# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_MAT15_0m
_database_code_depnum_ccdc_archive 'CCDC 1960508'
loop_
_audit_author_name
_audit_author_address
'Matthias Zeller'
;Purdue University
United States of America
;
_audit_update_record             
;
2020-03-21 deposited with the CCDC.	2020-04-21 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          392-394
_chemical_formula_moiety         ?
_chemical_formula_sum            'C17 H36 F3 N4 O3 P3 S'
_chemical_formula_weight         526.47

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'
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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      cubic
_space_group_IT_number           198
_space_group_name_H-M_alt        'P 21 3'
_space_group_name_Hall           'P 2ac 2ab 3'

_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, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'

_cell_length_a                   13.7390(2)
_cell_length_b                   13.7390(2)
_cell_length_c                   13.7390(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2593.38(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    7392
_cell_measurement_theta_min      2.096
_cell_measurement_theta_max      25.272

_exptl_crystal_description       cube
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.348
_exptl_crystal_F_000             1112
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.450
_exptl_crystal_size_min          0.390
_exptl_absorpt_coefficient_mu    0.356
_shelx_estimated_absorpt_T_min   0.842
_shelx_estimated_absorpt_T_max   0.874
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.842
_exptl_absorpt_correction_T_max  0.874
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            28648
_diffrn_reflns_av_unetI/netI     0.0122
_diffrn_reflns_av_R_equivalents  0.0269
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.096
_diffrn_reflns_theta_max         27.701
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             2033
_reflns_number_gt                1945
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.785
_reflns_Friedel_fraction_max     0.996
_reflns_Friedel_fraction_full    1.000

_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0657P)²+0.6070P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 838 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.01(2)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         2033
_refine_ls_number_parameters     179
_refine_ls_number_restraints     174
_refine_ls_R_factor_all          0.0361
_refine_ls_R_factor_gt           0.0339
_refine_ls_wR_factor_ref         0.1021
_refine_ls_wR_factor_gt          0.0992
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_restrained_S_all      1.120
_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
S1 S 0.86481(6) 0.63519(6) 0.36481(6) 0.0553(4) Uani 1 3 d S T P . .
P1 P 0.88403(4) 0.88403(4) 0.88403(4) 0.0281(3) Uani 1 3 d S T P . .
P2 P 0.79841(7) 0.87048(7) 0.71135(6) 0.0247(2) Uani 0.667 1 d . . P . .
F1 F 0.9194(2) 0.5666(2) 0.53539(19) 0.0826(9) Uani 1 1 d . . . . .
O1 O 0.8833(3) 0.7287(2) 0.4033(3) 0.0775(9) Uani 1 1 d . . . . .
N1 N 0.9172(4) 0.8322(4) 0.7725(4) 0.0444(12) Uani 0.816(7) 1 d D U P . 1
C10 C 1.0109(4) 0.8512(4) 0.7210(4) 0.0367(10) Uani 0.816(7) 1 d D U P . 1
C11 C 1.0135(3) 0.7882(5) 0.6313(4) 0.0651(15) Uani 0.816(7) 1 d D U P . 1
H11A H 0.999991 0.720541 0.649332 0.098 Uiso 0.816(7) 1 calc R U P . 1
H11B H 1.078041 0.792353 0.601175 0.098 Uiso 0.816(7) 1 calc R U P . 1
H11C H 0.964173 0.810776 0.584969 0.098 Uiso 0.816(7) 1 calc R U P . 1
C12 C 1.0917(3) 0.8236(5) 0.7908(4) 0.0670(15) Uani 0.816(7) 1 d D U P . 1
H12A H 1.088788 0.865782 0.848324 0.101 Uiso 0.816(7) 1 calc R U P . 1
H12B H 1.154811 0.831733 0.758605 0.101 Uiso 0.816(7) 1 calc R U P . 1
H12C H 1.083734 0.755628 0.810796 0.101 Uiso 0.816(7) 1 calc R U P . 1
C13 C 1.0213(4) 0.9587(4) 0.6953(6) 0.0797(18) Uani 0.816(7) 1 d D U P . 1
H13C H 0.967277 0.978353 0.653051 0.119 Uiso 0.816(7) 1 calc R U P . 1
H13B H 1.083104 0.969140 0.661237 0.119 Uiso 0.816(7) 1 calc R U P . 1
H13A H 1.020171 0.997619 0.755026 0.119 Uiso 0.816(7) 1 calc R U P . 1
N1B N 0.9118(14) 0.8687(14) 0.7614(15) 0.031(3) Uani 0.184(7) 1 d D U P . 2
C10B C 1.0075(19) 0.852(2) 0.714(2) 0.046(4) Uani 0.184(7) 1 d D U P . 2
C11B C 1.051(2) 0.7514(17) 0.706(2) 0.083(6) Uani 0.184(7) 1 d D U P . 2
H11D H 1.023012 0.718217 0.648796 0.125 Uiso 0.184(7) 1 calc R U P . 2
H11E H 1.035694 0.714229 0.764515 0.125 Uiso 0.184(7) 1 calc R U P . 2
H11F H 1.121414 0.756533 0.697955 0.125 Uiso 0.184(7) 1 calc R U P . 2
C12B C 1.0756(13) 0.9178(18) 0.7693(17) 0.062(5) Uani 0.184(7) 1 d D U P . 2
H12D H 1.070537 0.984167 0.743593 0.093 Uiso 0.184(7) 1 calc R U P . 2
H12E H 1.142588 0.894529 0.762074 0.093 Uiso 0.184(7) 1 calc R U P . 2
H12F H 1.057681 0.917693 0.838376 0.093 Uiso 0.184(7) 1 calc R U P . 2
C13B C 0.990(2) 0.895(2) 0.6101(18) 0.085(6) Uani 0.184(7) 1 d D U P . 2
H13D H 0.985989 0.966285 0.614551 0.128 Uiso 0.184(7) 1 calc R U P . 2
H13E H 0.928640 0.869677 0.583794 0.128 Uiso 0.184(7) 1 calc R U P . 2
H13F H 1.043696 0.876904 0.567131 0.128 Uiso 0.184(7) 1 calc R U P . 2
N2 N 0.7766(5) 0.7481(8) 0.7300(6) 0.0241(15) Uani 0.3333 1 d D . P . -1
C20 C 0.693134 0.693134 0.693134 0.034(2) Uani 0.3333 1 d DS . P . -1
C21 C 0.6644(12) 0.7164(18) 0.5922(12) 0.063(5) Uani 0.3333 1 d D . P . -1
H21A H 0.599718 0.689406 0.579090 0.094 Uiso 0.3333 1 calc R U P . -1
H21B H 0.711662 0.687995 0.546926 0.094 Uiso 0.3333 1 calc R U P . -1
H21C H 0.662864 0.787179 0.583654 0.094 Uiso 0.3333 1 calc R U P . -1
C22 C 0.7140(12) 0.5849(9) 0.7079(13) 0.049(3) Uani 0.3333 1 d D . P . -1
H22A H 0.656078 0.546944 0.690502 0.073 Uiso 0.3333 1 calc R U P . -1
H22B H 0.730599 0.572917 0.776175 0.073 Uiso 0.3333 1 calc R U P . -1
H22C H 0.768534 0.565279 0.666310 0.073 Uiso 0.3333 1 calc R U P . -1
C23 C 0.6061(8) 0.7197(8) 0.7666(9) 0.046(2) Uani 0.3333 1 d D . P . -1
H23A H 0.592900 0.789684 0.763449 0.069 Uiso 0.3333 1 calc R U P . -1
H23B H 0.624874 0.701927 0.833049 0.069 Uiso 0.3333 1 calc R U P . -1
H23C H 0.547480 0.683548 0.747960 0.069 Uiso 0.3333 1 calc R U P . -1
C1 C 0.9465(3) 0.5535(3) 0.4465(3) 0.0410(11) Uani 1 3 d S T P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 O1 1.413(3) 12_664 ?
S1 O1 1.413(3) 6_566 ?
S1 O1 1.413(3) . ?
S1 C1 1.944(6) . ?
P1 P1 0.000(2) 5 ?
P1 N1B 1.74(2) . ?
P1 N1B 1.74(2) 9 ?
P1 N1B 1.74(2) 5 ?
P1 N1 1.750(5) 9 ?
P1 N1 1.750(5) 5 ?
P1 N1 1.750(5) . ?
P1 P2 2.6546(12) . ?
P1 P2 2.6546(12) 9 ?
P1 P2 2.6546(12) 5 ?
P2 N1B 1.70(2) . ?
P2 N2 1.728(11) . ?
P2 N1 1.816(5) 5 ?
P2 N1 1.910(6) . ?
P2 N1B 2.292(19) 5 ?
P2 P2 2.6816(15) 5 ?
P2 P2 2.6816(15) 9 ?
F1 C1 1.289(3) . ?
N1 C10 1.492(6) . ?
C10 C11 1.506(7) . ?
C10 C12 1.515(8) . ?
C10 C13 1.526(8) . ?
N1B C10B 1.49(2) . ?
C10B C11B 1.50(2) . ?
C10B C12B 1.51(2) . ?
C10B C13B 1.56(2) . ?
N2 C20 1.463(6) . ?
C20 C21 1.476(15) . ?
C20 C22 1.528(13) . ?
C20 C23 1.606(9) . ?

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 S1 O1 115.93(10) 12_664 6_566 ?
O1 S1 O1 115.93(10) 12_664 . ?
O1 S1 O1 115.93(10) 6_566 . ?
O1 S1 C1 101.80(15) 12_664 . ?
O1 S1 C1 101.80(15) 6_566 . ?
O1 S1 C1 101.81(15) . . ?
P1 P1 N1B 0(10) 5 . ?
P1 P1 N1B 0(10) 5 9 ?
N1B P1 N1B 97.0(9) . 9 ?
P1 P1 N1B 0(10) 5 5 ?
N1B P1 N1B 97.0(9) . 5 ?
N1B P1 N1B 97.0(9) 9 5 ?
P1 P1 N1 0(10) 5 9 ?
N1B P1 N1 103.6(6) . 9 ?
N1B P1 N1 17.4(6) 9 9 ?
N1B P1 N1 80.2(6) 5 9 ?
P1 P1 N1 0(10) 5 5 ?
N1B P1 N1 80.2(6) . 5 ?
N1B P1 N1 103.6(6) 9 5 ?
N1B P1 N1 17.4(5) 5 5 ?
N1 P1 N1 88.7(2) 9 5 ?
P1 P1 N1 0(10) 5 . ?
N1 P1 N1 88.7(2) 9 . ?
N1 P1 N1 88.7(2) 5 . ?
P1 P1 P2 0(10) 5 . ?
N1B P1 P2 39.0(7) . . ?
N1B P1 P2 94.3(7) 9 . ?
N1B P1 P2 58.5(6) 5 . ?
N1 P1 P2 89.50(16) 9 . ?
N1 P1 P2 42.84(17) 5 . ?
N1 P1 P2 45.92(19) . . ?
P1 P1 P2 0(10) 5 9 ?
N1B P1 P2 58.5(6) . 9 ?
N1B P1 P2 39.0(7) 9 9 ?
N1B P1 P2 94.3(7) 5 9 ?
N1 P1 P2 45.92(19) 9 9 ?
N1 P1 P2 89.50(16) 5 9 ?
N1 P1 P2 42.85(17) . 9 ?
P2 P1 P2 60.67(4) . 9 ?
P1 P1 P2 0(10) 5 5 ?
N1B P1 P2 94.3(7) . 5 ?
N1B P1 P2 58.5(6) 9 5 ?
N1B P1 P2 39.0(7) 5 5 ?
N1 P1 P2 42.85(17) 9 5 ?
N1 P1 P2 45.9(2) 5 5 ?
N1 P1 P2 89.50(16) . 5 ?
P2 P1 P2 60.67(4) . 5 ?
P2 P1 P2 60.67(4) 9 5 ?
N1B P2 N1 79.3(6) . 5 ?
N2 P2 N1 100.1(3) . 5 ?
N2 P2 N1 79.3(3) . . ?
N1 P2 N1 82.1(3) 5 . ?
N1B P2 N1B 80.0(12) . 5 ?
N2 P2 N1B 93.6(5) . 5 ?
N1 P2 N1B 6.5(6) 5 5 ?
N1 P2 N1B 81.0(4) . 5 ?
N1B P2 P1 40.1(7) . 5 ?
N2 P2 P1 90.7(3) . 5 ?
N1 P2 P1 40.94(16) 5 5 ?
N1 P2 P1 41.17(15) . 5 ?
N1B P2 P1 40.4(5) 5 5 ?
N1B P2 P1 40.1(7) . . ?
N2 P2 P1 90.7(3) . . ?
N1 P2 P1 40.94(16) 5 . ?
N1 P2 P1 41.17(15) . . ?
N1B P2 P1 40.4(5) 5 . ?
P1 P2 P1 0.00(3) 5 . ?
N1B P2 P2 94.2(7) . 5 ?
N2 P2 P2 56.1(2) . 5 ?
N1 P2 P2 45.37(19) 5 5 ?
N1 P2 P2 85.47(15) . 5 ?
N1B P2 P2 39.1(5) 5 5 ?
P1 P2 P2 59.663(19) 5 5 ?
P1 P2 P2 59.663(19) . 5 ?
N1B P2 P2 58.0(6) . 9 ?
N2 P2 P2 37.3(3) . 9 ?
N1 P2 P2 87.29(15) 5 9 ?
N1 P2 P2 42.59(16) . 9 ?
N1B P2 P2 82.1(5) 5 9 ?
P1 P2 P2 59.663(19) 5 9 ?
P1 P2 P2 59.663(19) . 9 ?
P2 P2 P2 60.0 5 9 ?
C10 N1 P1 124.7(4) . 5 ?
C10 N1 P1 124.7(4) . . ?
P1 N1 P1 0.000(19) 5 . ?
C10 N1 P2 123.9(4) . 9 ?
P1 N1 P2 96.2(2) 5 9 ?
P1 N1 P2 96.2(2) . 9 ?
C10 N1 P2 118.7(4) . . ?
P1 N1 P2 92.9(2) 5 . ?
P1 N1 P2 92.9(2) . . ?
P2 N1 P2 92.0(2) 9 . ?
N1 C10 C11 108.0(5) . . ?
N1 C10 C12 106.7(5) . . ?
C11 C10 C12 111.0(5) . . ?
N1 C10 C13 111.0(5) . . ?
C11 C10 C13 111.4(6) . . ?
C12 C10 C13 108.6(5) . . ?
C10B N1B P2 129.3(17) . . ?
C10B N1B P1 129.7(17) . 5 ?
P2 N1B P1 100.9(10) . 5 ?
C10B N1B P1 129.7(17) . . ?
P2 N1B P1 100.9(10) . . ?
P1 N1B P1 0.00(8) 5 . ?
C10B N1B P2 99.7(14) . 9 ?
P2 N1B P2 82.9(8) . 9 ?
P1 N1B P2 81.1(7) 5 9 ?
P1 N1B P2 81.1(7) . 9 ?
N1B C10B C11B 122(2) . . ?
N1B C10B C12B 103.3(18) . . ?
C11B C10B C12B 110(2) . . ?
N1B C10B C13B 101.7(19) . . ?
C11B C10B C13B 110(2) . . ?
C12B C10B C13B 109(2) . . ?
C20 N2 P2 125.9(7) . . ?
N2 C20 C21 115.0(8) . . ?
N2 C20 C22 108.0(8) . . ?
C21 C20 C22 112.6(10) . . ?
N2 C20 C23 104.4(5) . . ?
C21 C20 C23 110.0(10) . . ?
C22 C20 C23 106.1(8) . . ?
F1 C1 F1 111.4(3) 12_664 6_566 ?
F1 C1 F1 111.4(3) 12_664 . ?
F1 C1 F1 111.4(3) 6_566 . ?
F1 C1 S1 107.4(3) 12_664 . ?
F1 C1 S1 107.4(3) 6_566 . ?
F1 C1 S1 107.4(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
P1 P1 N1 C10 0.00(10) 5 . . . ?
N1 P1 N1 C10 -141.1(6) 9 . . . ?
N1 P1 N1 C10 130.1(7) 5 . . . ?
P2 P1 N1 C10 128.4(6) . . . . ?
P2 P1 N1 C10 -139.2(7) 9 . . . ?
P2 P1 N1 C10 176.1(5) 5 . . . ?
N1 P1 N1 P1 0(100) 9 . . 5 ?
N1 P1 N1 P1 0(100) 5 . . 5 ?
P2 P1 N1 P1 0(100) . . . 5 ?
P2 P1 N1 P1 0(100) 9 . . 5 ?
P2 P1 N1 P1 0(100) 5 . . 5 ?
P1 P1 N1 P2 0.00(10) 5 . . 9 ?
N1 P1 N1 P2 -1.9(2) 9 . . 9 ?
N1 P1 N1 P2 -90.62(4) 5 . . 9 ?
P2 P1 N1 P2 -92.4(2) . . . 9 ?
P2 P1 N1 P2 -44.7(2) 5 . . 9 ?
P1 P1 N1 P2 0.00(10) 5 . . . ?
N1 P1 N1 P2 90.52(3) 9 . . . ?
N1 P1 N1 P2 1.8(2) 5 . . . ?
P2 P1 N1 P2 92.4(2) 9 . . . ?
P2 P1 N1 P2 47.68(17) 5 . . . ?
P1 N1 C10 C11 176.6(5) 5 . . . ?
P1 N1 C10 C11 176.6(5) . . . . ?
P2 N1 C10 C11 48.0(7) 9 . . . ?
P2 N1 C10 C11 -66.7(6) . . . . ?
P1 N1 C10 C12 57.2(7) 5 . . . ?
P1 N1 C10 C12 57.2(7) . . . . ?
P2 N1 C10 C12 -71.4(6) 9 . . . ?
P2 N1 C10 C12 174.0(4) . . . . ?
P1 N1 C10 C13 -61.1(7) 5 . . . ?
P1 N1 C10 C13 -61.1(7) . . . . ?
P2 N1 C10 C13 170.4(5) 9 . . . ?
P2 N1 C10 C13 55.7(6) . . . . ?
N1B P2 N1B C10B -176(2) 5 . . . ?
P1 P2 N1B C10B 176(3) 5 . . . ?
P1 P2 N1B C10B 176(3) . . . . ?
P2 P2 N1B C10B 147(2) 5 . . . ?
P2 P2 N1B C10B 97(2) 9 . . . ?
N1B P2 N1B P1 7.5(7) 5 . . 5 ?
P1 P2 N1B P1 0.000(4) . . . 5 ?
P2 P2 N1B P1 -29.1(8) 5 . . 5 ?
P2 P2 N1B P1 -79.5(8) 9 . . 5 ?
N1B P2 N1B P1 7.5(7) 5 . . . ?
P1 P2 N1B P1 0.000(4) 5 . . . ?
P2 P2 N1B P1 -29.1(8) 5 . . . ?
P2 P2 N1B P1 -79.5(8) 9 . . . ?
N1B P2 N1B P2 87.0(6) 5 . . 9 ?
P1 P2 N1B P2 79.5(8) 5 . . 9 ?
P1 P2 N1B P2 79.5(8) . . . 9 ?
P2 P2 N1B P2 50.4(5) 5 . . 9 ?
P1 P1 N1B C10B 0.00(17) 5 . . . ?
N1B P1 N1B C10B -88(2) 9 . . . ?
N1B P1 N1B C10B 174(2) 5 . . . ?
P2 P1 N1B C10B -176(3) . . . . ?
P2 P1 N1B C10B -95(2) 9 . . . ?
P2 P1 N1B C10B -147(2) 5 . . . ?
P1 P1 N1B P2 0.00(19) 5 . . . ?
N1B P1 N1B P2 88.2(2) 9 . . . ?
N1B P1 N1B P2 -9.8(11) 5 . . . ?
P2 P1 N1B P2 81.0(8) 9 . . . ?
P2 P1 N1B P2 29.4(8) 5 . . . ?
N1B P1 N1B P1 0(100) 9 . . 5 ?
N1B P1 N1B P1 0(100) 5 . . 5 ?
P2 P1 N1B P1 0(100) . . . 5 ?
P2 P1 N1B P1 0(100) 9 . . 5 ?
P2 P1 N1B P1 0(100) 5 . . 5 ?
P1 P1 N1B P2 0.00(19) 5 . . 9 ?
N1B P1 N1B P2 7.2(8) 9 . . 9 ?
N1B P1 N1B P2 -90.7(3) 5 . . 9 ?
P2 P1 N1B P2 -81.0(8) . . . 9 ?
P2 P1 N1B P2 -51.6(4) 5 . . 9 ?
P2 N1B C10B C11B -91(3) . . . . ?
P1 N1B C10B C11B 84(3) 5 . . . ?
P1 N1B C10B C11B 84(3) . . . . ?
P2 N1B C10B C11B -2(3) 9 . . . ?
P2 N1B C10B C12B 144.8(18) . . . . ?
P1 N1B C10B C12B -40(3) 5 . . . ?
P1 N1B C10B C12B -40(3) . . . . ?
P2 N1B C10B C12B -126.4(17) 9 . . . ?
P2 N1B C10B C13B 32(3) . . . . ?
P1 N1B C10B C13B -153.0(19) 5 . . . ?
P1 N1B C10B C13B -153.0(19) . . . . ?
P2 N1B C10B C13B 120.5(18) 9 . . . ?
N1 P2 N2 C20 107.7(4) 5 . . . ?
N1 P2 N2 C20 -172.4(5) . . . . ?
P1 P2 N2 C20 147.8(4) 5 . . . ?
P1 P2 N2 C20 147.8(4) . . . . ?
P2 P2 N2 C20 95.9(4) 5 . . . ?
P2 P2 N2 C20 179.5(7) 9 . . . ?
P2 N2 C20 C21 41.3(12) . . . . ?
P2 N2 C20 C22 168.0(7) . . . . ?
P2 N2 C20 C23 -79.4(7) . . . . ?

_refine_diff_density_max         0.396
_refine_diff_density_min         -0.376
_refine_diff_density_rms         0.044


_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: CHCl3'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Joseph9_0m
_database_code_depnum_ccdc_archive 'CCDC 1991878'
loop_
_audit_author_name
_audit_author_address
'Lothar Stahl'
;University of North Dakota
United States of America
;
_audit_update_record             
;
2020-03-21 deposited with the CCDC.	2020-04-21 downloaded from the CCDC.
;
_audit_creation_date             2020-03-16
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_chemical_formula_moiety         'C22 H41 As N4 P2'
_chemical_formula_sum            'C22 H41 As N4 P2'
_chemical_formula_weight         498.47
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
_atom_type_scat_dispersion_source
H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236
57.79970 0.0030380000826
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
As 0.07000 2.09310 16.67230 6.07010 3.43130 4.27790 2.63450 0.26470 12.94790
47.79720 2.53099989891
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
N 0.00653 0.00323 12.21260 3.13220 2.01250 1.16630 0.00570 9.89330 28.99750
0.58260 -11.5290002823
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
C 0.00347 0.00161 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870
51.65120 0.215599998832
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
P 0.10434 0.09671 6.43450 4.17910 1.78000 1.49080 1.90670 27.15700 0.52600
68.16450 1.11489999294
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'

_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_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,-y,-z

_symmetry_Int_Tables_number      2
_cell_length_a                   9.5164(5)
_cell_length_b                   9.9718(5)
_cell_length_c                   15.6775(9)
_cell_angle_alpha                79.744(3)
_cell_angle_beta                 87.738(3)
_cell_angle_gamma                63.228(3)
_cell_volume                     1305.62(13)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9965
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      27.57
_cell_measurement_theta_min      2.46
_exptl_absorpt_coefficient_mu    1.439
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6371
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1652 before and 0.0520 after correction.
The Ratio of minimum to maximum transmission is 0.8545.
The λ/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.2679
_exptl_crystal_description       plate
_exptl_crystal_F_000             528.6629
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.06
_diffrn_reflns_av_R_equivalents  0.0486
_diffrn_reflns_av_unetI/netI     0.0580
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            18771
_diffrn_reflns_theta_full        27.6105
_diffrn_reflns_theta_max         27.61
_diffrn_reflns_theta_min         1.32
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.9776
_diffrn_measured_fraction_theta_max 0.9776
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              12
_reflns_limit_k_min              -12
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                4863
_reflns_number_total             5942
_reflns_threshold_expression     I>=2u(I)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.7271
_refine_diff_density_min         -0.6024
_refine_diff_density_rms         0.1313
_refine_ls_d_res_high            0.7668
_refine_ls_d_res_low             15.4104
_refine_ls_goodness_of_fit_ref   1.0002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    58
_refine_ls_number_parameters     274
_refine_ls_number_reflns         5942
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0538
_refine_ls_R_factor_gt           0.0383
_refine_ls_restrained_S_all      1.0002
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0464P)²+1.3165P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0848
_refine_ls_wR_factor_ref         0.1031
_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:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6)
2.b Idealised Me refined as rotating group:
 C11(H11a,H11b,H11c), C12(H12a,H12b,H12c), C13(H13a,H13b,H13c), C21(H21a,H21b,
 H21c), C22(H22a,H22b,H22c), C23(H23a,H23b,H23c), C31(H31a,H31b,H31c), C32(H32a,
 H32b,H32c), C33(H33a,H33b,H33c), C41(H41a,H41b,H41c), C42(H42a,H42b,H42c),
 C43(H43a,H43b,H43c)
;
_atom_sites_solution_primary     direct
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_refinement_flags_posn
As1 As 0.89564(3) -0.01949(3) 0.242589(19) 0.01319(9) Uani 1.000000 .
P1 P 0.53649(7) 0.21839(7) 0.20866(5) 0.01272(15) Uani 1.000000 .
P2 P 0.59329(8) 0.02662(7) 0.35089(5) 0.01341(15) Uani 1.000000 .
N1 N 0.5545(2) 0.2150(2) 0.31799(15) 0.0139(5) Uani 1.000000 .
N2 N 0.5231(2) 0.0498(2) 0.24533(15) 0.0130(5) Uani 1.000000 .
N3 N 0.7243(2) 0.1487(2) 0.17613(15) 0.0130(4) Uani 1.000000 .
N4 N 0.7909(2) -0.0671(2) 0.34089(15) 0.0142(5) Uani 1.000000 .
C10 C 0.5914(3) 0.3131(3) 0.36398(19) 0.0174(6) Uani 1.000000 .
C11 C 0.7656(3) 0.2798(4) 0.3605(2) 0.0249(7) Uani 1.000000 .
H11a H 0.8318(4) 0.1744(9) 0.3891(12) 0.0374(10) Uiso 1.000000 GR
H11b H 0.7935(7) 0.294(2) 0.2998(2) 0.0374(10) Uiso 1.000000 GR
H11c H 0.7823(6) 0.3502(17) 0.3904(12) 0.0374(10) Uiso 1.000000 GR
C12 C 0.5480(4) 0.2892(4) 0.4586(2) 0.0282(7) Uani 1.000000 .
H12a H 0.4353(6) 0.317(2) 0.4608(2) 0.0423(11) Uiso 1.000000 GR
H12b H 0.6090(18) 0.1816(6) 0.4852(4) 0.0423(11) Uiso 1.000000 GR
H12c H 0.572(2) 0.3532(18) 0.4902(4) 0.0423(11) Uiso 1.000000 GR
C13 C 0.4877(4) 0.4789(3) 0.3206(2) 0.0289(7) Uani 1.000000 .
H13a H 0.5147(18) 0.4943(7) 0.2599(5) 0.0434(11) Uiso 1.000000 GR
H13b H 0.3766(4) 0.5006(8) 0.3232(13) 0.0434(11) Uiso 1.000000 GR
H13c H 0.506(2) 0.5480(3) 0.3511(9) 0.0434(11) Uiso 1.000000 GR
C20 C 0.3779(3) 0.0355(3) 0.22749(19) 0.0166(6) Uani 1.000000 .
C21 C 0.2340(3) 0.1463(3) 0.2702(2) 0.0212(6) Uani 1.000000 .
H21a H 0.2564(9) 0.1273(15) 0.3329(3) 0.0319(9) Uiso 1.000000 GR
H21b H 0.2118(14) 0.2517(3) 0.2455(9) 0.0319(9) Uiso 1.000000 GR
H21c H 0.1424(6) 0.1304(16) 0.2594(11) 0.0319(9) Uiso 1.000000 GR
C22 C 0.4108(4) -0.1292(3) 0.2643(2) 0.0288(7) Uani 1.000000 .
H22a H 0.5040(16) -0.1995(4) 0.2382(11) 0.0432(11) Uiso 1.000000 GR
H22b H 0.430(3) -0.1492(9) 0.3274(3) 0.0432(11) Uiso 1.000000 GR
H22c H 0.3197(11) -0.1444(8) 0.2510(13) 0.0432(11) Uiso 1.000000 GR
C23 C 0.3479(3) 0.0676(4) 0.1291(2) 0.0248(7) Uani 1.000000 .
H23a H 0.325(2) 0.1735(8) 0.1059(3) 0.0371(10) Uiso 1.000000 GR
H23b H 0.4415(9) -0.0016(16) 0.1026(2) 0.0371(10) Uiso 1.000000 GR
H23c H 0.2576(15) 0.051(2) 0.1158(2) 0.0371(10) Uiso 1.000000 GR
C30 C 0.7563(3) 0.2195(3) 0.08928(18) 0.0145(5) Uani 1.000000 .
C31 C 0.9334(3) 0.1582(3) 0.0775(2) 0.0202(6) Uani 1.000000 .
H31a H 0.9812(5) 0.181(2) 0.1239(7) 0.0303(9) Uiso 1.000000 GR
H31b H 0.9810(5) 0.0476(5) 0.0799(13) 0.0303(9) Uiso 1.000000 GR
H31c H 0.9515(3) 0.2074(17) 0.0212(6) 0.0303(9) Uiso 1.000000 GR
C32 C 0.6872(3) 0.3929(3) 0.0841(2) 0.0211(6) Uani 1.000000 .
H32a H 0.5733(5) 0.4360(4) 0.0910(13) 0.0317(9) Uiso 1.000000 GR
H32b H 0.7363(18) 0.4142(3) 0.1304(8) 0.0317(9) Uiso 1.000000 GR
H32c H 0.708(2) 0.4393(4) 0.0276(5) 0.0317(9) Uiso 1.000000 GR
C33 C 0.6823(3) 0.1843(3) 0.0165(2) 0.0213(6) Uani 1.000000 .
H33a H 0.7280(17) 0.0735(3) 0.0200(8) 0.0320(9) Uiso 1.000000 GR
H33b H 0.5683(5) 0.226(2) 0.0229(8) 0.0320(9) Uiso 1.000000 GR
H33c H 0.703(2) 0.2309(19) -0.0398(2) 0.0320(9) Uiso 1.000000 GR
C40 C 0.8854(3) -0.2094(3) 0.40616(19) 0.0183(6) Uani 1.000000 .
C41 C 0.8566(4) -0.3413(3) 0.3884(2) 0.0255(7) Uani 1.000000 .
H41a H 0.7443(6) -0.3141(11) 0.3927(14) 0.0383(10) Uiso 1.000000 GR
H41b H 0.889(2) -0.3609(16) 0.3300(6) 0.0383(10) Uiso 1.000000 GR
H41c H 0.918(2) -0.4332(7) 0.4312(9) 0.0383(10) Uiso 1.000000 GR
C42 C 0.8379(3) -0.1795(3) 0.4984(2) 0.0227(6) Uani 1.000000 .
H42a H 0.856(2) -0.0949(15) 0.5093(5) 0.0341(9) Uiso 1.000000 GR
H42b H 0.7259(6) -0.153(2) 0.5041(4) 0.0341(9) Uiso 1.000000 GR
H42c H 0.9010(16) -0.2716(8) 0.5407(2) 0.0341(9) Uiso 1.000000 GR
C43 C 1.0619(3) -0.2534(3) 0.4021(2) 0.0247(7) Uani 1.000000 .
H43a H 1.0981(6) -0.278(2) 0.3450(5) 0.0370(10) Uiso 1.000000 GR
H43b H 1.0797(4) -0.1676(10) 0.4116(14) 0.0370(10) Uiso 1.000000 GR
H43c H 1.1206(4) -0.3424(16) 0.4472(9) 0.0370(10) Uiso 1.000000 GR
C1 C 0.9268(3) -0.1863(3) 0.18018(19) 0.0154(5) Uani 1.000000 .
C2 C 1.0808(3) -0.2969(3) 0.17628(19) 0.0178(6) Uani 1.000000 .
H2 H 1.1651(3) -0.2844(3) 0.19792(19) 0.0213(7) Uiso 1.000000 R
C3 C 1.1131(4) -0.4258(3) 0.1411(2) 0.0226(6) Uani 1.000000 .
H3 H 1.2187(4) -0.5019(3) 0.1400(2) 0.0271(8) Uiso 1.000000 R
C4 C 0.9902(4) -0.4428(3) 0.1076(2) 0.0252(7) Uani 1.000000 .
H4 H 1.0111(4) -0.5315(3) 0.0845(2) 0.0303(8) Uiso 1.000000 R
C5 C 0.8359(4) -0.3289(3) 0.1082(2) 0.0229(6) Uani 1.000000 .
H5 H 0.7523(4) -0.3387(3) 0.0832(2) 0.0275(8) Uiso 1.000000 R
C6 C 0.8030(3) -0.2016(3) 0.1448(2) 0.0188(6) Uani 1.000000 .
H6 H 0.6974(3) -0.1255(3) 0.1458(2) 0.0226(7) Uiso 1.000000 R


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
As1 N3 1.899(2) . ?
As1 N4 1.908(2) . ?
As1 C1 1.981(3) . ?
P1 P2 2.5626(10) . ?
P1 N1 1.722(2) . ?
P1 N2 1.736(2) . ?
P1 N3 1.695(2) . ?
P2 N1 1.725(2) . ?
P2 N2 1.746(2) . ?
P2 N4 1.697(2) . ?
N1 C10 1.477(3) . ?
N2 C20 1.494(3) . ?
N3 C30 1.504(4) . ?
N4 C40 1.508(3) . ?
C10 C11 1.538(4) . ?
C10 C12 1.530(4) . ?
C10 C13 1.534(4) . ?
C20 C21 1.540(4) . ?
C20 C22 1.531(4) . ?
C20 C23 1.530(4) . ?
C30 C31 1.528(4) . ?
C30 C32 1.537(4) . ?
C30 C33 1.532(4) . ?
C40 C41 1.531(4) . ?
C40 C42 1.538(4) . ?
C40 C43 1.534(4) . ?
C1 C2 1.389(4) . ?
C1 C6 1.402(4) . ?
C2 C3 1.390(4) . ?
C3 C4 1.390(4) . ?
C4 C5 1.395(4) . ?
C5 C6 1.388(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N4 As1 N3 101.00(9) . . ?
C1 As1 N3 101.37(10) . . ?
C1 As1 N4 99.87(10) . . ?
N1 P1 P2 42.02(7) . . ?
N2 P1 P2 42.78(8) . . ?
N2 P1 N1 82.86(11) . . ?
N3 P1 P2 96.71(8) . . ?
N3 P1 N1 104.21(11) . . ?
N3 P1 N2 100.59(10) . . ?
N1 P2 P1 41.93(8) . . ?
N2 P2 P1 42.48(7) . . ?
N2 P2 N1 82.48(11) . . ?
N4 P2 P1 95.96(8) . . ?
N4 P2 N1 102.33(11) . . ?
N4 P2 N2 101.38(11) . . ?
P2 N1 P1 96.05(11) . . ?
C10 N1 P1 130.62(18) . . ?
C10 N1 P2 129.04(19) . . ?
P2 N2 P1 94.75(10) . . ?
C20 N2 P1 121.33(17) . . ?
C20 N2 P2 121.93(18) . . ?
P1 N3 As1 122.98(13) . . ?
C30 N3 As1 118.30(16) . . ?
C30 N3 P1 118.69(16) . . ?
P2 N4 As1 123.30(12) . . ?
C40 N4 As1 117.70(17) . . ?
C40 N4 P2 118.38(18) . . ?
C11 C10 N1 113.1(2) . . ?
C12 C10 N1 108.3(2) . . ?
C12 C10 C11 109.6(2) . . ?
C13 C10 N1 107.1(2) . . ?
C13 C10 C11 109.4(2) . . ?
C13 C10 C12 109.4(2) . . ?
C21 C20 N2 111.8(2) . . ?
C22 C20 N2 107.2(2) . . ?
C22 C20 C21 109.6(2) . . ?
C23 C20 N2 108.1(2) . . ?
C23 C20 C21 110.3(2) . . ?
C23 C20 C22 109.7(2) . . ?
C31 C30 N3 110.8(2) . . ?
C32 C30 N3 109.3(2) . . ?
C32 C30 C31 107.4(2) . . ?
C33 C30 N3 109.9(2) . . ?
C33 C30 C31 109.2(2) . . ?
C33 C30 C32 110.1(2) . . ?
C41 C40 N4 109.9(2) . . ?
C42 C40 N4 109.7(2) . . ?
C42 C40 C41 109.9(2) . . ?
C43 C40 N4 110.7(2) . . ?
C43 C40 C41 109.6(2) . . ?
C43 C40 C42 106.9(2) . . ?
C2 C1 As1 116.8(2) . . ?
C6 C1 As1 123.7(2) . . ?
C6 C1 C2 119.4(2) . . ?
C3 C2 C1 120.9(3) . . ?
C4 C3 C2 119.7(3) . . ?
C5 C4 C3 119.6(3) . . ?
C6 C5 C4 120.8(3) . . ?
C5 C6 C1 119.5(3) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_chemical_melting_point          412-414
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: toluene'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_joseph5_0m
_database_code_depnum_ccdc_archive 'CCDC 1991884'
loop_
_audit_author_name
_audit_author_address
'Lothar Stahl'
;University of North Dakota
United States of America
;
_audit_update_record             
;
2020-03-21 deposited with the CCDC.	2020-04-21 downloaded from the CCDC.
;
_audit_creation_date             2020-03-16
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C16 H36 As N7 P2'
_chemical_formula_sum            'C16 H36 As N7 P2'
_chemical_formula_weight         463.38
_chemical_melting_point          373-375
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As 0.0499 2.0058 '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           11
_space_group_name_H-M_alt        'P 1 21/m 1'
_space_group_name_Hall           '-P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'

_cell_length_a                   9.6134(5)
_cell_length_b                   11.6759(6)
_cell_length_c                   10.3557(5)
_cell_angle_alpha                90
_cell_angle_beta                 98.442(2)
_cell_angle_gamma                90
_cell_volume                     1149.78(10)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9866
_cell_measurement_temperature    100
_cell_measurement_theta_max      32.640
_cell_measurement_theta_min      2.645
_shelx_estimated_absorpt_T_max   0.547
_shelx_estimated_absorpt_T_min   0.441
_exptl_absorpt_coefficient_mu    1.632
_exptl_absorpt_correction_T_max  0.531
_exptl_absorpt_correction_T_min  0.387
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             488
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.53
_exptl_crystal_size_min          0.42
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0222
_diffrn_reflns_av_unetI/netI     0.0184
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            16118
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.664
_diffrn_reflns_theta_min         1.988
_diffrn_ambient_temperature      99.97
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4111
_reflns_number_total             4279
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         1.920
_refine_diff_density_min         -1.440
_refine_diff_density_rms         0.093
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     138
_refine_ls_number_reflns         4279
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0265
_refine_ls_R_factor_gt           0.0252
_refine_ls_restrained_S_all      1.090
_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)+(0.0308P)²+0.7093P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0683
_refine_ls_wR_factor_ref         0.0689
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: H12B(0.5) H12C(0.5) H22B(0.5) H22C(0.5)
3.a Me refined with riding coordinates:
 C12(H12A,H12B,H12C), C22(H22A,H22B,H22C)
3.b Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C21(H21A,H21B,H21C), C31(H31A,H31B,H31C), C32(H32A,H32B,
 H32C), C33(H33A,H33B,H33C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
As1 As 0.07266(2) 0.2500 0.25082(2) 0.01350(5) Uani 1 2 d S T P . .
P1 P 0.36892(3) 0.14092(2) 0.34663(3) 0.01059(6) Uani 1 1 d . . . . .
N1 N 0.37242(13) 0.2500 0.45839(12) 0.0105(2) Uani 1 2 d S T P . .
N2 N 0.41108(13) 0.2500 0.24474(12) 0.0119(2) Uani 1 2 d S T P . .
N3 N 0.19251(9) 0.12705(8) 0.29169(9) 0.01185(15) Uani 1 1 d . . . . .
N4 N 0.04851(19) 0.2500 0.05891(16) 0.0265(3) Uani 1 2 d S T P . .
N5 N 0.14590(18) 0.2500 0.00233(13) 0.0192(3) Uani 1 2 d S T P . .
N6 N 0.2370(3) 0.2500 -0.0593(2) 0.0531(7) Uani 1 2 d S T P . .
C10 C 0.33125(15) 0.2500 0.59047(14) 0.0121(2) Uani 1 2 d S T P . .
C12 C 0.17143(17) 0.2500 0.58787(16) 0.0181(3) Uani 1 2 d S T P . .
H12A H 0.1500 0.2500 0.6775 0.027 Uiso 1 2 calc RS T P . .
H12B H 0.1311 0.3185 0.5422 0.027 Uiso 0.5 1 calc R . . . .
H12C H 0.1311 0.1815 0.5422 0.027 Uiso 0.5 1 calc R . . . .
C11 C 0.39242(16) 0.14270(13) 0.66120(13) 0.0277(3) Uani 1 1 d . . . . .
H11A H 0.3534 0.0746 0.6138 0.042 Uiso 1 1 calc GR . . . .
H11B H 0.3683 0.1416 0.7499 0.042 Uiso 1 1 calc GR . . . .
H11C H 0.4949 0.1429 0.6654 0.042 Uiso 1 1 calc GR . . . .
C20 C 0.54807(17) 0.2500 0.19335(17) 0.0188(3) Uani 1 2 d S T P . .
C21 C 0.55392(16) 0.14272(12) 0.10990(15) 0.0275(3) Uani 1 1 d . . . . .
H21A H 0.5493 0.0745 0.1642 0.041 Uiso 1 1 calc GR . . . .
H21B H 0.6420 0.1421 0.0728 0.041 Uiso 1 1 calc GR . . . .
H21C H 0.4742 0.1427 0.0391 0.041 Uiso 1 1 calc GR . . . .
C22 C 0.67166(19) 0.2500 0.3059(2) 0.0322(5) Uani 1 2 d S T P . .
H22A H 0.7606 0.2500 0.2701 0.048 Uiso 1 2 calc RS T P . .
H22B H 0.6666 0.3185 0.3596 0.048 Uiso 0.5 1 calc R . . . .
H22C H 0.6666 0.1815 0.3596 0.048 Uiso 0.5 1 calc R . . . .
C30 C 0.13451(12) 0.00853(9) 0.26231(11) 0.01526(19) Uani 1 1 d . . . . .
C31 C -0.02613(13) 0.01150(12) 0.22813(14) 0.0231(2) Uani 1 1 d . . . . .
H31A H -0.0669 0.0435 0.3016 0.035 Uiso 1 1 calc GR . . . .
H31B H -0.0616 -0.0665 0.2103 0.035 Uiso 1 1 calc GR . . . .
H31C H -0.0526 0.0593 0.1506 0.035 Uiso 1 1 calc GR . . . .
C32 C 0.17196(14) -0.06758(11) 0.38312(13) 0.0219(2) Uani 1 1 d . . . . .
H32A H 0.2743 -0.0699 0.4076 0.033 Uiso 1 1 calc GR . . . .
H32B H 0.1366 -0.1453 0.3634 0.033 Uiso 1 1 calc GR . . . .
H32C H 0.1289 -0.0362 0.4556 0.033 Uiso 1 1 calc GR . . . .
C33 C 0.19828(16) -0.04133(11) 0.14704(13) 0.0242(2) Uani 1 1 d . . . . .
H33A H 0.1754 0.0086 0.0708 0.036 Uiso 1 1 calc GR . . . .
H33B H 0.1595 -0.1179 0.1264 0.036 Uiso 1 1 calc GR . . . .
H33C H 0.3006 -0.0465 0.1703 0.036 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
As1 N3 1.8505(9) 4_565 ?
As1 N3 1.8505(9) . ?
As1 N4 1.9668(17) . ?
P1 P1 2.5472(6) 4_565 ?
P1 N1 1.7180(9) . ?
P1 N2 1.7393(9) . ?
P1 N3 1.7154(9) . ?
N1 P1 1.7179(9) 4_565 ?
N1 C10 1.4786(19) . ?
N2 P1 1.7393(9) 4_565 ?
N2 C20 1.4910(19) . ?
N3 C30 1.5061(14) . ?
N4 N5 1.175(2) . ?
N5 N6 1.157(3) . ?
C10 C12 1.533(2) . ?
C10 C11 1.5249(15) . ?
C10 C11 1.5249(16) 4_565 ?
C20 C21 1.5275(17) 4_565 ?
C20 C21 1.5275(17) . ?
C20 C22 1.537(3) . ?
C30 C31 1.5332(17) . ?
C30 C32 1.5337(17) . ?
C30 C33 1.5345(17) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 As1 N3 101.75(6) 4_565 . ?
N3 As1 N4 102.02(4) . . ?
N3 As1 N4 102.02(4) 4_565 . ?
N1 P1 P1 42.15(3) . 4_565 ?
N1 P1 N2 83.26(5) . . ?
N2 P1 P1 42.93(3) . 4_565 ?
N3 P1 P1 95.42(3) . 4_565 ?
N3 P1 N1 102.36(5) . . ?
N3 P1 N2 100.08(5) . . ?
P1 N1 P1 95.69(6) 4_565 . ?
C10 N1 P1 129.92(4) . . ?
C10 N1 P1 129.92(4) . 4_565 ?
P1 N2 P1 94.15(6) . 4_565 ?
C20 N2 P1 120.88(7) . 4_565 ?
C20 N2 P1 120.88(7) . . ?
P1 N3 As1 123.69(5) . . ?
C30 N3 As1 117.83(7) . . ?
C30 N3 P1 118.19(7) . . ?
N5 N4 As1 121.29(13) . . ?
N6 N5 N4 176.5(2) . . ?
N1 C10 C12 112.80(12) . . ?
N1 C10 C11 107.91(8) . 4_565 ?
N1 C10 C11 107.91(8) . . ?
C11 C10 C12 108.86(9) 4_565 . ?
C11 C10 C12 108.86(9) . . ?
C11 C10 C11 110.49(16) 4_565 . ?
N2 C20 C21 108.04(10) . 4_565 ?
N2 C20 C21 108.04(10) . . ?
N2 C20 C22 110.75(14) . . ?
C21 C20 C21 110.17(15) 4_565 . ?
C21 C20 C22 109.90(10) . . ?
C21 C20 C22 109.90(10) 4_565 . ?
N3 C30 C31 110.88(9) . . ?
N3 C30 C32 109.39(9) . . ?
N3 C30 C33 109.11(9) . . ?
C31 C30 C32 108.02(10) . . ?
C31 C30 C33 109.44(10) . . ?
C32 C30 C33 110.00(10) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: toluene'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_J_MUS_04_CPTP2Ph2Cl2_0m
_database_code_depnum_ccdc_archive 'CCDC 1991877'
loop_
_audit_author_name
_audit_author_address
'Matthias Zeller'
;Purdue University
United States of America
;
_audit_update_record             
;
2020-03-21 deposited with the CCDC.	2020-04-21 downloaded from the CCDC.
;
_audit_creation_date             2020-03-16
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_chemical_formula_moiety         'C28 H46 Cl2 N4 P4'
_chemical_formula_sum            'C28 H46 Cl2 N4 P4'
_chemical_formula_weight         633.50
_chemical_absolute_configuration unk
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
_atom_type_scat_dispersion_source
H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236
57.79970 0.0030380000826
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
C 0.00347 0.00161 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870
51.65120 0.215599998832
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
Cl 0.14873 0.16029 11.46040 7.19640 6.25560 1.64550 0.01040 1.16620 18.51940
47.77840 -9.55739974976
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
P 0.10434 0.09671 6.43450 4.17910 1.78000 1.49080 1.90670 27.15700 0.52600
68.16450 1.11489999294
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
N 0.00653 0.00323 12.21260 3.13220 2.01250 1.16630 0.00570 9.89330 28.99750
0.58260 -11.5290002823
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'

_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_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,y+1/2,-z

_symmetry_Int_Tables_number      4
_cell_length_a                   9.8985(6)
_cell_length_b                   16.8686(10)
_cell_length_c                   11.0098(6)
_cell_angle_alpha                90
_cell_angle_beta                 114.4860(19)
_cell_angle_gamma                90
_cell_volume                     1673.01(17)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9971
_cell_measurement_temperature    150
_cell_measurement_theta_max      33.182
_cell_measurement_theta_min      2.365
_exptl_absorpt_coefficient_mu    0.410
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.7034
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0492 before and 0.0452 after correction. The Ratio of minimum to maximum transmission is 0.9423. The λ/2 correction factor is Not present.'
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.2575
_exptl_crystal_description       plate
_exptl_crystal_F_000             673.5818
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.41
_exptl_crystal_size_min          0.32
_diffrn_reflns_av_R_equivalents  0.0304
_diffrn_reflns_av_unetI/netI     0.0374
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            32695
_diffrn_reflns_theta_full        33.2335
_diffrn_reflns_theta_max         33.23
_diffrn_reflns_theta_min         2.26
_diffrn_ambient_temperature      150.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.9625
_diffrn_measured_fraction_theta_max 0.9625
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker Quest Photon100 CMOS'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.931
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              25
_reflns_limit_k_min              -25
_reflns_limit_l_max              16
_reflns_limit_l_min              -16
_reflns_number_gt                11204
_reflns_number_total             12362
_reflns_threshold_expression     I>=2u(I)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         0.3373
_refine_diff_density_min         -0.4547
_refine_diff_density_rms         0.0830
_refine_ls_abs_structure_details 
'Flack, H. D. (1983). Acta Cryst. A39, 876-881.'
_refine_ls_abs_structure_Flack   0.01(3)
_refine_ls_d_res_high            0.6484
_refine_ls_d_res_low             9.0083
_refine_ls_goodness_of_fit_ref   1.0314
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    68
_refine_ls_number_parameters     355
_refine_ls_number_reflns         12362
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0367
_refine_ls_R_factor_gt           0.0299
_refine_ls_restrained_S_all      1.0314
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0436P)²+0.0588P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0724
_refine_ls_wR_factor_ref         0.0762
_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:
 C6(H6), C5(H5), C4(H4), C3(H3), C2(H2), C56(H56), C55(H55), C54(H54),
 C53(H53), C52(H52)
2.b Idealised Me refined as rotating group:
 C32(H32a,H32b,H32c), C33(H33a,H33b,H33c), C31(H31a,H31b,H31c), C22(H22a,H22b,
 H22c), C23(H23a,H23b,H23c), C42(H42a,H42b,H42c), C43(H43a,H43b,H43c), C41(H41a,
 H41b,H41c), C11(H11a,H11b,H11c), C12(H12a,H12b,H12c), C13(H13a,H13b,H13c),
 C21(H21a,H21b,H21c)
;
_atom_sites_solution_primary     iterative
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_refinement_flags_posn
P1 P 0.37705(3) 0.119206(19) 0.59734(3) 0.01479(6) Uani 1.000000 .
N1 N 0.29998(11) 0.18080(6) 0.45951(10) 0.01691(18) Uani 1.000000 .
Cl1 Cl 0.38703(4) -0.127226(19) 0.50983(4) 0.02684(7) Uani 1.000000 .
C2 C -0.02804(15) -0.00354(9) 0.29597(15) 0.0269(3) Uani 1.000000 .
P2 P 0.44988(3) 0.183101(19) 0.41931(3) 0.01543(6) Uani 1.000000 .
N2 N 0.50740(11) 0.10610(6) 0.53389(10) 0.01541(18) Uani 1.000000 .
Cl2 Cl 0.07357(5) 0.15758(2) 0.02938(4) 0.03815(10) Uani 1.000000 .
C1 C 0.08751(14) -0.05847(8) 0.33543(12) 0.0180(2) Uani 1.000000 .
P3 P 0.27575(3) -0.019950(19) 0.42918(3) 0.01507(6) Uani 1.000000 .
N3 N 0.27427(11) 0.03088(6) 0.56047(10) 0.01577(18) Uani 1.000000 .
C6 C 0.06017(16) -0.13429(8) 0.28032(14) 0.0244(3) Uani 1.000000 .
P4 P 0.22195(4) 0.09387(2) 0.20216(3) 0.02028(7) Uani 1.000000 .
N4 N 0.38464(12) 0.14405(6) 0.25615(10) 0.0186(2) Uani 1.000000 .
C5 C -0.08171(18) -0.15524(10) 0.18808(16) 0.0329(3) Uani 1.000000 .
C4 C -0.19525(18) -0.10077(11) 0.14940(17) 0.0367(4) Uani 1.000000 .
C52 C 0.37456(19) -0.03948(9) 0.17139(14) 0.0299(3) Uani 1.000000 .
C53 C 0.3817(3) -0.11699(11) 0.12959(18) 0.0416(4) Uani 1.000000 .
C54 C 0.2561(3) -0.15227(11) 0.03503(18) 0.0464(5) Uani 1.000000 .
C55 C 0.1248(3) -0.11045(12) -0.01749(17) 0.0441(5) Uani 1.000000 .
C56 C 0.1167(2) -0.03295(10) 0.02303(14) 0.0329(3) Uani 1.000000 .
C51 C 0.24323(17) 0.00358(8) 0.11810(12) 0.0240(3) Uani 1.000000 .
C30 C 0.22788(15) 0.00211(8) 0.66963(13) 0.0208(2) Uani 1.000000 .
C32 C 0.14151(17) 0.06868(10) 0.70110(15) 0.0290(3) Uani 1.000000 .
C33 C 0.36607(17) -0.01880(10) 0.79533(13) 0.0266(3) Uani 1.000000 .
C31 C 0.12807(19) -0.07074(10) 0.62662(16) 0.0310(3) Uani 1.000000 .
C20 C 0.66462(13) 0.08139(8) 0.61174(13) 0.0189(2) Uani 1.000000 .
C22 C 0.67746(16) 0.03550(11) 0.73524(15) 0.0319(3) Uani 1.000000 .
C23 C 0.76593(15) 0.15415(10) 0.65473(16) 0.0291(3) Uani 1.000000 .
C40 C 0.45975(16) 0.18059(9) 0.17257(13) 0.0248(3) Uani 1.000000 .
C42 C 0.62932(17) 0.17961(11) 0.25061(15) 0.0316(3) Uani 1.000000 .
C43 C 0.4100(2) 0.26701(10) 0.14052(16) 0.0322(3) Uani 1.000000 .
C41 C 0.4243(2) 0.13420(11) 0.04370(16) 0.0376(4) Uani 1.000000 .
C11 C 0.1965(2) 0.30345(9) 0.33526(17) 0.0325(3) Uani 1.000000 .
C10 C 0.20049(14) 0.24927(8) 0.44824(15) 0.0228(2) Uani 1.000000 .
C12 C 0.2582(2) 0.29729(10) 0.57607(18) 0.0399(4) Uani 1.000000 .
C13 C 0.04519(18) 0.21788(11) 0.4136(3) 0.0527(6) Uani 1.000000 .
C21 C 0.70869(16) 0.02571(10) 0.52421(17) 0.0294(3) Uani 1.000000 .
C3 C -0.16912(17) -0.02492(12) 0.20344(18) 0.0373(4) Uani 1.000000 .
H6 H 0.13851(16) -0.17190(8) 0.30568(14) 0.0293(3) Uiso 1.000000 R
H5 H -0.09996(18) -0.20728(10) 0.15188(16) 0.0395(4) Uiso 1.000000 R
H4 H -0.29148(18) -0.11500(11) 0.08578(17) 0.0440(4) Uiso 1.000000 R
H3 H -0.24784(17) 0.01251(12) 0.17716(18) 0.0448(4) Uiso 1.000000 R
H2 H -0.01052(15) 0.04850(9) 0.33222(15) 0.0322(3) Uiso 1.000000 R
H56 H 0.0253(2) -0.00496(10) -0.01394(14) 0.0395(4) Uiso 1.000000 R
H55 H 0.0385(3) -0.13479(12) -0.08230(17) 0.0530(6) Uiso 1.000000 R
H54 H 0.2603(3) -0.20500(11) 0.00646(18) 0.0557(6) Uiso 1.000000 R
H53 H 0.4727(3) -0.14539(11) 0.16612(18) 0.0500(5) Uiso 1.000000 R
H52 H 0.46095(19) -0.01586(9) 0.23733(14) 0.0359(4) Uiso 1.000000 R
H32a H 0.2057(5) 0.1152(3) 0.7340(12) 0.0434(5) Uiso 1.000000 GR
H32b H 0.0544(8) 0.0828(5) 0.6199(3) 0.0434(5) Uiso 1.000000 GR
H32c H 0.1093(12) 0.0505(3) 0.7695(9) 0.0434(5) Uiso 1.000000 GR
H33a H 0.4197(8) -0.0621(5) 0.7754(4) 0.0400(4) Uiso 1.000000 GR
H33b H 0.4307(7) 0.0278(2) 0.8252(7) 0.0400(4) Uiso 1.000000 GR
H33c H 0.33626(19) -0.0355(7) 0.8659(4) 0.0400(4) Uiso 1.000000 GR
H31a H 0.0356(6) -0.0572(2) 0.5502(9) 0.0466(5) Uiso 1.000000 GR
H31b H 0.1790(6) -0.1131(3) 0.6012(13) 0.0466(5) Uiso 1.000000 GR
H31c H 0.1055(12) -0.0887(5) 0.7008(5) 0.0466(5) Uiso 1.000000 GR
H22a H 0.6526(15) 0.0705(2) 0.7941(7) 0.0478(5) Uiso 1.000000 GR
H22b H 0.6087(11) -0.0095(5) 0.70834(18) 0.0478(5) Uiso 1.000000 GR
H22c H 0.7793(4) 0.0160(7) 0.7827(8) 0.0478(5) Uiso 1.000000 GR
H23a H 0.7655(11) 0.1809(4) 0.57555(18) 0.0437(5) Uiso 1.000000 GR
H23b H 0.7299(8) 0.1907(4) 0.7039(11) 0.0437(5) Uiso 1.000000 GR
H23c H 0.8673(3) 0.13746(13) 0.7123(11) 0.0437(5) Uiso 1.000000 GR
H42a H 0.6569(2) 0.2098(7) 0.3335(7) 0.0474(5) Uiso 1.000000 GR
H42b H 0.6636(2) 0.12475(12) 0.2719(12) 0.0474(5) Uiso 1.000000 GR
H42c H 0.67566(18) 0.2036(7) 0.1962(6) 0.0474(5) Uiso 1.000000 GR
H43a H 0.3016(2) 0.26910(12) 0.0930(12) 0.0483(5) Uiso 1.000000 GR
H43b H 0.4414(14) 0.2973(2) 0.22372(18) 0.0483(5) Uiso 1.000000 GR
H43c H 0.4552(13) 0.2899(3) 0.0844(12) 0.0483(5) Uiso 1.000000 GR
H41a H 0.4587(15) 0.0794(3) 0.06545(16) 0.0564(6) Uiso 1.000000 GR
H41b H 0.3168(3) 0.1345(7) -0.0102(7) 0.0564(6) Uiso 1.000000 GR
H41c H 0.4745(14) 0.1589(5) -0.0068(7) 0.0564(6) Uiso 1.000000 GR
H11a H 0.2960(4) 0.3248(7) 0.3573(6) 0.0487(5) Uiso 1.000000 GR
H11b H 0.1637(15) 0.2730(2) 0.2521(3) 0.0487(5) Uiso 1.000000 GR
H11c H 0.1273(12) 0.3472(5) 0.3240(9) 0.0487(5) Uiso 1.000000 GR
H12a H 0.2540(16) 0.2651(3) 0.6485(4) 0.0598(6) Uiso 1.000000 GR
H12b H 0.3612(6) 0.3130(8) 0.5987(9) 0.0598(6) Uiso 1.000000 GR
H12c H 0.1968(11) 0.3448(5) 0.5636(5) 0.0598(6) Uiso 1.000000 GR
H13a H 0.0091(8) 0.1903(9) 0.3276(9) 0.0791(9) Uiso 1.000000 GR
H13b H 0.0474(4) 0.1809(8) 0.4831(10) 0.0791(9) Uiso 1.000000 GR
H13c H -0.0213(5) 0.26217(16) 0.4079(18) 0.0791(9) Uiso 1.000000 GR
H21a H 0.6413(9) -0.0199(4) 0.4975(11) 0.0441(4) Uiso 1.000000 GR
H21b H 0.7023(14) 0.0542(2) 0.4444(6) 0.0441(4) Uiso 1.000000 GR
H21c H 0.8107(5) 0.0072(6) 0.5747(5) 0.0441(4) Uiso 1.000000 GR


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1 N1 1.7334(11) . ?
P1 P2 2.5874(4) . ?
P1 N2 1.7172(10) . ?
P1 N3 1.7543(11) . ?
N1 P2 1.7156(11) . ?
N1 C10 1.4892(17) . ?
Cl1 P3 2.1132(5) . ?
C2 C1 1.3941(19) . ?
C2 C3 1.392(2) . ?
P2 N2 1.7342(11) . ?
P2 N4 1.7653(11) . ?
N2 C20 1.4915(15) . ?
Cl2 P4 2.1481(5) . ?
C1 P3 1.8344(13) . ?
C1 C6 1.3932(19) . ?
P3 N3 1.6859(11) . ?
N3 C30 1.5322(16) . ?
C6 C5 1.395(2) . ?
P4 N4 1.6941(11) . ?
P4 C51 1.8391(15) . ?
N4 C40 1.5318(17) . ?
C5 C4 1.376(3) . ?
C4 C3 1.389(2) . ?
C52 C53 1.397(2) . ?
C52 C51 1.389(2) . ?
C53 C54 1.382(3) . ?
C54 C55 1.378(3) . ?
C55 C56 1.394(3) . ?
C56 C51 1.399(2) . ?
C30 C32 1.535(2) . ?
C30 C33 1.530(2) . ?
C30 C31 1.524(2) . ?
C20 C22 1.5235(19) . ?
C20 C23 1.531(2) . ?
C20 C21 1.533(2) . ?
C40 C42 1.536(2) . ?
C40 C43 1.532(2) . ?
C40 C41 1.528(2) . ?
C11 C10 1.531(2) . ?
C10 C12 1.516(2) . ?
C10 C13 1.518(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
P2 P1 N1 41.13(3) . . ?
N2 P1 N1 81.56(5) . . ?
N2 P1 P2 41.69(4) . . ?
N3 P1 N1 107.70(5) . . ?
N3 P1 P2 119.70(4) . . ?
N3 P1 N2 104.95(5) . . ?
P2 N1 P1 97.21(5) . . ?
C10 N1 P1 125.01(9) . . ?
C10 N1 P2 125.01(9) . . ?
C3 C2 C1 120.03(14) . . ?
N1 P2 P1 41.65(4) . . ?
N2 P2 P1 41.19(3) . . ?
N2 P2 N1 81.59(5) . . ?
N4 P2 P1 121.08(4) . . ?
N4 P2 N1 105.27(5) . . ?
N4 P2 N2 109.39(5) . . ?
P2 N2 P1 97.12(5) . . ?
C20 N2 P1 125.67(8) . . ?
C20 N2 P2 125.25(8) . . ?
P3 C1 C2 116.79(10) . . ?
C6 C1 C2 119.22(12) . . ?
C6 C1 P3 122.61(10) . . ?
C1 P3 Cl1 99.44(4) . . ?
N3 P3 Cl1 105.28(4) . . ?
N3 P3 C1 107.14(5) . . ?
P3 N3 P1 114.84(6) . . ?
C30 N3 P1 114.90(8) . . ?
C30 N3 P3 128.56(9) . . ?
C5 C6 C1 120.32(14) . . ?
N4 P4 Cl2 105.21(4) . . ?
C51 P4 Cl2 98.49(5) . . ?
C51 P4 N4 107.45(6) . . ?
P4 N4 P2 115.92(6) . . ?
C40 N4 P2 113.41(8) . . ?
C40 N4 P4 128.15(8) . . ?
C4 C5 C6 120.20(14) . . ?
C3 C4 C5 119.96(14) . . ?
C51 C52 C53 121.08(16) . . ?
C54 C53 C52 119.9(2) . . ?
C55 C54 C53 119.54(17) . . ?
C56 C55 C54 121.01(17) . . ?
C51 C56 C55 120.01(18) . . ?
C52 C51 P4 120.19(10) . . ?
C56 C51 P4 119.19(13) . . ?
C56 C51 C52 118.45(14) . . ?
C32 C30 N3 108.74(11) . . ?
C33 C30 N3 109.65(10) . . ?
C33 C30 C32 109.70(11) . . ?
C31 C30 N3 112.21(10) . . ?
C31 C30 C32 108.06(12) . . ?
C31 C30 C33 108.44(13) . . ?
C22 C20 N2 109.64(10) . . ?
C23 C20 N2 110.33(11) . . ?
C23 C20 C22 109.26(12) . . ?
C21 C20 N2 108.12(11) . . ?
C21 C20 C22 108.04(12) . . ?
C21 C20 C23 111.41(12) . . ?
C42 C40 N4 110.45(11) . . ?
C43 C40 N4 109.35(12) . . ?
C43 C40 C42 108.14(13) . . ?
C41 C40 N4 111.69(12) . . ?
C41 C40 C42 106.93(13) . . ?
C41 C40 C43 110.19(13) . . ?
C11 C10 N1 108.91(12) . . ?
C12 C10 N1 110.82(12) . . ?
C12 C10 C11 107.96(13) . . ?
C13 C10 N1 108.45(11) . . ?
C13 C10 C11 108.79(14) . . ?
C13 C10 C12 111.86(16) . . ?
C4 C3 C2 120.27(16) . . ?

_olex2_submission_original_sample_id (1ab)2
_olex2_submission_special_instructions 'No special instructions were received'
_chemical_melting_point          427-429
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: toluene/THF'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Joseph7_0m
_database_code_depnum_ccdc_archive 'CCDC 1991883'
loop_
_audit_author_name
_audit_author_address
'Lothar Stahl'
;University of North Dakota
United States of America
;
_audit_update_record             
;
2020-03-21 deposited with the CCDC.	2020-04-21 downloaded from the CCDC.
;
_audit_creation_date             2020-03-16
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C22 H54 Bi N5 P2 Si2'
_chemical_formula_sum            'C22 H54 Bi N5 P2 Si2'
_chemical_formula_weight         715.80
_chemical_melting_point          484-486
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'
Bi Bi -4.1077 10.2566 '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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   16.4218(12)
_cell_length_b                   10.8323(8)
_cell_length_c                   18.0205(14)
_cell_angle_alpha                90
_cell_angle_beta                 96.409(3)
_cell_angle_gamma                90
_cell_volume                     3185.6(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9969
_cell_measurement_temperature    100.04
_cell_measurement_theta_max      33.10
_cell_measurement_theta_min      2.95
_shelx_estimated_absorpt_T_max   0.546
_shelx_estimated_absorpt_T_min   0.239
_exptl_absorpt_coefficient_mu    5.729
_exptl_absorpt_correction_T_max  0.522
_exptl_absorpt_correction_T_min  0.210
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.493
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1448
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0344
_diffrn_reflns_av_unetI/netI     0.0376
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            38046
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.145
_diffrn_reflns_theta_min         1.248
_diffrn_ambient_temperature      100.04
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_special_details          ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10762
_reflns_number_total             12020
_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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         4.031
_refine_diff_density_min         -3.499
_refine_diff_density_rms         0.195
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         12020
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0340
_refine_ls_R_factor_gt           0.0287
_refine_ls_restrained_S_all      1.050
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0484P)²+2.2705P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0747
_refine_ls_wR_factor_ref         0.0836
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C21(H21A,H21B,
 H21C), C23(H23A,H23B,H23C), C22(H22A,H22B,H22C), C31(H31A,H31B,H31C), C32(H32A,
 H32B,H32C), C33(H33A,H33B,H33C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C),
 C43(H43A,H43B,H43C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C53(H53A,H53B,
 H53C), C60(H60A,H60B,H60C), C61(H61A,H61B,H61C), C62(H62A,H62B,H62C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Bi1 Bi 0.21988(2) 0.30002(2) 0.31850(2) 0.00839(3) Uani 1 1 d . . . . .
P1 P 0.11911(4) 0.43776(6) 0.43750(3) 0.01031(11) Uani 1 1 d . . . . .
P2 P 0.16816(4) 0.58390(6) 0.33524(3) 0.00955(11) Uani 1 1 d . . . . .
Si1 Si 0.36784(4) 0.10342(7) 0.29347(4) 0.01229(12) Uani 1 1 d . . . . .
Si2 Si 0.42006(4) 0.28892(7) 0.41558(4) 0.01345(14) Uani 1 1 d . . . . .
N1 N 0.09783(12) 0.46272(19) 0.34097(11) 0.0097(3) Uani 1 1 d . . . . .
N2 N 0.18621(13) 0.5599(2) 0.43058(11) 0.0110(4) Uani 1 1 d . . . . .
N3 N 0.17524(14) 0.30933(19) 0.43031(13) 0.0124(4) Uani 1 1 d . . . . .
N4 N 0.24206(12) 0.50123(19) 0.30157(11) 0.0102(3) Uani 1 1 d . . . . .
N5 N 0.34609(13) 0.2296(2) 0.34803(12) 0.0120(4) Uani 1 1 d . . . . .
C10 C 0.01360(14) 0.4612(2) 0.30106(14) 0.0138(4) Uani 1 1 d . . . . .
C11 C 0.01925(17) 0.4720(3) 0.21753(15) 0.0205(5) Uani 1 1 d . . . . .
H11A H 0.0447 0.5510 0.2070 0.031 Uiso 1 1 calc GR . . . .
H11B H -0.0359 0.4678 0.1905 0.031 Uiso 1 1 calc GR . . . .
H11C H 0.0526 0.4041 0.2014 0.031 Uiso 1 1 calc GR . . . .
C12 C -0.03606(16) 0.5693(3) 0.32801(17) 0.0214(6) Uani 1 1 d . . . . .
H12A H -0.0388 0.5617 0.3819 0.032 Uiso 1 1 calc GR . . . .
H12B H -0.0916 0.5678 0.3018 0.032 Uiso 1 1 calc GR . . . .
H12C H -0.0094 0.6474 0.3176 0.032 Uiso 1 1 calc GR . . . .
C13 C -0.02655(17) 0.3388(3) 0.31796(17) 0.0217(6) Uani 1 1 d . . . . .
H13A H 0.0078 0.2703 0.3042 0.032 Uiso 1 1 calc GR . . . .
H13B H -0.0807 0.3333 0.2892 0.032 Uiso 1 1 calc GR . . . .
H13C H -0.0325 0.3341 0.3714 0.032 Uiso 1 1 calc GR . . . .
C20 C 0.20295(15) 0.6600(2) 0.48647(14) 0.0123(4) Uani 1 1 d . . . . .
C21 C 0.22824(17) 0.6016(3) 0.56258(14) 0.0174(5) Uani 1 1 d . . . . .
H21A H 0.1836 0.5496 0.5766 0.026 Uiso 1 1 calc GR . . . .
H21B H 0.2401 0.6667 0.6000 0.026 Uiso 1 1 calc GR . . . .
H21C H 0.2773 0.5509 0.5601 0.026 Uiso 1 1 calc GR . . . .
C23 C 0.27347(16) 0.7400(3) 0.46416(15) 0.0164(5) Uani 1 1 d . . . . .
H23A H 0.3218 0.6881 0.4606 0.025 Uiso 1 1 calc GR . . . .
H23B H 0.2867 0.8041 0.5019 0.025 Uiso 1 1 calc GR . . . .
H23C H 0.2570 0.7787 0.4157 0.025 Uiso 1 1 calc GR . . . .
C22 C 0.12663(17) 0.7405(3) 0.48965(16) 0.0180(5) Uani 1 1 d . . . . .
H22A H 0.1126 0.7809 0.4413 0.027 Uiso 1 1 calc GR . . . .
H22B H 0.1378 0.8033 0.5286 0.027 Uiso 1 1 calc GR . . . .
H22C H 0.0807 0.6887 0.5011 0.027 Uiso 1 1 calc GR . . . .
C30 C 0.17605(17) 0.2078(2) 0.48625(15) 0.0137(5) Uani 1 1 d . . . . .
C31 C 0.21582(19) 0.0930(3) 0.45793(17) 0.0206(5) Uani 1 1 d . . . . .
H31A H 0.1853 0.0666 0.4108 0.031 Uiso 1 1 calc GR . . . .
H31B H 0.2152 0.0268 0.4949 0.031 Uiso 1 1 calc GR . . . .
H31C H 0.2726 0.1116 0.4498 0.031 Uiso 1 1 calc GR . . . .
C32 C 0.08857(19) 0.1732(3) 0.5002(2) 0.0274(7) Uani 1 1 d . . . . .
H32A H 0.0627 0.2438 0.5223 0.041 Uiso 1 1 calc GR . . . .
H32B H 0.0902 0.1028 0.5345 0.041 Uiso 1 1 calc GR . . . .
H32C H 0.0569 0.1510 0.4527 0.041 Uiso 1 1 calc GR . . . .
C33 C 0.2231(2) 0.2513(3) 0.56003(17) 0.0291(7) Uani 1 1 d . . . . .
H33A H 0.2768 0.2833 0.5506 0.044 Uiso 1 1 calc GR . . . .
H33B H 0.2305 0.1817 0.5949 0.044 Uiso 1 1 calc GR . . . .
H33C H 0.1919 0.3167 0.5817 0.044 Uiso 1 1 calc GR . . . .
C40 C 0.28595(16) 0.5530(2) 0.24046(14) 0.0133(4) Uani 1 1 d . . . . .
C41 C 0.22616(18) 0.5777(3) 0.17029(15) 0.0205(5) Uani 1 1 d . . . . .
H41A H 0.1968 0.5015 0.1551 0.031 Uiso 1 1 calc GR . . . .
H41B H 0.2568 0.6061 0.1298 0.031 Uiso 1 1 calc GR . . . .
H41C H 0.1868 0.6414 0.1812 0.031 Uiso 1 1 calc GR . . . .
C42 C 0.35117(17) 0.4625(3) 0.22096(16) 0.0179(5) Uani 1 1 d . . . . .
H42A H 0.3903 0.4475 0.2652 0.027 Uiso 1 1 calc GR . . . .
H42B H 0.3801 0.4973 0.1811 0.027 Uiso 1 1 calc GR . . . .
H42C H 0.3251 0.3845 0.2040 0.027 Uiso 1 1 calc GR . . . .
C43 C 0.3277(2) 0.6745(3) 0.26714(19) 0.0233(6) Uani 1 1 d . . . . .
H43A H 0.2862 0.7337 0.2795 0.035 Uiso 1 1 calc GR . . . .
H43B H 0.3572 0.7085 0.2274 0.035 Uiso 1 1 calc GR . . . .
H43C H 0.3665 0.6588 0.3115 0.035 Uiso 1 1 calc GR . . . .
C51 C 0.42777(19) 0.1448(3) 0.21413(16) 0.0213(5) Uani 1 1 d . . . . .
H51A H 0.3950 0.1999 0.1795 0.032 Uiso 1 1 calc GR . . . .
H51B H 0.4409 0.0695 0.1878 0.032 Uiso 1 1 calc GR . . . .
H51C H 0.4786 0.1865 0.2337 0.032 Uiso 1 1 calc GR . . . .
C52 C 0.27132(17) 0.0280(3) 0.24871(17) 0.0203(5) Uani 1 1 d . . . . .
H52A H 0.2350 0.0102 0.2870 0.030 Uiso 1 1 calc GR . . . .
H52B H 0.2852 -0.0491 0.2246 0.030 Uiso 1 1 calc GR . . . .
H52C H 0.2435 0.0838 0.2112 0.030 Uiso 1 1 calc GR . . . .
C53 C 0.42511(17) -0.0209(3) 0.35007(16) 0.0191(5) Uani 1 1 d . . . . .
H53A H 0.4767 0.0127 0.3744 0.029 Uiso 1 1 calc GR . . . .
H53B H 0.4368 -0.0892 0.3172 0.029 Uiso 1 1 calc GR . . . .
H53C H 0.3917 -0.0510 0.3881 0.029 Uiso 1 1 calc GR . . . .
C60 C 0.52236(18) 0.3012(3) 0.37826(19) 0.0208(6) Uani 1 1 d . . . . .
H60A H 0.5431 0.2183 0.3695 0.031 Uiso 1 1 calc GR . . . .
H60B H 0.5611 0.3444 0.4146 0.031 Uiso 1 1 calc GR . . . .
H60C H 0.5161 0.3474 0.3312 0.031 Uiso 1 1 calc GR . . . .
C61 C 0.4402(2) 0.1885(3) 0.50087(18) 0.0244(6) Uani 1 1 d . . . . .
H61A H 0.3901 0.1817 0.5255 0.037 Uiso 1 1 calc GR . . . .
H61B H 0.4838 0.2254 0.5355 0.037 Uiso 1 1 calc GR . . . .
H61C H 0.4572 0.1062 0.4861 0.037 Uiso 1 1 calc GR . . . .
C62 C 0.39159(17) 0.4451(3) 0.44669(17) 0.0216(6) Uani 1 1 d . . . . .
H62A H 0.4035 0.5064 0.4094 0.032 Uiso 1 1 calc GR . . . .
H62B H 0.4233 0.4644 0.4946 0.032 Uiso 1 1 calc GR . . . .
H62C H 0.3330 0.4469 0.4525 0.032 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
Bi1 N1 2.733(2) . ?
Bi1 N3 2.222(2) . ?
Bi1 N4 2.236(2) . ?
Bi1 N5 2.217(2) . ?
P1 P2 2.6234(9) . ?
P1 N1 1.756(2) . ?
P1 N2 1.735(2) . ?
P1 N3 1.682(2) . ?
P2 N1 1.759(2) . ?
P2 N2 1.730(2) . ?
P2 N4 1.675(2) . ?
Si1 N5 1.744(2) . ?
Si1 C51 1.878(3) . ?
Si1 C52 1.883(3) . ?
Si1 C53 1.877(3) . ?
Si2 N5 1.743(2) . ?
Si2 C60 1.883(3) . ?
Si2 C61 1.882(3) . ?
Si2 C62 1.858(3) . ?
N1 C10 1.486(3) . ?
N2 C20 1.484(3) . ?
N3 C30 1.491(3) . ?
N4 C40 1.491(3) . ?
C10 C11 1.523(4) . ?
C10 C12 1.537(4) . ?
C10 C13 1.527(4) . ?
C20 C21 1.525(4) . ?
C20 C23 1.535(4) . ?
C20 C22 1.533(4) . ?
C30 C31 1.519(4) . ?
C30 C32 1.532(4) . ?
C30 C33 1.535(4) . ?
C40 C41 1.535(4) . ?
C40 C42 1.522(4) . ?
C40 C43 1.536(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 Bi1 N1 60.97(7) . . ?
N3 Bi1 N4 98.90(8) . . ?
N4 Bi1 N1 61.64(7) . . ?
N5 Bi1 N1 150.20(7) . . ?
N5 Bi1 N3 101.08(8) . . ?
N5 Bi1 N4 101.88(8) . . ?
N1 P1 P2 41.77(7) . . ?
N2 P1 P2 40.73(7) . . ?
N2 P1 N1 82.48(10) . . ?
N3 P1 P2 103.36(8) . . ?
N3 P1 N1 95.81(11) . . ?
N3 P1 N2 105.50(11) . . ?
N1 P2 P1 41.70(7) . . ?
N2 P2 P1 40.86(7) . . ?
N2 P2 N1 82.55(10) . . ?
N4 P2 P1 102.91(8) . . ?
N4 P2 N1 97.42(10) . . ?
N4 P2 N2 103.22(10) . . ?
N5 Si1 C51 113.57(13) . . ?
N5 Si1 C52 111.46(12) . . ?
N5 Si1 C53 112.19(12) . . ?
C51 Si1 C52 105.37(14) . . ?
C53 Si1 C51 108.14(14) . . ?
C53 Si1 C52 105.58(13) . . ?
N5 Si2 C60 110.89(13) . . ?
N5 Si2 C61 113.74(13) . . ?
N5 Si2 C62 111.52(12) . . ?
C61 Si2 C60 104.49(15) . . ?
C62 Si2 C60 107.94(14) . . ?
C62 Si2 C61 107.87(15) . . ?
P1 N1 Bi1 88.82(8) . . ?
P1 N1 P2 96.53(10) . . ?
P2 N1 Bi1 88.59(8) . . ?
C10 N1 Bi1 125.42(15) . . ?
C10 N1 P1 123.30(16) . . ?
C10 N1 P2 124.16(17) . . ?
P2 N2 P1 98.41(11) . . ?
C20 N2 P1 125.39(17) . . ?
C20 N2 P2 124.21(17) . . ?
P1 N3 Bi1 110.27(11) . . ?
C30 N3 Bi1 126.92(16) . . ?
C30 N3 P1 121.45(18) . . ?
P2 N4 Bi1 109.63(10) . . ?
C40 N4 Bi1 124.54(16) . . ?
C40 N4 P2 119.71(16) . . ?
Si1 N5 Bi1 112.28(10) . . ?
Si2 N5 Bi1 126.93(12) . . ?
Si2 N5 Si1 120.78(12) . . ?
N1 C10 C11 108.7(2) . . ?
N1 C10 C12 109.7(2) . . ?
N1 C10 C13 108.2(2) . . ?
C11 C10 C12 110.3(2) . . ?
C11 C10 C13 109.8(2) . . ?
C13 C10 C12 110.1(2) . . ?
N2 C20 C21 108.6(2) . . ?
N2 C20 C23 108.8(2) . . ?
N2 C20 C22 110.5(2) . . ?
C21 C20 C23 109.4(2) . . ?
C21 C20 C22 110.1(2) . . ?
C22 C20 C23 109.4(2) . . ?
N3 C30 C31 110.4(2) . . ?
N3 C30 C32 110.7(2) . . ?
N3 C30 C33 109.0(2) . . ?
C31 C30 C32 107.5(2) . . ?
C31 C30 C33 110.4(2) . . ?
C32 C30 C33 108.8(3) . . ?
N4 C40 C41 110.9(2) . . ?
N4 C40 C42 109.8(2) . . ?
N4 C40 C43 109.1(2) . . ?
C42 C40 C41 108.9(2) . . ?
C42 C40 C43 108.8(2) . . ?
C43 C40 C41 109.3(2) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: toluene'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_MAT41_0m
_database_code_depnum_ccdc_archive 'CCDC 1991882'
loop_
_audit_author_name
_audit_author_address
'Lothar Stahl'
;University of North Dakota
United States of America
;
_audit_update_record             
;
2020-03-21 deposited with the CCDC.	2020-04-21 downloaded from the CCDC.
;
_audit_creation_date             2019-02-25
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_chemical_formula_moiety         'C22 H41 N4 P2 Sb'
_chemical_formula_sum            'C22 H41 N4 P2 Sb'
_chemical_formula_weight         545.31
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
_atom_type_scat_dispersion_source
H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236
57.79970 0.0030380000826
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
C 0.00347 0.00161 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870
51.65120 0.215599998832
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
N 0.00653 0.00323 12.21260 3.13220 2.01250 1.16630 0.00570 9.89330 28.99750
0.58260 -11.5290002823
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
P 0.10434 0.09671 6.43450 4.17910 1.78000 1.49080 1.90670 27.15700 0.52600
68.16450 1.11489999294
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
Sb -0.60640 1.48759 19.64180 19.04550 5.03710 2.68270 5.30340 0.46070 27.90740
75.28250 4.59089994431
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2ybc (x-z,y,z)'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x+1/2,y+1/2,-z+1/2
3 -x,-y,-z
4 x-1/2,-y-1/2,z-1/2

_symmetry_Int_Tables_number      14
_cell_length_a                   16.0318(6)
_cell_length_b                   9.6090(4)
_cell_length_c                   18.2097(7)
_cell_angle_alpha                90
_cell_angle_beta                 110.3634(14)
_cell_angle_gamma                90
_cell_volume                     2629.88(18)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9719
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      37.67
_cell_measurement_theta_min      2.30
_exptl_absorpt_coefficient_mu    1.186
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.3771
_exptl_crystal_description       block
_exptl_crystal_F_000             1126.6618
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.75
_exptl_crystal_size_mid          0.74
_exptl_crystal_size_min          0.67
_diffrn_reflns_av_R_equivalents  0.0217
_diffrn_reflns_av_unetI/netI     0.0230
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            36559
_diffrn_reflns_theta_full        26.0000
_diffrn_reflns_theta_max         33.00
_diffrn_reflns_theta_min         2.52
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.9601
_diffrn_measured_fraction_theta_max 0.9468
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_special_details          ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              14
_reflns_limit_h_min              -24
_reflns_limit_k_max              14
_reflns_limit_k_min              0
_reflns_limit_l_max              27
_reflns_limit_l_min              -14
_reflns_number_gt                8743
_reflns_number_total             9401
_reflns_threshold_expression     I>=2u(I)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.5248
_refine_diff_density_min         -0.7472
_refine_diff_density_rms         0.0820
_refine_ls_d_res_high            0.6525
_refine_ls_d_res_low             8.0959
_refine_ls_goodness_of_fit_ref   1.0312
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    58
_refine_ls_number_parameters     274
_refine_ls_number_reflns         9401
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0231
_refine_ls_R_factor_gt           0.0205
_refine_ls_restrained_S_all      1.0312
_refine_ls_shift/su_max          0.0001
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0179P)²+1.8489P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0496
_refine_ls_wR_factor_ref         0.0516
_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:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6)
2.b Idealised Me refined as rotating group:
 C11(H11a,H11b,H11c), C12(H12a,H12b,H12c), C13(H13a,H13b,H13c), C21(H21a,H21b,
 H21c), C22(H22a,H22b,H22c), C23(H23a,H23b,H23c), C31(H31a,H31b,H31c), C32(H32a,
 H32b,H32c), C33(H33a,H33b,H33c), C41(H41a,H41b,H41c), C42(H42a,H42b,H42c),
 C43(H43a,H43b,H43c)
;
_atom_sites_solution_primary     direct
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_refinement_flags_posn
Sb1 Sb 0.150098(5) 1.010579(8) 0.983181(4) 0.01267(2) Uani 1.000000 .
P1 P 0.225503(19) 0.81167(3) 0.884521(17) 0.01157(5) Uani 1.000000 .
P2 P 0.205290(19) 0.69603(3) 1.007868(17) 0.01180(5) Uani 1.000000 .
N1 N 0.14012(6) 0.75366(10) 0.91490(6) 0.01278(16) Uani 1.000000 .
N2 N 0.29073(6) 0.75288(10) 0.97706(6) 0.01284(16) Uani 1.000000 .
N3 N 0.20995(7) 0.98011(10) 0.89787(6) 0.01409(17) Uani 1.000000 .
N4 N 0.18471(7) 0.83332(10) 1.05548(6) 0.01311(16) Uani 1.000000 .
C1 C 0.25952(8) 1.13292(12) 1.05902(7) 0.0159(2) Uani 1.000000 .
C2 C 0.24543(9) 1.26905(13) 1.07855(8) 0.0194(2) Uani 1.000000 .
H2 H 0.18751(9) 1.30825(13) 1.05796(8) 0.0233(3) Uiso 1.000000 R
C3 C 0.31522(11) 1.34812(15) 1.12783(8) 0.0254(3) Uani 1.000000 .
H3 H 0.30474(11) 1.44051(15) 1.14105(8) 0.0305(3) Uiso 1.000000 R
C4 C 0.39985(11) 1.29214(16) 1.15754(8) 0.0268(3) Uani 1.000000 .
H4 H 0.44762(11) 1.34629(16) 1.19090(8) 0.0322(3) Uiso 1.000000 R
C5 C 0.41505(9) 1.15645(16) 1.13859(8) 0.0243(3) Uani 1.000000 .
H5 H 0.47311(9) 1.11772(16) 1.15925(8) 0.0291(3) Uiso 1.000000 R
C6 C 0.34524(9) 1.07772(14) 1.08943(8) 0.0203(2) Uani 1.000000 .
H6 H 0.35596(9) 0.98534(14) 1.07637(8) 0.0244(3) Uiso 1.000000 R
C10 C 0.05468(8) 0.69496(14) 0.86336(7) 0.0175(2) Uani 1.000000 .
C11 C -0.00857(8) 0.68605(16) 0.90957(9) 0.0231(3) Uani 1.000000 .
H11a H 0.0159(4) 0.6219(10) 0.9537(4) 0.0347(4) Uiso 1.000000 GR
H11b H -0.0155(6) 0.7786(3) 0.9293(6) 0.0347(4) Uiso 1.000000 GR
H11c H -0.0667(3) 0.6519(12) 0.8753(2) 0.0347(4) Uiso 1.000000 GR
C12 C 0.06872(11) 0.54993(17) 0.83543(11) 0.0322(3) Uani 1.000000 .
H12a H 0.1084(8) 0.5561(3) 0.8050(7) 0.0482(5) Uiso 1.000000 GR
H12b H 0.0955(9) 0.4893(4) 0.88084(11) 0.0482(5) Uiso 1.000000 GR
H12c H 0.01130(17) 0.5113(6) 0.8025(7) 0.0482(5) Uiso 1.000000 GR
C13 C 0.01641(9) 0.79227(18) 0.79337(8) 0.0279(3) Uani 1.000000 .
H13a H 0.0096(8) 0.8858(4) 0.81201(9) 0.0419(4) Uiso 1.000000 GR
H13b H 0.0569(4) 0.7960(11) 0.7636(4) 0.0419(4) Uiso 1.000000 GR
H13c H -0.0417(4) 0.7575(7) 0.7596(4) 0.0419(4) Uiso 1.000000 GR
C20 C 0.37627(7) 0.67941(12) 0.99337(7) 0.01411(19) Uani 1.000000 .
C21 C 0.43260(8) 0.76188(15) 0.95608(9) 0.0228(3) Uani 1.000000 .
H21a H 0.4026(4) 0.7642(11) 0.89913(10) 0.0342(4) Uiso 1.000000 GR
H21b H 0.4405(7) 0.8571(4) 0.9766(5) 0.0342(4) Uiso 1.000000 GR
H21c H 0.4909(3) 0.7173(7) 0.9686(6) 0.0342(4) Uiso 1.000000 GR
C22 C 0.36107(9) 0.53169(14) 0.95934(8) 0.0201(2) Uani 1.000000 .
H22a H 0.3244(7) 0.4793(4) 0.9830(5) 0.0301(3) Uiso 1.000000 GR
H22b H 0.3306(7) 0.53654(14) 0.90250(13) 0.0301(3) Uiso 1.000000 GR
H22c H 0.41852(10) 0.4849(5) 0.9708(6) 0.0301(3) Uiso 1.000000 GR
C23 C 0.42417(8) 0.67335(14) 1.08196(7) 0.0184(2) Uani 1.000000 .
H23a H 0.4360(6) 0.76813(14) 1.10289(11) 0.0276(3) Uiso 1.000000 GR
H23b H 0.3867(3) 0.6248(10) 1.10628(10) 0.0276(3) Uiso 1.000000 GR
H23c H 0.4805(3) 0.6232(10) 1.09356(8) 0.0276(3) Uiso 1.000000 GR
C30 C 0.23145(9) 1.09473(13) 0.85221(7) 0.0184(2) Uani 1.000000 .
C31 C 0.17456(12) 1.22161(15) 0.85310(10) 0.0315(3) Uani 1.000000 .
H31a H 0.11156(13) 1.1953(4) 0.8332(7) 0.0473(5) Uiso 1.000000 GR
H31b H 0.1905(6) 1.2563(9) 0.90685(15) 0.0473(5) Uiso 1.000000 GR
H31c H 0.1851(7) 1.2947(5) 0.8198(6) 0.0473(5) Uiso 1.000000 GR
C32 C 0.20964(15) 1.05026(17) 0.76699(9) 0.0361(4) Uani 1.000000 .
H32a H 0.2464(7) 0.9700(10) 0.76478(11) 0.0542(6) Uiso 1.000000 GR
H32b H 0.1466(3) 1.0247(14) 0.7445(3) 0.0542(6) Uiso 1.000000 GR
H32c H 0.2219(9) 1.1275(5) 0.7371(2) 0.0542(6) Uiso 1.000000 GR
C33 C 0.32943(11) 1.13571(18) 0.88703(11) 0.0340(3) Uani 1.000000 .
H33a H 0.3433(2) 1.1655(14) 0.9414(3) 0.0510(5) Uiso 1.000000 GR
H33b H 0.36659(11) 1.0556(5) 0.8855(8) 0.0510(5) Uiso 1.000000 GR
H33c H 0.3413(2) 1.2123(10) 0.8565(5) 0.0510(5) Uiso 1.000000 GR
C40 C 0.17959(8) 0.82382(12) 1.13553(7) 0.01429(19) Uani 1.000000 .
C41 C 0.27227(9) 0.80413(18) 1.19646(8) 0.0276(3) Uani 1.000000 .
H41a H 0.2982(4) 0.7175(7) 1.1857(5) 0.0414(4) Uiso 1.000000 GR
H41b H 0.3101(3) 0.8828(7) 1.1940(5) 0.0414(4) Uiso 1.000000 GR
H41c H 0.26803(14) 0.7994(14) 1.24880(11) 0.0414(4) Uiso 1.000000 GR
C42 C 0.12051(12) 0.70085(17) 1.13983(10) 0.0333(4) Uani 1.000000 .
H42a H 0.0601(3) 0.7155(7) 1.1026(6) 0.0500(5) Uiso 1.000000 GR
H42b H 0.1448(5) 0.6147(3) 1.1266(8) 0.0500(5) Uiso 1.000000 GR
H42c H 0.1189(8) 0.6938(9) 1.1930(2) 0.0500(5) Uiso 1.000000 GR
C43 C 0.13836(10) 0.95607(15) 1.15381(8) 0.0240(3) Uani 1.000000 .
H43a H 0.1764(4) 1.0358(2) 1.1535(7) 0.0361(4) Uiso 1.000000 GR
H43b H 0.0793(4) 0.9699(7) 1.1141(4) 0.0361(4) Uiso 1.000000 GR
H43c H 0.1329(8) 0.9477(5) 1.2056(3) 0.0361(4) Uiso 1.000000 GR


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
Sb1 N3 2.1113(10) . ?
Sb1 N4 2.1057(10) . ?
Sb1 C1 2.1635(12) . ?
P1 P2 2.6252(4) . ?
P1 N1 1.7371(9) . ?
P1 N2 1.7395(10) . ?
P1 N3 1.6682(10) . ?
P2 N1 1.7416(10) . ?
P2 N2 1.7390(9) . ?
P2 N4 1.6734(10) . ?
N1 C10 1.4767(15) . ?
N2 C20 1.4778(14) . ?
N3 C30 1.4908(15) . ?
N4 C40 1.4911(14) . ?
C1 C2 1.3944(17) . ?
C1 C6 1.3953(18) . ?
C2 C3 1.391(2) . ?
C3 C4 1.383(2) . ?
C4 C5 1.392(2) . ?
C5 C6 1.3889(19) . ?
C10 C11 1.5288(17) . ?
C10 C12 1.5268(19) . ?
C10 C13 1.527(2) . ?
C20 C21 1.5270(16) . ?
C20 C22 1.5340(18) . ?
C20 C23 1.5276(17) . ?
C30 C31 1.5260(19) . ?
C30 C32 1.528(2) . ?
C30 C33 1.527(2) . ?
C40 C41 1.5256(19) . ?
C40 C42 1.5332(19) . ?
C40 C43 1.5217(17) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N4 Sb1 N3 105.04(4) . . ?
C1 Sb1 N3 94.01(4) . . ?
C1 Sb1 N4 93.54(4) . . ?
N1 P1 P2 41.07(3) . . ?
N2 P1 P2 40.99(3) . . ?
N2 P1 N1 82.06(5) . . ?
N3 P1 P2 102.52(4) . . ?
N3 P1 N1 95.20(5) . . ?
N3 P1 N2 104.12(5) . . ?
N1 P2 P1 40.94(3) . . ?
N2 P2 P1 41.01(3) . . ?
N2 P2 N1 81.95(5) . . ?
N4 P2 P1 102.41(3) . . ?
N4 P2 N1 95.35(5) . . ?
N4 P2 N2 103.82(5) . . ?
P2 N1 P1 97.99(5) . . ?
C10 N1 P1 125.42(8) . . ?
C10 N1 P2 127.33(8) . . ?
P2 N2 P1 98.00(5) . . ?
C20 N2 P1 123.56(7) . . ?
C20 N2 P2 124.41(8) . . ?
P1 N3 Sb1 111.77(5) . . ?
C30 N3 Sb1 124.09(7) . . ?
C30 N3 P1 124.07(8) . . ?
P2 N4 Sb1 111.73(5) . . ?
C40 N4 Sb1 124.65(7) . . ?
C40 N4 P2 123.10(8) . . ?
C2 C1 Sb1 120.34(10) . . ?
C6 C1 Sb1 120.97(9) . . ?
C6 C1 C2 118.69(12) . . ?
C3 C2 C1 120.76(13) . . ?
C4 C3 C2 119.95(13) . . ?
C5 C4 C3 120.00(13) . . ?
C6 C5 C4 119.92(14) . . ?
C5 C6 C1 120.68(13) . . ?
C11 C10 N1 108.53(10) . . ?
C12 C10 N1 110.41(11) . . ?
C12 C10 C11 109.58(11) . . ?
C13 C10 N1 108.12(10) . . ?
C13 C10 C11 110.06(11) . . ?
C13 C10 C12 110.11(12) . . ?
C21 C20 N2 108.29(9) . . ?
C22 C20 N2 110.80(10) . . ?
C22 C20 C21 109.63(10) . . ?
C23 C20 N2 108.71(9) . . ?
C23 C20 C21 109.37(10) . . ?
C23 C20 C22 110.00(10) . . ?
C31 C30 N3 109.22(10) . . ?
C32 C30 N3 110.13(11) . . ?
C32 C30 C31 107.92(13) . . ?
C33 C30 N3 111.29(11) . . ?
C33 C30 C31 108.78(13) . . ?
C33 C30 C32 109.43(13) . . ?
C41 C40 N4 110.33(9) . . ?
C42 C40 N4 110.01(10) . . ?
C42 C40 C41 109.27(12) . . ?
C43 C40 N4 109.79(10) . . ?
C43 C40 C41 109.38(11) . . ?
C43 C40 C42 108.02(11) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_chemical_melting_point          435-437
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: toluene'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_J_MUS_01_CPTPI_0m
_database_code_depnum_ccdc_archive 'CCDC 1991892'
loop_
_audit_author_name
_audit_author_address
'Matthias Zeller'
;Purdue University
United States of America
;
_audit_update_record             
;
2020-03-21 deposited with the CCDC.	2020-04-21 downloaded from the CCDC.
;
_audit_creation_date             2020-03-21
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_chemical_formula_moiety         'C16 H36 I N4 P3'
_chemical_formula_sum            'C16 H36 I N4 P3'
_chemical_formula_weight         504.32
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
_atom_type_scat_dispersion_source
I -0.41187 1.83264 20.14720 18.99490 7.51380 2.27350 4.34700 0.38140 27.76600
66.87760 4.07119989395
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236
57.79970 0.0030380000826
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
C 0.00347 0.00161 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870
51.65120 0.215599998832
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
N 0.00653 0.00323 12.21260 3.13220 2.01250 1.16630 0.00570 9.89330 28.99750
0.58260 -11.5290002823
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
P 0.10434 0.09671 6.43450 4.17910 1.78000 1.49080 1.90670 27.15700 0.52600
68.16450 1.11489999294
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'

_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_H-M_alt        'P 1 21/m 1'
_space_group_name_Hall           '-P 2yb'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,y+1/2,-z
3 -x,-y,-z
4 x,-y-1/2,z

_symmetry_Int_Tables_number      11
_cell_length_a                   9.5405(7)
_cell_length_b                   11.8694(8)
_cell_length_c                   10.3274(7)
_cell_angle_alpha                90
_cell_angle_beta                 96.573(2)
_cell_angle_gamma                90
_cell_volume                     1161.79(14)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9907
_cell_measurement_temperature    150
_cell_measurement_theta_max      33.203
_cell_measurement_theta_min      2.626
_exptl_absorpt_coefficient_mu    1.591
_exptl_absorpt_correction_T_max  0.564
_exptl_absorpt_correction_T_min  0.455
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.4415
_exptl_crystal_description       cube
_exptl_crystal_F_000             515.9084
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.41
_exptl_crystal_size_min          0.38
_diffrn_reflns_av_R_equivalents  0.0261
_diffrn_reflns_av_unetI/netI     0.0163
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            26788
_diffrn_reflns_theta_full        33.2216
_diffrn_reflns_theta_max         33.22
_diffrn_reflns_theta_min         2.62
_diffrn_ambient_temperature      149.99
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.9944
_diffrn_measured_fraction_theta_max 0.9940
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker Quest Photon100 CMOS'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'Incoatec I\ms'
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              18
_reflns_limit_k_min              0
_reflns_limit_l_max              15
_reflns_limit_l_min              0
_reflns_number_gt                4262
_reflns_number_total             4626
_reflns_threshold_expression     I>=2u(I)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         0.6691
_refine_diff_density_min         -0.7073
_refine_diff_density_rms         0.0709
_refine_ls_d_res_high            0.6486
_refine_ls_d_res_low             7.7618
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_goodness_of_fit_ref   1.0401
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    28
_refine_ls_number_parameters     127
_refine_ls_number_reflns         4626
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0225
_refine_ls_R_factor_gt           0.0192
_refine_ls_restrained_S_all      1.0401
_refine_ls_shift/su_max          0.0004
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0150P)²+0.5951P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0435
_refine_ls_wR_factor_ref         0.0452
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: H11b(0.5) H11c(0.5) H22b(0.5) H22c(0.5)
3.a Me refined with riding coordinates:
 C11(H11a,H11b,H11c), C22(H22a,H22b,H22c)
3.b Idealised Me refined as rotating group:
 C23(H23b,H23c,H23a), C32(H32a,H32b,H32c), C33(H33a,H33b,H33c), C13(H13c,H13a,
 H13b), C31(H31a,H31b,H31c)
;
_atom_sites_solution_primary     iterative
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_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_group
I1 I 0.857105(12) 0.25 0.519890(9) 0.02682(4) Uani 1.000000 2 S T P .
C23 C 0.43431(15) 0.35530(11) 0.39128(14) 0.0361(3) Uani 1.000000 1 . . . .
H23b H 0.3512(6) 0.3563(5) 0.4390(9) 0.0541(4) Uiso 1.000000 1 GR . . .
H23c H 0.5200(6) 0.3547(5) 0.4534(7) 0.0541(4) Uiso 1.000000 1 GR . . .
H23a H 0.4339(12) 0.42251(11) 0.33613(17) 0.0541(4) Uiso 1.000000 1 GR . . .
N3 N 0.78975(8) 0.13806(6) 0.20452(7) 0.01354(13) Uani 1.000000 1 . . . .
P1 P 0.88636(3) 0.25 0.25961(3) 0.01382(6) Uani 1.000000 2 S T P .
N1 N 0.61357(11) 0.25 0.02921(11) 0.01455(19) Uani 1.000000 2 S T P .
C30 C 0.85258(10) 0.02174(8) 0.23096(9) 0.01738(16) Uani 1.000000 1 . . . .
P2 P 0.61122(2) 0.14369(2) 0.14195(2) 0.01413(5) Uani 1.000000 1 . . . .
N2 N 0.56001(12) 0.25 0.23893(11) 0.01576(19) Uani 1.000000 2 S T P .
C32 C 0.82691(12) -0.04873(9) 0.10629(11) 0.0252(2) Uani 1.000000 1 . . . .
H32a H 0.72524(13) -0.0547(7) 0.0797(5) 0.0378(3) Uiso 1.000000 1 GR . . .
H32b H 0.8723(9) -0.0124(4) 0.0368(3) 0.0378(3) Uiso 1.000000 1 GR . . .
H32c H 0.8667(9) -0.1242(3) 0.1226(3) 0.0378(3) Uiso 1.000000 1 GR . . .
C33 C 0.78195(12) -0.03488(9) 0.34007(11) 0.02379(19) Uani 1.000000 1 . . . .
H33a H 0.7979(9) 0.0108(4) 0.4194(3) 0.0357(3) Uiso 1.000000 1 GR . . .
H33b H 0.6804(2) -0.0416(8) 0.3134(4) 0.0357(3) Uiso 1.000000 1 GR . . .
H33c H 0.8225(7) -0.1100(3) 0.3571(7) 0.0357(3) Uiso 1.000000 1 GR . . .
C10 C 0.66918(14) 0.25 -0.09890(13) 0.0174(2) Uani 1.000000 2 S T P .
C11 C 0.83054(15) 0.25 -0.08865(14) 0.0225(3) Uani 1.000000 2 S T P .
H11a H 0.86049(15) 0.25 -0.17631(14) 0.0337(4) Uiso 1.000000 2 RS T P -1
H11b H 0.86721(15) 0.317414245818 -0.04154(14) 0.0337(4) Uiso 0.500000 1 R . .
-1
H11c H 0.86721(15) 0.182585754182 -0.04154(14) 0.0337(4) Uiso 0.500000 1 R . .
-1
C13 C 0.61377(15) 0.35537(12) -0.17188(12) 0.0346(3) Uani 1.000000 1 . . . .
H13c H 0.51040(15) 0.3552(5) -0.1809(10) 0.0519(4) Uiso 1.000000 1 GR . . .
H13a H 0.6491(10) 0.42240(12) -0.1232(6) 0.0519(4) Uiso 1.000000 1 GR . . .
H13b H 0.6462(10) 0.3563(5) -0.2585(4) 0.0519(4) Uiso 1.000000 1 GR . . .
C20 C 0.43081(15) 0.25 0.30613(15) 0.0224(3) Uani 1.000000 2 S T P .
C22 C 0.29947(17) 0.25 0.2063(2) 0.0381(4) Uani 1.000000 2 S T P .
H22a H 0.21482(17) 0.25 0.2519(2) 0.0571(6) Uiso 1.000000 2 RS T P -1
H22b H 0.29969(17) 0.317414245818 0.1516(2) 0.0571(6) Uiso 0.500000 1 R . . -1
H22c H 0.29969(17) 0.182585754182 0.1516(2) 0.0571(6) Uiso 0.500000 1 R . . -1
C31 C 1.01204(11) 0.02923(9) 0.27082(12) 0.0254(2) Uani 1.000000 1 . . . .
H31a H 1.05687(17) 0.0667(7) 0.2017(4) 0.0381(3) Uiso 1.000000 1 GR . . .
H31b H 1.03026(12) 0.0726(7) 0.3518(5) 0.0381(3) Uiso 1.000000 1 GR . . .
H31c H 1.0509(2) -0.04681(10) 0.2845(9) 0.0381(3) Uiso 1.000000 1 GR . . .


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
I1 P1 2.7340(4) . ?
C23 C20 1.5263(15) 4_565 ?
N3 P1 1.6788(8) . ?
N3 C30 1.5174(12) . ?
N3 P2 1.7525(8) . ?
N1 P2 1.7188(8) 4_565 ?
N1 P2 1.7188(8) . ?
N1 C10 1.4808(17) . ?
C30 C32 1.5314(14) . ?
C30 C33 1.5327(14) . ?
C30 C31 1.5324(14) . ?
P2 P2 2.5236(5) 4_565 ?
P2 N2 1.7164(8) . ?
N2 C20 1.4822(17) . ?
C10 C11 1.531(2) . ?
C10 C13 1.5233(14) 4_565 ?
C10 C13 1.5233(14) . ?
C20 C22 1.529(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C30 N3 P1 117.96(6) . . ?
P2 N3 P1 124.57(5) . . ?
P2 N3 C30 116.64(6) . . ?
N3 P1 I1 102.67(3) 4_565 . ?
N3 P1 I1 102.67(3) . . ?
N3 P1 N3 104.64(5) 4_565 . ?
P2 N1 P2 94.46(6) 4_565 . ?
C10 N1 P2 129.72(4) . . ?
C10 N1 P2 129.72(4) . 4_565 ?
C32 C30 N3 108.90(8) . . ?
C33 C30 N3 109.47(8) . . ?
C33 C30 C32 109.70(8) . . ?
C31 C30 N3 110.80(8) . . ?
C31 C30 C32 108.41(8) . . ?
C31 C30 C33 109.54(8) . . ?
N1 P2 N3 100.97(4) . . ?
P2 P2 N3 92.19(3) 4_565 . ?
P2 P2 N1 42.77(3) 4_565 . ?
N2 P2 N3 98.19(5) . . ?
N2 P2 N1 83.24(4) . . ?
P2 N2 P2 94.64(6) 4_565 . ?
C20 N2 P2 125.50(5) . 4_565 ?
C20 N2 P2 125.50(5) . . ?
C11 C10 N1 113.49(11) . . ?
C13 C10 N1 107.61(8) 4_565 . ?
C13 C10 N1 107.61(8) . . ?
C13 C10 C11 108.87(9) . . ?
C13 C10 C11 108.87(9) 4_565 . ?
C13 C10 C13 110.38(14) . 4_565 ?
C23 C20 C23 109.94(14) . 4_565 ?
N2 C20 C23 107.77(8) . . ?
N2 C20 C23 107.77(8) . 4_565 ?
C22 C20 C23 110.53(9) . 4_565 ?
C22 C20 C23 110.53(9) . . ?
C22 C20 N2 110.23(13) . . ?

_olex2_submission_original_sample_id 1h
_olex2_submission_special_instructions 'No special instructions were received'
_chemical_melting_point          485-487
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: THF'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_J_MUS_02_CPTAsI_0m
_database_code_depnum_ccdc_archive 'CCDC 1991885'
loop_
_audit_author_name
_audit_author_address
'Matthias Zeller'
;Purdue University
United States of America
;
_audit_update_record             
;
2020-03-21 deposited with the CCDC.	2020-04-21 downloaded from the CCDC.
;
_audit_creation_date             2020-03-17
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_chemical_formula_moiety         'C16 H36 As I N4 P2'
_chemical_formula_sum            'C16 H36 As I N4 P2'
_chemical_formula_weight         548.26
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
_atom_type_scat_dispersion_source
C 0.00347 0.00161 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870
51.65120 0.215599998832
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
I -0.41187 1.83264 20.14720 18.99490 7.51380 2.27350 4.34700 0.38140 27.76600
66.87760 4.07119989395
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236
57.79970 0.0030380000826
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
N 0.00653 0.00323 12.21260 3.13220 2.01250 1.16630 0.00570 9.89330 28.99750
0.58260 -11.5290002823
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
P 0.10434 0.09671 6.43450 4.17910 1.78000 1.49080 1.90670 27.15700 0.52600
68.16450 1.11489999294
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
As 0.07000 2.09310 16.67230 6.07010 3.43130 4.27790 2.63450 0.26470 12.94790
47.79720 2.53099989891
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'

_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_H-M_alt        'P 1 21/m 1'
_space_group_name_Hall           '-P 2yb'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,y+1/2,-z
3 -x,-y,-z
4 x,-y-1/2,z

_symmetry_Int_Tables_number      11
_cell_length_a                   9.5274(8)
_cell_length_b                   11.9897(9)
_cell_length_c                   10.3478(7)
_cell_angle_alpha                90
_cell_angle_beta                 96.533(3)
_cell_angle_gamma                90
_cell_volume                     1174.36(15)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9007
_cell_measurement_temperature    150
_cell_measurement_theta_max      33.214
_cell_measurement_theta_min      2.742
_exptl_absorpt_coefficient_mu    2.904
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.4889
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1152 before and 0.0423 after correction. The Ratio of minimum to maximum transmission is 0.6549. The λ/2 correction factor is Not present.'
_exptl_crystal_colour            'dull yellowish yellow'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.5504
_exptl_crystal_description       plate
_exptl_crystal_F_000             551.8509
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.41
_exptl_crystal_size_min          0.22
_diffrn_reflns_av_R_equivalents  0.0307
_diffrn_reflns_av_unetI/netI     0.0196
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            28533
_diffrn_reflns_theta_full        33.2342
_diffrn_reflns_theta_max         33.23
_diffrn_reflns_theta_min         2.61
_diffrn_ambient_temperature      149.99
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.9964
_diffrn_measured_fraction_theta_max 0.9964
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker Quest Photon100 CMOS'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              18
_reflns_limit_k_min              0
_reflns_limit_l_max              15
_reflns_limit_l_min              0
_reflns_number_gt                4112
_reflns_number_total             4681
_reflns_threshold_expression     I>=2u(I)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         1.2625
_refine_diff_density_min         -0.8886
_refine_diff_density_rms         0.1008
_refine_ls_d_res_high            0.6484
_refine_ls_d_res_low             7.8044
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_goodness_of_fit_ref   1.0219
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    28
_refine_ls_number_parameters     127
_refine_ls_number_reflns         4681
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0294
_refine_ls_R_factor_gt           0.0225
_refine_ls_restrained_S_all      1.0219
_refine_ls_shift/su_max          0.0003
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0118P)²+1.1000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0463
_refine_ls_wR_factor_ref         0.0493
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: H11b(0.5) H11c(0.5) H21b(0.5) H21c(0.5)
3.a Me refined with riding coordinates:
 C11(H11a,H11b,H11c), C21(H21a,H21b,H21c)
3.b Idealised Me refined as rotating group:
 C32(H32a,H32b,H32c), C33(H33a,H33b,H33c), C12(H12a,H12b,H12c), C22(H22a,H22b,
 H22c), C31(H31a,H31b,H31c)
;
_atom_sites_solution_primary     iterative
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_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_group
I1 I 0.862430(17) 0.25 0.518786(12) 0.02999(5) Uani 1.000000 2 S T P .
N3 N 0.78668(11) 0.13062(8) 0.19924(10) 0.01518(18) Uani 1.000000 1 . . . .
As1 As 0.895863(18) 0.25 0.259529(17) 0.01512(5) Uani 1.000000 2 S T P .
C10 C 0.6730(2) 0.25 -0.09989(17) 0.0188(3) Uani 1.000000 2 S T P .
N2 N 0.56242(16) 0.25 0.23652(15) 0.0172(3) Uani 1.000000 2 S T P .
P1 P 0.61094(3) 0.14372(3) 0.13851(3) 0.01578(6) Uani 1.000000 1 . . . .
N1 N 0.61708(16) 0.25 0.02785(14) 0.0163(3) Uani 1.000000 2 S T P .
C32 C 0.81764(18) -0.05599(12) 0.10464(15) 0.0293(3) Uani 1.000000 1 . . . .
H32a H 0.7156(2) -0.0598(9) 0.0783(7) 0.0439(4) Uiso 1.000000 1 GR . . .
H32b H 0.8644(12) -0.0225(6) 0.0345(4) 0.0439(4) Uiso 1.000000 1 GR . . .
H32c H 0.8547(12) -0.1314(3) 0.1225(4) 0.0439(4) Uiso 1.000000 1 GR . . .
C33 C 0.77574(17) -0.03792(12) 0.33863(15) 0.0266(3) Uani 1.000000 1 . . . .
H33a H 0.7930(11) 0.0086(6) 0.4167(4) 0.0399(4) Uiso 1.000000 1 GR . . .
H33b H 0.6738(2) -0.0441(10) 0.3131(5) 0.0399(4) Uiso 1.000000 1 GR . . .
H33c H 0.8155(10) -0.1124(4) 0.3571(8) 0.0399(4) Uiso 1.000000 1 GR . . .
C11 C 0.8341(2) 0.25 -0.08883(19) 0.0240(4) Uani 1.000000 2 S T P .
H11a H 0.8647(2) 0.25 -0.17609(19) 0.0360(6) Uiso 1.000000 2 RS T P -1
H11b H 0.8705(2) 0.31673783742 -0.04165(19) 0.0360(6) Uiso 0.500000 1 R . . -1
H11c H 0.8705(2) 0.18326216258 -0.04165(19) 0.0360(6) Uiso 0.500000 1 R . . -1
C12 C 0.6181(2) 0.14573(16) -0.17273(16) 0.0390(4) Uani 1.000000 1 . . . .
H12a H 0.6527(13) 0.07944(16) -0.1236(7) 0.0585(6) Uiso 1.000000 1 GR . . .
H12b H 0.5146(2) 0.1461(6) -0.1827(13) 0.0585(6) Uiso 1.000000 1 GR . . .
H12c H 0.6517(13) 0.1445(6) -0.2588(6) 0.0585(6) Uiso 1.000000 1 GR . . .
C20 C 0.4350(2) 0.25 0.3061(2) 0.0246(4) Uani 1.000000 2 S T P .
C22 C 0.4402(2) 0.35417(15) 0.39130(18) 0.0394(4) Uani 1.000000 1 . . . .
H22a H 0.5280(7) 0.3543(6) 0.4507(10) 0.0590(6) Uiso 1.000000 1 GR . . .
H22b H 0.4368(16) 0.42077(15) 0.33611(19) 0.0590(6) Uiso 1.000000 1 GR . . .
H22c H 0.3593(9) 0.3543(6) 0.4418(11) 0.0590(6) Uiso 1.000000 1 GR . . .
C21 C 0.3021(2) 0.25 0.2095(3) 0.0453(7) Uani 1.000000 2 S T P .
H21a H 0.2187(2) 0.25 0.2568(3) 0.0679(10) Uiso 1.000000 2 RS T P -1
H21b H 0.3010(2) 0.31673783742 0.1547(3) 0.0679(10) Uiso 0.500000 1 R . . -1
H21c H 0.3010(2) 0.18326216258 0.1547(3) 0.0679(10) Uiso 0.500000 1 R . . -1
C31 C 1.00561(15) 0.02118(13) 0.26570(16) 0.0278(3) Uani 1.000000 1 . . . .
H31a H 1.0505(2) 0.0569(9) 0.1958(5) 0.0417(4) Uiso 1.000000 1 GR . . .
H31b H 1.02547(16) 0.0647(9) 0.3458(7) 0.0417(4) Uiso 1.000000 1 GR . . .
H31c H 1.0432(2) -0.05445(14) 0.2800(12) 0.0417(4) Uiso 1.000000 1 GR . . .
C30 C 0.84606(14) 0.01545(11) 0.22753(13) 0.0196(2) Uani 1.000000 1 . . . .


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
I1 As1 2.7373(3) . ?
N3 As1 1.8364(10) . ?
N3 P1 1.7273(11) . ?
N3 C30 1.5083(16) . ?
C10 N1 1.480(2) . ?
C10 C11 1.525(3) . ?
C10 C12 1.5214(19) . ?
C10 C12 1.5214(19) 4_565 ?
N2 P1 1.7242(10) 4_565 ?
N2 P1 1.7242(10) . ?
N2 C20 1.480(2) . ?
P1 P1 2.5486(7) 4_565 ?
P1 N1 1.7187(10) . ?
C32 C30 1.532(2) . ?
C33 C30 1.5347(18) . ?
C20 C22 1.526(2) . ?
C20 C22 1.526(2) 4_565 ?
C20 C21 1.521(3) . ?
C31 C30 1.528(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
P1 N3 As1 122.75(6) . . ?
C30 N3 As1 117.52(8) . . ?
C30 N3 P1 118.72(8) . . ?
N3 As1 I1 102.03(3) . . ?
N3 As1 I1 102.03(3) 4_565 . ?
N3 As1 N3 102.41(6) 4_565 . ?
C11 C10 N1 113.22(15) . . ?
C12 C10 N1 107.69(11) 4_565 . ?
C12 C10 N1 107.69(11) . . ?
C12 C10 C11 108.87(12) 4_565 . ?
C12 C10 C11 108.87(12) . . ?
C12 C10 C12 110.50(19) 4_565 . ?
P1 N2 P1 95.31(7) 4_565 . ?
C20 N2 P1 125.14(7) . 4_565 ?
C20 N2 P1 125.14(7) . . ?
N2 P1 N3 99.61(6) . . ?
P1 P1 N3 95.22(4) 4_565 . ?
P1 P1 N2 42.35(4) 4_565 . ?
N1 P1 N3 101.81(6) . . ?
N1 P1 N2 82.86(5) . . ?
P1 N1 C10 129.64(5) . . ?
P1 N1 C10 129.64(5) 4_565 . ?
P1 N1 P1 95.71(7) 4_565 . ?
C22 C20 N2 107.82(11) . . ?
C22 C20 N2 107.82(11) 4_565 . ?
C22 C20 C22 109.82(19) . 4_565 ?
C21 C20 N2 110.37(18) . . ?
C21 C20 C22 110.47(13) . 4_565 ?
C21 C20 C22 110.47(13) . . ?
C32 C30 N3 108.90(11) . . ?
C33 C30 N3 109.94(10) . . ?
C33 C30 C32 109.74(12) . . ?
C31 C30 N3 110.44(11) . . ?
C31 C30 C32 108.45(12) . . ?
C31 C30 C33 109.35(12) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_chemical_melting_point          459-461
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: THF'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_J_MUS_15_CPTSbI_0m
_database_code_depnum_ccdc_archive 'CCDC 1991886'
loop_
_audit_author_name
_audit_author_address
'Matthias Zeller'
;Purdue University
United States of America
;
_audit_update_record             
;
2020-03-21 deposited with the CCDC.	2020-04-21 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT919_J_MUS_15_CPTSbI_0m  
;
PROBLEM: Reflection # Likely Affected by the Beamstop ...          1 Check
RESPONSE: One reflection must have been blocked by the beamstop.
;
# Added during the CSD deposition process: Saturday 21 March 2020 07:19 PM
# end Validation Reply Form

_audit_creation_date             2020-03-17
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_chemical_formula_moiety         'C16 H36 I N4 P2 Sb'
_chemical_formula_sum            'C16 H36 I N4 P2 Sb'
_chemical_formula_weight         595.10
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
_atom_type_scat_dispersion_source
C 0.00347 0.00161 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870
51.65120 0.215599998832
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
I -0.41187 1.83264 20.14720 18.99490 7.51380 2.27350 4.34700 0.38140 27.76600
66.87760 4.07119989395
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236
57.79970 0.0030380000826
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
N 0.00653 0.00323 12.21260 3.13220 2.01250 1.16630 0.00570 9.89330 28.99750
0.58260 -11.5290002823
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
P 0.10434 0.09671 6.43450 4.17910 1.78000 1.49080 1.90670 27.15700 0.52600
68.16450 1.11489999294
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
Sb -0.60640 1.48759 19.64180 19.04550 5.03710 2.68270 5.30340 0.46070 27.90740
75.28250 4.59089994431
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,y+1/2,-z+1/2
3 -x,-y,-z
4 x,-y-1/2,z-1/2

_symmetry_Int_Tables_number      14
_cell_length_a                   9.6060(6)
_cell_length_b                   18.7374(12)
_cell_length_c                   26.7135(18)
_cell_angle_alpha                90
_cell_angle_beta                 93.325(3)
_cell_angle_gamma                90
_cell_volume                     4800.1(5)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    9778
_cell_measurement_temperature    150
_cell_measurement_theta_max      30.536
_cell_measurement_theta_min      2.304
_exptl_absorpt_coefficient_mu    2.576
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.4910
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1060 before and 0.0587 after correction. The Ratio of minimum to maximum transmission is 0.6581. The λ/2 correction factor is Not present.'
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.6468
_exptl_crystal_description       needle
_exptl_crystal_F_000             2346.0371
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.09
_diffrn_reflns_av_R_equivalents  0.0482
_diffrn_reflns_av_unetI/netI     0.0373
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            68044
_diffrn_reflns_theta_full        30.5841
_diffrn_reflns_theta_max         30.58
_diffrn_reflns_theta_min         2.30
_diffrn_ambient_temperature      150.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.9908
_diffrn_measured_fraction_theta_max 0.9908
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker Quest Photon100 CMOS'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              26
_reflns_limit_k_min              0
_reflns_limit_l_max              38
_reflns_limit_l_min              0
_reflns_number_gt                11523
_reflns_number_total             14615
_reflns_threshold_expression     I>=2u(I)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_refine_diff_density_max         1.8898
_refine_diff_density_min         -1.4551
_refine_diff_density_rms         0.2126
_refine_ls_d_res_high            0.6984
_refine_ls_d_res_low             8.8391
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_goodness_of_fit_ref   1.0235
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    96
_refine_ls_number_parameters     458
_refine_ls_number_reflns         14615
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0501
_refine_ls_R_factor_gt           0.0333
_refine_ls_restrained_S_all      1.0235
_refine_ls_shift/su_max          0.0008
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0314P)²+8.1471P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0732
_refine_ls_wR_factor_ref         0.0806
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C42B(H42a,H42b,H42c), C41B(H41a,H41b,H41c), C43B(H43a,H43b,H43c), C11B(H11a,
 H11b,H11c), C21A(H21d,H21e,H21f), C22A(H22d,H22e,H22f), C23A(H23d,H23e,H23f),
 C21B(H21a,H21b,H21c), C22B(H22a,H22b,H22c), C33A(H33d,H33e,H33f), C31A(H31d,
 H31e,H31f), C32A(H32d,H32e,H32f), C11A(H11d,H11e,H11f), C13A(H13d,H13e,H13f),
 C12A(H12d,H12e,H12f), C42A(H42d,H42e,H42f), C41A(H41d,H41e,H41f), C43A(H43d,
 H43e,H43f), C12B(H12a,H12b,H12c), C13B(H13a,H13b,H13c), C32B(H32a,H32b,H32c),
 C31B(H31a,H31b,H31c), C23B(H23a,H23b,H23c), C33B(H33a,H33b,H33c)
;
_atom_sites_solution_primary     direct
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_refinement_flags_posn
C40B C 0.0702(3) 0.31368(17) 1.21382(13) 0.0278(7) Uani 1.000000 .
C42B C 0.2298(4) 0.3196(2) 1.21314(17) 0.0400(9) Uani 1.000000 .
H42a H 0.2661(5) 0.3455(14) 1.2430(6) 0.0600(14) Uiso 1.000000 GR
H42b H 0.2706(4) 0.2716(2) 1.2130(11) 0.0600(14) Uiso 1.000000 GR
H42c H 0.2544(4) 0.3453(14) 1.1830(6) 0.0600(14) Uiso 1.000000 GR
C41B C 0.0336(4) 0.2719(2) 1.26020(16) 0.0390(9) Uani 1.000000 .
H41a H 0.071(3) 0.2235(5) 1.2584(5) 0.0584(13) Uiso 1.000000 GR
H41b H 0.074(2) 0.2958(8) 1.29028(17) 0.0584(13) Uiso 1.000000 GR
H41c H -0.0680(4) 0.2697(13) 1.2617(6) 0.0584(13) Uiso 1.000000 GR
P2A P 0.61475(7) 0.77863(4) 1.00185(3) 0.01720(14) Uani 1.000000 .
C43B C 0.0176(4) 0.2746(2) 1.16594(16) 0.0410(9) Uani 1.000000 .
H43a H 0.041(3) 0.3026(8) 1.13656(16) 0.0615(14) Uiso 1.000000 GR
H43b H 0.062(2) 0.2276(6) 1.1647(6) 0.0615(14) Uiso 1.000000 GR
H43c H -0.0838(6) 0.2687(14) 1.1659(5) 0.0615(14) Uiso 1.000000 GR
P1A P 0.39571(7) 0.86304(4) 1.01245(3) 0.01845(14) Uani 1.000000 .
P2B P 0.09526(7) 0.46120(4) 1.22988(3) 0.01819(14) Uani 1.000000 .
C30B C -0.3992(3) 0.52823(18) 1.22080(12) 0.0248(6) Uani 1.000000 .
P1B P -0.11190(7) 0.55482(4) 1.23471(3) 0.01825(14) Uani 1.000000 .
N4B N 0.0066(2) 0.38637(13) 1.21346(10) 0.0199(5) Uani 1.000000 .
N1B N -0.0114(2) 0.51489(13) 1.18863(9) 0.0186(5) Uani 1.000000 .
N3B N -0.2511(2) 0.50323(14) 1.21981(9) 0.0201(5) Uani 1.000000 .
C10B C 0.0439(3) 0.55384(18) 1.14535(12) 0.0253(6) Uani 1.000000 .
C11B C 0.1179(3) 0.49939(19) 1.11366(12) 0.0305(7) Uani 1.000000 .
H11a H 0.1941(17) 0.4771(10) 1.1341(3) 0.0457(11) Uiso 1.000000 GR
H11b H 0.0514(7) 0.4626(8) 1.1018(8) 0.0457(11) Uiso 1.000000 GR
H11c H 0.156(2) 0.5235(3) 1.0849(5) 0.0457(11) Uiso 1.000000 GR
C40A C 0.6081(3) 0.63194(16) 0.98180(11) 0.0199(5) Uani 1.000000 .
C20A C 0.5258(3) 0.80037(17) 1.10197(11) 0.0226(6) Uani 1.000000 .
C21A C 0.4883(4) 0.8675(2) 1.13003(14) 0.0382(9) Uani 1.000000 .
H21d H 0.494(3) 0.8579(5) 1.16615(15) 0.0572(13) Uiso 1.000000 GR
H21e H 0.5537(18) 0.9057(5) 1.1227(8) 0.0572(13) Uiso 1.000000 GR
H21f H 0.3933(11) 0.8822(9) 1.1193(8) 0.0572(13) Uiso 1.000000 GR
C22A C 0.6735(3) 0.7767(2) 1.11823(13) 0.0309(7) Uani 1.000000 .
H22d H 0.7396(4) 0.8144(6) 1.1105(9) 0.0464(11) Uiso 1.000000 GR
H22e H 0.6796(8) 0.7675(13) 1.1544(2) 0.0464(11) Uiso 1.000000 GR
H22f H 0.6962(10) 0.7330(8) 1.1003(7) 0.0464(11) Uiso 1.000000 GR
C23A C 0.4233(4) 0.7398(2) 1.11331(14) 0.0340(8) Uani 1.000000 .
H23d H 0.433(2) 0.7279(10) 1.1491(2) 0.0509(12) Uiso 1.000000 GR
H23e H 0.3276(4) 0.7555(6) 1.1046(9) 0.0509(12) Uiso 1.000000 GR
H23f H 0.4443(18) 0.6976(5) 1.0934(8) 0.0509(12) Uiso 1.000000 GR
C20B C -0.0050(3) 0.49108(18) 1.32699(11) 0.0249(6) Uani 1.000000 .
C21B C -0.0347(5) 0.5606(2) 1.35363(14) 0.0414(9) Uani 1.000000 .
H21a H -0.039(3) 0.5516(3) 1.3896(2) 0.0621(14) Uiso 1.000000 GR
H21b H 0.0400(16) 0.5948(6) 1.3482(9) 0.0621(14) Uiso 1.000000 GR
H21c H -0.1239(15) 0.5801(8) 1.3403(8) 0.0621(14) Uiso 1.000000 GR
C22B C 0.1357(4) 0.4615(2) 1.34676(13) 0.0378(8) Uani 1.000000 .
H22a H 0.2097(5) 0.4952(7) 1.3393(9) 0.0568(13) Uiso 1.000000 GR
H22b H 0.1350(11) 0.4546(14) 1.3831(2) 0.0568(13) Uiso 1.000000 GR
H22c H 0.1528(14) 0.4156(8) 1.3306(8) 0.0568(13) Uiso 1.000000 GR
C30A C 0.1129(3) 0.82391(17) 1.00258(12) 0.0217(6) Uani 1.000000 .
C33A C 0.0613(3) 0.7880(2) 1.04990(12) 0.0302(7) Uani 1.000000 .
H33d H -0.0391(6) 0.7962(12) 1.0515(5) 0.0452(11) Uiso 1.000000 GR
H33e H 0.080(2) 0.7366(3) 1.0486(5) 0.0452(11) Uiso 1.000000 GR
H33f H 0.1106(19) 0.8084(10) 1.07970(13) 0.0452(11) Uiso 1.000000 GR
C31A C 0.0264(3) 0.79718(18) 0.95655(12) 0.0267(6) Uani 1.000000 .
H31d H 0.036(2) 0.7453(2) 0.9539(5) 0.0401(10) Uiso 1.000000 GR
H31e H -0.0719(5) 0.8093(11) 0.9599(4) 0.0401(10) Uiso 1.000000 GR
H31f H 0.0593(17) 0.8199(10) 0.92637(15) 0.0401(10) Uiso 1.000000 GR
C32A C 0.0916(3) 0.90497(18) 1.00633(14) 0.0304(7) Uani 1.000000 .
H32d H -0.0075(5) 0.91523(19) 1.0095(10) 0.0456(11) Uiso 1.000000 GR
H32e H 0.146(2) 0.9234(3) 1.0358(5) 0.0456(11) Uiso 1.000000 GR
H32f H 0.123(2) 0.9280(2) 0.9761(4) 0.0456(11) Uiso 1.000000 GR
C10A C 0.5416(3) 0.87573(17) 0.92150(12) 0.0251(6) Uani 1.000000 .
C11A C 0.6138(4) 0.82768(19) 0.88455(13) 0.0302(7) Uani 1.000000 .
H11d H 0.5496(10) 0.7898(8) 0.8727(7) 0.0453(11) Uiso 1.000000 GR
H11e H 0.641(2) 0.8562(3) 0.8559(5) 0.0453(11) Uiso 1.000000 GR
H11f H 0.6971(15) 0.8063(11) 0.9013(3) 0.0453(11) Uiso 1.000000 GR
C13A C 0.4103(4) 0.9084(2) 0.89544(15) 0.0416(10) Uani 1.000000 .
H13d H 0.4367(5) 0.9382(13) 0.8674(7) 0.0624(14) Uiso 1.000000 GR
H13e H 0.3481(14) 0.8702(2) 0.8828(10) 0.0624(14) Uiso 1.000000 GR
H13f H 0.3623(17) 0.9377(13) 0.9194(3) 0.0624(14) Uiso 1.000000 GR
C12A C 0.6401(4) 0.93453(19) 0.94146(16) 0.0376(8) Uani 1.000000 .
H12d H 0.7236(14) 0.91295(19) 0.9579(9) 0.0564(13) Uiso 1.000000 GR
H12e H 0.667(2) 0.9645(9) 0.9136(2) 0.0564(13) Uiso 1.000000 GR
H12f H 0.5928(11) 0.9638(9) 0.9657(8) 0.0564(13) Uiso 1.000000 GR
C42A C 0.7661(3) 0.64304(18) 0.97944(14) 0.0298(7) Uani 1.000000 .
H42d H 0.8019(5) 0.6688(12) 1.0094(5) 0.0447(11) Uiso 1.000000 GR
H42e H 0.8125(4) 0.59656(18) 0.9779(10) 0.0447(11) Uiso 1.000000 GR
H42f H 0.7848(4) 0.6708(12) 0.9495(5) 0.0447(11) Uiso 1.000000 GR
C41A C 0.5808(3) 0.58800(17) 1.02871(13) 0.0272(6) Uani 1.000000 .
H41d H 0.626(2) 0.5414(5) 1.0266(4) 0.0408(10) Uiso 1.000000 GR
H41e H 0.618(2) 0.6133(6) 1.05861(14) 0.0408(10) Uiso 1.000000 GR
H41f H 0.4801(4) 0.5813(11) 1.0309(5) 0.0408(10) Uiso 1.000000 GR
C43A C 0.5555(3) 0.59241(17) 0.93435(12) 0.0251(6) Uani 1.000000 .
H43d H 0.573(2) 0.6214(6) 0.90486(13) 0.0376(9) Uiso 1.000000 GR
H43e H 0.6043(17) 0.5467(6) 0.9323(5) 0.0376(9) Uiso 1.000000 GR
H43f H 0.4551(6) 0.5838(11) 0.9355(4) 0.0376(9) Uiso 1.000000 GR
C12B C 0.1453(4) 0.61226(19) 1.16450(16) 0.0371(9) Uani 1.000000 .
H12a H 0.0958(8) 0.6467(8) 1.1846(9) 0.0556(13) Uiso 1.000000 GR
H12b H 0.2216(16) 0.5906(3) 1.1852(9) 0.0556(13) Uiso 1.000000 GR
H12c H 0.183(2) 0.6368(10) 1.13592(16) 0.0556(13) Uiso 1.000000 GR
C13B C -0.0786(4) 0.5866(2) 1.11495(14) 0.0380(9) Uani 1.000000 .
H13a H -0.1441(15) 0.5489(3) 1.1039(9) 0.0570(13) Uiso 1.000000 GR
H13b H -0.1259(18) 0.6210(11) 1.1357(4) 0.0570(13) Uiso 1.000000 GR
H13c H -0.0446(5) 0.6110(13) 1.0856(6) 0.0570(13) Uiso 1.000000 GR
C32B C -0.4056(4) 0.6097(2) 1.22298(16) 0.0369(8) Uani 1.000000 .
H32a H -0.358(2) 0.6264(2) 1.2543(5) 0.0553(12) Uiso 1.000000 GR
H32b H -0.359(2) 0.6298(2) 1.1944(6) 0.0553(12) Uiso 1.000000 GR
H32c H -0.5032(4) 0.6251(2) 1.2217(10) 0.0553(12) Uiso 1.000000 GR
C31B C -0.4798(3) 0.5035(2) 1.17324(14) 0.0394(9) Uani 1.000000 .
H31a H -0.4376(18) 0.5240(12) 1.14395(15) 0.0591(14) Uiso 1.000000 GR
H31b H -0.477(2) 0.4513(3) 1.1713(5) 0.0591(14) Uiso 1.000000 GR
H31c H -0.5769(8) 0.5194(13) 1.1738(5) 0.0591(14) Uiso 1.000000 GR
C23B C -0.1195(4) 0.4364(2) 1.33681(14) 0.0370(8) Uani 1.000000 .
H23a H -0.1180(19) 0.4257(11) 1.37275(19) 0.0556(12) Uiso 1.000000 GR
H23b H -0.2107(5) 0.4561(6) 1.3258(10) 0.0556(12) Uiso 1.000000 GR
H23c H -0.1029(17) 0.3925(6) 1.3182(8) 0.0556(12) Uiso 1.000000 GR
C33B C -0.4667(3) 0.4977(2) 1.26668(14) 0.0359(8) Uani 1.000000 .
H33a H -0.462(3) 0.4454(2) 1.2658(5) 0.0538(12) Uiso 1.000000 GR
H33b H -0.4169(18) 0.5152(12) 1.29729(14) 0.0538(12) Uiso 1.000000 GR
H33c H -0.5644(8) 0.5128(12) 1.2663(6) 0.0538(12) Uiso 1.000000 GR
Sb1B Sb -0.179982(19) 0.418890(11) 1.175757(7) 0.01993(5) Uani 1.000000 .
Sb1A Sb 0.342010(18) 0.729722(10) 0.948870(7) 0.01623(5) Uani 1.000000 .
I1A I 0.18580(2) 0.610806(11) 0.987618(8) 0.02619(5) Uani 1.000000 .
I1B I -0.35534(2) 0.309361(13) 1.217114(10) 0.03699(6) Uani 1.000000 .
N3A N 0.2633(2) 0.80687(13) 0.99687(9) 0.0176(5) Uani 1.000000 .
N1A N 0.4966(2) 0.83050(13) 0.96346(9) 0.0182(5) Uani 1.000000 .
N4A N 0.5357(2) 0.70213(13) 0.98351(9) 0.0173(4) Uani 1.000000 .
N2A N 0.5201(2) 0.81590(13) 1.04765(9) 0.0192(5) Uani 1.000000 .
N2B N 0.0003(2) 0.50510(13) 1.27313(9) 0.0185(5) Uani 1.000000 .


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
C40B C42B 1.538(5) . ?
C40B C41B 1.523(5) . ?
C40B C43B 1.534(5) . ?
C40B N4B 1.492(4) . ?
C42B H42a 0.9800 . ?
C42B H42b 0.9800 . ?
C42B H42c 0.9800 . ?
C41B H41a 0.9800 . ?
C41B H41b 0.9800 . ?
C41B H41c 0.9800 . ?
P2A P1A 2.6606(10) . ?
P2A N1A 1.775(2) . ?
P2A N4A 1.682(2) . ?
P2A N2A 1.715(2) . ?
C43B H43a 0.9800 . ?
C43B H43b 0.9800 . ?
C43B H43c 0.9800 . ?
P1A N3A 1.685(2) . ?
P1A N1A 1.781(2) . ?
P1A N2A 1.721(3) . ?
P2B P1B 2.6616(10) . ?
P2B N4B 1.685(3) . ?
P2B N1B 1.774(2) . ?
P2B N2B 1.722(2) . ?
C30B N3B 1.500(4) . ?
C30B C32B 1.529(5) . ?
C30B C31B 1.521(5) . ?
C30B C33B 1.531(5) . ?
P1B N1B 1.773(2) . ?
P1B N3B 1.679(2) . ?
P1B N2B 1.719(3) . ?
N4B Sb1B 2.095(2) . ?
N1B C10B 1.491(4) . ?
N1B Sb1B 2.431(2) . ?
N3B Sb1B 2.107(2) . ?
C10B C11B 1.528(5) . ?
C10B C12B 1.534(5) . ?
C10B C13B 1.520(4) . ?
C11B H11a 0.9800 . ?
C11B H11b 0.9800 . ?
C11B H11c 0.9800 . ?
C40A C42A 1.537(4) . ?
C40A C41A 1.535(4) . ?
C40A C43A 1.529(4) . ?
C40A N4A 1.490(4) . ?
C20A C21A 1.518(5) . ?
C20A C22A 1.525(4) . ?
C20A C23A 1.544(5) . ?
C20A N2A 1.478(4) . ?
C21A H21d 0.9800 . ?
C21A H21e 0.9800 . ?
C21A H21f 0.9800 . ?
C22A H22d 0.9800 . ?
C22A H22e 0.9800 . ?
C22A H22f 0.9800 . ?
C23A H23d 0.9800 . ?
C23A H23e 0.9800 . ?
C23A H23f 0.9800 . ?
C20B C21B 1.518(5) . ?
C20B C22B 1.527(4) . ?
C20B C23B 1.537(5) . ?
C20B N2B 1.466(4) . ?
C21B H21a 0.9800 . ?
C21B H21b 0.9800 . ?
C21B H21c 0.9800 . ?
C22B H22a 0.9800 . ?
C22B H22b 0.9800 . ?
C22B H22c 0.9800 . ?
C30A C33A 1.539(4) . ?
C30A C31A 1.528(4) . ?
C30A C32A 1.537(4) . ?
C30A N3A 1.496(3) . ?
C33A H33d 0.9800 . ?
C33A H33e 0.9800 . ?
C33A H33f 0.9800 . ?
C31A H31d 0.9800 . ?
C31A H31e 0.9800 . ?
C31A H31f 0.9800 . ?
C32A H32d 0.9800 . ?
C32A H32e 0.9800 . ?
C32A H32f 0.9800 . ?
C10A C11A 1.531(5) . ?
C10A C13A 1.533(5) . ?
C10A C12A 1.528(5) . ?
C10A N1A 1.489(4) . ?
C11A H11d 0.9800 . ?
C11A H11e 0.9800 . ?
C11A H11f 0.9800 . ?
C13A H13d 0.9800 . ?
C13A H13e 0.9800 . ?
C13A H13f 0.9800 . ?
C12A H12d 0.9800 . ?
C12A H12e 0.9800 . ?
C12A H12f 0.9800 . ?
C42A H42d 0.9800 . ?
C42A H42e 0.9800 . ?
C42A H42f 0.9800 . ?
C41A H41d 0.9800 . ?
C41A H41e 0.9800 . ?
C41A H41f 0.9800 . ?
C43A H43d 0.9800 . ?
C43A H43e 0.9800 . ?
C43A H43f 0.9800 . ?
C12B H12a 0.9800 . ?
C12B H12b 0.9800 . ?
C12B H12c 0.9800 . ?
C13B H13a 0.9800 . ?
C13B H13b 0.9800 . ?
C13B H13c 0.9800 . ?
C32B H32a 0.9800 . ?
C32B H32b 0.9800 . ?
C32B H32c 0.9800 . ?
C31B H31a 0.9800 . ?
C31B H31b 0.9800 . ?
C31B H31c 0.9800 . ?
C23B H23a 0.9800 . ?
C23B H23b 0.9800 . ?
C23B H23c 0.9800 . ?
C33B H33a 0.9800 . ?
C33B H33b 0.9800 . ?
C33B H33c 0.9800 . ?
Sb1B I1B 2.9131(3) . ?
Sb1A I1A 2.9100(3) . ?
Sb1A N3A 2.102(2) . ?
Sb1A N1A 2.420(2) . ?
Sb1A N4A 2.094(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C41B C40B C42B 108.9(3) . . ?
C43B C40B C42B 107.7(3) . . ?
C43B C40B C41B 110.7(3) . . ?
N4B C40B C42B 110.0(3) . . ?
N4B C40B C41B 111.1(3) . . ?
N4B C40B C43B 108.4(3) . . ?
H42a C42B C40B 109.5 . . ?
H42b C42B C40B 109.5 . . ?
H42b C42B H42a 109.5 . . ?
H42c C42B C40B 109.5 . . ?
H42c C42B H42a 109.5 . . ?
H42c C42B H42b 109.5 . . ?
H41a C41B C40B 109.5 . . ?
H41b C41B C40B 109.5 . . ?
H41b C41B H41a 109.5 . . ?
H41c C41B C40B 109.5 . . ?
H41c C41B H41a 109.5 . . ?
H41c C41B H41b 109.5 . . ?
N1A P2A P1A 41.64(8) . . ?
N4A P2A P1A 101.01(8) . . ?
N4A P2A N1A 92.03(12) . . ?
N2A P2A P1A 39.34(8) . . ?
N2A P2A N1A 80.88(12) . . ?
N2A P2A N4A 107.81(12) . . ?
H43a C43B C40B 109.5 . . ?
H43b C43B C40B 109.5 . . ?
H43b C43B H43a 109.5 . . ?
H43c C43B C40B 109.5 . . ?
H43c C43B H43a 109.5 . . ?
H43c C43B H43b 109.5 . . ?
N3A P1A P2A 101.12(8) . . ?
N1A P1A P2A 41.47(8) . . ?
N1A P1A N3A 92.27(11) . . ?
N2A P1A P2A 39.17(8) . . ?
N2A P1A N3A 107.75(12) . . ?
N2A P1A N1A 80.54(11) . . ?
N4B P2B P1B 101.14(9) . . ?
N1B P2B P1B 41.37(8) . . ?
N1B P2B N4B 92.60(12) . . ?
N2B P2B P1B 39.29(8) . . ?
N2B P2B N4B 107.03(12) . . ?
N2B P2B N1B 80.58(11) . . ?
C32B C30B N3B 110.7(3) . . ?
C31B C30B N3B 109.1(2) . . ?
C31B C30B C32B 108.4(3) . . ?
C33B C30B N3B 110.1(3) . . ?
C33B C30B C32B 108.9(3) . . ?
C33B C30B C31B 109.6(3) . . ?
N1B P1B P2B 41.38(8) . . ?
N3B P1B P2B 101.31(9) . . ?
N3B P1B N1B 92.88(12) . . ?
N2B P1B P2B 39.37(8) . . ?
N2B P1B N1B 80.68(11) . . ?
N2B P1B N3B 107.01(12) . . ?
P2B N4B C40B 123.9(2) . . ?
Sb1B N4B C40B 127.36(19) . . ?
Sb1B N4B P2B 106.76(12) . . ?
P1B N1B P2B 97.25(12) . . ?
C10B N1B P2B 122.71(18) . . ?
C10B N1B P1B 124.4(2) . . ?
Sb1B N1B P2B 91.39(10) . . ?
Sb1B N1B P1B 91.47(9) . . ?
Sb1B N1B C10B 121.11(19) . . ?
P1B N3B C30B 124.0(2) . . ?
Sb1B N3B C30B 125.63(19) . . ?
Sb1B N3B P1B 106.56(11) . . ?
C11B C10B N1B 107.5(3) . . ?
C12B C10B N1B 109.8(3) . . ?
C12B C10B C11B 110.7(3) . . ?
C13B C10B N1B 108.2(2) . . ?
C13B C10B C11B 110.2(3) . . ?
C13B C10B C12B 110.3(3) . . ?
H11a C11B C10B 109.5 . . ?
H11b C11B C10B 109.5 . . ?
H11b C11B H11a 109.5 . . ?
H11c C11B C10B 109.5 . . ?
H11c C11B H11a 109.5 . . ?
H11c C11B H11b 109.5 . . ?
C41A C40A C42A 108.8(3) . . ?
C43A C40A C42A 108.1(2) . . ?
C43A C40A C41A 110.7(3) . . ?
N4A C40A C42A 110.2(2) . . ?
N4A C40A C41A 110.3(2) . . ?
N4A C40A C43A 108.7(2) . . ?
C22A C20A C21A 110.1(3) . . ?
C23A C20A C21A 109.8(3) . . ?
C23A C20A C22A 108.9(3) . . ?
N2A C20A C21A 109.0(3) . . ?
N2A C20A C22A 108.5(2) . . ?
N2A C20A C23A 110.5(2) . . ?
H21d C21A C20A 109.5 . . ?
H21e C21A C20A 109.5 . . ?
H21e C21A H21d 109.5 . . ?
H21f C21A C20A 109.5 . . ?
H21f C21A H21d 109.5 . . ?
H21f C21A H21e 109.5 . . ?
H22d C22A C20A 109.5 . . ?
H22e C22A C20A 109.5 . . ?
H22e C22A H22d 109.5 . . ?
H22f C22A C20A 109.5 . . ?
H22f C22A H22d 109.5 . . ?
H22f C22A H22e 109.5 . . ?
H23d C23A C20A 109.5 . . ?
H23e C23A C20A 109.5 . . ?
H23e C23A H23d 109.5 . . ?
H23f C23A C20A 109.5 . . ?
H23f C23A H23d 109.5 . . ?
H23f C23A H23e 109.5 . . ?
C22B C20B C21B 109.6(3) . . ?
C23B C20B C21B 109.6(3) . . ?
C23B C20B C22B 109.1(3) . . ?
N2B C20B C21B 108.9(3) . . ?
N2B C20B C22B 108.9(3) . . ?
N2B C20B C23B 110.7(3) . . ?
H21a C21B C20B 109.5 . . ?
H21b C21B C20B 109.5 . . ?
H21b C21B H21a 109.5 . . ?
H21c C21B C20B 109.5 . . ?
H21c C21B H21a 109.5 . . ?
H21c C21B H21b 109.5 . . ?
H22a C22B C20B 109.5 . . ?
H22b C22B C20B 109.5 . . ?
H22b C22B H22a 109.5 . . ?
H22c C22B C20B 109.5 . . ?
H22c C22B H22a 109.5 . . ?
H22c C22B H22b 109.5 . . ?
C31A C30A C33A 109.4(3) . . ?
C32A C30A C33A 109.1(3) . . ?
C32A C30A C31A 107.9(3) . . ?
N3A C30A C33A 110.4(2) . . ?
N3A C30A C31A 109.4(2) . . ?
N3A C30A C32A 110.5(2) . . ?
H33d C33A C30A 109.5 . . ?
H33e C33A C30A 109.5 . . ?
H33e C33A H33d 109.5 . . ?
H33f C33A C30A 109.5 . . ?
H33f C33A H33d 109.5 . . ?
H33f C33A H33e 109.5 . . ?
H31d C31A C30A 109.5 . . ?
H31e C31A C30A 109.5 . . ?
H31e C31A H31d 109.5 . . ?
H31f C31A C30A 109.5 . . ?
H31f C31A H31d 109.5 . . ?
H31f C31A H31e 109.5 . . ?
H32d C32A C30A 109.5 . . ?
H32e C32A C30A 109.5 . . ?
H32e C32A H32d 109.5 . . ?
H32f C32A C30A 109.5 . . ?
H32f C32A H32d 109.5 . . ?
H32f C32A H32e 109.5 . . ?
C13A C10A C11A 109.5(3) . . ?
C12A C10A C11A 110.8(3) . . ?
C12A C10A C13A 110.3(3) . . ?
N1A C10A C11A 108.2(3) . . ?
N1A C10A C13A 107.6(2) . . ?
N1A C10A C12A 110.4(3) . . ?
H11d C11A C10A 109.5 . . ?
H11e C11A C10A 109.5 . . ?
H11e C11A H11d 109.5 . . ?
H11f C11A C10A 109.5 . . ?
H11f C11A H11d 109.5 . . ?
H11f C11A H11e 109.5 . . ?
H13d C13A C10A 109.5 . . ?
H13e C13A C10A 109.5 . . ?
H13e C13A H13d 109.5 . . ?
H13f C13A C10A 109.5 . . ?
H13f C13A H13d 109.5 . . ?
H13f C13A H13e 109.5 . . ?
H12d C12A C10A 109.5 . . ?
H12e C12A C10A 109.5 . . ?
H12e C12A H12d 109.5 . . ?
H12f C12A C10A 109.5 . . ?
H12f C12A H12d 109.5 . . ?
H12f C12A H12e 109.5 . . ?
H42d C42A C40A 109.5 . . ?
H42e C42A C40A 109.5 . . ?
H42e C42A H42d 109.5 . . ?
H42f C42A C40A 109.5 . . ?
H42f C42A H42d 109.5 . . ?
H42f C42A H42e 109.5 . . ?
H41d C41A C40A 109.5 . . ?
H41e C41A C40A 109.5 . . ?
H41e C41A H41d 109.5 . . ?
H41f C41A C40A 109.5 . . ?
H41f C41A H41d 109.5 . . ?
H41f C41A H41e 109.5 . . ?
H43d C43A C40A 109.5 . . ?
H43e C43A C40A 109.5 . . ?
H43e C43A H43d 109.5 . . ?
H43f C43A C40A 109.5 . . ?
H43f C43A H43d 109.5 . . ?
H43f C43A H43e 109.5 . . ?
H12a C12B C10B 109.5 . . ?
H12b C12B C10B 109.5 . . ?
H12b C12B H12a 109.5 . . ?
H12c C12B C10B 109.5 . . ?
H12c C12B H12a 109.5 . . ?
H12c C12B H12b 109.5 . . ?
H13a C13B C10B 109.5 . . ?
H13b C13B C10B 109.5 . . ?
H13b C13B H13a 109.5 . . ?
H13c C13B C10B 109.5 . . ?
H13c C13B H13a 109.5 . . ?
H13c C13B H13b 109.5 . . ?
H32a C32B C30B 109.5 . . ?
H32b C32B C30B 109.5 . . ?
H32b C32B H32a 109.5 . . ?
H32c C32B C30B 109.5 . . ?
H32c C32B H32a 109.5 . . ?
H32c C32B H32b 109.5 . . ?
H31a C31B C30B 109.5 . . ?
H31b C31B C30B 109.5 . . ?
H31b C31B H31a 109.5 . . ?
H31c C31B C30B 109.5 . . ?
H31c C31B H31a 109.5 . . ?
H31c C31B H31b 109.5 . . ?
H23a C23B C20B 109.5 . . ?
H23b C23B C20B 109.5 . . ?
H23b C23B H23a 109.5 . . ?
H23c C23B C20B 109.5 . . ?
H23c C23B H23a 109.5 . . ?
H23c C23B H23b 109.5 . . ?
H33a C33B C30B 109.5 . . ?
H33b C33B C30B 109.5 . . ?
H33b C33B H33a 109.5 . . ?
H33c C33B C30B 109.5 . . ?
H33c C33B H33a 109.5 . . ?
H33c C33B H33b 109.5 . . ?
N1B Sb1B N4B 66.61(9) . . ?
N3B Sb1B N4B 104.21(9) . . ?
N3B Sb1B N1B 66.47(8) . . ?
I1B Sb1B N4B 96.33(7) . . ?
I1B Sb1B N1B 149.61(6) . . ?
I1B Sb1B N3B 95.93(7) . . ?
N3A Sb1A I1A 95.65(6) . . ?
N1A Sb1A I1A 149.83(6) . . ?
N1A Sb1A N3A 66.68(8) . . ?
N4A Sb1A I1A 96.72(7) . . ?
N4A Sb1A N3A 104.01(9) . . ?
N4A Sb1A N1A 66.45(9) . . ?
C30A N3A P1A 124.15(19) . . ?
Sb1A N3A P1A 106.69(11) . . ?
Sb1A N3A C30A 126.35(18) . . ?
P1A N1A P2A 96.89(12) . . ?
C10A N1A P2A 122.85(18) . . ?
C10A N1A P1A 123.5(2) . . ?
Sb1A N1A P2A 91.81(10) . . ?
Sb1A N1A P1A 91.76(9) . . ?
Sb1A N1A C10A 121.68(19) . . ?
C40A N4A P2A 123.87(18) . . ?
Sb1A N4A P2A 107.04(12) . . ?
Sb1A N4A C40A 127.52(18) . . ?
P1A N2A P2A 101.49(13) . . ?
C20A N2A P2A 129.0(2) . . ?
C20A N2A P1A 128.50(19) . . ?
P1B N2B P2B 101.33(13) . . ?
C20B N2B P2B 128.5(2) . . ?
C20B N2B P1B 128.8(2) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: THF'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_MAT45_0m
_database_code_depnum_ccdc_archive 'CCDC 1991887'
loop_
_audit_author_name
_audit_author_address
'Lothar Stahl'
;University of North Dakota
United States of America
;
_audit_update_record             
;
2020-03-21 deposited with the CCDC.	2020-04-21 downloaded from the CCDC.
;
_audit_creation_date             2020-03-17
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_chemical_formula_moiety         'C17 H36 F3 N4 O3 P2 S Sb'
_chemical_formula_sum            'C17 H36 F3 N4 O3 P2 S Sb'
_chemical_formula_weight         617.27
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
_atom_type_scat_dispersion_source
C 0.00347 0.00161 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870
51.65120 0.215599998832
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
F 0.01794 0.01033 3.53920 2.64120 1.51700 1.02430 10.28250 4.29440 0.26150
26.14760 0.277599990368
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236
57.79970 0.0030380000826
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
O 0.01158 0.00611 3.04850 2.28680 1.54630 0.86700 13.27710 5.70110 0.32390
32.90890 0.250800013542
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
N 0.00653 0.00323 12.21260 3.13220 2.01250 1.16630 0.00570 9.89330 28.99750
0.58260 -11.5290002823
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
P 0.10434 0.09671 6.43450 4.17910 1.78000 1.49080 1.90670 27.15700 0.52600
68.16450 1.11489999294
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
S 0.12424 0.12443 6.90530 5.20340 1.43790 1.58630 1.46790 22.21510 0.25360
56.17200 0.866900026798
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
Sb -0.60640 1.48759 19.64180 19.04550 5.03710 2.68270 5.30340 0.46070 27.90740
75.28250 4.59089994431
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2ybc (x-z,y,z)'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x+1/2,y+1/2,-z+1/2
3 -x,-y,-z
4 x-1/2,-y-1/2,z-1/2

_symmetry_Int_Tables_number      14
_cell_length_a                   9.7212(3)
_cell_length_b                   18.6010(5)
_cell_length_c                   15.2849(4)
_cell_angle_alpha                90
_cell_angle_beta                 100.5301(12)
_cell_angle_gamma                90
_cell_volume                     2717.33(13)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9679
_cell_measurement_temperature    100
_cell_measurement_theta_max      37.99
_cell_measurement_theta_min      2.40
_exptl_absorpt_coefficient_mu    1.254
_exptl_absorpt_correction_T_max  0.612
_exptl_absorpt_correction_T_min  0.420
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.5087
_exptl_crystal_description       needle
_exptl_crystal_F_000             1255.4459
_exptl_crystal_size_max          0.68
_exptl_crystal_size_mid          0.56
_exptl_crystal_size_min          0.39
_diffrn_reflns_av_R_equivalents  0.0241
_diffrn_reflns_av_unetI/netI     0.0265
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            49097
_diffrn_reflns_theta_full        26.0000
_diffrn_reflns_theta_max         38.00
_diffrn_reflns_theta_min         2.40
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.9987
_diffrn_measured_fraction_theta_max 0.9922
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              12
_reflns_limit_h_min              -16
_reflns_limit_k_max              32
_reflns_limit_k_min              0
_reflns_limit_l_max              26
_reflns_limit_l_min              -12
_reflns_number_gt                12760
_reflns_number_total             14692
_reflns_threshold_expression     I>=2u(I)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_refine_diff_density_max         2.3216
_refine_diff_density_min         -1.8374
_refine_diff_density_rms         0.1856
_refine_ls_d_res_high            0.5771
_refine_ls_d_res_low             8.5010
_refine_ls_goodness_of_fit_ref   1.0568
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    48
_refine_ls_number_parameters     292
_refine_ls_number_reflns         14692
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0518
_refine_ls_R_factor_gt           0.0429
_refine_ls_restrained_S_all      1.0568
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0000P)²+7.7969P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0807
_refine_ls_wR_factor_ref         0.0859
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C11(H11a,H11b,H11c), C12(H12a,H12b,H12c), C13(H13a,H13b,H13c), C21(H21a,H21b,
 H21c), C22(H22a,H22b,H22c), C23(H23a,H23b,H23c), C31(H31a,H31b,H31c), C32(H32a,
 H32b,H32c), C33(H33a,H33b,H33c), C41(H41a,H41b,H41c), C42(H42a,H42b,H42c),
 C43(H43a,H43b,H43c)
;
_atom_sites_solution_primary     direct
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_refinement_flags_posn
Sb1 Sb 0.900733(13) 0.485774(6) 0.840116(7) 0.01470(3) Uani 1.000000 .
P1 P 0.91827(7) 0.42903(3) 0.65902(4) 0.02421(11) Uani 1.000000 .
P2 P 0.69488(6) 0.50983(3) 0.67127(3) 0.02016(9) Uani 1.000000 .
S1 S 0.83204(6) 0.37700(3) 1.02026(3) 0.02470(10) Uani 1.000000 .
F1 F 0.7633(3) 0.24599(10) 0.9690(2) 0.0825(9) Uani 1.000000 .
F2 F 0.5876(2) 0.31333(13) 0.97685(18) 0.0681(7) Uani 1.000000 .
F3 F 0.7180(4) 0.27465(18) 1.0957(2) 0.1207(15) Uani 1.000000 .
O1 O 0.7710(2) 0.42889(12) 1.07127(13) 0.0372(4) Uani 1.000000 .
O2 O 0.9681(2) 0.35019(11) 1.05919(12) 0.0358(4) Uani 1.000000 .
O3 O 0.81697(17) 0.39509(8) 0.92536(10) 0.0236(3) Uani 1.000000 .
N1 N 0.88253(17) 0.51851(9) 0.69314(10) 0.0174(3) Uani 1.000000 .
N2 N 0.7388(2) 0.42752(10) 0.63356(12) 0.0264(4) Uani 1.000000 .
N3 N 0.9664(2) 0.40428(9) 0.76616(12) 0.0229(3) Uani 1.000000 .
N4 N 0.69469(17) 0.50300(9) 0.78101(11) 0.0194(3) Uani 1.000000 .
C1 C 0.7184(4) 0.29859(18) 1.0144(2) 0.0565(10) Uani 1.000000 .
C10 C 0.9543(2) 0.58355(11) 0.66209(13) 0.0197(3) Uani 1.000000 .
C11 C 0.9040(3) 0.64928(12) 0.70727(15) 0.0277(4) Uani 1.000000 .
H11a H 0.9301(19) 0.6442(5) 0.77200(15) 0.0415(6) Uiso 1.000000 GR
H11b H 0.9476(17) 0.69266(17) 0.6882(11) 0.0415(6) Uiso 1.000000 GR
H11c H 0.8020(4) 0.6532(6) 0.6906(11) 0.0415(6) Uiso 1.000000 GR
C12 C 0.9118(3) 0.58940(13) 0.56106(14) 0.0277(4) Uani 1.000000 .
H12a H 0.9592(17) 0.6307(7) 0.5399(2) 0.0416(6) Uiso 1.000000 GR
H12b H 0.939(2) 0.5453(5) 0.53334(16) 0.0416(6) Uiso 1.000000 GR
H12c H 0.8103(4) 0.5959(11) 0.54515(16) 0.0416(6) Uiso 1.000000 GR
C13 C 1.1108(3) 0.57358(16) 0.69006(18) 0.0336(5) Uani 1.000000 .
H13a H 1.1341(4) 0.5678(12) 0.7548(2) 0.0504(8) Uiso 1.000000 GR
H13b H 1.1402(4) 0.5307(7) 0.6611(12) 0.0504(8) Uiso 1.000000 GR
H13c H 1.1593(3) 0.6158(6) 0.6724(14) 0.0504(8) Uiso 1.000000 GR
C20 C 0.6454(3) 0.36630(14) 0.60209(17) 0.0389(7) Uani 1.000000 .
C21 C 0.6144(4) 0.32364(17) 0.6809(2) 0.0520(9) Uani 1.000000 .
H21a H 0.7021(5) 0.3054(13) 0.7158(11) 0.0779(13) Uiso 1.000000 GR
H21b H 0.568(3) 0.3548(4) 0.7184(11) 0.0779(13) Uiso 1.000000 GR
H21c H 0.553(2) 0.2831(9) 0.6595(2) 0.0779(13) Uiso 1.000000 GR
C22 C 0.7207(6) 0.3174(2) 0.5451(3) 0.0775(15) Uani 1.000000 .
H22a H 0.737(4) 0.3439(7) 0.4927(13) 0.116(2) Uiso 1.000000 GR
H22b H 0.8102(19) 0.3017(17) 0.5802(8) 0.116(2) Uiso 1.000000 GR
H22c H 0.6623(19) 0.2753(11) 0.526(2) 0.116(2) Uiso 1.000000 GR
C23 C 0.5107(5) 0.3959(2) 0.5484(3) 0.093(2) Uani 1.000000 .
H23a H 0.467(2) 0.4284(19) 0.5856(9) 0.139(3) Uiso 1.000000 GR
H23b H 0.5314(8) 0.422(2) 0.4968(16) 0.139(3) Uiso 1.000000 GR
H23c H 0.4467(19) 0.3561(3) 0.528(3) 0.139(3) Uiso 1.000000 GR
C30 C 1.0705(3) 0.34707(14) 0.79907(18) 0.0369(6) Uani 1.000000 .
C31 C 1.1568(3) 0.36991(14) 0.88830(16) 0.0299(5) Uani 1.000000 .
H31a H 1.2009(18) 0.4165(6) 0.8817(4) 0.0449(7) Uiso 1.000000 GR
H31b H 1.0956(5) 0.3741(11) 0.9324(4) 0.0449(7) Uiso 1.000000 GR
H31c H 1.2293(15) 0.3339(6) 0.9082(7) 0.0449(7) Uiso 1.000000 GR
C32 C 1.1698(4) 0.3377(3) 0.7328(2) 0.0745(16) Uani 1.000000 .
H32a H 1.1175(9) 0.3192(19) 0.6764(8) 0.112(2) Uiso 1.000000 GR
H32b H 1.212(3) 0.3842(5) 0.7227(19) 0.112(2) Uiso 1.000000 GR
H32c H 1.244(2) 0.3036(15) 0.7570(11) 0.112(2) Uiso 1.000000 GR
C33 C 0.9934(5) 0.27686(14) 0.8113(3) 0.0696(14) Uani 1.000000 .
H33a H 0.928(3) 0.2850(5) 0.8521(18) 0.104(2) Uiso 1.000000 GR
H33b H 0.941(3) 0.2608(10) 0.7536(4) 0.104(2) Uiso 1.000000 GR
H33c H 1.0614(5) 0.2399(6) 0.836(2) 0.104(2) Uiso 1.000000 GR
C40 C 0.5807(2) 0.52901(13) 0.82645(15) 0.0245(4) Uani 1.000000 .
C41 C 0.4894(3) 0.46640(18) 0.8455(2) 0.0458(7) Uani 1.000000 .
H41a H 0.443(2) 0.4450(9) 0.7892(2) 0.0686(11) Uiso 1.000000 GR
H41b H 0.5479(5) 0.4301(7) 0.8809(15) 0.0686(11) Uiso 1.000000 GR
H41c H 0.4188(18) 0.4838(3) 0.8786(16) 0.0686(11) Uiso 1.000000 GR
C42 C 0.4896(3) 0.58401(18) 0.7681(2) 0.0415(7) Uani 1.000000 .
H42a H 0.5480(5) 0.6241(7) 0.7549(14) 0.0622(10) Uiso 1.000000 GR
H42b H 0.445(2) 0.5611(4) 0.7123(7) 0.0622(10) Uiso 1.000000 GR
H42c H 0.4174(17) 0.6021(10) 0.7995(7) 0.0622(10) Uiso 1.000000 GR
C43 C 0.6460(3) 0.56474(17) 0.91407(18) 0.0368(6) Uani 1.000000 .
H43a H 0.703(2) 0.5296(4) 0.9524(6) 0.0553(9) Uiso 1.000000 GR
H43b H 0.705(2) 0.6049(8) 0.9022(2) 0.0553(9) Uiso 1.000000 GR
H43c H 0.5717(3) 0.5827(11) 0.9439(8) 0.0553(9) Uiso 1.000000 GR


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
Sb1 O3 2.3651(15) . ?
Sb1 N1 2.3030(15) . ?
Sb1 N3 2.0610(17) . ?
Sb1 N4 2.0663(16) . ?
P1 P2 2.6755(9) . ?
P1 N1 1.7970(17) . ?
P1 N2 1.717(2) . ?
P1 N3 1.6831(18) . ?
P2 N1 1.8008(17) . ?
P2 N2 1.717(2) . ?
P2 N4 1.6825(17) . ?
S1 O1 1.436(2) . ?
S1 O2 1.4368(19) . ?
S1 O3 1.4701(15) . ?
S1 C1 1.822(3) . ?
F1 C1 1.319(5) . ?
F2 C1 1.325(4) . ?
F3 C1 1.321(4) . ?
N1 C10 1.515(3) . ?
N2 C20 1.481(3) . ?
N3 C30 1.491(3) . ?
N4 C40 1.492(3) . ?
C10 C11 1.528(3) . ?
C10 C12 1.528(3) . ?
C10 C13 1.515(3) . ?
C11 H11a 0.9800 . ?
C11 H11b 0.9800 . ?
C11 H11c 0.9800 . ?
C12 H12a 0.9800 . ?
C12 H12b 0.9800 . ?
C12 H12c 0.9800 . ?
C13 H13a 0.9800 . ?
C13 H13b 0.9800 . ?
C13 H13c 0.9800 . ?
C20 C21 1.518(4) . ?
C20 C22 1.534(5) . ?
C20 C23 1.516(5) . ?
C21 H21a 0.9800 . ?
C21 H21b 0.9800 . ?
C21 H21c 0.9800 . ?
C22 H22a 0.9800 . ?
C22 H22b 0.9800 . ?
C22 H22c 0.9800 . ?
C23 H23a 0.9800 . ?
C23 H23b 0.9800 . ?
C23 H23c 0.9800 . ?
C30 C31 1.525(3) . ?
C30 C32 1.531(5) . ?
C30 C33 1.534(5) . ?
C31 H31a 0.9800 . ?
C31 H31b 0.9800 . ?
C31 H31c 0.9800 . ?
C32 H32a 0.9800 . ?
C32 H32b 0.9800 . ?
C32 H32c 0.9800 . ?
C33 H33a 0.9800 . ?
C33 H33b 0.9800 . ?
C33 H33c 0.9800 . ?
C40 C41 1.524(4) . ?
C40 C42 1.529(3) . ?
C40 C43 1.526(4) . ?
C41 H41a 0.9800 . ?
C41 H41b 0.9800 . ?
C41 H41c 0.9800 . ?
C42 H42a 0.9800 . ?
C42 H42b 0.9800 . ?
C42 H42c 0.9800 . ?
C43 H43a 0.9800 . ?
C43 H43b 0.9800 . ?
C43 H43c 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Sb1 O3 138.87(5) . . ?
N3 Sb1 O3 87.14(7) . . ?
N3 Sb1 N1 68.63(6) . . ?
N4 Sb1 O3 87.00(6) . . ?
N4 Sb1 N1 68.71(6) . . ?
N4 Sb1 N3 104.30(7) . . ?
N1 P1 P2 42.01(6) . . ?
N2 P1 P2 38.82(7) . . ?
N2 P1 N1 80.71(9) . . ?
N3 P1 P2 99.82(7) . . ?
N3 P1 N1 90.29(8) . . ?
N3 P1 N2 107.85(10) . . ?
N1 P2 P1 41.90(5) . . ?
N2 P2 P1 38.82(7) . . ?
N2 P2 N1 80.61(9) . . ?
N4 P2 P1 100.14(6) . . ?
N4 P2 N1 90.42(8) . . ?
N4 P2 N2 108.24(9) . . ?
O2 S1 O1 116.69(12) . . ?
O3 S1 O1 113.92(11) . . ?
O3 S1 O2 113.97(11) . . ?
C1 S1 O1 104.94(18) . . ?
C1 S1 O2 104.26(15) . . ?
C1 S1 O3 100.62(13) . . ?
S1 O3 Sb1 136.44(9) . . ?
P1 N1 Sb1 93.08(7) . . ?
P2 N1 Sb1 92.98(7) . . ?
P2 N1 P1 96.09(8) . . ?
C10 N1 Sb1 123.98(11) . . ?
C10 N1 P1 121.62(13) . . ?
C10 N1 P2 121.47(13) . . ?
P2 N2 P1 102.35(9) . . ?
C20 N2 P1 128.55(19) . . ?
C20 N2 P2 128.3(2) . . ?
P1 N3 Sb1 105.87(9) . . ?
C30 N3 Sb1 126.81(14) . . ?
C30 N3 P1 125.06(16) . . ?
P2 N4 Sb1 105.67(9) . . ?
C40 N4 Sb1 126.15(13) . . ?
C40 N4 P2 125.16(13) . . ?
F1 C1 S1 111.3(3) . . ?
F2 C1 S1 112.4(2) . . ?
F2 C1 F1 108.0(3) . . ?
F3 C1 S1 109.2(3) . . ?
F3 C1 F1 107.7(3) . . ?
F3 C1 F2 108.0(4) . . ?
C11 C10 N1 107.09(16) . . ?
C12 C10 N1 108.59(17) . . ?
C12 C10 C11 110.51(18) . . ?
C13 C10 N1 108.05(17) . . ?
C13 C10 C11 111.0(2) . . ?
C13 C10 C12 111.45(19) . . ?
H11a C11 C10 109.5 . . ?
H11b C11 C10 109.5 . . ?
H11b C11 H11a 109.5 . . ?
H11c C11 C10 109.5 . . ?
H11c C11 H11a 109.5 . . ?
H11c C11 H11b 109.5 . . ?
H12a C12 C10 109.5 . . ?
H12b C12 C10 109.5 . . ?
H12b C12 H12a 109.5 . . ?
H12c C12 C10 109.5 . . ?
H12c C12 H12a 109.5 . . ?
H12c C12 H12b 109.5 . . ?
H13a C13 C10 109.5 . . ?
H13b C13 C10 109.5 . . ?
H13b C13 H13a 109.5 . . ?
H13c C13 C10 109.5 . . ?
H13c C13 H13a 109.5 . . ?
H13c C13 H13b 109.5 . . ?
C21 C20 N2 110.1(2) . . ?
C22 C20 N2 108.2(3) . . ?
C22 C20 C21 109.0(3) . . ?
C23 C20 N2 108.3(2) . . ?
C23 C20 C21 110.0(3) . . ?
C23 C20 C22 111.2(3) . . ?
H21a C21 C20 109.5 . . ?
H21b C21 C20 109.5 . . ?
H21b C21 H21a 109.5 . . ?
H21c C21 C20 109.5 . . ?
H21c C21 H21a 109.5 . . ?
H21c C21 H21b 109.5 . . ?
H22a C22 C20 109.5 . . ?
H22b C22 C20 109.5 . . ?
H22b C22 H22a 109.5 . . ?
H22c C22 C20 109.5 . . ?
H22c C22 H22a 109.5 . . ?
H22c C22 H22b 109.5 . . ?
H23a C23 C20 109.5 . . ?
H23b C23 C20 109.5 . . ?
H23b C23 H23a 109.5 . . ?
H23c C23 C20 109.5 . . ?
H23c C23 H23a 109.5 . . ?
H23c C23 H23b 109.5 . . ?
C31 C30 N3 109.34(18) . . ?
C32 C30 N3 109.2(3) . . ?
C32 C30 C31 108.3(3) . . ?
C33 C30 N3 109.4(2) . . ?
C33 C30 C31 109.2(3) . . ?
C33 C30 C32 111.4(3) . . ?
H31a C31 C30 109.5 . . ?
H31b C31 C30 109.5 . . ?
H31b C31 H31a 109.5 . . ?
H31c C31 C30 109.5 . . ?
H31c C31 H31a 109.5 . . ?
H31c C31 H31b 109.5 . . ?
H32a C32 C30 109.5 . . ?
H32b C32 C30 109.5 . . ?
H32b C32 H32a 109.5 . . ?
H32c C32 C30 109.5 . . ?
H32c C32 H32a 109.5 . . ?
H32c C32 H32b 109.5 . . ?
H33a C33 C30 109.5 . . ?
H33b C33 C30 109.5 . . ?
H33b C33 H33a 109.5 . . ?
H33c C33 C30 109.5 . . ?
H33c C33 H33a 109.5 . . ?
H33c C33 H33b 109.5 . . ?
C41 C40 N4 110.4(2) . . ?
C42 C40 N4 110.20(19) . . ?
C42 C40 C41 109.1(2) . . ?
C43 C40 N4 108.95(17) . . ?
C43 C40 C41 109.2(2) . . ?
C43 C40 C42 108.9(2) . . ?
H41a C41 C40 109.5 . . ?
H41b C41 C40 109.5 . . ?
H41b C41 H41a 109.5 . . ?
H41c C41 C40 109.5 . . ?
H41c C41 H41a 109.5 . . ?
H41c C41 H41b 109.5 . . ?
H42a C42 C40 109.5 . . ?
H42b C42 C40 109.5 . . ?
H42b C42 H42a 109.5 . . ?
H42c C42 C40 109.5 . . ?
H42c C42 H42a 109.5 . . ?
H42c C42 H42b 109.5 . . ?
H43a C43 C40 109.5 . . ?
H43b C43 C40 109.5 . . ?
H43b C43 H43a 109.5 . . ?
H43c C43 C40 109.5 . . ?
H43c C43 H43a 109.5 . . ?
H43c C43 H43b 109.5 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_chemical_melting_point          429-431
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: CHCl3'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
