85A(0.350014) H85B(0.303657)
 H85C(0.38822) H86A(0.488307) H86B(0.38335) H86C(0.458721) H89(0.612122)
 H90(0.615261) H91(0.545811) H95(0.396551) H97(0.669817) H99A(0.323505)
 H99B(0.386141) H99C(0.351221) H10A(0.45739) H10B(0.559297) H10C(0.545944)
 H10D(0.764675) H10E(0.71848) H10F(0.734976) H104(0.239333) H106(0.462509)
 H10G(0.346227) H10H(0.24813) H10I(0.316614) H10J(0.232702) H10K(0.315707)
 H10L(0.245943) H11A(0.627335) H11B(0.616876) H11C(0.610327) H111(0.689735)
 H112(0.684118) H113(0.817274) H114(0.956048) H115(0.961667) H116(0.828512)
 H117(0.143247) H118(-0.010739) H119(-0.118866) H120(-0.076877) H121(0.078436)
 H122(0.186316) H123(0.813415) H124(0.858554) H125(0.902302) H126(0.900912)
 H127(0.855774) H128(0.812026)
 Fixed Z: H4A(0.946316) H4B(0.924999) H4C(0.898819) H5A(0.783828) H5B(0.78708)
 H5C(0.812727) H6A(0.906934) H6B(0.876342) H6C(0.852145) H7A(0.961786)
 H7B(0.95411) H7C(0.980157) H10(0.834074) H11(0.874195) H12(0.866743)
 H16(0.778823) H18(0.673387) H20A(0.848153) H20B(0.864126) H20C(0.848032)
 H21A(0.664335) H21B(0.708733) H21C(0.680984) H22A(0.731425) H22B(0.680986)
 H22C(0.713609) H25(0.754097) H27(0.880082) H29A(0.924103) H29B(0.896407)
 H29C(0.917637) H30A(0.722899) H30B(0.756031) H30C(0.727732) H31A(0.826438)
 H31B(0.780519) H31C(0.829399) H35A(0.579491) H35B(0.592316) H35C(0.542269)
 H36A(0.671104) H36B(0.629899) H36C(0.668289) H37A(0.576644) H37B(0.579388)
 H37C(0.625493) H38A(0.536205) H38B(0.556074) H38C(0.514041) H41(0.945778)
 H42(0.90094) H43(0.827321) H47(1.000721) H49(0.99685) H51A(0.93572)
 H51B(0.959404) H51C(0.907163) H52A(0.94808) H52B(0.933575) H52C(0.898714)
 H53A(1.059022) H53B(1.051481) H53C(1.019365) H56(0.673552) H58(0.73998)
 H60A(0.762656) H60B(0.709207) H60C(0.746849) H61A(0.653167) H61B(0.630791)
 H61C(0.660304) H62A(0.819378) H62B(0.849541) H62C(0.830283) H65(0.546252)
 H66(0.536224) H67(0.59361) H71(0.766863) H73(0.695093) H75A(0.741155)
 H75B(0.718444) H75C(0.686783) H76A(0.780621) H76B(0.801286) H76C(0.762125)
 H77A(0.628881) H77B(0.596875) H77C(0.62459) H80(0.656037) H82(0.555022)
 H84A(0.68192) H84B(0.655171) H84C(0.69668) H85A(0.634202) H85B(0.582595)
 H85C(0.592204) H86A(0.522282) H86B(0.529651) H86C(0.562807) H89(0.691044)
 H90(0.615843) H91(0.556022) H95(0.793879) H97(0.830053) H99A(0.718301)
 H99B(0.681125) H99C(0.68763) H10A(0.871323) H10B(0.884708) H10C(0.884723)
 H10D(0.777944) H10E(0.729035) H10F(0.734525) H104(0.497169) H106(0.460726)
 H10G(0.582939) H10H(0.562442) H10I(0.605025) H10J(0.417395) H10K(0.409715)
 H10L(0.441533) H11A(0.528262) H11B(0.559448) H11C(0.505396) H111(0.853008)
 H112(0.931109) H113(0.986156) H114(0.963103) H115(0.885003) H116(0.829955)
 H117(0.604761) H118(0.612557) H119(0.558587) H120(0.496874) H121(0.488953)
 H122(0.541671) H123(1.066496) H124(1.095051) H125(1.046648) H126(0.96969)
 H127(0.941133) H128(0.989536)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
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
N1 N 0.9027(3) 0.6546(3) 0.89301(12) 0.0602(10) Uani 1 1 d . . . . .
N2 N 0.8803(3) 0.7400(2) 0.84401(11) 0.0519(8) Uani 1 1 d . . . . .
C1 C 0.8422(3) 0.6557(3) 0.85083(14) 0.0556(11) Uani 1 1 d . . . . .
C2 C 0.9616(4) 0.7890(3) 0.87987(16) 0.0628(12) Uani 1 1 d . . . . .
C3 C 0.9771(4) 0.7347(3) 0.91088(15) 0.0672(13) Uani 1 1 d . . . . .
C4 C 0.8855(4) 0.5813(4) 0.91778(17) 0.0800(16) Uani 1 1 d . . . . .
H4A H 0.867420 0.607130 0.946316 0.120 Uiso 1 1 calc R U . . .
H4B H 0.948660 0.553617 0.924999 0.120 Uiso 1 1 calc R U . . .
H4C H 0.828869 0.533625 0.898819 0.120 Uiso 1 1 calc R U . . .
C5 C 0.8385(4) 0.7749(3) 0.80371(15) 0.0668(13) Uani 1 1 d . . . . .
H5A H 0.780656 0.729536 0.783828 0.100 Uiso 1 1 calc R U . . .
H5B H 0.892379 0.785217 0.787080 0.100 Uiso 1 1 calc R U . . .
H5C H 0.814050 0.833613 0.812727 0.100 Uiso 1 1 calc R U . . .
C6 C 1.0158(5) 0.8828(4) 0.8787(2) 0.105(2) Uani 1 1 d . . . . .
H6A H 1.070426 0.905064 0.906934 0.158 Uiso 1 1 calc R U . . .
H6B H 0.965997 0.926437 0.876342 0.158 Uiso 1 1 calc R U . . .
H6C H 1.046499 0.878019 0.852145 0.158 Uiso 1 1 calc R U . . .
C7 C 1.0547(5) 0.7482(5) 0.95556(19) 0.112(2) Uani 1 1 d . . . . .
H7A H 1.097054 0.809572 0.961786 0.168 Uiso 1 1 calc R U . . .
H7B H 1.099202 0.700092 0.954110 0.168 Uiso 1 1 calc R U . . .
H7C H 1.018898 0.743870 0.980157 0.168 Uiso 1 1 calc R U . . .
O1 O 0.55248(18) 0.36705(17) 0.74469(8) 0.0400(6) Uani 1 1 d . . . . .
P1 P 0.54463(7) 0.28881(6) 0.77315(3) 0.0349(2) Uani 1 1 d . . . . .
C8 C 0.4413(3) 0.3054(2) 0.80494(11) 0.0360(8) Uani 1 1 d . . . . .
C9 C 0.3770(3) 0.2227(3) 0.80642(11) 0.0370(8) Uani 1 1 d . . . . .
C10 C 0.3026(3) 0.2254(3) 0.83250(12) 0.0434(9) Uani 1 1 d . . . . .
H10 H 0.263043 0.168995 0.834074 0.052 Uiso 1 1 calc R U . . .
C11 C 0.2857(3) 0.3084(3) 0.85588(13) 0.0459(9) Uani 1 1 d . . . . .
H11 H 0.236661 0.309810 0.874195 0.055 Uiso 1 1 calc R U . . .
C12 C 0.3421(3) 0.3893(3) 0.85194(12) 0.0439(9) Uani 1 1 d . . . . .
H12 H 0.328584 0.446866 0.866743 0.053 Uiso 1 1 calc R U . . .
C13 C 0.4181(3) 0.3901(2) 0.82717(11) 0.0376(8) Uani 1 1 d . . . . .
C14 C 0.3714(3) 0.1300(2) 0.77660(12) 0.0373(8) Uani 1 1 d . . . . .
C15 C 0.4083(3) 0.0550(3) 0.79437(13) 0.0428(9) Uani 1 1 d . . . . .
C16 C 0.3884(3) -0.0315(3) 0.76645(14) 0.0482(10) Uani 1 1 d . . . . .
H16 H 0.413928 -0.081621 0.778823 0.058 Uiso 1 1 calc R U . . .
C17 C 0.3329(3) -0.0491(3) 0.72108(15) 0.0491(10) Uani 1 1 d . . . . .
C18 C 0.2942(3) 0.0245(3) 0.70431(13) 0.0465(9) Uani 1 1 d . . . . .
H18 H 0.255427 0.014425 0.673387 0.056 Uiso 1 1 calc R U . . .
C19 C 0.3108(3) 0.1129(3) 0.73155(12) 0.0399(8) Uani 1 1 d . . . . .
C20 C 0.4712(3) 0.0691(3) 0.84288(14) 0.0547(11) Uani 1 1 d . . . . .
H20A H 0.497024 0.011417 0.848153 0.082 Uiso 1 1 calc R U . . .
H20B H 0.427838 0.086090 0.864126 0.082 Uiso 1 1 calc R U . . .
H20C H 0.529723 0.118870 0.848032 0.082 Uiso 1 1 calc R U . . .
C21 C 0.3156(4) -0.1447(3) 0.69115(17) 0.0671(13) Uani 1 1 d . . . . .
H21A H 0.258261 -0.149045 0.664335 0.101 Uiso 1 1 calc R U . . .
H21B H 0.298679 -0.191559 0.708733 0.101 Uiso 1 1 calc R U . . .
H21C H 0.378535 -0.155351 0.680984 0.101 Uiso 1 1 calc R U . . .
C22 C 0.2607(3) 0.1890(3) 0.71275(13) 0.0510(10) Uani 1 1 d . . . . .
H22A H 0.213904 0.210841 0.731425 0.076 Uiso 1 1 calc R U . . .
H22B H 0.221491 0.165057 0.680986 0.076 Uiso 1 1 calc R U . . .
H22C H 0.314249 0.240670 0.713609 0.076 Uiso 1 1 calc R U . . .
C23 C 0.4583(3) 0.4860(2) 0.82258(12) 0.0399(9) Uani 1 1 d . . . . .
C24 C 0.4139(3) 0.5182(3) 0.78274(13) 0.0431(9) Uani 1 1 d . . . . .
C25 C 0.4406(3) 0.6101(3) 0.78076(15) 0.0527(11) Uani 1 1 d . . . . .
H25 H 0.409633 0.631579 0.754097 0.063 Uiso 1 1 calc R U . . .
C26 C 0.5109(4) 0.6725(3) 0.81619(16) 0.0550(11) Uani 1 1 d . . . . .
C27 C 0.5513(3) 0.6405(3) 0.85528(14) 0.0499(10) Uani 1 1 d . . . . .
H27 H 0.598486 0.682436 0.880082 0.060 Uiso 1 1 calc R U . . .
C28 C 0.5258(3) 0.5493(3) 0.85987(13) 0.0435(9) Uani 1 1 d . . . . .
C29 C 0.5707(3) 0.5195(3) 0.90319(13) 0.0510(10) Uani 1 1 d . . . . .
H29A H 0.619462 0.571150 0.924103 0.076 Uiso 1 1 calc R U . . .
H29B H 0.607072 0.466843 0.896407 0.076 Uiso 1 1 calc R U . . .
H29C H 0.515183 0.500712 0.917637 0.076 Uiso 1 1 calc R U . . .
C30 C 0.3377(3) 0.4544(3) 0.74406(14) 0.0502(10) Uani 1 1 d . . . . .
H30A H 0.302932 0.490615 0.722899 0.075 Uiso 1 1 calc R U . . .
H30B H 0.286391 0.419835 0.756031 0.075 Uiso 1 1 calc R U . . .
H30C H 0.373632 0.410826 0.727732 0.075 Uiso 1 1 calc R U . . .
C31 C 0.5410(4) 0.7724(3) 0.81284(19) 0.0761(15) Uani 1 1 d . . . . .
H31A H 0.496465 0.811185 0.826438 0.114 Uiso 1 1 calc R U . . .
H31B H 0.532698 0.776717 0.780519 0.114 Uiso 1 1 calc R U . . .
H31C H 0.613290 0.794042 0.829399 0.114 Uiso 1 1 calc R U . . .
N3 N 0.5071(3) 0.1457(2) 0.62309(11) 0.0525(9) Uani 1 1 d . . . . .
N4 N 0.6280(3) 0.1727(2) 0.59097(11) 0.0477(8) Uani 1 1 d . . . . .
C32 C 0.5786(3) 0.2155(3) 0.62136(14) 0.0501(10) Uani 1 1 d . . . . .
C33 C 0.5132(4) 0.0613(3) 0.59614(15) 0.0582(11) Uani 1 1 d . . . . .
C34 C 0.5902(4) 0.0791(3) 0.57577(15) 0.0561(11) Uani 1 1 d . . . . .
C35 C 0.7081(4) 0.2218(3) 0.57497(16) 0.0646(12) Uani 1 1 d . . . . .
H35A H 0.769403 0.190774 0.579491 0.097 Uiso 1 1 calc R U . . .
H35B H 0.726214 0.285875 0.592316 0.097 Uiso 1 1 calc R U . . .
H35C H 0.683157 0.221923 0.542269 0.097 Uiso 1 1 calc R U . . .
C36 C 0.4312(4) 0.1588(4) 0.65032(16) 0.0735(14) Uani 1 1 d . . . . .
H36A H 0.434734 0.114729 0.671104 0.110 Uiso 1 1 calc R U . . .
H36B H 0.361777 0.148173 0.629899 0.110 Uiso 1 1 calc R U . . .
H36C H 0.445881 0.222403 0.668289 0.110 Uiso 1 1 calc R U . . .
C37 C 0.4430(5) -0.0261(4) 0.5943(2) 0.0921(18) Uani 1 1 d . . . . .
H37A H 0.465034 -0.078751 0.576644 0.138 Uiso 1 1 calc R U . . .
H37B H 0.371906 -0.020820 0.579388 0.138 Uiso 1 1 calc R U . . .
H37C H 0.445936 -0.036146 0.625493 0.138 Uiso 1 1 calc R U . . .
C38 C 0.6322(4) 0.0161(4) 0.54265(18) 0.0823(16) Uani 1 1 d . . . . .
H38A H 0.592962 -0.046638 0.536205 0.123 Uiso 1 1 calc R U . . .
H38B H 0.705207 0.014422 0.556074 0.123 Uiso 1 1 calc R U . . .
H38C H 0.625991 0.039424 0.514041 0.123 Uiso 1 1 calc R U . . .
O2 O 0.76871(18) 0.37084(17) 0.80109(8) 0.0406(6) Uani 1 1 d . . . . .
P2 P 0.69483(7) 0.34699(6) 0.83222(3) 0.0366(2) Uani 1 1 d . . . . .
C39 C 0.7219(3) 0.2360(2) 0.85194(12) 0.0384(8) Uani 1 1 d . . . . .
C40 C 0.7191(3) 0.2339(3) 0.89822(12) 0.0402(8) Uani 1 1 d . . . . .
C41 C 0.7285(3) 0.1524(3) 0.91539(13) 0.0483(10) Uani 1 1 d . . . . .
H41 H 0.722094 0.151289 0.945778 0.058 Uiso 1 1 calc R U . . .
C42 C 0.7465(3) 0.0747(3) 0.88925(14) 0.0555(11) Uani 1 1 d . . . . .
H42 H 0.751542 0.019249 0.900940 0.067 Uiso 1 1 calc R U . . .
C43 C 0.7574(3) 0.0777(3) 0.84527(14) 0.0510(10) Uani 1 1 d . . . . .
H43 H 0.772183 0.024144 0.827321 0.061 Uiso 1 1 calc R U . . .
C44 C 0.7474(3) 0.1567(2) 0.82662(12) 0.0392(8) Uani 1 1 d . . . . .
C45 C 0.7198(3) 0.3190(3) 0.93361(12) 0.0432(9) Uani 1 1 d . . . . .
C46 C 0.8130(3) 0.3760(3) 0.95325(13) 0.0496(10) Uani 1 1 d . . . . .
C47 C 0.8176(4) 0.4526(3) 0.98757(13) 0.0587(12) Uani 1 1 d . . . . .
H47 H 0.882071 0.491755 1.000721 0.070 Uiso 1 1 calc R U . . .
C48 C 0.7323(4) 0.4739(3) 1.00325(13) 0.0586(12) Uani 1 1 d . . . . .
C49 C 0.6408(4) 0.4112(3) 0.98514(13) 0.0574(11) Uani 1 1 d . . . . .
H49 H 0.582031 0.421685 0.996850 0.069 Uiso 1 1 calc R U . . .
C50 C 0.6322(3) 0.3339(3) 0.95053(13) 0.0494(10) Uani 1 1 d . . . . .
C51 C 0.9089(3) 0.3571(3) 0.93751(15) 0.0628(12) Uani 1 1 d . . . . .
H51A H 0.915121 0.291211 0.935720 0.094 Uiso 1 1 calc R U . . .
H51B H 0.969736 0.395116 0.959404 0.094 Uiso 1 1 calc R U . . .
H51C H 0.904405 0.372609 0.907163 0.094 Uiso 1 1 calc R U . . .
C52 C 0.5310(3) 0.2734(3) 0.93108(14) 0.0597(11) Uani 1 1 d . . . . .
H52A H 0.480765 0.294315 0.948080 0.090 Uiso 1 1 calc R U . . .
H52B H 0.538551 0.209156 0.933575 0.090 Uiso 1 1 calc R U . . .
H52C H 0.506572 0.276646 0.898714 0.090 Uiso 1 1 calc R U . . .
C53 C 0.7350(5) 0.5617(3) 1.03609(15) 0.0799(16) Uani 1 1 d . . . . .
H53A H 0.801235 0.575884 1.059022 0.120 Uiso 1 1 calc R U . . .
H53B H 0.678361 0.554258 1.051481 0.120 Uiso 1 1 calc R U . . .
H53C H 0.727152 0.612593 1.019365 0.120 Uiso 1 1 calc R U . . .
C54 C 0.7770(3) 0.1489(2) 0.78124(13) 0.0404(9) Uani 1 1 d . . . . .
C55 C 0.7112(3) 0.0944(2) 0.74089(13) 0.0420(9) Uani 1 1 d . . . . .
C56 C 0.7476(3) 0.0796(3) 0.70102(13) 0.0459(9) Uani 1 1 d . . . . .
H56 H 0.702839 0.043758 0.673552 0.055 Uiso 1 1 calc R U . . .
C57 C 0.8475(3) 0.1156(3) 0.70037(14) 0.0467(10) Uani 1 1 d . . . . .
C58 C 0.9097(3) 0.1679(3) 0.74012(15) 0.0497(10) Uani 1 1 d . . . . .
H58 H 0.977978 0.193183 0.739980 0.060 Uiso 1 1 calc R U . . .
C59 C 0.8778(3) 0.1860(3) 0.78093(14) 0.0447(9) Uani 1 1 d . . . . .
C60 C 0.6047(3) 0.0504(3) 0.73981(14) 0.0493(10) Uani 1 1 d . . . . .
H60A H 0.608262 0.010718 0.762656 0.074 Uiso 1 1 calc R U . . .
H60B H 0.572690 0.012814 0.709207 0.074 Uiso 1 1 calc R U . . .
H60C H 0.563065 0.098911 0.746849 0.074 Uiso 1 1 calc R U . . .
C61 C 0.8863(4) 0.0922(3) 0.65737(15) 0.0620(12) Uani 1 1 d . . . . .
H61A H 0.927978 0.147516 0.653167 0.093 Uiso 1 1 calc R U . . .
H61B H 0.827323 0.071085 0.630791 0.093 Uiso 1 1 calc R U . . .
H61C H 0.928878 0.042772 0.660304 0.093 Uiso 1 1 calc R U . . .
C62 C 0.9517(3) 0.2415(3) 0.82375(14) 0.0533(10) Uani 1 1 d . . . . .
H62A H 1.022237 0.246282 0.819378 0.080 Uiso 1 1 calc R U . . .
H62B H 0.947669 0.210693 0.849541 0.080 Uiso 1 1 calc R U . . .
H62C H 0.933330 0.303886 0.830283 0.080 Uiso 1 1 calc R U . . .
O3 O 0.70259(18) 0.57576(16) 0.71025(8) 0.0388(6) Uani 1 1 d . . . . .
P3 P 0.78711(7) 0.61707(6) 0.68751(3) 0.0340(2) Uani 1 1 d . . . . .
C63 C 0.7239(3) 0.6693(2) 0.63832(11) 0.0339(8) Uani 1 1 d . . . . .
C64 C 0.6288(3) 0.6335(2) 0.60564(11) 0.0346(8) Uani 1 1 d . . . . .
C65 C 0.5984(3) 0.6760(3) 0.56838(12) 0.0415(9) Uani 1 1 d . . . . .
H65 H 0.535585 0.650576 0.546252 0.050 Uiso 1 1 calc R U . . .
C66 C 0.6575(3) 0.7544(3) 0.56286(13) 0.0454(9) Uani 1 1 d . . . . .
H66 H 0.638050 0.779987 0.536224 0.054 Uiso 1 1 calc R U . . .
C67 C 0.7442(3) 0.7945(2) 0.59626(12) 0.0404(9) Uani 1 1 d . . . . .
H67 H 0.782494 0.850565 0.593610 0.048 Uiso 1 1 calc R U . . .
C68 C 0.7774(3) 0.7547(2) 0.63410(12) 0.0363(8) Uani 1 1 d . . . . .
C69 C 0.8622(3) 0.8148(2) 0.67106(12) 0.0357(8) Uani 1 1 d . . . . .
C70 C 0.8365(3) 0.8663(2) 0.70881(12) 0.0383(8) Uani 1 1 d . . . . .
C71 C 0.9130(3) 0.9298(2) 0.74104(13) 0.0404(8) Uani 1 1 d . . . . .
H71 H 0.895284 0.963828 0.766863 0.048 Uiso 1 1 calc R U . . .
C72 C 1.0134(3) 0.9452(2) 0.73692(13) 0.0419(9) Uani 1 1 d . . . . .
C73 C 1.0369(3) 0.8961(2) 0.69883(13) 0.0431(9) Uani 1 1 d . . . . .
H73 H 1.105561 0.906798 0.695093 0.052 Uiso 1 1 calc R U . . .
C74 C 0.9635(3) 0.8313(2) 0.66562(13) 0.0402(8) Uani 1 1 d . . . . .
C75 C 0.7275(3) 0.8536(3) 0.71427(13) 0.0430(9) Uani 1 1 d . . . . .
H75A H 0.722287 0.898008 0.741155 0.064 Uiso 1 1 calc R U . . .
H75B H 0.708467 0.790177 0.718444 0.064 Uiso 1 1 calc R U . . .
H75C H 0.680552 0.864297 0.686783 0.064 Uiso 1 1 calc R U . . .
C76 C 1.0955(3) 1.0135(3) 0.77349(14) 0.0540(10) Uani 1 1 d . . . . .
H76A H 1.158591 0.985614 0.780621 0.081 Uiso 1 1 calc R U . . .
H76B H 1.070112 1.028379 0.801286 0.081 Uiso 1 1 calc R U . . .
H76C H 1.110843 1.070433 0.762125 0.081 Uiso 1 1 calc R U . . .
C77 C 0.9953(3) 0.7776(3) 0.62547(13) 0.0495(10) Uani 1 1 d . . . . .
H77A H 1.069736 0.794798 0.628881 0.074 Uiso 1 1 calc R U . . .
H77B H 0.957314 0.792239 0.596875 0.074 Uiso 1 1 calc R U . . .
H77C H 0.979439 0.710844 0.624590 0.074 Uiso 1 1 calc R U . . .
C78 C 0.5474(3) 0.5584(2) 0.60815(11) 0.0339(8) Uani 1 1 d . . . . .
C79 C 0.4816(3) 0.5791(3) 0.63766(12) 0.0391(8) Uani 1 1 d . . . . .
C80 C 0.3967(3) 0.5144(3) 0.63572(13) 0.0431(9) Uani 1 1 d . . . . .
H80 H 0.353436 0.528510 0.656037 0.052 Uiso 1 1 calc R U . . .
C81 C 0.3729(3) 0.4303(3) 0.60531(13) 0.0425(9) Uani 1 1 d . . . . .
C82 C 0.4379(3) 0.4099(3) 0.57600(12) 0.0415(9) Uani 1 1 d . . . . .
H82 H 0.422812 0.352048 0.555022 0.050 Uiso 1 1 calc R U . . .
C83 C 0.5237(3) 0.4722(2) 0.57684(11) 0.0348(8) Uani 1 1 d . . . . .
C84 C 0.5014(3) 0.6702(3) 0.67072(13) 0.0461(9) Uani 1 1 d . . . . .
H84A H 0.439300 0.679418 0.681920 0.069 Uiso 1 1 calc R U . . .
H84B H 0.518614 0.720636 0.655171 0.069 Uiso 1 1 calc R U . . .
H84C H 0.559183 0.670146 0.696680 0.069 Uiso 1 1 calc R U . . .
C85 C 0.2779(3) 0.3620(3) 0.60341(16) 0.0636(12) Uani 1 1 d . . . . .
H85A H 0.279191 0.350014 0.634202 0.095 Uiso 1 1 calc R U . . .
H85B H 0.277730 0.303657 0.582595 0.095 Uiso 1 1 calc R U . . .
H85C H 0.215538 0.388220 0.592204 0.095 Uiso 1 1 calc R U . . .
C86 C 0.5919(3) 0.4486(3) 0.54518(12) 0.0433(9) Uani 1 1 d . . . . .
H86A H 0.584728 0.488307 0.522282 0.065 Uiso 1 1 calc R U . . .
H86B H 0.571724 0.383350 0.529651 0.065 Uiso 1 1 calc R U . . .
H86C H 0.663989 0.458721 0.562807 0.065 Uiso 1 1 calc R U . . .
O4 O 0.82285(18) 0.42107(16) 0.68631(8) 0.0386(6) Uani 1 1 d . . . . .
P4 P 0.81784(7) 0.47754(6) 0.64699(3) 0.0339(2) Uani 1 1 d . . . . .
C87 C 0.9523(3) 0.5156(2) 0.64105(11) 0.0340(8) Uani 1 1 d . . . . .
C88 C 1.0421(3) 0.5512(2) 0.67709(12) 0.0367(8) Uani 1 1 d . . . . .
C89 C 1.1325(3) 0.5871(3) 0.66670(13) 0.0413(9) Uani 1 1 d . . . . .
H89 H 1.191630 0.612122 0.691044 0.050 Uiso 1 1 calc R U . . .
C90 C 1.1392(3) 0.5877(3) 0.62199(13) 0.0442(9) Uani 1 1 d . . . . .
H90 H 1.200866 0.615261 0.615843 0.053 Uiso 1 1 calc R U . . .
C91 C 1.0554(3) 0.5479(3) 0.58683(13) 0.0422(9) Uani 1 1 d . . . . .
H91 H 1.060289 0.545811 0.556022 0.051 Uiso 1 1 calc R U . . .
C92 C 0.9631(3) 0.5102(2) 0.59536(12) 0.0366(8) Uani 1 1 d . . . . .
C93 C 1.0542(3) 0.5455(3) 0.72670(12) 0.0379(8) Uani 1 1 d . . . . .
C94 C 1.0666(3) 0.4590(3) 0.73927(12) 0.0394(8) Uani 1 1 d . . . . .
C95 C 1.0895(3) 0.4547(3) 0.78545(14) 0.0481(10) Uani 1 1 d . . . . .
H95 H 1.098447 0.396551 0.793879 0.058 Uiso 1 1 calc R U . . .
C96 C 1.0998(3) 0.5316(3) 0.81949(13) 0.0482(10) Uani 1 1 d . . . . .
C97 C 1.0895(3) 0.6162(3) 0.80688(13) 0.0470(9) Uani 1 1 d . . . . .
H97 H 1.096421 0.669817 0.830053 0.056 Uiso 1 1 calc R U . . .
C98 C 1.0692(3) 0.6249(3) 0.76085(13) 0.0394(8) Uani 1 1 d . . . . .
C99 C 1.0576(3) 0.3723(3) 0.70343(13) 0.0467(9) Uani 1 1 d . . . . .
H99A H 1.085129 0.323505 0.718301 0.070 Uiso 1 1 calc R U . . .
H99B H 1.097008 0.386141 0.681125 0.070 Uiso 1 1 calc R U . . .
H99C H 0.984694 0.351221 0.687630 0.070 Uiso 1 1 calc R U . . .
C100 C 1.1193(4) 0.5228(4) 0.86949(14) 0.0688(14) Uani 1 1 d . . . . .
H10A H 1.103140 0.457390 0.871323 0.103 Uiso 1 1 calc R U . . .
H10B H 1.075305 0.559297 0.884708 0.103 Uiso 1 1 calc R U . . .
H10C H 1.192129 0.545944 0.884723 0.103 Uiso 1 1 calc R U . . .
C101 C 1.0635(3) 0.7188(3) 0.74963(13) 0.0471(9) Uani 1 1 d . . . . .
H10D H 1.071814 0.764675 0.777944 0.071 Uiso 1 1 calc R U . . .
H10E H 0.996141 0.718480 0.729035 0.071 Uiso 1 1 calc R U . . .
H10F H 1.118634 0.734976 0.734525 0.071 Uiso 1 1 calc R U . . .
C102 C 0.8862(3) 0.4535(2) 0.55396(12) 0.0362(8) Uani 1 1 d . . . . .
C103 C 0.8895(3) 0.3578(3) 0.54372(12) 0.0411(9) Uani 1 1 d . . . . .
C104 C 0.8267(3) 0.3038(3) 0.50383(13) 0.0427(9) Uani 1 1 d . . . . .
H104 H 0.830261 0.239333 0.497169 0.051 Uiso 1 1 calc R U . . .
C105 C 0.7582(3) 0.3408(3) 0.47304(12) 0.0398(8) Uani 1 1 d . . . . .
C106 C 0.7603(3) 0.4354(3) 0.48220(12) 0.0398(8) Uani 1 1 d . . . . .
H106 H 0.716920 0.462509 0.460726 0.048 Uiso 1 1 calc R U . . .
C107 C 0.8228(3) 0.4926(2) 0.52132(12) 0.0365(8) Uani 1 1 d . . . . .
C108 C 0.9602(3) 0.3133(3) 0.57639(15) 0.0558(11) Uani 1 1 d . . . . .
H10G H 1.031050 0.346227 0.582939 0.084 Uiso 1 1 calc R U . . .
H10H H 0.958081 0.248130 0.562442 0.084 Uiso 1 1 calc R U . . .
H10I H 0.937393 0.316614 0.605025 0.084 Uiso 1 1 calc R U . . .
C109 C 0.6845(3) 0.2783(3) 0.43181(13) 0.0544(11) Uani 1 1 d . . . . .
H10J H 0.721295 0.232702 0.417395 0.082 Uiso 1 1 calc R U . . .
H10K H 0.656594 0.315707 0.409715 0.082 Uiso 1 1 calc R U . . .
H10L H 0.627653 0.245943 0.441533 0.082 Uiso 1 1 calc R U . . .
C110 C 0.8229(3) 0.5958(3) 0.52930(13) 0.0486(10) Uani 1 1 d . . . . .
H11A H 0.890459 0.627335 0.528262 0.073 Uiso 1 1 calc R U . . .
H11B H 0.809512 0.616876 0.559448 0.073 Uiso 1 1 calc R U . . .
H11C H 0.768896 0.610327 0.505396 0.073 Uiso 1 1 calc R U . . .
K1 K 0.73247(6) 0.28641(5) 0.71556(3) 0.0413(2) Uani 1 1 d . . . . .
K2 K 0.65109(6) 0.53383(6) 0.78548(3) 0.0435(2) Uani 1 1 d . . . . .
K3 K 0.87003(6) 0.50537(6) 0.77225(3) 0.0419(2) Uani 1 1 d . . . . .
K4 K 0.58777(6) 0.41445(5) 0.66919(3) 0.0397(2) Uani 1 1 d . . . . .
C111 C 1.3236(4) 0.7438(5) 0.8754(2) 0.151(3) Uani 1 1 d G U . . .
H111 H 1.320803 0.689735 0.853008 0.181 Uiso 1 1 calc R U . . .
C112 C 1.3484(5) 0.7405(4) 0.9217(3) 0.163(3) Uani 1 1 d G U . . .
H112 H 1.362449 0.684118 0.931109 0.196 Uiso 1 1 calc R U . . .
C113 C 1.3525(5) 0.8196(6) 0.95445(17) 0.180(3) Uani 1 1 d G U . . .
H113 H 1.369369 0.817274 0.986156 0.216 Uiso 1 1 calc R U . . .
C114 C 1.3318(5) 0.9020(5) 0.9408(3) 0.194(3) Uani 1 1 d G U . . .
H114 H 1.334641 0.956048 0.963103 0.233 Uiso 1 1 calc R U . . .
C115 C 1.3071(5) 0.9053(5) 0.8944(3) 0.172(3) Uani 1 1 d G U . . .
H115 H 1.292993 0.961667 0.885003 0.206 Uiso 1 1 calc R U . . .
C116 C 1.3030(4) 0.8262(6) 0.86166(18) 0.153(3) Uani 1 1 d G U . . .
H116 H 1.286074 0.828512 0.829955 0.184 Uiso 1 1 calc R U . . .
C117 C 0.0960(6) 0.0981(6) 0.5824(2) 0.114(2) Uani 1 1 d . . . . .
H117 H 0.079740 0.143247 0.604761 0.136 Uiso 1 1 calc R U . . .
C118 C 0.0898(5) 0.0075(6) 0.5871(2) 0.108(2) Uani 1 1 d . . . . .
H118 H 0.068464 -0.010739 0.612557 0.130 Uiso 1 1 calc R U . . .
C119 C 0.1142(5) -0.0558(5) 0.5554(2) 0.102(2) Uani 1 1 d . . . . .
H119 H 0.109269 -0.118866 0.558587 0.123 Uiso 1 1 calc R U . . .
C120 C 0.1459(6) -0.0312(4) 0.5188(3) 0.112(2) Uani 1 1 d . . . . .
H120 H 0.162911 -0.076877 0.496874 0.134 Uiso 1 1 calc R U . . .
C121 C 0.1533(5) 0.0600(5) 0.5138(3) 0.112(2) Uani 1 1 d . . . . .
H121 H 0.177086 0.078436 0.488953 0.135 Uiso 1 1 calc R U . . .
C122 C 0.1254(5) 0.1238(5) 0.5455(3) 0.112(2) Uani 1 1 d . . . . .
H122 H 0.126610 0.186316 0.541671 0.134 Uiso 1 1 calc R U . . .
C123 C 0.7364(8) 0.8312(6) 1.0468(3) 0.225(4) Uani 1 1 d G U . . .
H123 H 0.694757 0.813415 1.066496 0.270 Uiso 1 1 calc R U . . .
C124 C 0.8424(9) 0.8580(6) 1.0638(2) 0.222(4) Uani 1 1 d G U . . .
H124 H 0.873332 0.858554 1.095051 0.266 Uiso 1 1 calc R U . . .
C125 C 0.9033(5) 0.8840(6) 1.0351(4) 0.241(4) Uani 1 1 d G U . . .
H125 H 0.975829 0.902302 1.046648 0.289 Uiso 1 1 calc R U . . .
C126 C 0.8581(8) 0.8832(6) 0.9893(4) 0.258(4) Uani 1 1 d G U . . .
H126 H 0.899752 0.900912 0.969690 0.310 Uiso 1 1 calc R U . . .
C127 C 0.7521(9) 0.8563(7) 0.9724(2) 0.257(4) Uani 1 1 d G U . . .
H127 H 0.721177 0.855774 0.941133 0.308 Uiso 1 1 calc R U . . .
C128 C 0.6912(6) 0.8304(6) 1.0011(4) 0.241(4) Uani 1 1 d G U . . .
H128 H 0.618678 0.812026 0.989536 0.289 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C1 1.366(5) . ?
N1 C3 1.406(6) . ?
N1 C4 1.444(5) . ?
N1 K2 4.145(4) . ?
N1 K3 3.865(4) . ?
N2 C1 1.360(5) . ?
N2 C2 1.395(5) . ?
N2 C5 1.437(5) . ?
N2 K2 3.950(4) . ?
N2 K3 3.747(4) . ?
C1 K2 3.052(5) . ?
C1 K3 3.097(5) . ?
C2 C3 1.337(6) . ?
C2 C6 1.500(7) . ?
C3 C7 1.491(6) . ?
C4 K3 4.338(5) . ?
C5 K2 4.004(5) . ?
C5 K3 4.030(5) . ?
O1 P1 1.565(2) . ?
O1 K1 3.041(3) . ?
O1 K2 2.626(3) . ?
O1 K4 2.634(2) . ?
P1 C8 1.870(4) . ?
P1 P2 2.3559(16) . ?
P1 K1 3.3660(15) . ?
P1 K2 3.6665(16) . ?
P1 K4 4.0412(15) . ?
C8 C9 1.427(5) . ?
C8 C13 1.420(5) . ?
C8 K2 4.350(4) . ?
C9 C10 1.403(5) . ?
C9 C14 1.496(5) . ?
C10 C11 1.379(5) . ?
C11 C12 1.378(5) . ?
C12 C13 1.393(5) . ?
C13 C23 1.499(5) . ?
C13 K2 4.124(4) . ?
C14 C15 1.405(5) . ?
C14 C19 1.400(5) . ?
C15 C16 1.374(5) . ?
C15 C20 1.501(5) . ?
C16 C17 1.386(5) . ?
C17 C18 1.382(5) . ?
C17 C21 1.511(6) . ?
C18 C19 1.392(5) . ?
C19 C22 1.504(5) . ?
C23 C24 1.414(5) . ?
C23 C28 1.410(5) . ?
C23 K2 3.094(4) . ?
C24 C25 1.380(5) . ?
C24 C30 1.486(5) . ?
C24 K2 3.144(4) . ?
C25 C26 1.390(6) . ?
C25 K2 3.139(4) . ?
C26 C27 1.379(6) . ?
C26 C31 1.513(6) . ?
C26 K2 3.098(4) . ?
C27 C28 1.391(5) . ?
C27 K2 3.062(4) . ?
C28 C29 1.486(5) . ?
C28 K2 3.093(4) . ?
C29 K2 3.991(4) . ?
C30 K2 4.088(4) . ?
C31 K2 4.004(5) . ?
N3 C32 1.343(5) . ?
N3 C33 1.395(6) . ?
N3 C36 1.455(5) . ?
N3 K1 3.783(4) . ?
N3 K4 3.927(4) . ?
N4 C32 1.363(5) . ?
N4 C34 1.382(5) . ?
N4 C35 1.445(5) . ?
N4 K1 3.769(4) . ?
N4 K4 4.107(4) . ?
C32 K1 3.086(4) . ?
C32 K4 3.031(4) . ?
C33 C34 1.338(6) . ?
C33 C37 1.496(6) . ?
C34 C38 1.500(6) . ?
C35 K1 4.159(5) . ?
C36 K1 4.167(5) . ?
C36 K4 3.997(5) . ?
O2 P2 1.563(3) . ?
O2 K1 2.608(3) . ?
O2 K2 3.071(3) . ?
O2 K3 2.658(2) . ?
P2 C39 1.885(3) . ?
P2 K1 3.6720(15) . ?
P2 K2 3.3649(14) . ?
P2 K3 4.0481(17) . ?
C39 C40 1.423(5) . ?
C39 C44 1.410(5) . ?
C40 C41 1.400(5) . ?
C40 C45 1.510(5) . ?
C41 C42 1.360(6) . ?
C42 C43 1.386(5) . ?
C43 C44 1.388(5) . ?
C44 C54 1.508(5) . ?
C44 K1 4.138(3) . ?
C45 C46 1.378(6) . ?
C45 C50 1.406(6) . ?
C46 C47 1.392(6) . ?
C46 C51 1.505(6) . ?
C47 C48 1.379(6) . ?
C48 C49 1.395(6) . ?
C48 C53 1.491(6) . ?
C49 C50 1.394(6) . ?
C50 C52 1.481(6) . ?
C54 C55 1.405(5) . ?
C54 C59 1.402(5) . ?
C54 K1 3.101(3) . ?
C55 C56 1.397(5) . ?
C55 C60 1.492(5) . ?
C55 K1 3.062(3) . ?
C56 C57 1.389(6) . ?
C56 K1 3.052(4) . ?
C57 C58 1.364(6) . ?
C57 C61 1.513(5) . ?
C57 K1 3.124(4) . ?
C58 C59 1.394(5) . ?
C58 K1 3.144(4) . ?
C59 C62 1.501(6) . ?
C59 K1 3.151(4) . ?
C60 K1 3.964(4) . ?
C61 K1 4.104(5) . ?
C62 K1 4.112(4) . ?
O3 P3 1.569(2) . ?
O3 K2 2.678(2) . ?
O3 K3 3.006(3) . ?
O3 K4 2.638(3) . ?
P3 C63 1.882(3) . ?
P3 P4 2.3458(15) . ?
P3 K2 4.1014(16) . ?
P3 K3 3.3500(15) . ?
P3 K4 3.6624(18) . ?
C63 C64 1.420(5) . ?
C63 C68 1.420(5) . ?
C63 K4 4.335(4) . ?
C64 C65 1.395(4) . ?
C64 C78 1.490(5) . ?
C64 K4 4.086(3) . ?
C65 C66 1.383(5) . ?
C66 C67 1.366(5) . ?
C67 C68 1.391(4) . ?
C68 C69 1.494(5) . ?
C69 C70 1.399(5) . ?
C69 C74 1.403(5) . ?
C70 C71 1.390(5) . ?
C70 C75 1.501(5) . ?
C71 C72 1.376(5) . ?
C72 C73 1.378(5) . ?
C72 C76 1.520(5) . ?
C73 C74 1.393(5) . ?
C74 C77 1.510(5) . ?
C78 C79 1.411(5) . ?
C78 C83 1.415(5) . ?
C78 K4 3.071(3) . ?
C79 C80 1.385(5) . ?
C79 C84 1.499(5) . ?
C79 K4 3.138(3) . ?
C80 C81 1.379(5) . ?
C80 K4 3.164(4) . ?
C81 C82 1.397(5) . ?
C81 C85 1.517(5) . ?
C81 K4 3.164(4) . ?
C82 C83 1.383(5) . ?
C82 K4 3.087(4) . ?
C83 C86 1.492(5) . ?
C83 K4 3.050(3) . ?
C84 K4 4.073(4) . ?
C85 K4 4.125(5) . ?
C86 K4 3.904(4) . ?
O4 P4 1.565(2) . ?
O4 K1 2.597(2) . ?
O4 K3 2.610(3) . ?
O4 K4 3.068(3) . ?
P4 C87 1.883(4) . ?
P4 K1 3.9925(15) . ?
P4 K3 3.6685(15) . ?
P4 K4 3.3625(15) . ?
C87 C88 1.422(5) . ?
C87 C92 1.420(5) . ?
C88 C89 1.388(5) . ?
C88 C93 1.502(5) . ?
C88 K3 4.169(4) . ?
C89 C90 1.385(5) . ?
C90 C91 1.368(5) . ?
C91 C92 1.393(5) . ?
C92 C102 1.497(5) . ?
C93 C94 1.412(5) . ?
C93 C98 1.395(5) . ?
C93 K3 3.131(4) . ?
C94 C95 1.387(5) . ?
C94 C99 1.511(5) . ?
C94 K3 3.121(4) . ?
C95 C96 1.376(6) . ?
C95 K3 3.077(4) . ?
C96 C97 1.381(5) . ?
C96 C100 1.518(5) . ?
C96 K3 3.054(4) . ?
C97 C98 1.399(5) . ?
C97 K3 3.073(4) . ?
C98 C101 1.490(5) . ?
C98 K3 3.149(4) . ?
C99 K3 4.073(4) . ?
C100 K3 3.907(5) . ?
C101 K3 4.100(4) . ?
C102 C103 1.405(5) . ?
C102 C107 1.408(5) . ?
C103 C104 1.378(5) . ?
C103 C108 1.507(5) . ?
C104 C105 1.390(5) . ?
C105 C106 1.375(5) . ?
C105 C109 1.508(5) . ?
C106 C107 1.381(5) . ?
C107 C110 1.503(5) . ?
C111 C112 1.3900 . ?
C111 C116 1.3900 . ?
C112 C113 1.3900 . ?
C113 C114 1.3900 . ?
C114 C115 1.3900 . ?
C115 C116 1.3900 . ?
C117 C118 1.366(9) . ?
C117 C122 1.365(9) . ?
C118 C119 1.349(8) . ?
C119 C120 1.363(8) . ?
C120 C121 1.378(8) . ?
C121 C122 1.374(9) . ?
C123 C124 1.3900 . ?
C123 C128 1.3900 . ?
C124 C125 1.3900 . ?
C125 C126 1.3900 . ?
C126 C127 1.3900 . ?
C127 C128 1.3900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 N1 C3 113.1(4) . . ?
C1 N1 C4 122.7(4) . . ?
C1 N1 K2 30.8(2) . . ?
C1 N1 K3 46.9(2) . . ?
C3 N1 C4 124.0(4) . . ?
C3 N1 K2 143.6(3) . . ?
C3 N1 K3 123.1(3) . . ?
C4 N1 K2 91.9(3) . . ?
C4 N1 K3 99.2(3) . . ?
K3 N1 K2 45.57(5) . . ?
C1 N2 C2 113.7(3) . . ?
C1 N2 C5 122.4(4) . . ?
C1 N2 K2 40.8(2) . . ?
C1 N2 K3 51.8(2) . . ?
C2 N2 C5 123.9(4) . . ?
C2 N2 K2 154.1(3) . . ?
C2 N2 K3 127.2(3) . . ?
C5 N2 K2 81.7(3) . . ?
C5 N2 K3 90.7(2) . . ?
K3 N2 K2 47.61(5) . . ?
N1 C1 K2 136.0(3) . . ?
N1 C1 K3 114.3(3) . . ?
N2 C1 N1 101.2(4) . . ?
N2 C1 K2 122.3(3) . . ?
N2 C1 K3 108.0(3) . . ?
K2 C1 K3 60.82(9) . . ?
N2 C2 C6 122.2(4) . . ?
C3 C2 N2 106.1(4) . . ?
C3 C2 C6 131.7(5) . . ?
N1 C3 C7 123.2(5) . . ?
C2 C3 N1 105.8(4) . . ?
C2 C3 C7 131.0(5) . . ?
N1 C4 K3 61.6(2) . . ?
N2 C5 K2 77.5(2) . . ?
N2 C5 K3 68.4(2) . . ?
K2 C5 K3 45.59(6) . . ?
P1 O1 K1 87.78(10) . . ?
P1 O1 K2 119.94(13) . . ?
P1 O1 K4 147.40(14) . . ?
K2 O1 K1 98.08(8) . . ?
K2 O1 K4 85.03(8) . . ?
K4 O1 K1 66.80(6) . . ?
O1 P1 C8 109.11(14) . . ?
O1 P1 P2 97.98(11) . . ?
O1 P1 K1 64.54(9) . . ?
O1 P1 K2 38.35(10) . . ?
O1 P1 K4 20.56(9) . . ?
C8 P1 P2 101.21(12) . . ?
C8 P1 K1 173.08(11) . . ?
C8 P1 K2 98.31(12) . . ?
C8 P1 K4 125.42(10) . . ?
P2 P1 K1 77.63(4) . . ?
P2 P1 K2 63.64(5) . . ?
P2 P1 K4 104.33(5) . . ?
K1 P1 K2 75.01(4) . . ?
K1 P1 K4 49.18(3) . . ?
K2 P1 K4 54.66(3) . . ?
P1 C8 K2 56.52(10) . . ?
C9 C8 P1 115.8(3) . . ?
C9 C8 K2 172.1(2) . . ?
C13 C8 P1 128.0(3) . . ?
C13 C8 C9 116.2(3) . . ?
C13 C8 K2 71.4(2) . . ?
C8 C9 C14 124.6(3) . . ?
C10 C9 C8 121.1(3) . . ?
C10 C9 C14 113.8(3) . . ?
C11 C10 C9 121.2(4) . . ?
C12 C11 C10 118.2(4) . . ?
C11 C12 C13 122.8(4) . . ?
C8 C13 C23 126.5(3) . . ?
C8 C13 K2 89.5(2) . . ?
C12 C13 C8 120.3(3) . . ?
C12 C13 C23 112.8(3) . . ?
C12 C13 K2 150.1(3) . . ?
C23 C13 K2 38.47(17) . . ?
C15 C14 C9 122.2(3) . . ?
C19 C14 C9 118.1(3) . . ?
C19 C14 C15 118.6(3) . . ?
C14 C15 C20 120.7(3) . . ?
C16 C15 C14 119.3(3) . . ?
C16 C15 C20 120.0(3) . . ?
C15 C16 C17 123.0(4) . . ?
C16 C17 C21 121.3(4) . . ?
C18 C17 C16 117.3(4) . . ?
C18 C17 C21 121.4(4) . . ?
C17 C18 C19 121.7(4) . . ?
C14 C19 C22 120.4(3) . . ?
C18 C19 C14 120.0(3) . . ?
C18 C19 C22 119.6(3) . . ?
C13 C23 K2 124.0(2) . . ?
C24 C23 C13 118.6(3) . . ?
C24 C23 K2 78.9(2) . . ?
C28 C23 C13 121.3(3) . . ?
C28 C23 C24 119.2(3) . . ?
C28 C23 K2 76.8(2) . . ?
C23 C24 C30 120.4(3) . . ?
C23 C24 K2 75.0(2) . . ?
C25 C24 C23 119.0(4) . . ?
C25 C24 C30 120.6(3) . . ?
C25 C24 K2 77.1(2) . . ?
C30 C24 K2 119.6(2) . . ?
C24 C25 C26 122.7(4) . . ?
C24 C25 K2 77.5(2) . . ?
C26 C25 K2 75.5(2) . . ?
C25 C26 C31 121.8(4) . . ?
C25 C26 K2 78.8(2) . . ?
C27 C26 C25 117.4(4) . . ?
C27 C26 C31 120.7(4) . . ?
C27 C26 K2 75.6(2) . . ?
C31 C26 K2 116.2(3) . . ?
C26 C27 C28 122.7(4) . . ?
C26 C27 K2 78.5(2) . . ?
C28 C27 K2 78.2(2) . . ?
C23 C28 C29 121.1(3) . . ?
C23 C28 K2 76.9(2) . . ?
C27 C28 C23 118.8(3) . . ?
C27 C28 C29 120.1(4) . . ?
C27 C28 K2 75.7(2) . . ?
C29 C28 K2 116.9(3) . . ?
C28 C29 K2 43.71(19) . . ?
C24 C30 K2 41.95(18) . . ?
C26 C31 K2 44.0(2) . . ?
C32 N3 C33 113.2(4) . . ?
C32 N3 C36 122.4(4) . . ?
C32 N3 K1 49.5(2) . . ?
C32 N3 K4 40.3(2) . . ?
C33 N3 C36 124.4(4) . . ?
C33 N3 K1 123.2(3) . . ?
C33 N3 K4 153.4(3) . . ?
C36 N3 K1 94.9(2) . . ?
C36 N3 K4 82.1(3) . . ?
K1 N3 K4 48.06(5) . . ?
C32 N4 C34 113.0(3) . . ?
C32 N4 C35 123.0(4) . . ?
C32 N4 K1 50.5(2) . . ?
C32 N4 K4 31.6(2) . . ?
C34 N4 C35 124.0(4) . . ?
C34 N4 K1 123.9(2) . . ?
C34 N4 K4 144.4(3) . . ?
C35 N4 K1 95.3(2) . . ?
C35 N4 K4 91.4(2) . . ?
K1 N4 K4 46.80(5) . . ?
N3 C32 N4 101.9(4) . . ?
N3 C32 K1 111.2(3) . . ?
N3 C32 K4 123.0(3) . . ?
N4 C32 K1 109.6(3) . . ?
N4 C32 K4 134.8(3) . . ?
K4 C32 K1 61.83(9) . . ?
N3 C33 C37 122.0(4) . . ?
C34 C33 N3 105.8(4) . . ?
C34 C33 C37 132.2(5) . . ?
N4 C34 C38 123.5(4) . . ?
C33 C34 N4 106.1(4) . . ?
C33 C34 C38 130.5(4) . . ?
N4 C35 K1 64.5(2) . . ?
N3 C36 K1 64.8(2) . . ?
N3 C36 K4 76.7(2) . . ?
K4 C36 K1 45.22(6) . . ?
P2 O2 K1 121.34(13) . . ?
P2 O2 K2 86.68(11) . . ?
P2 O2 K3 145.85(15) . . ?
K1 O2 K2 97.73(8) . . ?
K1 O2 K3 83.34(8) . . ?
K3 O2 K2 65.34(6) . . ?
P1 P2 K1 63.56(4) . . ?
P1 P2 K2 77.51(5) . . ?
P1 P2 K3 102.96(4) . . ?
O2 P2 P1 97.41(10) . . ?
O2 P2 C39 109.23(15) . . ?
O2 P2 K1 37.34(10) . . ?
O2 P2 K2 65.68(9) . . ?
O2 P2 K3 21.63(9) . . ?
C39 P2 P1 99.63(12) . . ?
C39 P2 K1 98.53(12) . . ?
C39 P2 K2 173.47(12) . . ?
C39 P2 K3 127.52(12) . . ?
K1 P2 K3 53.66(3) . . ?
K2 P2 K1 74.95(4) . . ?
K2 P2 K3 48.58(3) . . ?
C40 C39 P2 115.7(3) . . ?
C44 C39 P2 127.5(3) . . ?
C44 C39 C40 116.8(3) . . ?
C39 C40 C45 123.9(3) . . ?
C41 C40 C39 120.7(3) . . ?
C41 C40 C45 114.9(3) . . ?
C42 C41 C40 121.0(4) . . ?
C41 C42 C43 118.9(4) . . ?
C42 C43 C44 122.1(4) . . ?
C39 C44 C54 126.8(3) . . ?
C39 C44 K1 89.88(19) . . ?
C43 C44 C39 120.1(3) . . ?
C43 C44 C54 112.8(3) . . ?
C43 C44 K1 149.8(3) . . ?
C54 C44 K1 38.36(16) . . ?
C46 C45 C40 117.7(4) . . ?
C46 C45 C50 120.2(4) . . ?
C50 C45 C40 121.6(4) . . ?
C45 C46 C47 119.3(4) . . ?
C45 C46 C51 120.8(4) . . ?
C47 C46 C51 119.9(4) . . ?
C48 C47 C46 122.6(4) . . ?
C47 C48 C49 116.7(4) . . ?
C47 C48 C53 122.3(5) . . ?
C49 C48 C53 120.9(5) . . ?
C50 C49 C48 122.6(4) . . ?
C45 C50 C52 122.1(4) . . ?
C49 C50 C45 118.2(4) . . ?
C49 C50 C52 119.6(4) . . ?
C44 C54 K1 124.1(2) . . ?
C55 C54 C44 121.1(3) . . ?
C55 C54 K1 75.31(19) . . ?
C59 C54 C44 118.6(3) . . ?
C59 C54 C55 119.7(4) . . ?
C59 C54 K1 79.05(19) . . ?
C54 C55 C60 121.8(4) . . ?
C54 C55 K1 78.34(19) . . ?
C56 C55 C54 118.9(4) . . ?
C56 C55 C60 119.3(4) . . ?
C56 C55 K1 76.4(2) . . ?
C60 C55 K1 116.7(2) . . ?
C55 C56 K1 77.2(2) . . ?
C57 C56 C55 121.9(4) . . ?
C57 C56 K1 79.9(2) . . ?
C56 C57 C61 120.2(4) . . ?
C56 C57 K1 74.1(2) . . ?
C58 C57 C56 117.8(4) . . ?
C58 C57 C61 121.9(4) . . ?
C58 C57 K1 78.2(2) . . ?
C61 C57 K1 120.5(2) . . ?
C57 C58 C59 123.1(4) . . ?
C57 C58 K1 76.6(2) . . ?
C59 C58 K1 77.5(2) . . ?
C54 C59 C62 121.2(4) . . ?
C54 C59 K1 75.04(19) . . ?
C58 C59 C54 118.6(4) . . ?
C58 C59 C62 120.1(4) . . ?
C58 C59 K1 76.9(2) . . ?
C62 C59 K1 120.0(2) . . ?
C55 C60 K1 43.63(17) . . ?
C57 C61 K1 41.00(18) . . ?
C59 C62 K1 41.58(17) . . ?
P3 O3 K2 148.75(14) . . ?
P3 O3 K3 88.33(10) . . ?
P3 O3 K4 118.86(13) . . ?
K2 O3 K3 66.10(6) . . ?
K4 O3 K2 83.92(8) . . ?
K4 O3 K3 98.24(8) . . ?
O3 P3 C63 109.63(14) . . ?
O3 P3 P4 98.56(10) . . ?
O3 P3 K2 19.80(9) . . ?
O3 P3 K3 63.76(9) . . ?
O3 P3 K4 39.11(10) . . ?
C63 P3 P4 100.15(11) . . ?
C63 P3 K2 126.31(11) . . ?
C63 P3 K3 172.46(12) . . ?
C63 P3 K4 97.64(12) . . ?
P4 P3 K2 103.43(4) . . ?
P4 P3 K3 78.00(4) . . ?
P4 P3 K4 63.71(4) . . ?
K3 P3 K2 48.09(3) . . ?
K3 P3 K4 74.95(4) . . ?
K4 P3 K2 54.13(3) . . ?
P3 C63 K4 56.87(10) . . ?
C64 C63 P3 127.3(3) . . ?
C64 C63 K4 70.49(18) . . ?
C68 C63 P3 115.7(3) . . ?
C68 C63 C64 116.9(3) . . ?
C68 C63 K4 172.4(2) . . ?
C63 C64 C78 127.4(3) . . ?
C63 C64 K4 90.38(19) . . ?
C65 C64 C63 119.8(3) . . ?
C65 C64 C78 112.5(3) . . ?
C65 C64 K4 149.4(2) . . ?
C78 C64 K4 38.83(15) . . ?
C66 C65 C64 121.6(4) . . ?
C67 C66 C65 119.0(3) . . ?
C66 C67 C68 121.3(3) . . ?
C63 C68 C69 124.4(3) . . ?
C67 C68 C63 120.8(3) . . ?
C67 C68 C69 114.4(3) . . ?
C70 C69 C68 118.6(3) . . ?
C70 C69 C74 119.2(3) . . ?
C74 C69 C68 121.5(3) . . ?
C69 C70 C75 120.3(3) . . ?
C71 C70 C69 119.2(3) . . ?
C71 C70 C75 120.4(3) . . ?
C72 C71 C70 122.4(4) . . ?
C71 C72 C73 117.7(4) . . ?
C71 C72 C76 120.9(4) . . ?
C73 C72 C76 121.3(4) . . ?
C72 C73 C74 122.2(4) . . ?
C69 C74 C77 121.3(3) . . ?
C73 C74 C69 119.1(4) . . ?
C73 C74 C77 119.5(3) . . ?
C64 C78 K4 123.5(2) . . ?
C79 C78 C64 118.7(3) . . ?
C79 C78 C83 118.8(3) . . ?
C79 C78 K4 79.54(18) . . ?
C83 C78 C64 121.7(3) . . ?
C83 C78 K4 75.82(18) . . ?
C78 C79 C84 121.1(3) . . ?
C78 C79 K4 74.21(18) . . ?
C80 C79 C78 119.4(4) . . ?
C80 C79 C84 119.5(3) . . ?
C80 C79 K4 78.4(2) . . ?
C84 C79 K4 118.6(2) . . ?
C79 C80 K4 76.26(19) . . ?
C81 C80 C79 122.3(4) . . ?
C81 C80 K4 77.4(2) . . ?
C80 C81 C82 118.3(3) . . ?
C80 C81 C85 120.8(4) . . ?
C80 C81 K4 77.4(2) . . ?
C82 C81 C85 120.9(4) . . ?
C82 C81 K4 74.0(2) . . ?
C85 C81 K4 119.3(2) . . ?
C81 C82 K4 80.2(2) . . ?
C83 C82 C81 121.5(4) . . ?
C83 C82 K4 75.48(19) . . ?
C78 C83 C86 119.9(3) . . ?
C78 C83 K4 77.46(18) . . ?
C82 C83 C78 119.8(3) . . ?
C82 C83 C86 120.3(3) . . ?
C82 C83 K4 78.48(19) . . ?
C86 C83 K4 114.1(2) . . ?
C79 C84 K4 42.58(16) . . ?
C81 C85 K4 41.98(18) . . ?
C83 C86 K4 45.49(15) . . ?
P4 O4 K1 146.14(14) . . ?
P4 O4 K3 120.94(13) . . ?
P4 O4 K4 86.68(10) . . ?
K1 O4 K3 84.51(8) . . ?
K1 O4 K4 66.79(6) . . ?
K3 O4 K4 97.32(8) . . ?
P3 P4 K1 104.16(4) . . ?
P3 P4 K3 63.28(4) . . ?
P3 P4 K4 77.57(5) . . ?
O4 P4 P3 97.51(10) . . ?
O4 P4 C87 109.92(14) . . ?
O4 P4 K1 21.25(9) . . ?
O4 P4 K3 37.60(10) . . ?
O4 P4 K4 65.64(10) . . ?
C87 P4 P3 99.76(12) . . ?
C87 P4 K1 127.04(10) . . ?
C87 P4 K3 99.46(11) . . ?
C87 P4 K4 174.18(11) . . ?
K3 P4 K1 54.18(3) . . ?
K4 P4 K1 49.69(3) . . ?
K4 P4 K3 74.73(4) . . ?
C88 C87 P4 127.1(3) . . ?
C92 C87 P4 115.6(3) . . ?
C92 C87 C88 117.3(3) . . ?
C87 C88 C93 126.1(3) . . ?
C87 C88 K3 89.4(2) . . ?
C89 C88 C87 119.5(3) . . ?
C89 C88 C93 114.0(3) . . ?
C89 C88 K3 150.8(2) . . ?
C93 C88 K3 38.25(17) . . ?
C90 C89 C88 122.1(3) . . ?
C91 C90 C89 118.9(3) . . ?
C90 C91 C92 121.2(3) . . ?
C87 C92 C102 124.1(3) . . ?
C91 C92 C87 120.6(3) . . ?
C91 C92 C102 114.7(3) . . ?
C88 C93 K3 124.5(2) . . ?
C94 C93 C88 118.2(3) . . ?
C94 C93 K3 76.6(2) . . ?
C98 C93 C88 121.6(3) . . ?
C98 C93 C94 119.5(3) . . ?
C98 C93 K3 77.9(2) . . ?
C93 C94 C99 121.1(3) . . ?
C93 C94 K3 77.3(2) . . ?
C95 C94 C93 118.9(4) . . ?
C95 C94 C99 120.0(3) . . ?
C95 C94 K3 75.3(2) . . ?
C99 C94 K3 118.9(2) . . ?
C94 C95 K3 78.9(2) . . ?
C96 C95 C94 122.3(4) . . ?
C96 C95 K3 76.1(2) . . ?
C95 C96 C97 118.3(3) . . ?
C95 C96 C100 120.6(4) . . ?
C95 C96 K3 77.9(2) . . ?
C97 C96 C100 121.1(4) . . ?
C97 C96 K3 77.7(2) . . ?
C100 C96 K3 113.1(3) . . ?
C96 C97 C98 121.7(4) . . ?
C96 C97 K3 76.2(2) . . ?
C98 C97 K3 80.1(2) . . ?
C93 C98 C97 119.1(3) . . ?
C93 C98 C101 121.8(3) . . ?
C93 C98 K3 76.4(2) . . ?
C97 C98 C101 119.1(4) . . ?
C97 C98 K3 74.0(2) . . ?
C101 C98 K3 119.9(2) . . ?
C94 C99 K3 42.13(18) . . ?
C96 C100 K3 46.0(2) . . ?
C98 C101 K3 41.74(18) . . ?
C103 C102 C92 117.6(3) . . ?
C103 C102 C107 118.3(3) . . ?
C107 C102 C92 123.4(3) . . ?
C102 C103 C108 120.4(3) . . ?
C104 C103 C102 119.9(3) . . ?
C104 C103 C108 119.7(3) . . ?
C103 C104 C105 122.1(3) . . ?
C104 C105 C109 120.5(3) . . ?
C106 C105 C104 117.3(3) . . ?
C106 C105 C109 122.2(3) . . ?
C105 C106 C107 122.7(3) . . ?
C102 C107 C110 120.1(3) . . ?
C106 C107 C102 119.4(3) . . ?
C106 C107 C110 120.5(3) . . ?
O1 K1 C32 85.09(10) . . ?
O1 K1 C55 102.51(9) . . ?
O1 K1 C56 123.43(10) . . ?
O2 K1 O1 64.13(8) . . ?
O2 K1 C32 149.15(10) . . ?
O2 K1 C55 92.27(9) . . ?
O2 K1 C56 115.05(9) . . ?
C55 K1 C32 92.46(11) . . ?
C56 K1 C32 79.31(11) . . ?
C56 K1 C55 26.42(10) . . ?
O4 K1 O1 103.02(7) . . ?
O4 K1 C32 91.93(10) . . ?
O4 K1 O2 96.78(8) . . ?
O4 K1 C55 154.38(9) . . ?
O4 K1 C56 131.29(10) . . ?
C1 K2 C27 79.60(12) . . ?
C1 K2 C28 92.45(12) . . ?
C1 K2 O2 85.48(10) . . ?
O1 K2 C1 148.88(10) . . ?
O1 K2 C27 115.31(10) . . ?
O1 K2 C28 92.86(10) . . ?
O1 K2 O2 63.49(7) . . ?
O1 K2 O3 94.91(8) . . ?
C27 K2 C28 26.12(10) . . ?
C27 K2 O2 125.01(9) . . ?
O2 K2 C28 104.14(9) . . ?
O3 K2 C1 93.74(10) . . ?
O3 K2 C27 131.56(9) . . ?
O3 K2 C28 153.72(9) . . ?
O3 K2 O2 101.80(7) . . ?
O2 K3 O3 104.01(8) . . ?
O2 K3 C95 102.75(9) . . ?
O2 K3 C96 109.27(9) . . ?
O2 K3 C97 132.87(9) . . ?
O3 K3 C95 145.12(9) . . ?
O3 K3 C96 146.53(9) . . ?
O3 K3 C97 121.10(9) . . ?
O4 K3 O2 95.24(8) . . ?
O4 K3 O3 64.69(7) . . ?
O4 K3 C95 91.01(10) . . ?
O4 K3 C96 114.62(10) . . ?
O4 K3 C97 114.92(10) . . ?
C96 K3 C95 25.93(11) . . ?
C96 K3 C97 26.05(10) . . ?
C97 K3 C95 45.28(11) . . ?
O1 K4 C32 93.73(10) . . ?
O1 K4 O3 95.69(8) . . ?
O1 K4 C78 142.29(9) . . ?
O1 K4 C83 153.70(9) . . ?
O1 K4 O4 101.41(7) . . ?
C32 K4 C78 117.19(10) . . ?
C32 K4 C83 90.69(11) . . ?
C32 K4 O4 84.45(10) . . ?
O3 K4 C32 147.74(10) . . ?
O3 K4 C78 70.09(8) . . ?
O3 K4 C83 94.28(9) . . ?
O3 K4 O4 63.46(7) . . ?
C83 K4 C78 26.73(9) . . ?
C83 K4 O4 104.82(9) . . ?
O4 K4 C78 102.52(8) . . ?
C112 C111 C116 120.0 . . ?
C113 C112 C111 120.0 . . ?
C114 C113 C112 120.0 . . ?
C113 C114 C115 120.0 . . ?
C116 C115 C114 120.0 . . ?
C115 C116 C111 120.0 . . ?
C122 C117 C118 120.1(7) . . ?
C119 C118 C117 119.4(7) . . ?
C118 C119 C120 121.4(7) . . ?
C119 C120 C121 119.8(7) . . ?
C122 C121 C120 118.6(7) . . ?
C117 C122 C121 120.6(7) . . ?
C124 C123 C128 120.0 . . ?
C123 C124 C125 120.0 . . ?
C126 C125 C124 120.0 . . ?
C125 C126 C127 120.0 . . ?
C128 C127 C126 120.0 . . ?
C127 C128 C123 120.0 . . ?

_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_AJ1026
_database_code_depnum_ccdc_archive 'CCDC 2082011'
_audit_update_record             
;
2021-08-04 deposited with the CCDC.	2021-08-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C31 H38 N2 P, F6 Sb'
_chemical_formula_sum            'C31 H38 F6 N2 P Sb'
_chemical_formula_weight         705.35

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'
F F 0.0171 0.0103 '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'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           34
_space_group_name_H-M_alt        'P n n 2'
_space_group_name_Hall           'P 2 -2n'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1/2'

_cell_length_a                   38.1631(19)
_cell_length_b                   9.9045(6)
_cell_length_c                   8.5781(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3242.4(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    7838
_cell_measurement_theta_min      2.8430
_cell_measurement_theta_max      26.0490

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.445
_exptl_crystal_F_000             1432
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.160
_exptl_absorpt_coefficient_mu    0.957
_shelx_estimated_absorpt_T_min   0.796
_shelx_estimated_absorpt_T_max   0.862
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.92167
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.29d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            24941
_diffrn_reflns_av_unetI/netI     0.0863
_diffrn_reflns_av_R_equivalents  0.1157
_diffrn_reflns_limit_h_min       -51
_diffrn_reflns_limit_h_max       47
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.864
_diffrn_reflns_theta_max         28.909
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.900
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.900
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.833
_diffrn_reflns_point_group_measured_fraction_full 0.980
_reflns_number_total             7122
_reflns_number_gt                4681
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.740
_reflns_Friedel_fraction_max     0.757
_reflns_Friedel_fraction_full    0.959

_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.
;

_computing_data_collection       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_structure_solution    'ShelXT-2018 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'CIFTAB (Sheldrick, 2015)'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0923P)²+0.1900P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmp
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 1632 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.00(3)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         7122
_refine_ls_number_parameters     515
_refine_ls_number_restraints     922
_refine_ls_R_factor_all          0.0940
_refine_ls_R_factor_gt           0.0624
_refine_ls_wR_factor_ref         0.1737
_refine_ls_wR_factor_gt          0.1564
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_restrained_S_all      0.989
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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 0.40584(4) 0.13028(18) 0.4537(3) 0.0798(6) Uani 1 1 d . . . . .
H1 H 0.420(2) 0.010(10) 0.344(14) 0.120 Uiso 1 1 d . U . . .
N1 N 0.3339(4) 0.1641(17) 0.545(2) 0.065(3) Uani 0.58(2) 1 d D U P A 1
N2 N 0.3446(4) -0.014(2) 0.405(3) 0.069(3) Uani 0.58(2) 1 d D U P A 1
C1 C 0.3592(4) 0.098(3) 0.469(5) 0.068(3) Uani 0.58(2) 1 d D U P A 1
C2 C 0.3088(4) -0.0076(19) 0.433(2) 0.071(3) Uani 0.58(2) 1 d D U P A 1
C3 C 0.3019(4) 0.099(2) 0.510(3) 0.073(4) Uani 0.58(2) 1 d D U P A 1
C4 C 0.3389(6) 0.279(2) 0.647(3) 0.094(5) Uani 0.58(2) 1 d D U P A 1
H4A H 0.316608 0.307865 0.686812 0.140 Uiso 0.58(2) 1 calc R U P A 1
H4B H 0.353878 0.253878 0.731754 0.140 Uiso 0.58(2) 1 calc R U P A 1
H4C H 0.349451 0.351604 0.589351 0.140 Uiso 0.58(2) 1 calc R U P A 1
C5 C 0.2681(4) 0.154(3) 0.571(3) 0.105(6) Uani 0.58(2) 1 d D U P A 1
H5A H 0.272331 0.237586 0.624625 0.157 Uiso 0.58(2) 1 calc R U P A 1
H5B H 0.252358 0.169853 0.485388 0.157 Uiso 0.58(2) 1 calc R U P A 1
H5C H 0.257784 0.090290 0.641518 0.157 Uiso 0.58(2) 1 calc R U P A 1
C6 C 0.2843(5) -0.112(2) 0.372(3) 0.101(6) Uani 0.58(2) 1 d D U P A 1
H6A H 0.297356 -0.180307 0.318042 0.152 Uiso 0.58(2) 1 calc R U P A 1
H6B H 0.271588 -0.151649 0.456468 0.152 Uiso 0.58(2) 1 calc R U P A 1
H6C H 0.268081 -0.070324 0.300462 0.152 Uiso 0.58(2) 1 calc R U P A 1
C7 C 0.3636(7) -0.126(2) 0.331(4) 0.103(7) Uani 0.58(2) 1 d D U P A 1
H7A H 0.347104 -0.192119 0.295065 0.155 Uiso 0.58(2) 1 calc R U P A 1
H7B H 0.376791 -0.092144 0.243781 0.155 Uiso 0.58(2) 1 calc R U P A 1
H7C H 0.379204 -0.166022 0.405048 0.155 Uiso 0.58(2) 1 calc R U P A 1
N1' N 0.3381(5) 0.206(2) 0.554(4) 0.072(4) Uani 0.42(2) 1 d D U P A 2
N2' N 0.3376(5) 0.019(3) 0.420(4) 0.068(4) Uani 0.42(2) 1 d D U P A 2
C1' C 0.3586(6) 0.115(5) 0.485(7) 0.069(4) Uani 0.42(2) 1 d D U P A 2
C2' C 0.3038(5) 0.043(3) 0.476(3) 0.071(4) Uani 0.42(2) 1 d D U P A 2
C3' C 0.3035(5) 0.155(3) 0.553(3) 0.073(4) Uani 0.42(2) 1 d D U P A 2
C4' C 0.3511(8) 0.317(2) 0.648(3) 0.078(6) Uani 0.42(2) 1 d D U P A 2
H4D H 0.331721 0.369545 0.685325 0.118 Uiso 0.42(2) 1 calc R U P A 2
H4E H 0.364068 0.281921 0.734859 0.118 Uiso 0.42(2) 1 calc R U P A 2
H4F H 0.366144 0.372995 0.585676 0.118 Uiso 0.42(2) 1 calc R U P A 2
C5' C 0.2732(6) 0.229(4) 0.626(5) 0.115(7) Uani 0.42(2) 1 d D U P A 2
H5D H 0.281545 0.309288 0.675453 0.172 Uiso 0.42(2) 1 calc R U P A 2
H5E H 0.256544 0.251820 0.546516 0.172 Uiso 0.42(2) 1 calc R U P A 2
H5F H 0.262211 0.171538 0.701984 0.172 Uiso 0.42(2) 1 calc R U P A 2
C6' C 0.2736(7) -0.045(3) 0.429(4) 0.103(8) Uani 0.42(2) 1 d D U P A 2
H6D H 0.282184 -0.121902 0.372153 0.155 Uiso 0.42(2) 1 calc R U P A 2
H6E H 0.261442 -0.075265 0.520421 0.155 Uiso 0.42(2) 1 calc R U P A 2
H6F H 0.257893 0.005545 0.364078 0.155 Uiso 0.42(2) 1 calc R U P A 2
C7' C 0.3505(8) -0.098(2) 0.335(4) 0.088(8) Uani 0.42(2) 1 d D U P A 2
H7D H 0.331079 -0.151431 0.299524 0.132 Uiso 0.42(2) 1 calc R U P A 2
H7E H 0.364008 -0.068616 0.246666 0.132 Uiso 0.42(2) 1 calc R U P A 2
H7F H 0.365066 -0.151666 0.402169 0.132 Uiso 0.42(2) 1 calc R U P A 2
C8 C 0.41100(17) 0.3019(6) 0.3716(11) 0.0717(19) Uani 1 1 d . . . . .
C9 C 0.39061(17) 0.3558(7) 0.2540(9) 0.0676(18) Uani 1 1 d . . . . .
C10 C 0.3977(2) 0.4836(8) 0.1934(11) 0.085(2) Uani 1 1 d . . . . .
H10 H 0.383782 0.519843 0.114991 0.103 Uiso 1 1 calc R U . . .
C11 C 0.4262(2) 0.5563(9) 0.2524(13) 0.102(3) Uani 1 1 d . . . . .
H11 H 0.431104 0.642438 0.215145 0.122 Uiso 1 1 calc R U . . .
C12 C 0.4470(2) 0.4994(8) 0.3662(14) 0.098(3) Uani 1 1 d . . . . .
H12 H 0.465970 0.548315 0.404038 0.117 Uiso 1 1 calc R U . . .
C13 C 0.44066(16) 0.3738(7) 0.4252(10) 0.0714(18) Uani 1 1 d . . . . .
C14 C 0.46592(18) 0.3149(7) 0.5402(14) 0.081(3) Uani 1 1 d . . . . .
C15 C 0.49143(19) 0.2258(8) 0.4873(14) 0.087(3) Uani 1 1 d . . . . .
C16 C 0.5155(2) 0.1698(10) 0.593(2) 0.112(4) Uani 1 1 d . . . . .
H16 H 0.532798 0.111978 0.556330 0.134 Uiso 1 1 calc R U . . .
C17 C 0.5141(3) 0.1987(10) 0.752(2) 0.118(6) Uani 1 1 d . . . . .
C18 C 0.4895(2) 0.2893(9) 0.799(2) 0.112(3) Uani 1 1 d . . . . .
H18 H 0.488367 0.312491 0.903613 0.134 Uiso 1 1 calc R U . . .
C19 C 0.4656(2) 0.3493(8) 0.6946(13) 0.087(2) Uani 1 1 d . . . . .
C20 C 0.4393(2) 0.4491(11) 0.7575(16) 0.117(4) Uani 1 1 d . . . . .
H20A H 0.443235 0.535815 0.710675 0.175 Uiso 1 1 calc R U . . .
H20B H 0.441958 0.456205 0.868527 0.175 Uiso 1 1 calc R U . . .
H20C H 0.416047 0.418816 0.733448 0.175 Uiso 1 1 calc R U . . .
C21 C 0.5406(4) 0.1352(16) 0.856(3) 0.183(8) Uani 1 1 d . . . . .
H21A H 0.548687 0.052474 0.810606 0.274 Uiso 1 1 calc R U . . .
H21B H 0.530072 0.116525 0.955765 0.274 Uiso 1 1 calc R U . . .
H21C H 0.559983 0.195666 0.870085 0.274 Uiso 1 1 calc R U . . .
C22 C 0.4944(2) 0.1951(8) 0.319(2) 0.101(3) Uani 1 1 d . . . . .
H22A H 0.474574 0.142150 0.287030 0.151 Uiso 1 1 calc R U . . .
H22B H 0.515534 0.145459 0.300345 0.151 Uiso 1 1 calc R U . . .
H22C H 0.494861 0.277926 0.261029 0.151 Uiso 1 1 calc R U . . .
C23 C 0.35975(18) 0.2812(7) 0.1792(10) 0.0684(18) Uani 1 1 d . . . . .
C24 C 0.32539(18) 0.3284(8) 0.2052(10) 0.0709(19) Uani 1 1 d . . . . .
C25 C 0.29791(19) 0.2552(10) 0.1446(11) 0.080(2) Uani 1 1 d . . . . .
H25 H 0.275141 0.282941 0.166146 0.096 Uiso 1 1 calc R U . . .
C26 C 0.3027(2) 0.1450(11) 0.0553(12) 0.085(3) Uani 1 1 d . . . . .
C27 C 0.3364(2) 0.1049(10) 0.0186(15) 0.095(3) Uani 1 1 d . . . . .
H27 H 0.339768 0.032528 -0.048708 0.113 Uiso 1 1 calc R U . . .
C28 C 0.3654(2) 0.1718(8) 0.0813(12) 0.077(2) Uani 1 1 d . . . . .
C29 C 0.4028(2) 0.1281(11) 0.0346(17) 0.110(3) Uani 1 1 d . . . . .
H29A H 0.401580 0.051137 -0.033193 0.166 Uiso 1 1 calc R U . . .
H29B H 0.414295 0.201115 -0.018635 0.166 Uiso 1 1 calc R U . . .
H29C H 0.415903 0.105010 0.126397 0.166 Uiso 1 1 calc R U . . .
C30 C 0.2714(3) 0.0620(12) -0.0110(16) 0.128(4) Uani 1 1 d . . . . .
H30A H 0.264075 -0.003744 0.064563 0.193 Uiso 1 1 calc R U . . .
H30B H 0.278478 0.016946 -0.104912 0.193 Uiso 1 1 calc R U . . .
H30C H 0.252202 0.121726 -0.033523 0.193 Uiso 1 1 calc R U . . .
C31 C 0.3173(2) 0.4529(8) 0.2932(14) 0.093(2) Uani 1 1 d . . . . .
H31A H 0.315818 0.527768 0.222416 0.140 Uiso 1 1 calc R U . . .
H31B H 0.335485 0.469546 0.368099 0.140 Uiso 1 1 calc R U . . .
H31C H 0.295317 0.442317 0.346294 0.140 Uiso 1 1 calc R U . . .
Sb1 Sb 0.33354(2) 0.69694(6) 0.80198(12) 0.0961(3) Uani 1 1 d . U . . .
F1 F 0.3282(6) 0.750(3) 1.0059(17) 0.163(6) Uani 0.597(12) 1 d D U P B 1
F2 F 0.3327(5) 0.6480(19) 0.5981(15) 0.149(5) Uani 0.597(12) 1 d D U P B 1
F3 F 0.2919(4) 0.7972(14) 0.7613(18) 0.160(6) Uani 0.597(12) 1 d D U P B 1
F4 F 0.3048(5) 0.5513(13) 0.840(2) 0.169(6) Uani 0.597(12) 1 d D U P B 1
F5 F 0.3695(4) 0.5979(18) 0.834(2) 0.182(6) Uani 0.597(12) 1 d D U P B 1
F6 F 0.3572(4) 0.8541(18) 0.759(2) 0.153(5) Uani 0.597(12) 1 d D U P B 1
F1' F 0.3123(8) 0.743(4) 0.978(3) 0.179(9) Uani 0.403(12) 1 d D U P B 2
F2' F 0.3620(7) 0.627(2) 0.644(3) 0.159(7) Uani 0.403(12) 1 d D U P B 2
F3' F 0.3353(8) 0.8569(19) 0.737(2) 0.146(7) Uani 0.403(12) 1 d D U P B 2
F4' F 0.3759(5) 0.724(3) 0.921(3) 0.156(7) Uani 0.403(12) 1 d D U P B 2
F5' F 0.3402(8) 0.5141(19) 0.881(3) 0.174(7) Uani 0.403(12) 1 d D U P B 2
F6' F 0.2961(5) 0.646(3) 0.711(3) 0.197(8) Uani 0.403(12) 1 d D U P B 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1 C1 1.814(16) . ?
P1 C1' 1.83(2) . ?
P1 C8 1.851(6) . ?
P1 H1 1.62(11) . ?
N1 C1 1.335(16) . ?
N1 C3 1.410(18) . ?
N1 C4 1.45(2) . ?
N2 C1 1.357(16) . ?
N2 C2 1.392(16) . ?
N2 C7 1.467(19) . ?
C2 C3 1.28(2) . ?
C2 C6 1.488(19) . ?
C3 C5 1.49(2) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
N1' C1' 1.330(19) . ?
N1' C3' 1.41(2) . ?
N1' C4' 1.45(2) . ?
N2' C1' 1.36(2) . ?
N2' C2' 1.39(2) . ?
N2' C7' 1.46(2) . ?
C2' C3' 1.30(3) . ?
C2' C6' 1.50(2) . ?
C3' C5' 1.50(2) . ?
C4' H4D 0.9600 . ?
C4' H4E 0.9600 . ?
C4' H4F 0.9600 . ?
C5' H5D 0.9600 . ?
C5' H5E 0.9600 . ?
C5' H5F 0.9600 . ?
C6' H6D 0.9600 . ?
C6' H6E 0.9600 . ?
C6' H6F 0.9600 . ?
C7' H7D 0.9600 . ?
C7' H7E 0.9600 . ?
C7' H7F 0.9600 . ?
C8 C9 1.381(11) . ?
C8 C13 1.414(10) . ?
C9 C10 1.395(11) . ?
C9 C23 1.531(11) . ?
C10 C11 1.399(12) . ?
C10 H10 0.9300 . ?
C11 C12 1.377(13) . ?
C11 H11 0.9300 . ?
C12 C13 1.365(11) . ?
C12 H12 0.9300 . ?
C13 C14 1.497(12) . ?
C14 C19 1.368(14) . ?
C14 C15 1.390(13) . ?
C15 C16 1.406(16) . ?
C15 C22 1.48(2) . ?
C16 C17 1.39(2) . ?
C16 H16 0.9300 . ?
C17 C18 1.360(18) . ?
C17 C21 1.489(17) . ?
C18 C19 1.407(15) . ?
C18 H18 0.9300 . ?
C19 C20 1.508(13) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 C28 1.388(12) . ?
C23 C24 1.410(10) . ?
C24 C25 1.377(12) . ?
C24 C31 1.479(13) . ?
C25 C26 1.346(15) . ?
C25 H25 0.9300 . ?
C26 C27 1.379(13) . ?
C26 C30 1.560(13) . ?
C27 C28 1.400(13) . ?
C27 H27 0.9300 . ?
C28 C29 1.545(12) . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
Sb1 F3' 1.682(18) . ?
Sb1 F6' 1.702(18) . ?
Sb1 F5 1.710(10) . ?
Sb1 F1' 1.77(2) . ?
Sb1 F2 1.815(13) . ?
Sb1 F1 1.837(14) . ?
Sb1 F6 1.837(15) . ?
Sb1 F4 1.842(12) . ?
Sb1 F2' 1.871(16) . ?
Sb1 F3 1.907(10) . ?
Sb1 F4' 1.932(16) . ?
Sb1 F5' 1.951(18) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 P1 C8 107.0(15) . . ?
C1' P1 C8 104(2) . . ?
C1 P1 H1 104(3) . . ?
C1' P1 H1 111(3) . . ?
C8 P1 H1 115(4) . . ?
C1 N1 C3 107.6(14) . . ?
C1 N1 C4 125.7(13) . . ?
C3 N1 C4 126.7(14) . . ?
C1 N2 C2 107.2(12) . . ?
C1 N2 C7 126.3(14) . . ?
C2 N2 C7 126.4(14) . . ?
N1 C1 N2 107.5(12) . . ?
N1 C1 P1 131.2(12) . . ?
N2 C1 P1 121.1(12) . . ?
C3 C2 N2 109.2(12) . . ?
C3 C2 C6 129.1(16) . . ?
N2 C2 C6 121.7(16) . . ?
C2 C3 N1 107.9(12) . . ?
C2 C3 C5 131.2(17) . . ?
N1 C3 C5 120.7(19) . . ?
N1 C4 H4A 109.5 . . ?
N1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C2 C6 H6A 109.5 . . ?
C2 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C2 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N2 C7 H7A 109.5 . . ?
N2 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
N2 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C1' N1' C3' 107.8(17) . . ?
C1' N1' C4' 124.0(18) . . ?
C3' N1' C4' 126(2) . . ?
C1' N2' C2' 106.9(16) . . ?
C1' N2' C7' 124.0(17) . . ?
C2' N2' C7' 128.0(18) . . ?
N1' C1' N2' 107.8(16) . . ?
N1' C1' P1 125.9(18) . . ?
N2' C1' P1 125.4(16) . . ?
C3' C2' N2' 108.9(15) . . ?
C3' C2' C6' 129(2) . . ?
N2' C2' C6' 122(2) . . ?
C2' C3' N1' 107.5(15) . . ?
C2' C3' C5' 129(2) . . ?
N1' C3' C5' 123(2) . . ?
N1' C4' H4D 109.5 . . ?
N1' C4' H4E 109.5 . . ?
H4D C4' H4E 109.5 . . ?
N1' C4' H4F 109.5 . . ?
H4D C4' H4F 109.5 . . ?
H4E C4' H4F 109.5 . . ?
C3' C5' H5D 109.5 . . ?
C3' C5' H5E 109.5 . . ?
H5D C5' H5E 109.5 . . ?
C3' C5' H5F 109.5 . . ?
H5D C5' H5F 109.5 . . ?
H5E C5' H5F 109.5 . . ?
C2' C6' H6D 109.5 . . ?
C2' C6' H6E 109.5 . . ?
H6D C6' H6E 109.5 . . ?
C2' C6' H6F 109.5 . . ?
H6D C6' H6F 109.5 . . ?
H6E C6' H6F 109.5 . . ?
N2' C7' H7D 109.5 . . ?
N2' C7' H7E 109.5 . . ?
H7D C7' H7E 109.5 . . ?
N2' C7' H7F 109.5 . . ?
H7D C7' H7F 109.5 . . ?
H7E C7' H7F 109.5 . . ?
C9 C8 C13 119.6(6) . . ?
C9 C8 P1 125.0(5) . . ?
C13 C8 P1 115.1(6) . . ?
C8 C9 C10 120.9(7) . . ?
C8 C9 C23 123.6(6) . . ?
C10 C9 C23 115.6(6) . . ?
C9 C10 C11 118.9(8) . . ?
C9 C10 H10 120.5 . . ?
C11 C10 H10 120.5 . . ?
C12 C11 C10 119.5(7) . . ?
C12 C11 H11 120.2 . . ?
C10 C11 H11 120.2 . . ?
C13 C12 C11 122.3(7) . . ?
C13 C12 H12 118.9 . . ?
C11 C12 H12 118.9 . . ?
C12 C13 C8 118.7(7) . . ?
C12 C13 C14 119.0(6) . . ?
C8 C13 C14 122.3(6) . . ?
C19 C14 C15 118.7(9) . . ?
C19 C14 C13 122.4(8) . . ?
C15 C14 C13 118.9(10) . . ?
C14 C15 C16 119.8(12) . . ?
C14 C15 C22 120.1(9) . . ?
C16 C15 C22 120.0(10) . . ?
C17 C16 C15 121.8(11) . . ?
C17 C16 H16 119.1 . . ?
C15 C16 H16 119.1 . . ?
C18 C17 C16 116.8(12) . . ?
C18 C17 C21 124.7(18) . . ?
C16 C17 C21 118.4(14) . . ?
C17 C18 C19 122.6(17) . . ?
C17 C18 H18 118.7 . . ?
C19 C18 H18 118.7 . . ?
C14 C19 C18 120.2(10) . . ?
C14 C19 C20 121.1(9) . . ?
C18 C19 C20 118.7(12) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C17 C21 H21A 109.5 . . ?
C17 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C17 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C15 C22 H22A 109.5 . . ?
C15 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C15 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C28 C23 C24 120.0(7) . . ?
C28 C23 C9 120.7(6) . . ?
C24 C23 C9 119.3(7) . . ?
C25 C24 C23 118.3(8) . . ?
C25 C24 C31 118.2(7) . . ?
C23 C24 C31 123.5(7) . . ?
C26 C25 C24 122.5(7) . . ?
C26 C25 H25 118.7 . . ?
C24 C25 H25 118.7 . . ?
C25 C26 C27 119.3(8) . . ?
C25 C26 C30 122.0(9) . . ?
C27 C26 C30 118.7(11) . . ?
C26 C27 C28 120.9(10) . . ?
C26 C27 H27 119.5 . . ?
C28 C27 H27 119.5 . . ?
C23 C28 C27 118.6(8) . . ?
C23 C28 C29 121.3(8) . . ?
C27 C28 C29 120.0(9) . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C26 C30 H30A 109.5 . . ?
C26 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C26 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C24 C31 H31A 109.5 . . ?
C24 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C24 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
F3' Sb1 F6' 99.2(13) . . ?
F3' Sb1 F1' 93.5(14) . . ?
F6' Sb1 F1' 94.6(14) . . ?
F5 Sb1 F2 91.0(9) . . ?
F5 Sb1 F1 95.6(9) . . ?
F2 Sb1 F1 172.6(8) . . ?
F5 Sb1 F6 97.1(9) . . ?
F2 Sb1 F6 92.4(8) . . ?
F1 Sb1 F6 90.3(10) . . ?
F5 Sb1 F4 90.0(9) . . ?
F2 Sb1 F4 87.3(7) . . ?
F1 Sb1 F4 89.2(10) . . ?
F6 Sb1 F4 172.8(9) . . ?
F3' Sb1 F2' 94.8(11) . . ?
F6' Sb1 F2' 92.7(12) . . ?
F1' Sb1 F2' 168.0(14) . . ?
F5 Sb1 F3 176.3(8) . . ?
F2 Sb1 F3 87.0(8) . . ?
F1 Sb1 F3 86.3(8) . . ?
F6 Sb1 F3 86.1(8) . . ?
F4 Sb1 F3 86.8(7) . . ?
F3' Sb1 F4' 90.7(10) . . ?
F6' Sb1 F4' 170.1(14) . . ?
F1' Sb1 F4' 84.2(12) . . ?
F2' Sb1 F4' 87.0(11) . . ?
F3' Sb1 F5' 170.2(12) . . ?
F6' Sb1 F5' 89.6(12) . . ?
F1' Sb1 F5' 90.0(14) . . ?
F2' Sb1 F5' 80.4(11) . . ?
F4' Sb1 F5' 80.6(10) . . ?

_refine_diff_density_max         0.663
_refine_diff_density_min         -0.462
_refine_diff_density_rms         0.073



####################################################################### 
# 
# 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_AJ1028
_database_code_depnum_ccdc_archive 'CCDC 2082009'
_audit_update_record             
;
2021-08-04 deposited with the CCDC.	2021-08-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C31 H38 N2 O2 P), 2(F6 Sb), C H2 Cl2'
_chemical_formula_sum            'C63 H78 Cl2 F12 N4 O4 P2 Sb2'
_chemical_formula_weight         1559.63

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'
F F 0.0171 0.0103 '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'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.6743(2)
_cell_length_b                   14.2432(3)
_cell_length_c                   20.3249(7)
_cell_angle_alpha                93.375(2)
_cell_angle_beta                 91.737(2)
_cell_angle_gamma                108.005(2)
_cell_volume                     3478.82(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    16269
_cell_measurement_theta_min      2.7610
_cell_measurement_theta_max      27.6500

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_F_000             1580
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.140
_exptl_absorpt_coefficient_mu    0.978
_shelx_estimated_absorpt_T_min   0.785
_shelx_estimated_absorpt_T_max   0.875
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.84588
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.29d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            12154
_diffrn_reflns_av_unetI/netI     0.1054
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -2
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.561
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_full        24.999
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             12154
_reflns_number_gt                9862
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_structure_solution    'ShelXT-2018 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'CIFTAB (Sheldrick, 2015)'
_refine_special_details          
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1301P)²+5.0292P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         12154
_refine_ls_number_parameters     978
_refine_ls_number_restraints     876
_refine_ls_R_factor_all          0.1003
_refine_ls_R_factor_gt           0.0886
_refine_ls_wR_factor_ref         0.2498
_refine_ls_wR_factor_gt          0.2396
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_restrained_S_all      1.057
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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 0.75995(10) 0.19725(8) 0.31867(6) 0.0341(3) Uani 1 1 d . . . . .
P2 P 0.66675(10) 0.43407(8) 0.28319(6) 0.0308(3) Uani 1 1 d . . . . .
O1 O 0.6427(3) 0.1946(3) 0.3272(2) 0.0440(8) Uani 1 1 d . . . . .
O2 O 0.8478(3) 0.2971(2) 0.34291(19) 0.0409(8) Uani 1 1 d . . . . .
H2 H 0.816754 0.338880 0.350740 0.061 Uiso 1 1 calc R U . . .
O3 O 0.7760(3) 0.4427(2) 0.31678(18) 0.0391(8) Uani 1 1 d . . . . .
O4 O 0.5739(3) 0.3351(2) 0.29044(18) 0.0384(8) Uani 1 1 d . . . . .
H4 H 0.602005 0.292207 0.298769 0.058 Uiso 1 1 calc R U . . .
N1 N 0.8832(4) 0.2025(3) 0.2049(2) 0.0466(11) Uani 1 1 d . . . . .
N2 N 0.7072(4) 0.1697(3) 0.1797(2) 0.0451(11) Uani 1 1 d . . . . .
N3 N 0.5947(4) 0.4073(3) 0.1494(2) 0.0377(9) Uani 1 1 d . . . . .
N4 N 0.7734(4) 0.4406(3) 0.1610(2) 0.0401(9) Uani 1 1 d . . . . .
C1 C 0.7831(4) 0.1875(3) 0.2306(2) 0.0375(11) Uani 1 1 d . . . . .
C2 C 0.7603(6) 0.1740(5) 0.1211(3) 0.0567(16) Uani 1 1 d . . . . .
C3 C 0.8698(7) 0.1942(5) 0.1360(3) 0.0618(17) Uani 1 1 d . . . . .
C4 C 0.9910(5) 0.2266(5) 0.2411(3) 0.0593(15) Uani 1 1 d . . . . .
H4A H 1.030042 0.295821 0.239371 0.089 Uiso 1 1 calc R U . . .
H4B H 1.033829 0.188411 0.221335 0.089 Uiso 1 1 calc R U . . .
H4C H 0.979719 0.211343 0.286198 0.089 Uiso 1 1 calc R U . . .
C5 C 0.9653(9) 0.2050(8) 0.0921(4) 0.097(3) Uani 1 1 d . . . . .
H5A H 1.027750 0.259243 0.109470 0.146 Uiso 1 1 calc R U . . .
H5B H 0.944030 0.217469 0.048523 0.146 Uiso 1 1 calc R U . . .
H5C H 0.985186 0.145117 0.090136 0.146 Uiso 1 1 calc R U . . .
C6 C 0.6999(9) 0.1554(7) 0.0562(4) 0.089(3) Uani 1 1 d . . . . .
H6A H 0.660493 0.086075 0.048551 0.134 Uiso 1 1 calc R U . . .
H6B H 0.751719 0.175847 0.022400 0.134 Uiso 1 1 calc R U . . .
H6C H 0.648006 0.192289 0.055391 0.134 Uiso 1 1 calc R U . . .
C7 C 0.5866(5) 0.1492(4) 0.1819(3) 0.0554(16) Uani 1 1 d . . . . .
H7A H 0.562811 0.126837 0.224201 0.083 Uiso 1 1 calc R U . . .
H7B H 0.549816 0.098826 0.147977 0.083 Uiso 1 1 calc R U . . .
H7C H 0.568233 0.208481 0.174796 0.083 Uiso 1 1 calc R U . . .
C8 C 0.7996(4) 0.1018(3) 0.3573(3) 0.0365(10) Uani 1 1 d . . . . .
C9 C 0.7757(4) 0.0072(4) 0.3244(3) 0.0414(11) Uani 1 1 d . . . . .
C10 C 0.8161(5) -0.0631(4) 0.3534(3) 0.0551(15) Uani 1 1 d . . . . .
H10 H 0.803599 -0.125220 0.331691 0.066 Uiso 1 1 calc R U . . .
C11 C 0.8740(6) -0.0407(4) 0.4135(4) 0.0606(17) Uani 1 1 d . . . . .
H11 H 0.902467 -0.087045 0.431371 0.073 Uiso 1 1 calc R U . . .
C12 C 0.8901(5) 0.0475(5) 0.4470(3) 0.0539(15) Uani 1 1 d . . . . .
H12 H 0.926103 0.059191 0.488640 0.065 Uiso 1 1 calc R U . . .
C13 C 0.8544(4) 0.1222(4) 0.4213(3) 0.0407(11) Uani 1 1 d . . . . .
C14 C 0.8681(5) 0.2120(4) 0.4661(2) 0.0425(12) Uani 1 1 d . . . . .
C15 C 0.9717(5) 0.2853(4) 0.4767(3) 0.0495(13) Uani 1 1 d . . . . .
C16 C 0.9819(6) 0.3651(5) 0.5234(3) 0.0572(15) Uani 1 1 d . . . . .
H16 H 1.049326 0.415606 0.528872 0.069 Uiso 1 1 calc R U . . .
C17 C 0.8950(6) 0.3706(5) 0.5613(3) 0.0582(16) Uani 1 1 d . . . . .
C18 C 0.7959(6) 0.2972(6) 0.5513(3) 0.0663(18) Uani 1 1 d . . . . .
H18 H 0.737145 0.300366 0.576645 0.080 Uiso 1 1 calc R U . . .
C19 C 0.7790(5) 0.2168(4) 0.5040(3) 0.0504(13) Uani 1 1 d . . . . .
C20 C 0.6677(6) 0.1365(6) 0.4962(4) 0.0733(19) Uani 1 1 d . . . . .
H20A H 0.627868 0.145009 0.457241 0.110 Uiso 1 1 calc R U . . .
H20B H 0.625565 0.140528 0.534084 0.110 Uiso 1 1 calc R U . . .
H20C H 0.679207 0.072855 0.492260 0.110 Uiso 1 1 calc R U . . .
C21 C 0.9095(9) 0.4543(7) 0.6128(4) 0.091(3) Uani 1 1 d . . . . .
H21A H 0.873692 0.499601 0.597077 0.136 Uiso 1 1 calc R U . . .
H21B H 0.987285 0.488233 0.621603 0.136 Uiso 1 1 calc R U . . .
H21C H 0.876928 0.428500 0.652587 0.136 Uiso 1 1 calc R U . . .
C22 C 1.0700(5) 0.2809(5) 0.4395(4) 0.0666(18) Uani 1 1 d . . . . .
H22A H 1.079477 0.216940 0.442336 0.100 Uiso 1 1 calc R U . . .
H22B H 1.135221 0.330996 0.458251 0.100 Uiso 1 1 calc R U . . .
H22C H 1.058506 0.291996 0.394107 0.100 Uiso 1 1 calc R U . . .
C23 C 0.7006(5) -0.0282(3) 0.2636(3) 0.0428(12) Uani 1 1 d . . . . .
C24 C 0.5852(5) -0.0527(4) 0.2704(3) 0.0506(14) Uani 1 1 d . . . . .
C25 C 0.5155(6) -0.0920(4) 0.2153(4) 0.0639(18) Uani 1 1 d . . . . .
H25 H 0.439041 -0.110741 0.219615 0.077 Uiso 1 1 calc R U . . .
C26 C 0.5563(7) -0.1044(5) 0.1533(4) 0.070(2) Uani 1 1 d . . . . .
C27 C 0.6676(6) -0.0848(4) 0.1490(4) 0.0620(17) Uani 1 1 d . . . . .
H27 H 0.694983 -0.096093 0.108348 0.074 Uiso 1 1 calc R U . . .
C28 C 0.7431(5) -0.0481(4) 0.2035(3) 0.0524(14) Uani 1 1 d . . . . .
C29 C 0.8634(6) -0.0344(5) 0.1956(4) 0.0685(18) Uani 1 1 d . . . . .
H29A H 0.878447 -0.095074 0.203003 0.103 Uiso 1 1 calc R U . . .
H29B H 0.907009 0.017037 0.226911 0.103 Uiso 1 1 calc R U . . .
H29C H 0.882206 -0.016328 0.151648 0.103 Uiso 1 1 calc R U . . .
C30 C 0.4763(8) -0.1425(6) 0.0938(5) 0.092(3) Uani 1 1 d . . . . .
H30A H 0.517040 -0.149016 0.055647 0.138 Uiso 1 1 calc R U . . .
H30B H 0.435881 -0.096795 0.086335 0.138 Uiso 1 1 calc R U . . .
H30C H 0.425138 -0.205878 0.101618 0.138 Uiso 1 1 calc R U . . .
C31 C 0.5357(6) -0.0442(5) 0.3361(4) 0.0605(16) Uani 1 1 d . . . . .
H31A H 0.585128 -0.051634 0.370686 0.091 Uiso 1 1 calc R U . . .
H31B H 0.465511 -0.095064 0.336989 0.091 Uiso 1 1 calc R U . . .
H31C H 0.525051 0.019520 0.342357 0.091 Uiso 1 1 calc R U . . .
C32 C 0.6805(4) 0.4306(3) 0.1944(2) 0.0345(10) Uani 1 1 d . . . . .
C33 C 0.6326(6) 0.4032(4) 0.0872(3) 0.0512(14) Uani 1 1 d . . . . .
C34 C 0.7447(6) 0.4235(5) 0.0948(3) 0.0580(15) Uani 1 1 d . . . . .
C35 C 0.8882(5) 0.4651(5) 0.1886(3) 0.0513(13) Uani 1 1 d . . . . .
H35A H 0.890857 0.485278 0.234696 0.077 Uiso 1 1 calc R U . . .
H35B H 0.935750 0.517973 0.165887 0.077 Uiso 1 1 calc R U . . .
H35C H 0.912841 0.407884 0.183259 0.077 Uiso 1 1 calc R U . . .
C36 C 0.8288(8) 0.4315(8) 0.0443(4) 0.086(2) Uani 1 1 d . . . . .
H36A H 0.868223 0.500006 0.039896 0.130 Uiso 1 1 calc R U . . .
H36B H 0.792356 0.401612 0.002727 0.130 Uiso 1 1 calc R U . . .
H36C H 0.880199 0.398061 0.057724 0.130 Uiso 1 1 calc R U . . .
C37 C 0.5566(7) 0.3782(6) 0.0271(3) 0.073(2) Uani 1 1 d . . . . .
H37A H 0.499110 0.316887 0.031517 0.109 Uiso 1 1 calc R U . . .
H37B H 0.597827 0.371702 -0.010863 0.109 Uiso 1 1 calc R U . . .
H37C H 0.523844 0.429877 0.021714 0.109 Uiso 1 1 calc R U . . .
C38 C 0.4769(5) 0.3870(5) 0.1633(3) 0.0529(14) Uani 1 1 d . . . . .
H38A H 0.444589 0.317987 0.169902 0.079 Uiso 1 1 calc R U . . .
H38B H 0.438363 0.403883 0.126659 0.079 Uiso 1 1 calc R U . . .
H38C H 0.470683 0.425848 0.202339 0.079 Uiso 1 1 calc R U . . .
C39 C 0.6090(4) 0.5316(3) 0.3043(2) 0.0346(10) Uani 1 1 d . . . . .
C40 C 0.5226(4) 0.5153(4) 0.3491(3) 0.0413(11) Uani 1 1 d . . . . .
C41 C 0.4705(6) 0.5876(5) 0.3589(3) 0.0571(15) Uani 1 1 d . . . . .
H41 H 0.412084 0.576793 0.387074 0.069 Uiso 1 1 calc R U . . .
C42 C 0.5033(6) 0.6741(5) 0.3283(4) 0.0634(17) Uani 1 1 d . . . . .
H42 H 0.466302 0.720722 0.335082 0.076 Uiso 1 1 calc R U . . .
C43 C 0.5899(5) 0.6921(4) 0.2879(3) 0.0522(14) Uani 1 1 d . . . . .
H43 H 0.612542 0.752308 0.268617 0.063 Uiso 1 1 calc R U . . .
C44 C 0.6461(4) 0.6233(3) 0.2744(2) 0.0371(11) Uani 1 1 d . . . . .
C45 C 0.7415(4) 0.6526(3) 0.2313(3) 0.0396(11) Uani 1 1 d . . . . .
C46 C 0.8509(5) 0.6833(4) 0.2593(3) 0.0518(14) Uani 1 1 d . . . . .
C47 C 0.9384(6) 0.7165(5) 0.2187(4) 0.0687(19) Uani 1 1 d . . . . .
H47 H 1.010409 0.736740 0.237429 0.082 Uiso 1 1 calc R U . . .
C48 C 0.9236(7) 0.7210(6) 0.1514(5) 0.082(2) Uani 1 1 d . . . . .
C49 C 0.8162(7) 0.6951(5) 0.1255(4) 0.072(2) Uani 1 1 d . . . . .
H49 H 0.804653 0.699998 0.080557 0.086 Uiso 1 1 calc R U . . .
C50 C 0.7237(6) 0.6619(4) 0.1633(3) 0.0520(14) Uani 1 1 d . . . . .
C51 C 0.6102(6) 0.6409(5) 0.1319(4) 0.0671(19) Uani 1 1 d . . . . .
H51A H 0.557526 0.593753 0.156185 0.101 Uiso 1 1 calc R U . . .
H51B H 0.608811 0.614302 0.087242 0.101 Uiso 1 1 calc R U . . .
H51C H 0.591054 0.701061 0.132011 0.101 Uiso 1 1 calc R U . . .
C52 C 1.0192(9) 0.7591(9) 0.1079(7) 0.120(4) Uani 1 1 d . . . . .
H52A H 1.077312 0.810545 0.132011 0.180 Uiso 1 1 calc R U . . .
H52B H 0.994436 0.785187 0.069925 0.180 Uiso 1 1 calc R U . . .
H52C H 1.046963 0.706061 0.093806 0.180 Uiso 1 1 calc R U . . .
C53 C 0.8738(6) 0.6853(5) 0.3326(3) 0.0623(17) Uani 1 1 d . . . . .
H53A H 0.827046 0.716588 0.355529 0.093 Uiso 1 1 calc R U . . .
H53B H 0.950282 0.721776 0.343601 0.093 Uiso 1 1 calc R U . . .
H53C H 0.858633 0.618812 0.345474 0.093 Uiso 1 1 calc R U . . .
C54 C 0.4856(5) 0.4252(4) 0.3878(3) 0.0408(11) Uani 1 1 d . . . . .
C55 C 0.3826(5) 0.3557(5) 0.3724(3) 0.0516(14) Uani 1 1 d . . . . .
C56 C 0.3505(5) 0.2733(5) 0.4098(3) 0.0601(16) Uani 1 1 d . . . . .
H56 H 0.281284 0.226447 0.400303 0.072 Uiso 1 1 calc R U . . .
C57 C 0.4177(6) 0.2588(5) 0.4602(4) 0.0650(17) Uani 1 1 d . . . . .
C58 C 0.5177(6) 0.3310(5) 0.4749(3) 0.0578(15) Uani 1 1 d . . . . .
H58 H 0.562992 0.323109 0.509585 0.069 Uiso 1 1 calc R U . . .
C59 C 0.5536(5) 0.4146(4) 0.4406(3) 0.0465(12) Uani 1 1 d . . . . .
C60 C 0.6622(6) 0.4927(5) 0.4618(3) 0.0603(16) Uani 1 1 d . . . . .
H60A H 0.706663 0.509225 0.424172 0.090 Uiso 1 1 calc R U . . .
H60B H 0.701282 0.467800 0.494185 0.090 Uiso 1 1 calc R U . . .
H60C H 0.647789 0.550769 0.480391 0.090 Uiso 1 1 calc R U . . .
C61 C 0.3796(9) 0.1677(7) 0.4993(6) 0.107(3) Uani 1 1 d . . . . .
H61A H 0.440561 0.142468 0.506986 0.161 Uiso 1 1 calc R U . . .
H61B H 0.320241 0.117925 0.474849 0.161 Uiso 1 1 calc R U . . .
H61C H 0.353896 0.185123 0.540817 0.161 Uiso 1 1 calc R U . . .
C62 C 0.3065(5) 0.3629(6) 0.3165(4) 0.0672(18) Uani 1 1 d . . . . .
H62A H 0.244256 0.379411 0.333747 0.101 Uiso 1 1 calc R U . . .
H62B H 0.280496 0.300561 0.290932 0.101 Uiso 1 1 calc R U . . .
H62C H 0.345824 0.413412 0.288966 0.101 Uiso 1 1 calc R U . . .
Cl1 Cl 0.2093(7) 0.8739(8) 0.3215(8) 0.246(6) Uani 0.798(11) 1 d D U P A 1
Cl2 Cl 0.1161(4) 1.0445(6) 0.3297(4) 0.193(3) Uani 0.798(11) 1 d D U P A 1
C63 C 0.192(2) 0.9791(16) 0.2863(11) 0.179(7) Uani 0.798(11) 1 d D U P A 1
H63A H 0.265772 1.024716 0.280590 0.215 Uiso 0.798(11) 1 calc R U P A 1
H63B H 0.156706 0.958364 0.242709 0.215 Uiso 0.798(11) 1 calc R U P A 1
Cl1' Cl 0.340(3) 1.074(3) 0.308(2) 0.232(14) Uani 0.202(11) 1 d D U P A 2
Cl2' Cl 0.194(3) 0.904(2) 0.3515(12) 0.174(9) Uani 0.202(11) 1 d D U P A 2
C63' C 0.197(3) 1.006(4) 0.306(4) 0.160(13) Uani 0.202(11) 1 d D U P A 2
H63C H 0.155278 1.045375 0.327096 0.193 Uiso 0.202(11) 1 calc R U P A 2
H63D H 0.167650 0.985345 0.261528 0.193 Uiso 0.202(11) 1 calc R U P A 2
Sb1 Sb 0.2608(3) 0.0838(3) 0.0924(2) 0.0951(9) Uani 0.718(10) 1 d D U P B 1
F1 F 0.196833 0.023685 0.014624 0.186(5) Uani 0.718(10) 1 d D U P B 1
F2 F 0.1270(8) 0.0604(11) 0.1311(8) 0.167(4) Uani 0.718(10) 1 d D U P B 1
F3 F 0.2700(11) -0.0322(8) 0.1214(8) 0.169(4) Uani 0.718(10) 1 d D U P B 1
F4 F 0.3957(8) 0.1009(14) 0.0555(8) 0.183(5) Uani 0.718(10) 1 d D U P B 1
F5 F 0.2532(14) 0.2014(9) 0.0658(10) 0.204(5) Uani 0.718(10) 1 d D U P B 1
F6 F 0.3352(10) 0.1426(11) 0.1697(7) 0.170(5) Uani 0.718(10) 1 d . U P B 1
Sb1' Sb 0.2478(8) 0.0937(8) 0.0899(5) 0.100(3) Uani 0.282(10) 1 d D . P B 2
F1' F 0.268(3) -0.0077(19) 0.0396(15) 0.189(10) Uani 0.282(10) 1 d D U P B 2
F2' F 0.1154(18) 0.016(2) 0.1146(17) 0.191(12) Uani 0.282(10) 1 d D U P B 2
F3' F 0.315(2) 0.051(3) 0.1616(13) 0.171(9) Uani 0.282(10) 1 d D U P B 2
F4' F 0.3917(15) 0.1700(18) 0.0743(14) 0.144(9) Uani 0.282(10) 1 d D U P B 2
F5' F 0.190(3) 0.135(3) 0.0204(14) 0.203(11) Uani 0.282(10) 1 d D U P B 2
F6' F 0.247(2) 0.1971(17) 0.1457(15) 0.164(9) Uani 0.282(10) 1 d D U P B 2
Sb2 Sb 0.2194(4) 0.5479(4) 0.1627(3) 0.0841(9) Uani 0.573(13) 1 d D U P C 1
F7 F 0.1404(14) 0.4338(13) 0.1999(9) 0.175(6) Uani 0.573(13) 1 d D U P C 1
F8 F 0.3362(13) 0.5579(18) 0.2185(10) 0.185(7) Uani 0.573(13) 1 d D U P C 1
F9 F 0.2748(16) 0.4703(13) 0.1024(9) 0.169(5) Uani 0.573(13) 1 d D U P C 1
F10 F 0.1004(9) 0.5233(16) 0.1014(6) 0.138(5) Uani 0.573(13) 1 d D U P C 1
F11 F 0.1554(16) 0.6158(17) 0.2148(8) 0.188(6) Uani 0.573(13) 1 d D U P C 1
F12 F 0.2964(15) 0.6465(11) 0.1154(8) 0.162(6) Uani 0.573(13) 1 d D U P C 1
Sb2' Sb 0.2215(4) 0.5145(7) 0.1539(3) 0.0818(14) Uani 0.427(13) 1 d D . P C 2
F7' F 0.2071(16) 0.3854(10) 0.1724(9) 0.137(6) Uani 0.427(13) 1 d D U P C 2
F8' F 0.3491(12) 0.5491(15) 0.2054(9) 0.114(5) Uani 0.427(13) 1 d D U P C 2
F9' F 0.3070(13) 0.4972(14) 0.0842(8) 0.132(6) Uani 0.427(13) 1 d D U P C 2
F10' F 0.0973(12) 0.4616(15) 0.0970(8) 0.114(6) Uani 0.427(13) 1 d D U P C 2
F11' F 0.1331(13) 0.519(2) 0.2218(7) 0.152(7) Uani 0.427(13) 1 d D U P C 2
F12' F 0.235(2) 0.6324(14) 0.1240(12) 0.166(8) Uani 0.427(13) 1 d D U P C 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1 O1 1.490(4) . ?
P1 O2 1.553(4) . ?
P1 C8 1.800(5) . ?
P1 C1 1.826(5) . ?
P2 O3 1.492(4) . ?
P2 O4 1.550(4) . ?
P2 C39 1.796(5) . ?
P2 C32 1.818(5) . ?
N1 C1 1.347(7) . ?
N1 C3 1.398(8) . ?
N1 C4 1.464(8) . ?
N2 C1 1.349(7) . ?
N2 C2 1.380(8) . ?
N2 C7 1.468(8) . ?
N3 C32 1.345(7) . ?
N3 C33 1.370(7) . ?
N3 C38 1.470(7) . ?
N4 C32 1.350(7) . ?
N4 C34 1.372(8) . ?
N4 C35 1.472(7) . ?
C2 C3 1.347(10) . ?
C2 C6 1.473(9) . ?
C3 C5 1.502(11) . ?
C8 C9 1.408(7) . ?
C8 C13 1.426(7) . ?
C9 C10 1.408(7) . ?
C9 C23 1.500(7) . ?
C10 C11 1.374(9) . ?
C11 C12 1.348(9) . ?
C12 C13 1.400(8) . ?
C13 C14 1.487(8) . ?
C14 C19 1.403(8) . ?
C14 C15 1.403(8) . ?
C15 C16 1.408(9) . ?
C15 C22 1.491(10) . ?
C16 C17 1.383(10) . ?
C17 C18 1.363(10) . ?
C17 C21 1.502(10) . ?
C18 C19 1.410(10) . ?
C19 C20 1.513(9) . ?
C23 C28 1.399(9) . ?
C23 C24 1.407(8) . ?
C24 C25 1.381(9) . ?
C24 C31 1.507(10) . ?
C25 C26 1.400(12) . ?
C26 C27 1.358(11) . ?
C26 C30 1.514(10) . ?
C27 C28 1.406(9) . ?
C28 C29 1.491(10) . ?
C33 C34 1.362(10) . ?
C33 C37 1.489(9) . ?
C34 C36 1.485(10) . ?
C39 C40 1.418(7) . ?
C39 C44 1.424(7) . ?
C40 C41 1.393(8) . ?
C40 C54 1.502(7) . ?
C41 C42 1.367(10) . ?
C42 C43 1.361(10) . ?
C43 C44 1.399(8) . ?
C44 C45 1.482(8) . ?
C45 C46 1.409(8) . ?
C45 C50 1.414(8) . ?
C46 C47 1.384(10) . ?
C46 C53 1.506(9) . ?
C47 C48 1.382(13) . ?
C48 C49 1.376(12) . ?
C48 C52 1.504(12) . ?
C49 C50 1.394(10) . ?
C50 C51 1.491(9) . ?
C54 C55 1.386(8) . ?
C54 C59 1.400(8) . ?
C55 C56 1.396(9) . ?
C55 C62 1.497(9) . ?
C56 C57 1.377(10) . ?
C57 C58 1.375(10) . ?
C57 C61 1.519(10) . ?
C58 C59 1.375(9) . ?
C59 C60 1.510(9) . ?
Cl1 C63 1.765(16) . ?
Cl2 C63 1.760(16) . ?
Cl1' C63' 1.76(2) . ?
Cl2' C63' 1.76(2) . ?
Sb1 F1 1.795(3) . ?
Sb1 F5 1.819(11) . ?
Sb1 F3 1.822(10) . ?
Sb1 F6 1.825(12) . ?
Sb1 F2 1.836(9) . ?
Sb1 F4 1.839(10) . ?
Sb1' F5' 1.789(15) . ?
Sb1' F2' 1.808(14) . ?
Sb1' F6' 1.808(16) . ?
Sb1' F1' 1.808(14) . ?
Sb1' F4' 1.859(13) . ?
Sb1' F3' 1.885(15) . ?
Sb2 F11 1.769(12) . ?
Sb2 F12 1.794(11) . ?
Sb2 F8 1.803(10) . ?
Sb2 F7 1.845(10) . ?
Sb2 F10 1.859(9) . ?
Sb2 F9 1.895(12) . ?
Sb2' F12' 1.781(14) . ?
Sb2' F11' 1.813(12) . ?
Sb2' F8' 1.816(11) . ?
Sb2' F7' 1.852(12) . ?
Sb2' F10' 1.855(11) . ?
Sb2' F9' 1.860(12) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 P1 O2 114.4(2) . . ?
O1 P1 C8 114.9(2) . . ?
O2 P1 C8 106.6(2) . . ?
O1 P1 C1 109.0(2) . . ?
O2 P1 C1 102.7(2) . . ?
C8 P1 C1 108.4(2) . . ?
O3 P2 O4 115.11(19) . . ?
O3 P2 C39 116.0(2) . . ?
O4 P2 C39 106.8(2) . . ?
O3 P2 C32 109.3(2) . . ?
O4 P2 C32 101.4(2) . . ?
C39 P2 C32 106.9(2) . . ?
C1 N1 C3 109.0(5) . . ?
C1 N1 C4 127.1(5) . . ?
C3 N1 C4 123.8(5) . . ?
C1 N2 C2 109.2(5) . . ?
C1 N2 C7 128.4(5) . . ?
C2 N2 C7 122.4(5) . . ?
C32 N3 C33 109.8(5) . . ?
C32 N3 C38 126.3(5) . . ?
C33 N3 C38 123.9(5) . . ?
C32 N4 C34 108.8(5) . . ?
C32 N4 C35 127.5(4) . . ?
C34 N4 C35 123.7(5) . . ?
N1 C1 N2 107.3(5) . . ?
N1 C1 P1 124.9(4) . . ?
N2 C1 P1 127.8(4) . . ?
C3 C2 N2 107.8(5) . . ?
C3 C2 C6 129.6(7) . . ?
N2 C2 C6 122.5(7) . . ?
C2 C3 N1 106.7(6) . . ?
C2 C3 C5 130.7(7) . . ?
N1 C3 C5 122.6(7) . . ?
C9 C8 C13 120.3(4) . . ?
C9 C8 P1 119.9(4) . . ?
C13 C8 P1 119.8(4) . . ?
C10 C9 C8 118.5(5) . . ?
C10 C9 C23 116.6(5) . . ?
C8 C9 C23 124.7(4) . . ?
C11 C10 C9 120.5(5) . . ?
C12 C11 C10 120.9(5) . . ?
C11 C12 C13 122.2(5) . . ?
C12 C13 C8 117.3(5) . . ?
C12 C13 C14 116.3(5) . . ?
C8 C13 C14 126.1(4) . . ?
C19 C14 C15 119.9(5) . . ?
C19 C14 C13 118.6(5) . . ?
C15 C14 C13 121.0(5) . . ?
C14 C15 C16 118.6(6) . . ?
C14 C15 C22 121.7(5) . . ?
C16 C15 C22 119.7(6) . . ?
C17 C16 C15 122.1(6) . . ?
C18 C17 C16 118.1(6) . . ?
C18 C17 C21 120.8(7) . . ?
C16 C17 C21 121.0(7) . . ?
C17 C18 C19 122.7(6) . . ?
C14 C19 C18 118.4(6) . . ?
C14 C19 C20 121.3(6) . . ?
C18 C19 C20 120.2(6) . . ?
C28 C23 C24 120.8(5) . . ?
C28 C23 C9 120.7(5) . . ?
C24 C23 C9 118.1(5) . . ?
C25 C24 C23 118.3(6) . . ?
C25 C24 C31 119.2(6) . . ?
C23 C24 C31 122.3(5) . . ?
C24 C25 C26 122.0(7) . . ?
C27 C26 C25 118.2(6) . . ?
C27 C26 C30 121.9(8) . . ?
C25 C26 C30 119.9(8) . . ?
C26 C27 C28 122.7(7) . . ?
C23 C28 C27 117.7(6) . . ?
C23 C28 C29 123.0(6) . . ?
C27 C28 C29 119.3(6) . . ?
N3 C32 N4 107.1(4) . . ?
N3 C32 P2 124.5(4) . . ?
N4 C32 P2 128.1(4) . . ?
C34 C33 N3 106.5(5) . . ?
C34 C33 C37 131.2(6) . . ?
N3 C33 C37 122.3(6) . . ?
C33 C34 N4 107.7(5) . . ?
C33 C34 C36 130.1(6) . . ?
N4 C34 C36 122.2(7) . . ?
C40 C39 C44 120.0(4) . . ?
C40 C39 P2 119.5(4) . . ?
C44 C39 P2 120.5(4) . . ?
C41 C40 C39 118.4(5) . . ?
C41 C40 C54 118.0(5) . . ?
C39 C40 C54 123.6(4) . . ?
C42 C41 C40 121.6(6) . . ?
C43 C42 C41 120.1(5) . . ?
C42 C43 C44 122.3(5) . . ?
C43 C44 C39 117.5(5) . . ?
C43 C44 C45 117.3(5) . . ?
C39 C44 C45 125.1(4) . . ?
C46 C45 C50 119.3(5) . . ?
C46 C45 C44 119.9(5) . . ?
C50 C45 C44 120.3(5) . . ?
C47 C46 C45 118.9(6) . . ?
C47 C46 C53 119.6(6) . . ?
C45 C46 C53 121.4(6) . . ?
C48 C47 C46 123.0(7) . . ?
C49 C48 C47 117.3(7) . . ?
C49 C48 C52 120.0(9) . . ?
C47 C48 C52 122.5(9) . . ?
C48 C49 C50 123.1(7) . . ?
C49 C50 C45 118.3(6) . . ?
C49 C50 C51 119.5(6) . . ?
C45 C50 C51 122.1(6) . . ?
C55 C54 C59 121.0(5) . . ?
C55 C54 C40 119.4(5) . . ?
C59 C54 C40 119.5(5) . . ?
C54 C55 C56 117.9(6) . . ?
C54 C55 C62 123.4(6) . . ?
C56 C55 C62 118.7(6) . . ?
C57 C56 C55 122.4(6) . . ?
C58 C57 C56 117.6(6) . . ?
C58 C57 C61 121.8(7) . . ?
C56 C57 C61 120.6(7) . . ?
C57 C58 C59 122.9(6) . . ?
C58 C59 C54 118.2(6) . . ?
C58 C59 C60 119.6(6) . . ?
C54 C59 C60 122.2(5) . . ?
Cl2 C63 Cl1 117.4(14) . . ?
Cl2' C63' Cl1' 104(3) . . ?
F1 Sb1 F5 90.0(7) . . ?
F1 Sb1 F3 91.7(6) . . ?
F5 Sb1 F3 178.3(8) . . ?
F1 Sb1 F6 175.7(6) . . ?
F5 Sb1 F6 91.9(8) . . ?
F3 Sb1 F6 86.5(8) . . ?
F1 Sb1 F2 92.9(5) . . ?
F5 Sb1 F2 91.1(7) . . ?
F3 Sb1 F2 88.6(6) . . ?
F6 Sb1 F2 90.9(7) . . ?
F1 Sb1 F4 87.4(5) . . ?
F5 Sb1 F4 92.1(7) . . ?
F3 Sb1 F4 88.1(6) . . ?
F6 Sb1 F4 88.7(7) . . ?
F2 Sb1 F4 176.8(7) . . ?
F5' Sb1' F2' 94.5(12) . . ?
F5' Sb1' F6' 94.9(14) . . ?
F2' Sb1' F6' 93.6(12) . . ?
F5' Sb1' F1' 91.3(13) . . ?
F2' Sb1' F1' 91.4(12) . . ?
F6' Sb1' F1' 171.7(13) . . ?
F5' Sb1' F4' 92.8(12) . . ?
F2' Sb1' F4' 172.7(13) . . ?
F6' Sb1' F4' 85.0(11) . . ?
F1' Sb1' F4' 89.2(11) . . ?
F5' Sb1' F3' 177.5(13) . . ?
F2' Sb1' F3' 87.9(11) . . ?
F6' Sb1' F3' 85.8(13) . . ?
F1' Sb1' F3' 87.8(12) . . ?
F4' Sb1' F3' 84.8(10) . . ?
F11 Sb2 F12 98.7(9) . . ?
F11 Sb2 F8 96.5(9) . . ?
F12 Sb2 F8 93.7(9) . . ?
F11 Sb2 F7 89.3(9) . . ?
F12 Sb2 F7 171.1(10) . . ?
F8 Sb2 F7 89.4(8) . . ?
F11 Sb2 F10 89.3(8) . . ?
F12 Sb2 F10 88.8(7) . . ?
F8 Sb2 F10 173.2(10) . . ?
F7 Sb2 F10 87.2(7) . . ?
F11 Sb2 F9 174.6(9) . . ?
F12 Sb2 F9 82.6(8) . . ?
F8 Sb2 F9 88.6(8) . . ?
F7 Sb2 F9 89.1(9) . . ?
F10 Sb2 F9 85.4(7) . . ?
F12' Sb2' F11' 99.0(11) . . ?
F12' Sb2' F8' 98.2(9) . . ?
F11' Sb2' F8' 94.8(8) . . ?
F12' Sb2' F7' 171.7(10) . . ?
F11' Sb2' F7' 87.6(9) . . ?
F8' Sb2' F7' 86.1(8) . . ?
F12' Sb2' F10' 88.3(9) . . ?
F11' Sb2' F10' 90.3(7) . . ?
F8' Sb2' F10' 170.9(9) . . ?
F7' Sb2' F10' 86.6(7) . . ?
F12' Sb2' F9' 85.9(9) . . ?
F11' Sb2' F9' 174.7(11) . . ?
F8' Sb2' F9' 86.6(8) . . ?
F7' Sb2' F9' 87.4(8) . . ?
F10' Sb2' F9' 87.6(8) . . ?

_refine_diff_density_max         0.641
_refine_diff_density_min         -0.630
_refine_diff_density_rms         0.133



