# 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_g480_mn
_database_code_depnum_ccdc_archive 'CCDC 1992146'
loop_
_audit_author_name
_audit_author_address
'Christoph Feil'
;Universitity of Stuttgart
Germany
;
_audit_update_record             
;
2020-03-23 deposited with the CCDC.	2020-11-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C5 H10 N2 P, I'
_chemical_formula_sum            'C5 H10 I N2 P'
_chemical_formula_weight         256.02

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'
I I -0.4742 1.8119 '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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           59
_space_group_name_H-M_alt        'P m m n'
_space_group_name_Hall           '-P 2ab 2a'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   8.4133(14)
_cell_length_b                   7.1479(11)
_cell_length_c                   7.5050(11)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     451.33(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    130(2)
_cell_measurement_reflns_used    409
_cell_measurement_theta_min      2.714
_cell_measurement_theta_max      24.971

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.884
_exptl_crystal_F_000             244
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.111
_exptl_crystal_size_mid          0.097
_exptl_crystal_size_min          0.081
_exptl_absorpt_coefficient_mu    3.653
_shelx_estimated_absorpt_T_min   0.687
_shelx_estimated_absorpt_T_max   0.756
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.5327
_exptl_absorpt_correction_T_max  0.8917
_exptl_absorpt_process_details   'BLESSING 1995'
_exptl_absorpt_special_details   ?

_diffrn_ambient_temperature      130(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker Kappa ApexII Duo'
_diffrn_measurement_method       'Omega and phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            4551
_diffrn_reflns_av_unetI/netI     0.0366
_diffrn_reflns_av_R_equivalents  0.0645
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         2.714
_diffrn_reflns_theta_max         25.014
_diffrn_reflns_theta_full        25.014
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measured_fraction_theta_full 0.959
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_Laue_measured_fraction_full 0.959
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_point_group_measured_fraction_full 0.959
_reflns_number_total             447
_reflns_number_gt                409
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker ApexII Software Suite, 2008'
_computing_cell_refinement       'Bruker ApexII Software Suite, 2008'
_computing_data_reduction        'Bruker ApexII Software Suite, 2008'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXS plus XP (Sheldrick, 1991)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'

_refine_special_details          
;
due to the bad quality of the data and possible disorder perpendicular the 
CNCCN-plane use of constraints (general RIGU restraint, ISOR) for the refinement.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0290P)²+12.3500P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         447
_refine_ls_number_parameters     38
_refine_ls_number_restraints     45
_refine_ls_R_factor_all          0.0735
_refine_ls_R_factor_gt           0.0639
_refine_ls_wR_factor_ref         0.1480
_refine_ls_wR_factor_gt          0.1431
_refine_ls_goodness_of_fit_ref   1.288
_refine_ls_restrained_S_all      1.276
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.7500 0.7500 1.0068(8) 0.0454(19) Uani 1 4 d DS TU P . .
H1A H 0.612(17) 0.69(5) 1.01(6) 0.068 Uiso 0.25 1 d D U P A -1
H1B H 0.76(5) 0.914(17) 1.06(4) 0.068 Uiso 0.25 1 d D U P B -1
N1 N 0.8783(15) 0.7500 0.6596(15) 0.024(3) Uani 1 2 d S TU P . .
C1 C 0.7500 0.7500 0.764(3) 0.025(4) Uani 1 4 d S TU P . .
C2 C 0.8292(18) 0.7500 0.4850(18) 0.025(3) Uani 1 2 d S TU P . .
H2 H 0.8960 0.7500 0.3830 0.030 Uiso 1 2 calc R U P . .
C3 C 1.0428(19) 0.7500 0.721(2) 0.038(4) Uani 1 2 d S TU P . .
H3A H 1.0518 0.8264 0.8285 0.057 Uiso 0.5 1 calc R U P . .
H3B H 1.1112 0.8022 0.6273 0.057 Uiso 0.5 1 calc R U P . .
H3C H 1.0759 0.6215 0.7469 0.057 Uiso 0.5 1 calc R U P . .
I1 I 0.7500 0.2500 0.78027(18) 0.0304(6) Uani 1 4 d S TU P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1 C1 1.83(2) . ?
P1 H1A 1.250(11) . ?
P1 H1B 1.250(11) . ?
N1 C1 1.332(16) . ?
N1 C2 1.373(17) . ?
N1 C3 1.46(2) . ?
C1 N1 1.332(16) 2_665 ?
C2 C2 1.33(3) 2_665 ?
C2 H2 0.9500 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 P1 H1A 90(10) . . ?
C1 P1 H1B 110(10) . . ?
H1A P1 H1B 114(2) . . ?
C1 N1 C2 108.4(13) . . ?
C1 N1 C3 125.8(12) . . ?
C2 N1 C3 125.8(13) . . ?
N1 C1 N1 108.2(16) 2_665 . ?
N1 C1 P1 125.9(8) 2_665 . ?
N1 C1 P1 125.9(8) . . ?
C2 C2 N1 107.5(8) 2_665 . ?
C2 C2 H2 126.3 2_665 . ?
N1 C2 H2 126.3 . . ?
N1 C3 H3A 109.5 . . ?
N1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
N1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 N1 C1 N1 0.000(3) . . . 2_665 ?
C3 N1 C1 N1 180.000(3) . . . 2_665 ?
C2 N1 C1 P1 180.000(1) . . . . ?
C3 N1 C1 P1 0.000(3) . . . . ?
C1 N1 C2 C2 0.000(3) . . . 2_665 ?
C3 N1 C2 C2 180.000(3) . . . 2_665 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
P1 H1B I1 1.250(11) 3.2(3) 3.958(3) 119(19) 1_565
C2 H2 I1 0.95 3.22 4.062(15) 148.6 5_766
C3 H3B I1 0.98 3.30 4.143(17) 145.9 5_766

_refine_diff_density_max         2.867
_refine_diff_density_min         -2.254
_refine_diff_density_rms         0.272


# start Validation Reply Form

_vrf_PLAT029_g480_mn             
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.959 Why?  
RESPONSE: due to the bad quality of the data
;
_vrf_PLAT971_g480_mn             
;
PROBLEM: Check Calcd Resid. Dens.  1.13A   From I1              3.00 eA-3  
RESPONSE: possible disorder of the I-atom
;

# end Validation Reply Form
####################################################################### 
# 
# 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_g477_mn
_database_code_depnum_ccdc_archive 'CCDC 1992147'
loop_
_audit_author_name
_audit_author_address
'Christoph Feil'
;Universitity of Stuttgart
Germany
;
_audit_update_record             
;
2020-03-23 deposited with the CCDC.	2020-11-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C9 H18 N2 P, I'
_chemical_formula_sum            'C9 H18 I N2 P'
_chemical_formula_weight         312.12

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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_H-M_alt        'P 21/m'
_space_group_name_Hall           '-P 2yb'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   9.2450(5)
_cell_length_b                   7.4965(4)
_cell_length_c                   10.4442(6)
_cell_angle_alpha                90
_cell_angle_beta                 115.069(3)
_cell_angle_gamma                90
_cell_volume                     655.65(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    130(2)
_cell_measurement_reflns_used    2559
_cell_measurement_theta_min      2.153
_cell_measurement_theta_max      33.265

_exptl_crystal_description       prism
_exptl_crystal_colour            light-yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.581
_exptl_crystal_F_000             308
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.635
_exptl_crystal_size_mid          0.512
_exptl_crystal_size_min          0.280
_exptl_absorpt_coefficient_mu    2.530
_shelx_estimated_absorpt_T_min   0.296
_shelx_estimated_absorpt_T_max   0.538
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.1110
_exptl_absorpt_correction_T_max  0.3096
_exptl_absorpt_process_details   'BLESSING 1995'
_exptl_absorpt_special_details   ?

_diffrn_ambient_temperature      130(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker Kappa ApexII Duo'
_diffrn_measurement_method       'Omega and phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            17628
_diffrn_reflns_av_unetI/netI     0.0145
_diffrn_reflns_av_R_equivalents  0.0253
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.153
_diffrn_reflns_theta_max         33.265
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             2681
_reflns_number_gt                2559
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker ApexII Software Suite, 2008'
_computing_cell_refinement       'Bruker ApexII Software Suite, 2008'
_computing_data_reduction        'Bruker ApexII Software Suite, 2008'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXS plus XP (Sheldrick, 1991)'
_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)+(0.0235P)²+0.2339P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014)'
_refine_ls_extinction_coef       0.0374(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2681
_refine_ls_number_parameters     77
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0210
_refine_ls_R_factor_gt           0.0194
_refine_ls_wR_factor_ref         0.0496
_refine_ls_wR_factor_gt          0.0483
_refine_ls_goodness_of_fit_ref   1.188
_refine_ls_restrained_S_all      1.188
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 1.03094(5) 0.7500 0.82083(5) 0.02286(9) Uani 1 2 d S T P . .
H1 H 1.031(2) 0.619(3) 0.902(2) 0.034 Uiso 1 1 d . U . . .
C1 C 0.81547(19) 0.7500 0.71390(16) 0.0174(2) Uani 1 2 d S T P . .
N1 N 0.74580(16) 0.7500 0.57149(14) 0.0181(2) Uani 1 2 d S T P . .
N2 N 0.69774(16) 0.7500 0.75722(14) 0.0196(2) Uani 1 2 d S T P . .
C2 C 0.58273(19) 0.7500 0.52487(17) 0.0222(3) Uani 1 2 d S T P . .
H2 H 0.5057 0.7500 0.4292 0.027 Uiso 1 2 calc R U P . .
C3 C 0.5523(2) 0.7500 0.64072(18) 0.0234(3) Uani 1 2 d S T P . .
H3 H 0.4500 0.7500 0.6416 0.028 Uiso 1 2 calc R U P . .
C4 C 0.8286(2) 0.7500 0.47709(16) 0.0202(3) Uani 1 2 d S T P . .
H4 H 0.9463 0.7500 0.5375 0.024 Uiso 1 2 calc R U P . .
C5 C 0.78715(19) 0.5812(2) 0.38849(15) 0.0299(3) Uani 1 1 d . . . . .
H5A H 0.8421 0.5817 0.3263 0.045 Uiso 1 1 calc R U . . .
H5B H 0.8211 0.4769 0.4508 0.045 Uiso 1 1 calc R U . . .
H5C H 0.6715 0.5760 0.3312 0.045 Uiso 1 1 calc R U . . .
C6 C 0.7183(2) 0.7500 0.90543(18) 0.0255(3) Uani 1 2 d S T P . .
H6 H 0.8353 0.7500 0.9682 0.031 Uiso 1 2 calc R U P . .
C7 C 0.6467(2) 0.5809(3) 0.93479(16) 0.0371(3) Uani 1 1 d . . . . .
H7A H 0.6606 0.5814 1.0332 0.056 Uiso 1 1 calc R U . . .
H7B H 0.5327 0.5756 0.8714 0.056 Uiso 1 1 calc R U . . .
H7C H 0.7009 0.4766 0.9187 0.056 Uiso 1 1 calc R U . . .
I1 I 0.86010(2) 0.2500 0.73553(2) 0.02437(5) Uani 1 2 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
P1 C1 1.8249(16) . ?
P1 H1 1.30(2) . ?
C1 N2 1.344(2) . ?
C1 N1 1.347(2) . ?
N1 C2 1.374(2) . ?
N1 C4 1.482(2) . ?
N2 C3 1.379(2) . ?
N2 C6 1.478(2) . ?
C2 C3 1.353(2) . ?
C2 H2 0.9500 . ?
C3 H3 0.9500 . ?
C4 C5 1.5179(16) 4_575 ?
C4 C5 1.5179(16) . ?
C4 H4 1.0000 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 C7 1.5199(19) 4_575 ?
C6 C7 1.5199(19) . ?
C6 H6 1.0000 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 P1 H1 95.7(9) . . ?
N2 C1 N1 107.16(14) . . ?
N2 C1 P1 128.59(12) . . ?
N1 C1 P1 124.25(12) . . ?
C1 N1 C2 109.31(13) . . ?
C1 N1 C4 126.45(13) . . ?
C2 N1 C4 124.24(13) . . ?
C1 N2 C3 109.20(14) . . ?
C1 N2 C6 126.14(14) . . ?
C3 N2 C6 124.67(14) . . ?
C3 C2 N1 107.20(14) . . ?
C3 C2 H2 126.4 . . ?
N1 C2 H2 126.4 . . ?
C2 C3 N2 107.14(14) . . ?
C2 C3 H3 126.4 . . ?
N2 C3 H3 126.4 . . ?
N1 C4 C5 109.71(9) . 4_575 ?
N1 C4 C5 109.71(9) . . ?
C5 C4 C5 112.96(15) 4_575 . ?
N1 C4 H4 108.1 . . ?
C5 C4 H4 108.1 4_575 . ?
C5 C4 H4 108.1 . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N2 C6 C7 109.73(10) . 4_575 ?
N2 C6 C7 109.73(10) . . ?
C7 C6 C7 113.04(17) 4_575 . ?
N2 C6 H6 108.1 . . ?
C7 C6 H6 108.1 4_575 . ?
C7 C6 H6 108.1 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 C1 N1 C2 0.000(1) . . . . ?
P1 C1 N1 C2 180.000(1) . . . . ?
N2 C1 N1 C4 180.000(1) . . . . ?
P1 C1 N1 C4 0.000(1) . . . . ?
N1 C1 N2 C3 0.000(1) . . . . ?
P1 C1 N2 C3 180.000(1) . . . . ?
N1 C1 N2 C6 180.000(1) . . . . ?
P1 C1 N2 C6 0.000(1) . . . . ?
C1 N1 C2 C3 0.000(1) . . . . ?
C4 N1 C2 C3 180.000(0) . . . . ?
N1 C2 C3 N2 0.000(1) . . . . ?
C1 N2 C3 C2 0.000(1) . . . . ?
C6 N2 C3 C2 180.000(1) . . . . ?
C1 N1 C4 C5 -117.68(10) . . . 4_575 ?
C2 N1 C4 C5 62.32(10) . . . 4_575 ?
C1 N1 C4 C5 117.68(10) . . . . ?
C2 N1 C4 C5 -62.32(10) . . . . ?
C1 N2 C6 C7 117.61(11) . . . 4_575 ?
C3 N2 C6 C7 -62.39(11) . . . 4_575 ?
C1 N2 C6 C7 -117.61(11) . . . . ?
C3 N2 C6 C7 62.39(11) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
P1 H1 I1 1.30(2) 3.30(2) 4.0181(2) 114.8(11) .
C2 H2 I1 0.95 3.08 3.8369(16) 138.1 3_666
C5 H5B I1 0.98 3.31 4.2053(15) 152.7 .
C6 H6 I1 1.00 3.18 4.1073(18) 154.7 3_767

_refine_diff_density_max         0.787
_refine_diff_density_min         -0.907
_refine_diff_density_rms         0.095

####################################################################### 
# 
# 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_g483_mn
_database_code_depnum_ccdc_archive 'CCDC 1992150'
loop_
_audit_author_name
_audit_author_address
'Christoph Feil'
;Universitity of Stuttgart
Germany
;
_audit_update_record             
;
2020-03-23 deposited with the CCDC.	2020-11-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H40 N2 P, I, 2 (C2 H3 N)'
_chemical_formula_sum            'C32 H46 I N4 P'
_chemical_formula_weight         644.60

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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_H-M_alt        'P b c n'
_space_group_name_Hall           '-P 2n 2ab'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   21.5771(13)
_cell_length_b                   14.8112(8)
_cell_length_c                   21.4093(11)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6842.0(7)
_cell_formula_units_Z            8
_cell_measurement_temperature    130(2)
_cell_measurement_reflns_used    4801
_cell_measurement_theta_min      1.668
_cell_measurement_theta_max      26.403

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.252
_exptl_crystal_F_000             2672
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.195
_exptl_crystal_size_mid          0.167
_exptl_crystal_size_min          0.055
_exptl_absorpt_coefficient_mu    1.007
_shelx_estimated_absorpt_T_min   0.828
_shelx_estimated_absorpt_T_max   0.947
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.8868
_exptl_absorpt_correction_T_max  0.9728
_exptl_absorpt_process_details   'BLESSING 1995'
_exptl_absorpt_special_details   ?

_diffrn_ambient_temperature      130(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker Kappa ApexII Duo'
_diffrn_measurement_method       'Omega and phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            53388
_diffrn_reflns_av_unetI/netI     0.0375
_diffrn_reflns_av_R_equivalents  0.0473
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.668
_diffrn_reflns_theta_max         26.403
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_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             7008
_reflns_number_gt                4801
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker ApexII Software Suite, 2008'
_computing_cell_refinement       'Bruker ApexII Software Suite, 2008'
_computing_data_reduction        'Bruker ApexII Software Suite, 2008'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXS plus XP (Sheldrick, 1991)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'

_refine_special_details          
;
One solvent molecule acetonitrile disorderd about 2 position with the occupancy 0.5
and about the center of symmetry. Use of restraints (SADI, RIGU) for the refinement
of the solvent molecules.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0290P)²+8.7991P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7008
_refine_ls_number_parameters     376
_refine_ls_number_restraints     37
_refine_ls_R_factor_all          0.0726
_refine_ls_R_factor_gt           0.0383
_refine_ls_wR_factor_ref         0.0861
_refine_ls_wR_factor_gt          0.0759
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_restrained_S_all      1.013
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.46337(4) 0.23927(7) 0.42724(5) 0.0469(2) Uani 1 1 d D . . . .
H1P H 0.4731(16) 0.218(2) 0.4843(9) 0.056 Uiso 1 1 d D U . . .
C1 C 0.4888(2) 0.3553(3) 0.4285(3) 0.0846(15) Uani 1 1 d . . . . .
H1A H 0.5340 0.3573 0.4330 0.127 Uiso 1 1 calc R U . . .
H1B H 0.4768 0.3850 0.3895 0.127 Uiso 1 1 calc R U . . .
H1C H 0.4696 0.3866 0.4639 0.127 Uiso 1 1 calc R U . . .
C2 C 0.37899(13) 0.25034(19) 0.41883(12) 0.0220(6) Uani 1 1 d . . . . .
N1 N 0.33855(10) 0.27957(14) 0.46234(10) 0.0197(5) Uani 1 1 d . . . . .
N2 N 0.34445(10) 0.21604(15) 0.37218(10) 0.0202(5) Uani 1 1 d . . . . .
C3 C 0.27876(13) 0.26414(19) 0.44325(13) 0.0231(6) Uani 1 1 d . . . . .
H3 H 0.2420 0.2788 0.4655 0.028 Uiso 1 1 calc R U . . .
C4 C 0.28230(12) 0.22405(18) 0.38672(12) 0.0227(6) Uani 1 1 d . . . . .
H4 H 0.2484 0.2049 0.3616 0.027 Uiso 1 1 calc R U . . .
C5 C 0.35789(13) 0.3259(2) 0.51922(12) 0.0243(7) Uani 1 1 d . . . . .
C6 C 0.37702(13) 0.2722(2) 0.56958(13) 0.0281(7) Uani 1 1 d . . . . .
C7 C 0.40077(15) 0.3192(2) 0.62101(14) 0.0360(8) Uani 1 1 d . . . . .
H7 H 0.4147 0.2864 0.6564 0.043 Uiso 1 1 calc R U . . .
C8 C 0.40440(15) 0.4114(3) 0.62144(15) 0.0425(9) Uani 1 1 d . . . . .
H8 H 0.4220 0.4413 0.6565 0.051 Uiso 1 1 calc R U . . .
C9 C 0.38277(15) 0.4617(2) 0.57160(15) 0.0392(8) Uani 1 1 d . . . . .
H9 H 0.3842 0.5258 0.5735 0.047 Uiso 1 1 calc R U . . .
C10 C 0.35890(14) 0.4198(2) 0.51871(13) 0.0308(7) Uani 1 1 d . . . . .
C11 C 0.36951(13) 0.17983(19) 0.31448(12) 0.0236(6) Uani 1 1 d . . . . .
C12 C 0.37863(14) 0.2403(2) 0.26495(13) 0.0289(7) Uani 1 1 d . . . . .
C13 C 0.40468(15) 0.2052(2) 0.21110(14) 0.0372(8) Uani 1 1 d . . . . .
H13 H 0.4116 0.2438 0.1763 0.045 Uiso 1 1 calc R U . . .
C14 C 0.42076(15) 0.1154(3) 0.20707(14) 0.0412(9) Uani 1 1 d . . . . .
H14 H 0.4390 0.0931 0.1697 0.049 Uiso 1 1 calc R U . . .
C15 C 0.41081(15) 0.0574(2) 0.25625(14) 0.0356(8) Uani 1 1 d . . . . .
H15 H 0.4222 -0.0043 0.2524 0.043 Uiso 1 1 calc R U . . .
C16 C 0.38409(13) 0.0884(2) 0.31198(13) 0.0268(7) Uani 1 1 d . . . . .
C17 C 0.36930(15) 0.1707(2) 0.57029(14) 0.0351(7) Uani 1 1 d . . . . .
H17 H 0.3592 0.1510 0.5268 0.042 Uiso 1 1 calc R U . . .
C18 C 0.42771(19) 0.1209(3) 0.59065(19) 0.0577(11) Uani 1 1 d . . . . .
H18A H 0.4200 0.0557 0.5902 0.087 Uiso 1 1 calc R U . . .
H18B H 0.4616 0.1351 0.5618 0.087 Uiso 1 1 calc R U . . .
H18C H 0.4391 0.1398 0.6330 0.087 Uiso 1 1 calc R U . . .
C19 C 0.31440(19) 0.1462(3) 0.61182(18) 0.0583(11) Uani 1 1 d . . . . .
H19A H 0.3092 0.0805 0.6124 0.087 Uiso 1 1 calc R U . . .
H19B H 0.3220 0.1680 0.6544 0.087 Uiso 1 1 calc R U . . .
H19C H 0.2767 0.1744 0.5954 0.087 Uiso 1 1 calc R U . . .
C20 C 0.33254(18) 0.4747(2) 0.46479(16) 0.0444(9) Uani 1 1 d . . . . .
H20 H 0.3250 0.4326 0.4291 0.053 Uiso 1 1 calc R U . . .
C21 C 0.26989(19) 0.5154(3) 0.48397(19) 0.0614(11) Uani 1 1 d . . . . .
H21A H 0.2530 0.5508 0.4492 0.092 Uiso 1 1 calc R U . . .
H21B H 0.2410 0.4667 0.4946 0.092 Uiso 1 1 calc R U . . .
H21C H 0.2757 0.5547 0.5203 0.092 Uiso 1 1 calc R U . . .
C22 C 0.3759(2) 0.5493(3) 0.4419(2) 0.0713(13) Uani 1 1 d . . . . .
H22A H 0.3563 0.5819 0.4073 0.107 Uiso 1 1 calc R U . . .
H22B H 0.3844 0.5913 0.4762 0.107 Uiso 1 1 calc R U . . .
H22C H 0.4149 0.5225 0.4275 0.107 Uiso 1 1 calc R U . . .
C23 C 0.35922(16) 0.3390(2) 0.26850(14) 0.0373(8) Uani 1 1 d . . . . .
H23 H 0.3459 0.3515 0.3124 0.045 Uiso 1 1 calc R U . . .
C24 C 0.3044(2) 0.3565(3) 0.2264(2) 0.0688(13) Uani 1 1 d . . . . .
H24A H 0.2708 0.3147 0.2369 0.103 Uiso 1 1 calc R U . . .
H24B H 0.2901 0.4188 0.2321 0.103 Uiso 1 1 calc R U . . .
H24C H 0.3167 0.3475 0.1828 0.103 Uiso 1 1 calc R U . . .
C25 C 0.4120(2) 0.4027(3) 0.2533(2) 0.0791(14) Uani 1 1 d . . . . .
H25A H 0.4471 0.3903 0.2810 0.119 Uiso 1 1 calc R U . . .
H25B H 0.4248 0.3939 0.2098 0.119 Uiso 1 1 calc R U . . .
H25C H 0.3982 0.4652 0.2591 0.119 Uiso 1 1 calc R U . . .
C26 C 0.37253(15) 0.0239(2) 0.36604(14) 0.0332(7) Uani 1 1 d . . . . .
H26 H 0.3528 0.0590 0.4007 0.040 Uiso 1 1 calc R U . . .
C27 C 0.43352(16) -0.0154(2) 0.39072(16) 0.0438(9) Uani 1 1 d . . . . .
H27A H 0.4248 -0.0566 0.4254 0.066 Uiso 1 1 calc R U . . .
H27B H 0.4545 -0.0485 0.3572 0.066 Uiso 1 1 calc R U . . .
H27C H 0.4603 0.0337 0.4053 0.066 Uiso 1 1 calc R U . . .
C28 C 0.32772(17) -0.0511(2) 0.34696(18) 0.0489(9) Uani 1 1 d . . . . .
H28A H 0.3210 -0.0917 0.3824 0.073 Uiso 1 1 calc R U . . .
H28B H 0.2881 -0.0244 0.3342 0.073 Uiso 1 1 calc R U . . .
H28C H 0.3453 -0.0852 0.3120 0.073 Uiso 1 1 calc R U . . .
I1 I 0.12751(2) 0.29852(2) 0.53244(2) 0.04539(9) Uani 1 1 d . . . . .
N1S N 0.29681(15) 0.3633(3) 0.76734(15) 0.0622(9) Uani 1 1 d D U . . .
C1S C 0.27317(16) 0.3756(2) 0.72094(16) 0.0402(8) Uani 1 1 d D U . . .
C2S C 0.24263(17) 0.3921(3) 0.66205(16) 0.0479(9) Uani 1 1 d D U . . .
H2S1 H 0.2265 0.3351 0.6454 0.072 Uiso 1 1 calc R U . . .
H2S2 H 0.2723 0.4179 0.6324 0.072 Uiso 1 1 calc R U . . .
H2S3 H 0.2083 0.4345 0.6683 0.072 Uiso 1 1 calc R U . . .
N2SA N 0.4758(3) 0.6028(4) 0.2726(3) 0.0537(16) Uani 0.5 1 d D U P A -1
C3SA C 0.4547(3) 0.6561(5) 0.3042(3) 0.0414(16) Uani 0.5 1 d D U P A -1
C4SA C 0.4321(13) 0.7246(9) 0.3462(9) 0.053(6) Uani 0.5 1 d D U P A -1
H4S1 H 0.4451 0.7842 0.3312 0.080 Uiso 0.5 1 calc R U P A -1
H4S2 H 0.4490 0.7142 0.3880 0.080 Uiso 0.5 1 calc R U P A -1
H4S3 H 0.3867 0.7220 0.3478 0.080 Uiso 0.5 1 calc R U P A -1
N2SB N 0.4755(3) 0.8333(4) 0.2579(3) 0.0550(19) Uani 0.5 1 d D U P B -2
C3SB C 0.4556(3) 0.7859(4) 0.2944(3) 0.0414(16) Uani 0.5 1 d D U P B -2
C4SB C 0.4281(13) 0.7246(10) 0.3388(9) 0.049(4) Uani 0.5 1 d D U P B -2
H4S4 H 0.4492 0.6661 0.3365 0.073 Uiso 0.5 1 calc R U P B -2
H4S5 H 0.3841 0.7167 0.3290 0.073 Uiso 0.5 1 calc R U P B -2
H4S6 H 0.4324 0.7494 0.3810 0.073 Uiso 0.5 1 calc R U P B -2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1 C1 1.805(4) . ?
P1 C2 1.837(3) . ?
P1 H1P 1.279(18) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 N2 1.346(3) . ?
C2 N1 1.348(3) . ?
N1 C3 1.373(3) . ?
N1 C5 1.459(3) . ?
N2 C4 1.382(3) . ?
N2 C11 1.451(3) . ?
C3 C4 1.350(4) . ?
C3 H3 0.9500 . ?
C4 H4 0.9500 . ?
C5 C10 1.391(4) . ?
C5 C6 1.402(4) . ?
C6 C7 1.400(4) . ?
C6 C17 1.513(4) . ?
C7 C8 1.368(5) . ?
C7 H7 0.9500 . ?
C8 C9 1.382(5) . ?
C8 H8 0.9500 . ?
C9 C10 1.391(4) . ?
C9 H9 0.9500 . ?
C10 C20 1.523(4) . ?
C11 C16 1.391(4) . ?
C11 C12 1.402(4) . ?
C12 C13 1.384(4) . ?
C12 C23 1.523(5) . ?
C13 C14 1.378(5) . ?
C13 H13 0.9500 . ?
C14 C15 1.376(5) . ?
C14 H14 0.9500 . ?
C15 C16 1.402(4) . ?
C15 H15 0.9500 . ?
C16 C26 1.521(4) . ?
C17 C18 1.524(5) . ?
C17 C19 1.525(5) . ?
C17 H17 1.0000 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 C22 1.528(5) . ?
C20 C21 1.536(5) . ?
C20 H20 1.0000 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C24 1.510(5) . ?
C23 C25 1.515(5) . ?
C23 H23 1.0000 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 C28 1.528(5) . ?
C26 C27 1.533(4) . ?
C26 H26 1.0000 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
N1S C1S 1.131(4) . ?
C1S C2S 1.443(5) . ?
C2S H2S1 0.9800 . ?
C2S H2S2 0.9800 . ?
C2S H2S3 0.9800 . ?
N2SA C3SA 1.136(6) . ?
C3SA C4SA 1.441(9) . ?
C4SA H4S1 0.9800 . ?
C4SA H4S2 0.9800 . ?
C4SA H4S3 0.9800 . ?
N2SB C3SB 1.135(6) . ?
C3SB C4SB 1.441(9) . ?
C4SB H4S4 0.9800 . ?
C4SB H4S5 0.9800 . ?
C4SB H4S6 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 P1 C2 102.61(17) . . ?
C1 P1 H1P 99.9(15) . . ?
C2 P1 H1P 106.2(16) . . ?
P1 C1 H1A 109.5 . . ?
P1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
P1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N2 C2 N1 106.0(2) . . ?
N2 C2 P1 126.0(2) . . ?
N1 C2 P1 127.1(2) . . ?
C2 N1 C3 110.4(2) . . ?
C2 N1 C5 122.9(2) . . ?
C3 N1 C5 126.6(2) . . ?
C2 N2 C4 109.8(2) . . ?
C2 N2 C11 124.4(2) . . ?
C4 N2 C11 125.8(2) . . ?
C4 C3 N1 106.7(2) . . ?
C4 C3 H3 126.7 . . ?
N1 C3 H3 126.7 . . ?
C3 C4 N2 107.1(2) . . ?
C3 C4 H4 126.4 . . ?
N2 C4 H4 126.4 . . ?
C10 C5 C6 124.6(3) . . ?
C10 C5 N1 117.9(2) . . ?
C6 C5 N1 117.4(2) . . ?
C7 C6 C5 115.5(3) . . ?
C7 C6 C17 121.8(3) . . ?
C5 C6 C17 122.6(3) . . ?
C8 C7 C6 121.5(3) . . ?
C8 C7 H7 119.2 . . ?
C6 C7 H7 119.2 . . ?
C7 C8 C9 120.9(3) . . ?
C7 C8 H8 119.6 . . ?
C9 C8 H8 119.6 . . ?
C8 C9 C10 120.8(3) . . ?
C8 C9 H9 119.6 . . ?
C10 C9 H9 119.6 . . ?
C9 C10 C5 116.5(3) . . ?
C9 C10 C20 121.1(3) . . ?
C5 C10 C20 122.3(3) . . ?
C16 C11 C12 124.1(3) . . ?
C16 C11 N2 118.5(2) . . ?
C12 C11 N2 117.4(2) . . ?
C13 C12 C11 116.6(3) . . ?
C13 C12 C23 120.9(3) . . ?
C11 C12 C23 122.5(3) . . ?
C14 C13 C12 121.1(3) . . ?
C14 C13 H13 119.4 . . ?
C12 C13 H13 119.4 . . ?
C15 C14 C13 121.0(3) . . ?
C15 C14 H14 119.5 . . ?
C13 C14 H14 119.5 . . ?
C14 C15 C16 120.7(3) . . ?
C14 C15 H15 119.6 . . ?
C16 C15 H15 119.6 . . ?
C11 C16 C15 116.4(3) . . ?
C11 C16 C26 123.0(2) . . ?
C15 C16 C26 120.6(3) . . ?
C6 C17 C18 113.1(3) . . ?
C6 C17 C19 109.1(3) . . ?
C18 C17 C19 111.1(3) . . ?
C6 C17 H17 107.7 . . ?
C18 C17 H17 107.7 . . ?
C19 C17 H17 107.7 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C10 C20 C22 113.6(3) . . ?
C10 C20 C21 109.6(3) . . ?
C22 C20 C21 110.0(3) . . ?
C10 C20 H20 107.8 . . ?
C22 C20 H20 107.8 . . ?
C21 C20 H20 107.8 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C24 C23 C25 110.7(3) . . ?
C24 C23 C12 110.5(3) . . ?
C25 C23 C12 112.4(3) . . ?
C24 C23 H23 107.7 . . ?
C25 C23 H23 107.7 . . ?
C12 C23 H23 107.7 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C16 C26 C28 110.9(3) . . ?
C16 C26 C27 111.1(3) . . ?
C28 C26 C27 111.0(3) . . ?
C16 C26 H26 107.9 . . ?
C28 C26 H26 107.9 . . ?
C27 C26 H26 107.9 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
N1S C1S C2S 179.4(5) . . ?
C1S C2S H2S1 109.5 . . ?
C1S C2S H2S2 109.5 . . ?
H2S1 C2S H2S2 109.5 . . ?
C1S C2S H2S3 109.5 . . ?
H2S1 C2S H2S3 109.5 . . ?
H2S2 C2S H2S3 109.5 . . ?
N2SA C3SA C4SA 176.0(14) . . ?
C3SA C4SA H4S1 109.5 . . ?
C3SA C4SA H4S2 109.5 . . ?
H4S1 C4SA H4S2 109.5 . . ?
C3SA C4SA H4S3 109.5 . . ?
H4S1 C4SA H4S3 109.5 . . ?
H4S2 C4SA H4S3 109.5 . . ?
N2SB C3SB C4SB 177.4(14) . . ?
C3SB C4SB H4S4 109.5 . . ?
C3SB C4SB H4S5 109.5 . . ?
H4S4 C4SB H4S5 109.5 . . ?
C3SB C4SB H4S6 109.5 . . ?
H4S4 C4SB H4S6 109.5 . . ?
H4S5 C4SB H4S6 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 P1 C2 N2 121.4(3) . . . . ?
C1 P1 C2 N1 -71.2(3) . . . . ?
N2 C2 N1 C3 -0.2(3) . . . . ?
P1 C2 N1 C3 -169.6(2) . . . . ?
N2 C2 N1 C5 -176.7(2) . . . . ?
P1 C2 N1 C5 13.9(4) . . . . ?
N1 C2 N2 C4 0.1(3) . . . . ?
P1 C2 N2 C4 169.6(2) . . . . ?
N1 C2 N2 C11 177.7(2) . . . . ?
P1 C2 N2 C11 -12.8(4) . . . . ?
C2 N1 C3 C4 0.3(3) . . . . ?
C5 N1 C3 C4 176.6(2) . . . . ?
N1 C3 C4 N2 -0.2(3) . . . . ?
C2 N2 C4 C3 0.1(3) . . . . ?
C11 N2 C4 C3 -177.5(2) . . . . ?
C2 N1 C5 C10 94.0(3) . . . . ?
C3 N1 C5 C10 -81.9(3) . . . . ?
C2 N1 C5 C6 -83.0(3) . . . . ?
C3 N1 C5 C6 101.1(3) . . . . ?
C10 C5 C6 C7 -2.6(4) . . . . ?
N1 C5 C6 C7 174.1(2) . . . . ?
C10 C5 C6 C17 174.0(3) . . . . ?
N1 C5 C6 C17 -9.3(4) . . . . ?
C5 C6 C7 C8 0.4(4) . . . . ?
C17 C6 C7 C8 -176.3(3) . . . . ?
C6 C7 C8 C9 2.1(5) . . . . ?
C7 C8 C9 C10 -2.5(5) . . . . ?
C8 C9 C10 C5 0.3(5) . . . . ?
C8 C9 C10 C20 177.4(3) . . . . ?
C6 C5 C10 C9 2.3(4) . . . . ?
N1 C5 C10 C9 -174.4(3) . . . . ?
C6 C5 C10 C20 -174.8(3) . . . . ?
N1 C5 C10 C20 8.5(4) . . . . ?
C2 N2 C11 C16 90.1(3) . . . . ?
C4 N2 C11 C16 -92.6(3) . . . . ?
C2 N2 C11 C12 -88.6(3) . . . . ?
C4 N2 C11 C12 88.6(3) . . . . ?
C16 C11 C12 C13 -1.0(4) . . . . ?
N2 C11 C12 C13 177.7(3) . . . . ?
C16 C11 C12 C23 177.0(3) . . . . ?
N2 C11 C12 C23 -4.3(4) . . . . ?
C11 C12 C13 C14 -0.2(5) . . . . ?
C23 C12 C13 C14 -178.2(3) . . . . ?
C12 C13 C14 C15 0.7(5) . . . . ?
C13 C14 C15 C16 -0.1(5) . . . . ?
C12 C11 C16 C15 1.5(4) . . . . ?
N2 C11 C16 C15 -177.2(2) . . . . ?
C12 C11 C16 C26 -178.8(3) . . . . ?
N2 C11 C16 C26 2.6(4) . . . . ?
C14 C15 C16 C11 -0.9(4) . . . . ?
C14 C15 C16 C26 179.4(3) . . . . ?
C7 C6 C17 C18 -50.8(4) . . . . ?
C5 C6 C17 C18 132.8(3) . . . . ?
C7 C6 C17 C19 73.5(4) . . . . ?
C5 C6 C17 C19 -102.9(3) . . . . ?
C9 C10 C20 C22 50.8(4) . . . . ?
C5 C10 C20 C22 -132.2(3) . . . . ?
C9 C10 C20 C21 -72.6(4) . . . . ?
C5 C10 C20 C21 104.3(3) . . . . ?
C13 C12 C23 C24 68.5(4) . . . . ?
C11 C12 C23 C24 -109.5(3) . . . . ?
C13 C12 C23 C25 -55.7(4) . . . . ?
C11 C12 C23 C25 126.3(3) . . . . ?
C11 C16 C26 C28 119.0(3) . . . . ?
C15 C16 C26 C28 -61.2(4) . . . . ?
C11 C16 C26 C27 -117.0(3) . . . . ?
C15 C16 C26 C27 62.8(4) . . . . ?

_refine_diff_density_max         0.679
_refine_diff_density_min         -0.767
_refine_diff_density_rms         0.065

####################################################################### 
# 
# 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_g479_mn
_database_code_depnum_ccdc_archive 'CCDC 1992151'
loop_
_audit_author_name
_audit_author_address
'Christoph Feil'
;Universitity of Stuttgart
Germany
;
_audit_update_record             
;
2020-03-23 deposited with the CCDC.	2020-11-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C21 H26 N2 P, I, 0.5(C2 H3 N)'
_chemical_formula_sum            'C22 H27.50 I N2.50 P'
_chemical_formula_weight         484.83

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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   17.8150(8)
_cell_length_b                   19.1134(9)
_cell_length_c                   14.7481(7)
_cell_angle_alpha                90
_cell_angle_beta                 114.254(2)
_cell_angle_gamma                90
_cell_volume                     4578.5(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    130(2)
_cell_measurement_reflns_used    13048
_cell_measurement_theta_min      1.645
_cell_measurement_theta_max      33.170

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_F_000             1960
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.489
_exptl_crystal_size_mid          0.421
_exptl_crystal_size_min          0.266
_exptl_absorpt_coefficient_mu    1.478
_shelx_estimated_absorpt_T_min   0.532
_shelx_estimated_absorpt_T_max   0.695
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.5919
_exptl_absorpt_correction_T_max  0.7353
_exptl_absorpt_process_details   'BLESSING 1995'
_exptl_absorpt_special_details   ?

_diffrn_ambient_temperature      130(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker Kappa ApexII Duo'
_diffrn_measurement_method       'Omega and phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            81625
_diffrn_reflns_av_unetI/netI     0.0285
_diffrn_reflns_av_R_equivalents  0.0304
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.645
_diffrn_reflns_theta_max         33.170
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             17413
_reflns_number_gt                13044
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker ApexII Software Suite, 2008'
_computing_cell_refinement       'Bruker ApexII Software Suite, 2008'
_computing_data_reduction        'Bruker ApexII Software Suite, 2008'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXS plus XP (Sheldrick, 1991)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'

_refine_special_details          
;
Use of restraints (RIGU) for the solvent acetone. PH2 moieties disordered.
s.o.f. (= 0.600(3)) determined from isotropic refinement using EADP constraint for the 
pair of P-atoms. Fixed to 0.60 and 0.40, respectively, for the anisotropic refinement.
Use of restraints (SADI) for the C-P distandes and the geormetry of the PH2 moiety
(1,2 and 1,3 distances, C---H, P-H and H---H).
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0346P)²+3.2003P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         17413
_refine_ls_number_parameters     533
_refine_ls_number_restraints     85
_refine_ls_R_factor_all          0.0530
_refine_ls_R_factor_gt           0.0323
_refine_ls_wR_factor_ref         0.0830
_refine_ls_wR_factor_gt          0.0734
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_restrained_S_all      1.008
_refine_ls_shift/su_max          0.003
_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
C1 C 0.60927(12) 0.58516(8) 0.77798(12) 0.0224(3) Uani 1 1 d D . . . .
P1 P 0.60322(9) 0.68180(7) 0.76704(10) 0.0296(3) Uani 0.6 1 d D . P A 1
H1P1 H 0.6767(10) 0.6906(12) 0.772(3) 0.044 Uiso 0.6 1 d D U P B 1
H1P2 H 0.602(2) 0.6940(12) 0.8524(14) 0.044 Uiso 0.6 1 d D U P C 1
P1A P 0.62737(14) 0.67951(10) 0.80373(15) 0.0314(4) Uani 0.4 1 d D . P A 2
H1P3 H 0.666(3) 0.6905(13) 0.748(3) 0.047 Uiso 0.4 1 d D U P D 2
H1P4 H 0.676(3) 0.6743(13) 0.8964(12) 0.047 Uiso 0.4 1 d D U P E 2
N1 N 0.64861(9) 0.54059(7) 0.74180(11) 0.0216(3) Uani 1 1 d . . . . .
N2 N 0.55851(10) 0.54622(7) 0.80442(11) 0.0234(3) Uani 1 1 d . . . . .
C2 C 0.62150(12) 0.47275(9) 0.74487(14) 0.0266(4) Uani 1 1 d . . . . .
H2 H 0.6394 0.4316 0.7236 0.032 Uiso 1 1 calc R U . . .
C3 C 0.56500(13) 0.47638(9) 0.78371(14) 0.0275(4) Uani 1 1 d . . . . .
H3 H 0.5354 0.4384 0.7947 0.033 Uiso 1 1 calc R U . . .
C4 C 0.50885(12) 0.57276(9) 0.85383(13) 0.0231(3) Uani 1 1 d . . . . .
C5 C 0.42680(12) 0.58997(9) 0.79626(13) 0.0261(3) Uani 1 1 d . . . . .
C6 C 0.38023(13) 0.61446(10) 0.84579(15) 0.0281(4) Uani 1 1 d . . . . .
H6 H 0.3242 0.6266 0.8084 0.034 Uiso 1 1 calc R U . . .
C7 C 0.41396(13) 0.62166(9) 0.94899(15) 0.0278(4) Uani 1 1 d . . . . .
C8 C 0.49620(13) 0.60410(9) 1.00300(14) 0.0272(4) Uani 1 1 d . . . . .
H8 H 0.5194 0.6092 1.0733 0.033 Uiso 1 1 calc R U . . .
C9 C 0.54573(12) 0.57918(9) 0.95709(13) 0.0241(3) Uani 1 1 d . . . . .
C10 C 0.71075(11) 0.55717(8) 0.70571(13) 0.0208(3) Uani 1 1 d . . . . .
C11 C 0.68887(11) 0.55373(9) 0.60339(13) 0.0218(3) Uani 1 1 d . . . . .
C12 C 0.75105(12) 0.56379(9) 0.57057(15) 0.0269(3) Uani 1 1 d . . . . .
H12 H 0.7377 0.5624 0.5012 0.032 Uiso 1 1 calc R U . . .
C13 C 0.83241(12) 0.57580(10) 0.63664(17) 0.0309(4) Uani 1 1 d . . . . .
C14 C 0.85073(12) 0.58098(10) 0.73722(16) 0.0312(4) Uani 1 1 d . . . . .
H14 H 0.9057 0.5910 0.7823 0.037 Uiso 1 1 calc R U . . .
C15 C 0.79089(12) 0.57186(9) 0.77421(14) 0.0266(4) Uani 1 1 d . . . . .
C16 C 0.38949(14) 0.58180(12) 0.68490(15) 0.0365(4) Uani 1 1 d . . . . .
H16A H 0.3802 0.5321 0.6678 0.055 Uiso 1 1 calc R U . . .
H16B H 0.4271 0.6012 0.6580 0.055 Uiso 1 1 calc R U . . .
H16C H 0.3369 0.6069 0.6564 0.055 Uiso 1 1 calc R U . . .
C17 C 0.36198(15) 0.64961(11) 0.99938(18) 0.0368(5) Uani 1 1 d . . . . .
H17A H 0.3196 0.6152 0.9942 0.055 Uiso 1 1 calc R U . . .
H17B H 0.3356 0.6933 0.9672 0.055 Uiso 1 1 calc R U . . .
H17C H 0.3968 0.6586 1.0697 0.055 Uiso 1 1 calc R U . . .
C18 C 0.63463(13) 0.56126(10) 1.01694(15) 0.0307(4) Uani 1 1 d . . . . .
H18A H 0.6474 0.5658 1.0879 0.046 Uiso 1 1 calc R U . . .
H18B H 0.6696 0.5932 0.9994 0.046 Uiso 1 1 calc R U . . .
H18C H 0.6449 0.5130 1.0025 0.046 Uiso 1 1 calc R U . . .
C19 C 0.60203(12) 0.53923(11) 0.53067(14) 0.0290(4) Uani 1 1 d . . . . .
H19A H 0.5919 0.4887 0.5272 0.044 Uiso 1 1 calc R U . . .
H19B H 0.5940 0.5566 0.4648 0.044 Uiso 1 1 calc R U . . .
H19C H 0.5636 0.5629 0.5526 0.044 Uiso 1 1 calc R U . . .
C20 C 0.89950(15) 0.58106(13) 0.5995(2) 0.0456(6) Uani 1 1 d . . . . .
H20A H 0.9477 0.6043 0.6498 0.068 Uiso 1 1 calc R U . . .
H20B H 0.8795 0.6083 0.5378 0.068 Uiso 1 1 calc R U . . .
H20C H 0.9149 0.5340 0.5868 0.068 Uiso 1 1 calc R U . . .
C21 C 0.81282(15) 0.57609(12) 0.88424(15) 0.0377(5) Uani 1 1 d . . . . .
H21A H 0.8727 0.5724 0.9210 0.057 Uiso 1 1 calc R U . . .
H21B H 0.7861 0.5377 0.9037 0.057 Uiso 1 1 calc R U . . .
H21C H 0.7940 0.6209 0.8996 0.057 Uiso 1 1 calc R U . . .
I1 I 0.36336(2) 0.36051(2) 0.70745(2) 0.03095(4) Uani 1 1 d . . . . .
C22 C 1.08670(10) 0.80322(8) 0.71093(12) 0.0194(3) Uani 1 1 d D . . . .
P2 P 1.10013(13) 0.72545(9) 0.79075(11) 0.0322(3) Uani 0.6 1 d D . P F 1
H2P1 H 1.0232(7) 0.7124(15) 0.765(2) 0.048 Uiso 0.6 1 d D U P G 1
H2P2 H 1.134(2) 0.6861(11) 0.747(2) 0.048 Uiso 0.6 1 d D U P H 1
P2A P 1.0916(2) 0.71351(13) 0.75973(19) 0.0385(6) Uani 0.4 1 d D . P F 2
H2P3 H 1.064(3) 0.6817(12) 0.6756(12) 0.058 Uiso 0.4 1 d D U P I 2
H2P4 H 1.1704(7) 0.7103(17) 0.807(4) 0.058 Uiso 0.4 1 d D U P J 2
N3 N 1.14884(8) 0.84241(7) 0.70868(11) 0.0192(3) Uani 1 1 d . . . . .
N4 N 1.01696(8) 0.83854(8) 0.65835(11) 0.0209(3) Uani 1 1 d . . . . .
C23 C 1.11777(11) 0.90240(9) 0.65407(14) 0.0257(3) Uani 1 1 d . . . . .
H23 H 1.1486 0.9383 0.6406 0.031 Uiso 1 1 calc R U . . .
C24 C 1.03499(11) 0.90047(9) 0.62334(14) 0.0261(4) Uani 1 1 d . . . . .
H24 H 0.9967 0.9350 0.5851 0.031 Uiso 1 1 calc R U . . .
C25 C 1.23526(10) 0.82783(8) 0.76314(13) 0.0195(3) Uani 1 1 d . . . . .
C26 C 1.27137(10) 0.84749(9) 0.86269(13) 0.0219(3) Uani 1 1 d . . . . .
C27 C 1.35554(11) 0.83356(10) 0.91403(14) 0.0261(3) Uani 1 1 d . . . . .
H27 H 1.3823 0.8460 0.9823 0.031 Uiso 1 1 calc R U . . .
C28 C 1.40114(11) 0.80202(9) 0.86816(16) 0.0275(4) Uani 1 1 d . . . . .
C29 C 1.36196(11) 0.78398(9) 0.76838(15) 0.0262(4) Uani 1 1 d . . . . .
H29 H 1.3931 0.7629 0.7367 0.031 Uiso 1 1 calc R U . . .
C30 C 1.27814(11) 0.79597(9) 0.71331(14) 0.0227(3) Uani 1 1 d . . . . .
C31 C 0.93481(10) 0.81474(9) 0.63900(13) 0.0213(3) Uani 1 1 d . . . . .
C32 C 0.89279(10) 0.77646(9) 0.55268(13) 0.0232(3) Uani 1 1 d . . . . .
C33 C 0.81281(11) 0.75525(10) 0.53483(14) 0.0252(3) Uani 1 1 d . . . . .
H33 H 0.7821 0.7289 0.4767 0.030 Uiso 1 1 calc R U . . .
C34 C 0.77726(10) 0.77176(9) 0.59992(14) 0.0250(3) Uani 1 1 d . . . . .
C35 C 0.82181(11) 0.81034(10) 0.68534(14) 0.0260(3) Uani 1 1 d . . . . .
H35 H 0.7973 0.8216 0.7298 0.031 Uiso 1 1 calc R U . . .
C36 C 0.90203(11) 0.83287(10) 0.70676(14) 0.0244(3) Uani 1 1 d . . . . .
C37 C 1.22237(12) 0.88091(11) 0.91308(14) 0.0295(4) Uani 1 1 d . . . . .
H37A H 1.1853 0.9162 0.8689 0.044 Uiso 1 1 calc R U . . .
H37B H 1.2599 0.9033 0.9749 0.044 Uiso 1 1 calc R U . . .
H37C H 1.1899 0.8451 0.9283 0.044 Uiso 1 1 calc R U . . .
C38 C 1.49156(12) 0.78718(12) 0.92591(19) 0.0388(5) Uani 1 1 d . . . . .
H38A H 1.5028 0.7381 0.9167 0.058 Uiso 1 1 calc R U . . .
H38B H 1.5068 0.7962 0.9967 0.058 Uiso 1 1 calc R U . . .
H38C H 1.5238 0.8176 0.9019 0.058 Uiso 1 1 calc R U . . .
C39 C 1.23523(13) 0.77449(11) 0.60635(15) 0.0315(4) Uani 1 1 d . . . . .
H39A H 1.2748 0.7521 0.5851 0.047 Uiso 1 1 calc R U . . .
H39B H 1.2118 0.8159 0.5652 0.047 Uiso 1 1 calc R U . . .
H39C H 1.1910 0.7414 0.5989 0.047 Uiso 1 1 calc R U . . .
C40 C 0.93156(13) 0.75770(12) 0.48242(16) 0.0333(4) Uani 1 1 d . . . . .
H40A H 0.9547 0.7999 0.4660 0.050 Uiso 1 1 calc R U . . .
H40B H 0.8897 0.7377 0.4214 0.050 Uiso 1 1 calc R U . . .
H40C H 0.9755 0.7234 0.5141 0.050 Uiso 1 1 calc R U . . .
C41 C 0.69121(12) 0.74726(11) 0.57827(17) 0.0325(4) Uani 1 1 d . . . . .
H41A H 0.6615 0.7386 0.5068 0.049 Uiso 1 1 calc R U . . .
H41B H 0.6624 0.7833 0.5990 0.049 Uiso 1 1 calc R U . . .
H41C H 0.6938 0.7039 0.6150 0.049 Uiso 1 1 calc R U . . .
C42 C 0.95077(13) 0.87496(12) 0.79838(16) 0.0346(4) Uani 1 1 d . . . . .
H42A H 1.0036 0.8518 0.8361 0.052 Uiso 1 1 calc R U . . .
H42B H 0.9198 0.8786 0.8398 0.052 Uiso 1 1 calc R U . . .
H42C H 0.9607 0.9219 0.7789 0.052 Uiso 1 1 calc R U . . .
I2 I 1.11111(2) 0.56229(2) 0.89567(2) 0.03531(4) Uani 1 1 d . . . . .
N1S N 0.1229(3) 0.6087(2) 0.5742(3) 0.1027(12) Uani 1 1 d . U . . .
C1S C 0.1532(3) 0.5633(2) 0.6254(4) 0.0847(13) Uani 1 1 d . U . . .
C2S C 0.1944(3) 0.50619(19) 0.6959(3) 0.0871(12) Uani 1 1 d . U . . .
H2S1 H 0.2539 0.5150 0.7272 0.131 Uiso 1 1 calc R U . . .
H2S2 H 0.1839 0.4616 0.6599 0.131 Uiso 1 1 calc R U . . .
H2S3 H 0.1729 0.5041 0.7471 0.131 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.345(2) . ?
C1 N2 1.347(2) . ?
C1 P1A 1.844(3) . ?
C1 P1 1.853(2) . ?
P1 H1P1 1.292(9) . ?
P1 H1P2 1.292(9) . ?
P1A H1P3 1.287(9) . ?
P1A H1P4 1.287(9) . ?
N1 C2 1.391(2) . ?
N1 C10 1.447(2) . ?
N2 C3 1.385(2) . ?
N2 C4 1.449(2) . ?
C2 C3 1.349(3) . ?
C2 H2 0.9500 . ?
C3 H3 0.9500 . ?
C4 C9 1.394(2) . ?
C4 C5 1.395(3) . ?
C5 C6 1.393(3) . ?
C5 C16 1.506(3) . ?
C6 C7 1.395(3) . ?
C6 H6 0.9500 . ?
C7 C8 1.391(3) . ?
C7 C17 1.504(3) . ?
C8 C9 1.398(3) . ?
C8 H8 0.9500 . ?
C9 C18 1.502(3) . ?
C10 C11 1.397(2) . ?
C10 C15 1.397(3) . ?
C11 C12 1.392(3) . ?
C11 C19 1.502(3) . ?
C12 C13 1.394(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.385(3) . ?
C13 C20 1.509(3) . ?
C14 C15 1.394(3) . ?
C14 H14 0.9500 . ?
C15 C21 1.507(3) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 N4 1.345(2) . ?
C22 N3 1.348(2) . ?
C22 P2A 1.848(3) . ?
C22 P2 1.850(2) . ?
P2 H2P1 1.287(9) . ?
P2 H2P2 1.286(9) . ?
P2A H2P3 1.284(9) . ?
P2A H2P4 1.286(9) . ?
N3 C23 1.380(2) . ?
N3 C25 1.441(2) . ?
N4 C24 1.381(2) . ?
N4 C31 1.445(2) . ?
C23 C24 1.354(2) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 C26 1.391(2) . ?
C25 C30 1.399(2) . ?
C26 C27 1.400(2) . ?
C26 C37 1.502(3) . ?
C27 C28 1.390(3) . ?
C27 H27 0.9500 . ?
C28 C29 1.388(3) . ?
C28 C38 1.508(3) . ?
C29 C30 1.395(2) . ?
C29 H29 0.9500 . ?
C30 C39 1.500(3) . ?
C31 C32 1.390(2) . ?
C31 C36 1.392(3) . ?
C32 C33 1.399(2) . ?
C32 C40 1.506(3) . ?
C33 C34 1.386(3) . ?
C33 H33 0.9500 . ?
C34 C35 1.393(3) . ?
C34 C41 1.506(2) . ?
C35 C36 1.399(2) . ?
C35 H35 0.9500 . ?
C36 C42 1.504(3) . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
N1S C1S 1.131(6) . ?
C1S C2S 1.478(7) . ?
C2S H2S1 0.9800 . ?
C2S H2S2 0.9800 . ?
C2S H2S3 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 C1 N2 106.63(14) . . ?
N1 C1 P1A 128.73(15) . . ?
N2 C1 P1A 124.22(15) . . ?
N1 C1 P1 128.16(14) . . ?
N2 C1 P1 123.65(14) . . ?
C1 P1 H1P1 96.0(10) . . ?
C1 P1 H1P2 96.8(10) . . ?
H1P1 P1 H1P2 110.4(19) . . ?
C1 P1A H1P3 97.0(11) . . ?
C1 P1A H1P4 97.4(11) . . ?
H1P3 P1A H1P4 113(2) . . ?
C1 N1 C2 109.46(15) . . ?
C1 N1 C10 127.54(14) . . ?
C2 N1 C10 122.99(14) . . ?
C1 N2 C3 110.00(15) . . ?
C1 N2 C4 124.99(14) . . ?
C3 N2 C4 124.88(15) . . ?
C3 C2 N1 107.18(15) . . ?
C3 C2 H2 126.4 . . ?
N1 C2 H2 126.4 . . ?
C2 C3 N2 106.73(16) . . ?
C2 C3 H3 126.6 . . ?
N2 C3 H3 126.6 . . ?
C9 C4 C5 123.36(16) . . ?
C9 C4 N2 117.96(17) . . ?
C5 C4 N2 118.68(15) . . ?
C6 C5 C4 117.46(17) . . ?
C6 C5 C16 121.06(18) . . ?
C4 C5 C16 121.47(17) . . ?
C5 C6 C7 121.54(19) . . ?
C5 C6 H6 119.2 . . ?
C7 C6 H6 119.2 . . ?
C8 C7 C6 118.79(17) . . ?
C8 C7 C17 121.36(18) . . ?
C6 C7 C17 119.84(19) . . ?
C7 C8 C9 122.05(17) . . ?
C7 C8 H8 119.0 . . ?
C9 C8 H8 119.0 . . ?
C4 C9 C8 116.80(17) . . ?
C4 C9 C18 122.13(17) . . ?
C8 C9 C18 121.06(17) . . ?
C11 C10 C15 122.64(17) . . ?
C11 C10 N1 118.10(15) . . ?
C15 C10 N1 119.14(15) . . ?
C12 C11 C10 117.41(17) . . ?
C12 C11 C19 120.69(16) . . ?
C10 C11 C19 121.90(16) . . ?
C11 C12 C13 121.81(18) . . ?
C11 C12 H12 119.1 . . ?
C13 C12 H12 119.1 . . ?
C14 C13 C12 118.70(18) . . ?
C14 C13 C20 120.7(2) . . ?
C12 C13 C20 120.6(2) . . ?
C13 C14 C15 121.91(18) . . ?
C13 C14 H14 119.0 . . ?
C15 C14 H14 119.0 . . ?
C14 C15 C10 117.44(17) . . ?
C14 C15 C21 120.86(18) . . ?
C10 C15 C21 121.68(18) . . ?
C5 C16 H16A 109.5 . . ?
C5 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C5 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C7 C17 H17A 109.5 . . ?
C7 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C7 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C9 C18 H18A 109.5 . . ?
C9 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C9 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C11 C19 H19A 109.5 . . ?
C11 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C11 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C13 C20 H20A 109.5 . . ?
C13 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C13 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C15 C21 H21A 109.5 . . ?
C15 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C15 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N4 C22 N3 106.29(14) . . ?
N4 C22 P2A 125.11(17) . . ?
N3 C22 P2A 128.09(17) . . ?
N4 C22 P2 128.14(14) . . ?
N3 C22 P2 124.69(14) . . ?
C22 P2 H2P1 97.0(11) . . ?
C22 P2 H2P2 96.7(10) . . ?
H2P1 P2 H2P2 113(2) . . ?
C22 P2A H2P3 97.2(11) . . ?
C22 P2A H2P4 97.0(11) . . ?
H2P3 P2A H2P4 114(2) . . ?
C22 N3 C23 109.84(14) . . ?
C22 N3 C25 125.38(14) . . ?
C23 N3 C25 124.50(14) . . ?
C22 N4 C24 110.12(14) . . ?
C22 N4 C31 125.23(14) . . ?
C24 N4 C31 124.64(14) . . ?
C24 C23 N3 107.06(15) . . ?
C24 C23 H23 126.5 . . ?
N3 C23 H23 126.5 . . ?
C23 C24 N4 106.68(15) . . ?
C23 C24 H24 126.7 . . ?
N4 C24 H24 126.7 . . ?
C26 C25 C30 123.82(15) . . ?
C26 C25 N3 117.46(15) . . ?
C30 C25 N3 118.71(15) . . ?
C25 C26 C27 116.60(17) . . ?
C25 C26 C37 121.76(15) . . ?
C27 C26 C37 121.64(17) . . ?
C28 C27 C26 121.98(18) . . ?
C28 C27 H27 119.0 . . ?
C26 C27 H27 119.0 . . ?
C29 C28 C27 118.92(16) . . ?
C29 C28 C38 120.48(19) . . ?
C27 C28 C38 120.60(19) . . ?
C28 C29 C30 121.88(17) . . ?
C28 C29 H29 119.1 . . ?
C30 C29 H29 119.1 . . ?
C29 C30 C25 116.80(17) . . ?
C29 C30 C39 121.91(17) . . ?
C25 C30 C39 121.28(16) . . ?
C32 C31 C36 124.15(16) . . ?
C32 C31 N4 117.85(16) . . ?
C36 C31 N4 117.99(15) . . ?
C31 C32 C33 116.64(17) . . ?
C31 C32 C40 121.93(16) . . ?
C33 C32 C40 121.42(17) . . ?
C34 C33 C32 121.58(17) . . ?
C34 C33 H33 119.2 . . ?
C32 C33 H33 119.2 . . ?
C33 C34 C35 119.61(16) . . ?
C33 C34 C41 119.81(18) . . ?
C35 C34 C41 120.58(18) . . ?
C34 C35 C36 121.14(17) . . ?
C34 C35 H35 119.4 . . ?
C36 C35 H35 119.4 . . ?
C31 C36 C35 116.87(17) . . ?
C31 C36 C42 121.35(16) . . ?
C35 C36 C42 121.78(17) . . ?
C26 C37 H37A 109.5 . . ?
C26 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C26 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C28 C38 H38A 109.5 . . ?
C28 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C28 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C30 C39 H39A 109.5 . . ?
C30 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C30 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C32 C40 H40A 109.5 . . ?
C32 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C32 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C34 C41 H41A 109.5 . . ?
C34 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C34 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C36 C42 H42A 109.5 . . ?
C36 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C36 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
N1S C1S C2S 177.5(5) . . ?
C1S C2S H2S1 109.5 . . ?
C1S C2S H2S2 109.5 . . ?
H2S1 C2S H2S2 109.5 . . ?
C1S C2S H2S3 109.5 . . ?
H2S1 C2S H2S3 109.5 . . ?
H2S2 C2S H2S3 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 C1 N1 C2 0.5(2) . . . . ?
P1A C1 N1 C2 173.20(16) . . . . ?
P1 C1 N1 C2 -165.43(15) . . . . ?
N2 C1 N1 C10 -178.60(16) . . . . ?
P1A C1 N1 C10 -5.9(3) . . . . ?
P1 C1 N1 C10 15.5(3) . . . . ?
N1 C1 N2 C3 -0.7(2) . . . . ?
P1A C1 N2 C3 -173.82(16) . . . . ?
P1 C1 N2 C3 166.03(14) . . . . ?
N1 C1 N2 C4 175.17(16) . . . . ?
P1A C1 N2 C4 2.1(3) . . . . ?
P1 C1 N2 C4 -18.1(3) . . . . ?
C1 N1 C2 C3 -0.1(2) . . . . ?
C10 N1 C2 C3 179.04(16) . . . . ?
N1 C2 C3 N2 -0.3(2) . . . . ?
C1 N2 C3 C2 0.6(2) . . . . ?
C4 N2 C3 C2 -175.25(17) . . . . ?
C1 N2 C4 C9 -84.3(2) . . . . ?
C3 N2 C4 C9 91.0(2) . . . . ?
C1 N2 C4 C5 96.3(2) . . . . ?
C3 N2 C4 C5 -88.4(2) . . . . ?
C9 C4 C5 C6 -0.3(3) . . . . ?
N2 C4 C5 C6 179.17(16) . . . . ?
C9 C4 C5 C16 -179.68(18) . . . . ?
N2 C4 C5 C16 -0.3(3) . . . . ?
C4 C5 C6 C7 0.0(3) . . . . ?
C16 C5 C6 C7 179.44(18) . . . . ?
C5 C6 C7 C8 0.3(3) . . . . ?
C5 C6 C7 C17 178.83(18) . . . . ?
C6 C7 C8 C9 -0.4(3) . . . . ?
C17 C7 C8 C9 -178.88(17) . . . . ?
C5 C4 C9 C8 0.2(3) . . . . ?
N2 C4 C9 C8 -179.25(15) . . . . ?
C5 C4 C9 C18 -179.05(17) . . . . ?
N2 C4 C9 C18 1.5(2) . . . . ?
C7 C8 C9 C4 0.1(3) . . . . ?
C7 C8 C9 C18 179.37(17) . . . . ?
C1 N1 C10 C11 -107.6(2) . . . . ?
C2 N1 C10 C11 73.4(2) . . . . ?
C1 N1 C10 C15 76.1(2) . . . . ?
C2 N1 C10 C15 -102.9(2) . . . . ?
C15 C10 C11 C12 1.7(2) . . . . ?
N1 C10 C11 C12 -174.49(15) . . . . ?
C15 C10 C11 C19 -178.80(17) . . . . ?
N1 C10 C11 C19 5.0(2) . . . . ?
C10 C11 C12 C13 1.0(3) . . . . ?
C19 C11 C12 C13 -178.59(17) . . . . ?
C11 C12 C13 C14 -3.0(3) . . . . ?
C11 C12 C13 C20 175.33(19) . . . . ?
C12 C13 C14 C15 2.5(3) . . . . ?
C20 C13 C14 C15 -175.81(19) . . . . ?
C13 C14 C15 C10 0.0(3) . . . . ?
C13 C14 C15 C21 178.56(18) . . . . ?
C11 C10 C15 C14 -2.1(3) . . . . ?
N1 C10 C15 C14 174.00(15) . . . . ?
C11 C10 C15 C21 179.30(17) . . . . ?
N1 C10 C15 C21 -4.6(2) . . . . ?
N4 C22 N3 C23 -0.2(2) . . . . ?
P2A C22 N3 C23 171.80(16) . . . . ?
P2 C22 N3 C23 -170.25(15) . . . . ?
N4 C22 N3 C25 173.93(15) . . . . ?
P2A C22 N3 C25 -14.0(3) . . . . ?
P2 C22 N3 C25 3.9(3) . . . . ?
N3 C22 N4 C24 -0.4(2) . . . . ?
P2A C22 N4 C24 -172.80(16) . . . . ?
P2 C22 N4 C24 169.10(15) . . . . ?
N3 C22 N4 C31 178.20(16) . . . . ?
P2A C22 N4 C31 5.9(3) . . . . ?
P2 C22 N4 C31 -12.3(3) . . . . ?
C22 N3 C23 C24 0.8(2) . . . . ?
C25 N3 C23 C24 -173.39(17) . . . . ?
N3 C23 C24 N4 -1.1(2) . . . . ?
C22 N4 C24 C23 1.0(2) . . . . ?
C31 N4 C24 C23 -177.69(17) . . . . ?
C22 N3 C25 C26 -80.9(2) . . . . ?
C23 N3 C25 C26 92.4(2) . . . . ?
C22 N3 C25 C30 100.0(2) . . . . ?
C23 N3 C25 C30 -86.6(2) . . . . ?
C30 C25 C26 C27 -0.3(2) . . . . ?
N3 C25 C26 C27 -179.35(15) . . . . ?
C30 C25 C26 C37 -179.35(16) . . . . ?
N3 C25 C26 C37 1.6(2) . . . . ?
C25 C26 C27 C28 0.3(3) . . . . ?
C37 C26 C27 C28 179.36(17) . . . . ?
C26 C27 C28 C29 0.1(3) . . . . ?
C26 C27 C28 C38 -179.46(17) . . . . ?
C27 C28 C29 C30 -0.6(3) . . . . ?
C38 C28 C29 C30 178.95(17) . . . . ?
C28 C29 C30 C25 0.6(3) . . . . ?
C28 C29 C30 C39 -178.09(17) . . . . ?
C26 C25 C30 C29 -0.2(2) . . . . ?
N3 C25 C30 C29 178.87(15) . . . . ?
C26 C25 C30 C39 178.59(16) . . . . ?
N3 C25 C30 C39 -2.4(2) . . . . ?
C22 N4 C31 C32 -91.3(2) . . . . ?
C24 N4 C31 C32 87.1(2) . . . . ?
C22 N4 C31 C36 90.1(2) . . . . ?
C24 N4 C31 C36 -91.5(2) . . . . ?
C36 C31 C32 C33 -0.3(3) . . . . ?
N4 C31 C32 C33 -178.80(15) . . . . ?
C36 C31 C32 C40 -179.40(18) . . . . ?
N4 C31 C32 C40 2.1(3) . . . . ?
C31 C32 C33 C34 0.1(3) . . . . ?
C40 C32 C33 C34 179.26(18) . . . . ?
C32 C33 C34 C35 0.0(3) . . . . ?
C32 C33 C34 C41 -179.43(17) . . . . ?
C33 C34 C35 C36 0.0(3) . . . . ?
C41 C34 C35 C36 179.43(17) . . . . ?
C32 C31 C36 C35 0.3(3) . . . . ?
N4 C31 C36 C35 178.80(15) . . . . ?
C32 C31 C36 C42 -179.49(18) . . . . ?
N4 C31 C36 C42 -1.0(3) . . . . ?
C34 C35 C36 C31 -0.2(3) . . . . ?
C34 C35 C36 C42 179.62(18) . . . . ?

_refine_diff_density_max         1.232
_refine_diff_density_min         -0.832
_refine_diff_density_rms         0.086

####################################################################### 
# 
# 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_g535_mn
_database_code_depnum_ccdc_archive 'CCDC 1992148'
loop_
_audit_author_name
_audit_author_address
'Christoph Feil'
;Universitity of Stuttgart
Germany
;
_audit_update_record             
;
2020-03-23 deposited with the CCDC.	2020-11-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C29 H41 N2 P'
_chemical_formula_sum            'C29 H41 N2 P'
_chemical_formula_weight         448.61

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   40.4446(12)
_cell_length_b                   10.7492(3)
_cell_length_c                   12.5916(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5474.2(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    135(2)
_cell_measurement_reflns_used    6627
_cell_measurement_theta_min      2.185
_cell_measurement_theta_max      66.619

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.089
_exptl_crystal_F_000             1952
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.126
_exptl_crystal_size_mid          0.101
_exptl_crystal_size_min          0.037
_exptl_absorpt_coefficient_mu    1.003
_shelx_estimated_absorpt_T_min   0.884
_shelx_estimated_absorpt_T_max   0.964
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7731
_exptl_absorpt_correction_T_max  0.8642
_exptl_absorpt_process_details   'BLESSING 1995'
_exptl_absorpt_special_details   ?

_diffrn_ambient_temperature      135(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker Kappa ApexII Duo'
_diffrn_measurement_method       'Omega and phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            22897
_diffrn_reflns_av_unetI/netI     0.0516
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.185
_diffrn_reflns_theta_max         66.619
_diffrn_reflns_theta_full        66.619
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measured_fraction_theta_full 0.967
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_Laue_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.806
_diffrn_reflns_point_group_measured_fraction_full 0.806
_reflns_number_total             7792
_reflns_number_gt                6627
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.588
_reflns_Friedel_fraction_max     0.628
_reflns_Friedel_fraction_full    0.628

_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       'Bruker ApexII Software Suite, 2008'
_computing_cell_refinement       'Bruker ApexII Software Suite, 2008'
_computing_data_reduction        'Bruker ApexII Software Suite, 2008'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXS plus XP (Sheldrick, 1991)'
_computing_publication_material  ?

_refine_special_details          
;
4 iPr groups disordered, use of constraints (EADP) and restraints (SADI)
for the refinement. Disordered atoms refined isotropically.
Use of general RIGU restraint.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0505P)²+1.2200P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 2043 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.029(13)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         7792
_refine_ls_number_parameters     565
_refine_ls_number_restraints     1085
_refine_ls_R_factor_all          0.0574
_refine_ls_R_factor_gt           0.0449
_refine_ls_wR_factor_ref         0.1085
_refine_ls_wR_factor_gt          0.1025
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.285
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.48756(2) 0.18987(9) 0.67553(8) 0.0296(2) Uani 1 1 d . U . . .
C1 C 0.53243(9) 0.1919(4) 0.6404(3) 0.0321(9) Uani 1 1 d . U . . .
H1A H 0.5447 0.2486 0.6883 0.039 Uiso 1 1 calc R U . . .
H1B H 0.5420 0.1074 0.6469 0.039 Uiso 1 1 calc R U . . .
C2 C 0.53470(10) 0.2371(4) 0.5264(3) 0.0367(10) Uani 1 1 d . U . . .
H2A H 0.5579 0.2397 0.5045 0.055 Uiso 1 1 calc R U . . .
H2B H 0.5225 0.1802 0.4800 0.055 Uiso 1 1 calc R U . . .
H2C H 0.5251 0.3207 0.5212 0.055 Uiso 1 1 calc R U . . .
C3 C 0.48547(9) 0.1531(3) 0.8113(3) 0.0236(8) Uani 1 1 d . U . . .
N1 N 0.50749(7) 0.1295(3) 0.8922(2) 0.0237(6) Uani 1 1 d . U . . .
N2 N 0.45478(7) 0.1422(3) 0.8603(2) 0.0230(7) Uani 1 1 d . U . . .
C4 C 0.49078(10) 0.1025(3) 0.9863(3) 0.0275(8) Uani 1 1 d . U . . .
H4 H 0.5006 0.0817 1.0526 0.033 Uiso 1 1 calc R U . . .
C5 C 0.45848(10) 0.1112(3) 0.9658(3) 0.0289(9) Uani 1 1 d . U . . .
H5 H 0.4411 0.0984 1.0153 0.035 Uiso 1 1 calc R U . . .
C6 C 0.54302(8) 0.1468(3) 0.8881(3) 0.0245(8) Uani 1 1 d . U . . .
C7 C 0.55513(9) 0.2680(3) 0.8932(3) 0.0324(9) Uani 1 1 d D U . . .
C8 C 0.58942(10) 0.2825(4) 0.8905(4) 0.0396(10) Uani 1 1 d . U . . .
H8 H 0.5987 0.3636 0.8942 0.047 Uiso 1 1 calc R U . . .
C9 C 0.61002(10) 0.1813(4) 0.8826(4) 0.0430(11) Uani 1 1 d . U . . .
H9 H 0.6333 0.1931 0.8794 0.052 Uiso 1 1 calc R U . . .
C10 C 0.59713(10) 0.0627(4) 0.8794(3) 0.0368(10) Uani 1 1 d . U . . .
H10 H 0.6117 -0.0063 0.8745 0.044 Uiso 1 1 calc R U . . .
C11 C 0.56312(9) 0.0419(3) 0.8833(3) 0.0281(8) Uani 1 1 d D U . . .
C12 C 0.42391(9) 0.1687(3) 0.8071(3) 0.0252(8) Uani 1 1 d . U . . .
C13 C 0.40612(9) 0.0706(3) 0.7640(3) 0.0271(8) Uani 1 1 d D U . . .
C14 C 0.37700(9) 0.1002(4) 0.7105(3) 0.0345(10) Uani 1 1 d . U . . .
H14 H 0.3640 0.0355 0.6807 0.041 Uiso 1 1 calc R U . . .
C15 C 0.36682(10) 0.2218(4) 0.7004(3) 0.0394(10) Uani 1 1 d . U . . .
H15 H 0.3471 0.2403 0.6623 0.047 Uiso 1 1 calc R U . . .
C16 C 0.38490(10) 0.3166(4) 0.7449(4) 0.0392(10) Uani 1 1 d . U . . .
H16 H 0.3774 0.3999 0.7378 0.047 Uiso 1 1 calc R U . . .
C17 C 0.41384(9) 0.2929(3) 0.8000(3) 0.0297(9) Uani 1 1 d D U . . .
C18 C 0.53267(11) 0.3804(3) 0.9057(3) 0.0451(11) Uani 1 1 d D U . . .
H18A H 0.5093 0.3499 0.9057 0.054 Uiso 0.682(14) 1 calc R U P A 1
H18B H 0.5114 0.3577 0.8702 0.054 Uiso 0.318(14) 1 calc R U P A 2
C19A C 0.5392(3) 0.4426(8) 1.0146(5) 0.0549(19) Uiso 0.682(14) 1 d D . P A 1
H19A H 0.5371 0.3804 1.0710 0.082 Uiso 0.682(14) 1 calc R U P A 1
H19B H 0.5616 0.4777 1.0154 0.082 Uiso 0.682(14) 1 calc R U P A 1
H19C H 0.5230 0.5091 1.0261 0.082 Uiso 0.682(14) 1 calc R U P A 1
C20A C 0.5359(2) 0.4768(7) 0.8180(6) 0.0544(19) Uiso 0.682(14) 1 d D . P A 1
H20A H 0.5206 0.5458 0.8319 0.082 Uiso 0.682(14) 1 calc R U P A 1
H20B H 0.5586 0.5081 0.8160 0.082 Uiso 0.682(14) 1 calc R U P A 1
H20C H 0.5304 0.4385 0.7496 0.082 Uiso 0.682(14) 1 calc R U P A 1
C19B C 0.5239(5) 0.4096(15) 1.0186(8) 0.0549(19) Uiso 0.318(14) 1 d D . P A 2
H19D H 0.5095 0.4827 1.0206 0.082 Uiso 0.318(14) 1 calc R U P A 2
H19E H 0.5124 0.3383 1.0502 0.082 Uiso 0.318(14) 1 calc R U P A 2
H19F H 0.5442 0.4268 1.0588 0.082 Uiso 0.318(14) 1 calc R U P A 2
C20B C 0.5470(5) 0.4891(11) 0.8413(14) 0.0544(19) Uiso 0.318(14) 1 d D . P A 2
H20D H 0.5519 0.4610 0.7689 0.082 Uiso 0.318(14) 1 calc R U P A 2
H20E H 0.5308 0.5570 0.8387 0.082 Uiso 0.318(14) 1 calc R U P A 2
H20F H 0.5673 0.5186 0.8751 0.082 Uiso 0.318(14) 1 calc R U P A 2
C21 C 0.54863(10) -0.0887(3) 0.8828(3) 0.0349(9) Uani 1 1 d D U . . .
H21 H 0.5284 -0.0860 0.9284 0.042 Uiso 1 1 calc R U . . .
C22 C 0.57173(11) -0.1852(4) 0.9319(4) 0.0443(11) Uani 1 1 d D U . . .
H22A H 0.5786 -0.1572 1.0026 0.066 Uiso 1 1 calc R U . . .
H22B H 0.5601 -0.2649 0.9381 0.066 Uiso 1 1 calc R U . . .
H22C H 0.5912 -0.1955 0.8866 0.066 Uiso 1 1 calc R U . . .
C23 C 0.53748(14) -0.1286(4) 0.7739(4) 0.0581(14) Uani 1 1 d D U . . .
H23A H 0.5284 -0.2130 0.7776 0.087 Uiso 1 1 calc R U . . .
H23B H 0.5204 -0.0713 0.7480 0.087 Uiso 1 1 calc R U . . .
H23C H 0.5564 -0.1276 0.7251 0.087 Uiso 1 1 calc R U . . .
C24 C 0.41725(10) -0.0641(3) 0.7754(3) 0.0305(9) Uani 1 1 d D U . . .
H24 H 0.4380 -0.0655 0.8188 0.037 Uiso 1 1 calc R U . . .
C25 C 0.42490(13) -0.1212(4) 0.6667(4) 0.0542(13) Uani 1 1 d D U . . .
H25A H 0.4320 -0.2077 0.6759 0.081 Uiso 1 1 calc R U . . .
H25B H 0.4050 -0.1188 0.6223 0.081 Uiso 1 1 calc R U . . .
H25C H 0.4426 -0.0737 0.6323 0.081 Uiso 1 1 calc R U . . .
C26 C 0.39119(11) -0.1414(4) 0.8327(4) 0.0453(11) Uani 1 1 d D U . . .
H26A H 0.3989 -0.2275 0.8390 0.068 Uiso 1 1 calc R U . . .
H26B H 0.3874 -0.1068 0.9037 0.068 Uiso 1 1 calc R U . . .
H26C H 0.3705 -0.1395 0.7922 0.068 Uiso 1 1 calc R U . . .
C27 C 0.43314(10) 0.3968(3) 0.8546(3) 0.0361(10) Uani 1 1 d D U . . .
H27 H 0.4568 0.3703 0.8582 0.043 Uiso 1 1 calc R U . . .
C28 C 0.42113(12) 0.4152(5) 0.9674(3) 0.0533(13) Uani 1 1 d D U . . .
H28A H 0.4221 0.3358 1.0056 0.080 Uiso 1 1 calc R U . . .
H28B H 0.4352 0.4762 1.0033 0.080 Uiso 1 1 calc R U . . .
H28C H 0.3983 0.4454 0.9664 0.080 Uiso 1 1 calc R U . . .
C29 C 0.43183(18) 0.5194(4) 0.7936(4) 0.083(2) Uani 1 1 d D U . . .
H29A H 0.4397 0.5061 0.7208 0.124 Uiso 1 1 calc R U . . .
H29B H 0.4090 0.5500 0.7919 0.124 Uiso 1 1 calc R U . . .
H29C H 0.4460 0.5808 0.8289 0.124 Uiso 1 1 calc R U . . .
P2 P 0.26956(3) 0.44761(10) 0.23994(9) 0.0357(3) Uani 1 1 d . U . . .
C30 C 0.23993(9) 0.4353(4) 0.3527(3) 0.0378(10) Uani 1 1 d . U . . .
H30A H 0.2400 0.3497 0.3818 0.045 Uiso 1 1 calc R U . . .
H30B H 0.2462 0.4937 0.4101 0.045 Uiso 1 1 calc R U . . .
C31 C 0.20589(11) 0.4678(5) 0.3092(4) 0.0490(12) Uani 1 1 d . U . . .
H31A H 0.1895 0.4624 0.3664 0.074 Uiso 1 1 calc R U . . .
H31B H 0.2062 0.5526 0.2808 0.074 Uiso 1 1 calc R U . . .
H31C H 0.2000 0.4093 0.2526 0.074 Uiso 1 1 calc R U . . .
C32 C 0.30935(9) 0.4220(3) 0.2943(3) 0.0249(8) Uani 1 1 d . U . . .
N3 N 0.33686(7) 0.4244(3) 0.2295(2) 0.0261(7) Uani 1 1 d . U . . .
N4 N 0.32161(7) 0.3966(3) 0.3934(2) 0.0243(7) Uani 1 1 d . U . . .
C33 C 0.36502(9) 0.4000(3) 0.2873(3) 0.0285(8) Uani 1 1 d . U . . .
H33 H 0.3869 0.3958 0.2602 0.034 Uiso 1 1 calc R U . . .
C34 C 0.35596(9) 0.3832(3) 0.3888(3) 0.0283(8) Uani 1 1 d . U . . .
H34 H 0.3702 0.3655 0.4468 0.034 Uiso 1 1 calc R U . . .
C35 C 0.33437(9) 0.4357(4) 0.1162(3) 0.0306(9) Uani 1 1 d . U . . .
C36 C 0.33621(10) 0.5541(4) 0.0721(4) 0.0410(10) Uani 1 1 d D U . . .
C37 C 0.33212(12) 0.5632(6) -0.0368(4) 0.0639(15) Uani 1 1 d . U . . .
H37 H 0.3333 0.6423 -0.0702 0.077 Uiso 1 1 calc R U . . .
C38 C 0.32637(12) 0.4600(7) -0.0964(4) 0.0741(17) Uani 1 1 d . U . . .
H38 H 0.3228 0.4688 -0.1706 0.089 Uiso 1 1 calc R U . . .
C39 C 0.32565(12) 0.3437(7) -0.0522(4) 0.0653(15) Uani 1 1 d . U . . .
H39 H 0.3222 0.2731 -0.0963 0.078 Uiso 1 1 calc R U . . .
C40 C 0.32996(10) 0.3276(4) 0.0576(4) 0.0418(11) Uani 1 1 d D U . . .
C41 C 0.30330(9) 0.3836(3) 0.4902(3) 0.0239(8) Uani 1 1 d . U . . .
C42 C 0.30125(9) 0.4867(3) 0.5580(3) 0.0264(8) Uani 1 1 d D U . . .
C43 C 0.28322(10) 0.4713(4) 0.6511(3) 0.0314(9) Uani 1 1 d . U . . .
H43 H 0.2807 0.5396 0.6982 0.038 Uiso 1 1 calc R U . . .
C44 C 0.26888(9) 0.3579(4) 0.6765(3) 0.0338(9) Uani 1 1 d . U . . .
H44 H 0.2571 0.3489 0.7414 0.041 Uiso 1 1 calc R U . . .
C45 C 0.27155(9) 0.2580(3) 0.6081(3) 0.0289(8) Uani 1 1 d . U . . .
H45 H 0.2615 0.1810 0.6265 0.035 Uiso 1 1 calc R U . . .
C46 C 0.28867(9) 0.2683(3) 0.5126(3) 0.0249(8) Uani 1 1 d D U . . .
C47 C 0.34376(10) 0.6689(4) 0.1385(4) 0.0530(13) Uani 1 1 d D U . . .
H47A H 0.3391 0.6550 0.2156 0.064 Uiso 0.506(12) 1 calc R U P B 1
H47B H 0.3464 0.6344 0.2118 0.064 Uiso 0.494(12) 1 calc R U P B 2
C48A C 0.37997(19) 0.6979(11) 0.1183(13) 0.0566(19) Uiso 0.506(12) 1 d D . P B
1
H48A H 0.3864 0.7716 0.1593 0.085 Uiso 0.506(12) 1 calc R U P B 1
H48B H 0.3935 0.6268 0.1402 0.085 Uiso 0.506(12) 1 calc R U P B 1
H48C H 0.3833 0.7139 0.0425 0.085 Uiso 0.506(12) 1 calc R U P B 1
C49A C 0.3213(2) 0.7721(8) 0.0903(11) 0.060(2) Uiso 0.506(12) 1 d D . P B 1
H49A H 0.2981 0.7519 0.1040 0.090 Uiso 0.506(12) 1 calc R U P B 1
H49B H 0.3267 0.8523 0.1230 0.090 Uiso 0.506(12) 1 calc R U P B 1
H49C H 0.3250 0.7769 0.0135 0.090 Uiso 0.506(12) 1 calc R U P B 1
C48B C 0.3771(2) 0.7281(12) 0.1166(13) 0.0566(19) Uiso 0.494(12) 1 d D . P B 2
H48D H 0.3937 0.6629 0.1074 0.085 Uiso 0.494(12) 1 calc R U P B 2
H48E H 0.3757 0.7782 0.0518 0.085 Uiso 0.494(12) 1 calc R U P B 2
H48F H 0.3833 0.7815 0.1765 0.085 Uiso 0.494(12) 1 calc R U P B 2
C49B C 0.3179(2) 0.7686(8) 0.1528(12) 0.060(2) Uiso 0.494(12) 1 d D . P B 2
H49D H 0.2964 0.7297 0.1669 0.090 Uiso 0.494(12) 1 calc R U P B 2
H49E H 0.3240 0.8220 0.2127 0.090 Uiso 0.494(12) 1 calc R U P B 2
H49F H 0.3165 0.8188 0.0880 0.090 Uiso 0.494(12) 1 calc R U P B 2
C50 C 0.33012(10) 0.1999(4) 0.1078(4) 0.0524(13) Uani 1 1 d D U . . .
H50A H 0.3376 0.2110 0.1829 0.063 Uiso 0.48(2) 1 calc R U P C 1
H50B H 0.3283 0.2124 0.1863 0.063 Uiso 0.52(2) 1 calc R U P C 2
C51A C 0.3578(3) 0.1281(10) 0.0498(14) 0.057(2) Uiso 0.48(2) 1 d D . P C 1
H51A H 0.3593 0.0436 0.0786 0.086 Uiso 0.48(2) 1 calc R U P C 1
H51B H 0.3528 0.1240 -0.0262 0.086 Uiso 0.48(2) 1 calc R U P C 1
H51C H 0.3789 0.1711 0.0602 0.086 Uiso 0.48(2) 1 calc R U P C 1
C52A C 0.2990(2) 0.1219(10) 0.1115(14) 0.057(2) Uiso 0.48(2) 1 d D . P C 1
H52A H 0.3038 0.0425 0.1467 0.086 Uiso 0.48(2) 1 calc R U P C 1
H52B H 0.2819 0.1664 0.1511 0.086 Uiso 0.48(2) 1 calc R U P C 1
H52C H 0.2913 0.1061 0.0390 0.086 Uiso 0.48(2) 1 calc R U P C 1
C51B C 0.3611(2) 0.1224(9) 0.0885(13) 0.057(2) Uiso 0.52(2) 1 d D . P C 2
H51D H 0.3588 0.0418 0.1240 0.086 Uiso 0.52(2) 1 calc R U P C 2
H51E H 0.3639 0.1094 0.0120 0.086 Uiso 0.52(2) 1 calc R U P C 2
H51F H 0.3804 0.1662 0.1169 0.086 Uiso 0.52(2) 1 calc R U P C 2
C52B C 0.2974(2) 0.1405(10) 0.0710(13) 0.057(2) Uiso 0.52(2) 1 d D . P C 2
H52D H 0.2955 0.0564 0.1005 0.086 Uiso 0.52(2) 1 calc R U P C 2
H52E H 0.2788 0.1912 0.0958 0.086 Uiso 0.52(2) 1 calc R U P C 2
H52F H 0.2970 0.1361 -0.0067 0.086 Uiso 0.52(2) 1 calc R U P C 2
C53 C 0.31703(10) 0.6109(3) 0.5303(3) 0.0344(9) Uani 1 1 d D U . . .
H53A H 0.3356 0.5930 0.4801 0.041 Uiso 0.474(12) 1 calc R U P D 1
H53B H 0.3274 0.6019 0.4587 0.041 Uiso 0.526(12) 1 calc R U P D 2
C54A C 0.3321(3) 0.6743(9) 0.6270(7) 0.0446(17) Uiso 0.474(12) 1 d D . P D 1
H54A H 0.3473 0.6167 0.6626 0.067 Uiso 0.474(12) 1 calc R U P D 1
H54B H 0.3443 0.7486 0.6044 0.067 Uiso 0.474(12) 1 calc R U P D 1
H54C H 0.3145 0.6985 0.6763 0.067 Uiso 0.474(12) 1 calc R U P D 1
C55A C 0.2933(2) 0.6972(9) 0.4728(11) 0.0498(18) Uiso 0.474(12) 1 d D . P D 1
H55A H 0.3045 0.7758 0.4566 0.075 Uiso 0.474(12) 1 calc R U P D 1
H55B H 0.2860 0.6580 0.4066 0.075 Uiso 0.474(12) 1 calc R U P D 1
H55C H 0.2741 0.7136 0.5181 0.075 Uiso 0.474(12) 1 calc R U P D 1
C54B C 0.3443(2) 0.6444(9) 0.6082(8) 0.0446(17) Uiso 0.526(12) 1 d D . P D 2
H54D H 0.3540 0.7247 0.5883 0.067 Uiso 0.526(12) 1 calc R U P D 2
H54E H 0.3351 0.6500 0.6800 0.067 Uiso 0.526(12) 1 calc R U P D 2
H54F H 0.3615 0.5801 0.6065 0.067 Uiso 0.526(12) 1 calc R U P D 2
C55B C 0.2914(2) 0.7157(7) 0.5226(11) 0.0498(18) Uiso 0.526(12) 1 d D . P D 2
H55D H 0.2741 0.6920 0.4720 0.075 Uiso 0.526(12) 1 calc R U P D 2
H55E H 0.2815 0.7298 0.5926 0.075 Uiso 0.526(12) 1 calc R U P D 2
H55F H 0.3022 0.7921 0.4982 0.075 Uiso 0.526(12) 1 calc R U P D 2
C56 C 0.29123(9) 0.1594(3) 0.4360(3) 0.0290(9) Uani 1 1 d D U . . .
H56 H 0.2951 0.1941 0.3633 0.035 Uiso 1 1 calc R U . . .
C57 C 0.32074(11) 0.0779(4) 0.4640(4) 0.0539(14) Uani 1 1 d D U . . .
H57A H 0.3221 0.0082 0.4140 0.081 Uiso 1 1 calc R U . . .
H57B H 0.3411 0.1273 0.4598 0.081 Uiso 1 1 calc R U . . .
H57C H 0.3181 0.0457 0.5363 0.081 Uiso 1 1 calc R U . . .
C58 C 0.25997(11) 0.0794(4) 0.4316(4) 0.0495(12) Uani 1 1 d D U . . .
H58A H 0.2632 0.0112 0.3810 0.074 Uiso 1 1 calc R U . . .
H58B H 0.2554 0.0451 0.5022 0.074 Uiso 1 1 calc R U . . .
H58C H 0.2412 0.1307 0.4087 0.074 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1 C3 1.757(4) . ?
P1 C1 1.868(4) . ?
C1 C2 1.518(5) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 N1 1.377(5) . ?
C3 N2 1.391(5) . ?
N1 C4 1.395(5) . ?
N1 C6 1.450(4) . ?
N2 C5 1.377(5) . ?
N2 C12 1.445(5) . ?
C4 C5 1.335(5) . ?
C4 H4 0.9500 . ?
C5 H5 0.9500 . ?
C6 C11 1.391(5) . ?
C6 C7 1.394(5) . ?
C7 C8 1.396(5) . ?
C7 C18 1.520(5) . ?
C8 C9 1.374(6) . ?
C8 H8 0.9500 . ?
C9 C10 1.378(6) . ?
C9 H9 0.9500 . ?
C10 C11 1.394(5) . ?
C10 H10 0.9500 . ?
C11 C21 1.521(4) . ?
C12 C13 1.388(5) . ?
C12 C17 1.399(5) . ?
C13 C14 1.393(5) . ?
C13 C24 1.523(4) . ?
C14 C15 1.376(6) . ?
C14 H14 0.9500 . ?
C15 C16 1.374(6) . ?
C15 H15 0.9500 . ?
C16 C17 1.385(6) . ?
C16 H16 0.9500 . ?
C17 C27 1.525(5) . ?
C18 C19B 1.498(8) . ?
C18 C20A 1.519(6) . ?
C18 C20B 1.535(8) . ?
C18 C19A 1.547(6) . ?
C18 H18A 1.0000 . ?
C18 H18B 1.0000 . ?
C19A H19A 0.9800 . ?
C19A H19B 0.9800 . ?
C19A H19C 0.9800 . ?
C20A H20A 0.9800 . ?
C20A H20B 0.9800 . ?
C20A H20C 0.9800 . ?
C19B H19D 0.9800 . ?
C19B H19E 0.9800 . ?
C19B H19F 0.9800 . ?
C20B H20D 0.9800 . ?
C20B H20E 0.9800 . ?
C20B H20F 0.9800 . ?
C21 C23 1.506(5) . ?
C21 C22 1.527(5) . ?
C21 H21 1.0000 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 C26 1.523(5) . ?
C24 C25 1.531(5) . ?
C24 H24 1.0000 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 C28 1.514(5) . ?
C27 C29 1.526(5) . ?
C27 H27 1.0000 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
P2 C32 1.770(4) . ?
P2 C30 1.863(4) . ?
C30 C31 1.522(6) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 N4 1.370(5) . ?
C32 N3 1.380(5) . ?
N3 C33 1.377(5) . ?
N3 C35 1.435(5) . ?
N4 C34 1.398(5) . ?
N4 C41 1.433(5) . ?
C33 C34 1.342(6) . ?
C33 H33 0.9500 . ?
C34 H34 0.9500 . ?
C35 C40 1.387(6) . ?
C35 C36 1.391(5) . ?
C36 C37 1.385(7) . ?
C36 C47 1.521(6) . ?
C37 C38 1.359(8) . ?
C37 H37 0.9500 . ?
C38 C39 1.369(9) . ?
C38 H38 0.9500 . ?
C39 C40 1.404(7) . ?
C39 H39 0.9500 . ?
C40 C50 1.512(5) . ?
C41 C42 1.401(5) . ?
C41 C46 1.402(5) . ?
C42 C43 1.391(5) . ?
C42 C53 1.521(5) . ?
C43 C44 1.387(5) . ?
C43 H43 0.9500 . ?
C44 C45 1.381(5) . ?
C44 H44 0.9500 . ?
C45 C46 1.392(5) . ?
C45 H45 0.9500 . ?
C46 C56 1.520(4) . ?
C47 C49B 1.508(7) . ?
C47 C48B 1.515(7) . ?
C47 C48A 1.519(7) . ?
C47 C49A 1.557(7) . ?
C47 H47A 1.0000 . ?
C47 H47B 1.0000 . ?
C48A H48A 0.9800 . ?
C48A H48B 0.9800 . ?
C48A H48C 0.9800 . ?
C49A H49A 0.9800 . ?
C49A H49B 0.9800 . ?
C49A H49C 0.9800 . ?
C48B H48D 0.9800 . ?
C48B H48E 0.9800 . ?
C48B H48F 0.9800 . ?
C49B H49D 0.9800 . ?
C49B H49E 0.9800 . ?
C49B H49F 0.9800 . ?
C50 C52A 1.512(7) . ?
C50 C51B 1.523(7) . ?
C50 C52B 1.542(7) . ?
C50 C51A 1.545(7) . ?
C50 H50A 1.0000 . ?
C50 H50B 1.0000 . ?
C51A H51A 0.9800 . ?
C51A H51B 0.9800 . ?
C51A H51C 0.9800 . ?
C52A H52A 0.9800 . ?
C52A H52B 0.9800 . ?
C52A H52C 0.9800 . ?
C51B H51D 0.9800 . ?
C51B H51E 0.9800 . ?
C51B H51F 0.9800 . ?
C52B H52D 0.9800 . ?
C52B H52E 0.9800 . ?
C52B H52F 0.9800 . ?
C53 C55A 1.518(7) . ?
C53 C54B 1.520(7) . ?
C53 C54A 1.524(7) . ?
C53 C55B 1.535(7) . ?
C53 H53A 1.0000 . ?
C53 H53B 1.0000 . ?
C54A H54A 0.9800 . ?
C54A H54B 0.9800 . ?
C54A H54C 0.9800 . ?
C55A H55A 0.9800 . ?
C55A H55B 0.9800 . ?
C55A H55C 0.9800 . ?
C54B H54D 0.9800 . ?
C54B H54E 0.9800 . ?
C54B H54F 0.9800 . ?
C55B H55D 0.9800 . ?
C55B H55E 0.9800 . ?
C55B H55F 0.9800 . ?
C56 C57 1.522(5) . ?
C56 C58 1.530(5) . ?
C56 H56 1.0000 . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 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
C3 P1 C1 106.26(18) . . ?
C2 C1 P1 106.6(3) . . ?
C2 C1 H1A 110.4 . . ?
P1 C1 H1A 110.4 . . ?
C2 C1 H1B 110.4 . . ?
P1 C1 H1B 110.4 . . ?
H1A C1 H1B 108.6 . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N1 C3 N2 103.5(3) . . ?
N1 C3 P1 136.9(3) . . ?
N2 C3 P1 119.6(3) . . ?
C3 N1 C4 110.7(3) . . ?
C3 N1 C6 126.2(3) . . ?
C4 N1 C6 122.5(3) . . ?
C5 N2 C3 110.6(3) . . ?
C5 N2 C12 126.1(3) . . ?
C3 N2 C12 123.2(3) . . ?
C5 C4 N1 107.1(3) . . ?
C5 C4 H4 126.4 . . ?
N1 C4 H4 126.4 . . ?
C4 C5 N2 108.1(3) . . ?
C4 C5 H5 126.0 . . ?
N2 C5 H5 126.0 . . ?
C11 C6 C7 123.6(3) . . ?
C11 C6 N1 118.5(3) . . ?
C7 C6 N1 117.8(3) . . ?
C6 C7 C8 116.9(3) . . ?
C6 C7 C18 122.5(3) . . ?
C8 C7 C18 120.5(3) . . ?
C9 C8 C7 121.1(4) . . ?
C9 C8 H8 119.5 . . ?
C7 C8 H8 119.5 . . ?
C8 C9 C10 120.3(4) . . ?
C8 C9 H9 119.8 . . ?
C10 C9 H9 119.8 . . ?
C9 C10 C11 121.4(4) . . ?
C9 C10 H10 119.3 . . ?
C11 C10 H10 119.3 . . ?
C6 C11 C10 116.6(3) . . ?
C6 C11 C21 121.5(3) . . ?
C10 C11 C21 121.9(3) . . ?
C13 C12 C17 123.3(3) . . ?
C13 C12 N2 118.6(3) . . ?
C17 C12 N2 118.0(3) . . ?
C12 C13 C14 117.0(3) . . ?
C12 C13 C24 122.2(3) . . ?
C14 C13 C24 120.9(3) . . ?
C15 C14 C13 121.0(4) . . ?
C15 C14 H14 119.5 . . ?
C13 C14 H14 119.5 . . ?
C14 C15 C16 120.5(4) . . ?
C14 C15 H15 119.8 . . ?
C16 C15 H15 119.8 . . ?
C15 C16 C17 121.2(4) . . ?
C15 C16 H16 119.4 . . ?
C17 C16 H16 119.4 . . ?
C16 C17 C12 116.9(3) . . ?
C16 C17 C27 121.6(3) . . ?
C12 C17 C27 121.4(3) . . ?
C19B C18 C7 114.0(6) . . ?
C20A C18 C7 114.6(5) . . ?
C19B C18 C20B 115.5(8) . . ?
C7 C18 C20B 108.9(7) . . ?
C20A C18 C19A 109.5(5) . . ?
C7 C18 C19A 109.5(4) . . ?
C20A C18 H18A 107.7 . . ?
C7 C18 H18A 107.7 . . ?
C19A C18 H18A 107.7 . . ?
C19B C18 H18B 105.9 . . ?
C7 C18 H18B 105.9 . . ?
C20B C18 H18B 105.9 . . ?
C18 C19A H19A 109.5 . . ?
C18 C19A H19B 109.5 . . ?
H19A C19A H19B 109.5 . . ?
C18 C19A H19C 109.5 . . ?
H19A C19A H19C 109.5 . . ?
H19B C19A H19C 109.5 . . ?
C18 C20A H20A 109.5 . . ?
C18 C20A H20B 109.5 . . ?
H20A C20A H20B 109.5 . . ?
C18 C20A H20C 109.5 . . ?
H20A C20A H20C 109.5 . . ?
H20B C20A H20C 109.5 . . ?
C18 C19B H19D 109.5 . . ?
C18 C19B H19E 109.5 . . ?
H19D C19B H19E 109.5 . . ?
C18 C19B H19F 109.5 . . ?
H19D C19B H19F 109.5 . . ?
H19E C19B H19F 109.5 . . ?
C18 C20B H20D 109.5 . . ?
C18 C20B H20E 109.5 . . ?
H20D C20B H20E 109.5 . . ?
C18 C20B H20F 109.5 . . ?
H20D C20B H20F 109.5 . . ?
H20E C20B H20F 109.5 . . ?
C23 C21 C11 112.5(3) . . ?
C23 C21 C22 111.0(3) . . ?
C11 C21 C22 112.9(3) . . ?
C23 C21 H21 106.7 . . ?
C11 C21 H21 106.7 . . ?
C22 C21 H21 106.7 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C13 C24 C26 111.0(3) . . ?
C13 C24 C25 110.9(3) . . ?
C26 C24 C25 110.2(3) . . ?
C13 C24 H24 108.2 . . ?
C26 C24 H24 108.2 . . ?
C25 C24 H24 108.2 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C28 C27 C29 110.4(4) . . ?
C28 C27 C17 110.7(3) . . ?
C29 C27 C17 112.8(4) . . ?
C28 C27 H27 107.6 . . ?
C29 C27 H27 107.6 . . ?
C17 C27 H27 107.6 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C32 P2 C30 106.20(18) . . ?
C31 C30 P2 106.9(3) . . ?
C31 C30 H30A 110.3 . . ?
P2 C30 H30A 110.3 . . ?
C31 C30 H30B 110.3 . . ?
P2 C30 H30B 110.3 . . ?
H30A C30 H30B 108.6 . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
N4 C32 N3 104.5(3) . . ?
N4 C32 P2 135.4(3) . . ?
N3 C32 P2 120.1(3) . . ?
C33 N3 C32 110.5(3) . . ?
C33 N3 C35 126.9(3) . . ?
C32 N3 C35 122.2(3) . . ?
C32 N4 C34 110.1(3) . . ?
C32 N4 C41 127.4(3) . . ?
C34 N4 C41 122.6(3) . . ?
C34 C33 N3 107.7(3) . . ?
C34 C33 H33 126.2 . . ?
N3 C33 H33 126.2 . . ?
C33 C34 N4 107.3(3) . . ?
C33 C34 H34 126.4 . . ?
N4 C34 H34 126.4 . . ?
C40 C35 C36 124.1(4) . . ?
C40 C35 N3 117.8(4) . . ?
C36 C35 N3 118.0(4) . . ?
C37 C36 C35 116.9(5) . . ?
C37 C36 C47 120.8(5) . . ?
C35 C36 C47 122.3(4) . . ?
C38 C37 C36 120.7(5) . . ?
C38 C37 H37 119.7 . . ?
C36 C37 H37 119.7 . . ?
C37 C38 C39 121.6(5) . . ?
C37 C38 H38 119.2 . . ?
C39 C38 H38 119.2 . . ?
C38 C39 C40 120.6(5) . . ?
C38 C39 H39 119.7 . . ?
C40 C39 H39 119.7 . . ?
C35 C40 C39 115.9(5) . . ?
C35 C40 C50 122.5(4) . . ?
C39 C40 C50 121.6(5) . . ?
C42 C41 C46 123.5(3) . . ?
C42 C41 N4 118.1(3) . . ?
C46 C41 N4 118.4(3) . . ?
C43 C42 C41 116.8(3) . . ?
C43 C42 C53 121.2(3) . . ?
C41 C42 C53 122.0(3) . . ?
C44 C43 C42 121.2(4) . . ?
C44 C43 H43 119.4 . . ?
C42 C43 H43 119.4 . . ?
C45 C44 C43 120.5(4) . . ?
C45 C44 H44 119.8 . . ?
C43 C44 H44 119.8 . . ?
C44 C45 C46 121.1(4) . . ?
C44 C45 H45 119.5 . . ?
C46 C45 H45 119.5 . . ?
C45 C46 C41 117.0(3) . . ?
C45 C46 C56 121.4(3) . . ?
C41 C46 C56 121.6(3) . . ?
C49B C47 C48B 109.8(6) . . ?
C49B C47 C36 120.2(6) . . ?
C48B C47 C36 114.8(6) . . ?
C48A C47 C36 105.6(6) . . ?
C48A C47 C49A 110.5(7) . . ?
C36 C47 C49A 104.2(5) . . ?
C48A C47 H47A 112.0 . . ?
C36 C47 H47A 112.0 . . ?
C49A C47 H47A 112.0 . . ?
C49B C47 H47B 103.2 . . ?
C48B C47 H47B 103.2 . . ?
C36 C47 H47B 103.2 . . ?
C47 C48A H48A 109.5 . . ?
C47 C48A H48B 109.5 . . ?
H48A C48A H48B 109.5 . . ?
C47 C48A H48C 109.5 . . ?
H48A C48A H48C 109.5 . . ?
H48B C48A H48C 109.5 . . ?
C47 C49A H49A 109.5 . . ?
C47 C49A H49B 109.5 . . ?
H49A C49A H49B 109.5 . . ?
C47 C49A H49C 109.5 . . ?
H49A C49A H49C 109.5 . . ?
H49B C49A H49C 109.5 . . ?
C47 C48B H48D 109.5 . . ?
C47 C48B H48E 109.5 . . ?
H48D C48B H48E 109.5 . . ?
C47 C48B H48F 109.5 . . ?
H48D C48B H48F 109.5 . . ?
H48E C48B H48F 109.5 . . ?
C47 C49B H49D 109.5 . . ?
C47 C49B H49E 109.5 . . ?
H49D C49B H49E 109.5 . . ?
C47 C49B H49F 109.5 . . ?
H49D C49B H49F 109.5 . . ?
H49E C49B H49F 109.5 . . ?
C40 C50 C52A 120.9(7) . . ?
C40 C50 C51B 115.7(6) . . ?
C40 C50 C52B 104.3(6) . . ?
C51B C50 C52B 115.6(6) . . ?
C40 C50 C51A 105.0(6) . . ?
C52A C50 C51A 109.9(6) . . ?
C40 C50 H50A 106.8 . . ?
C52A C50 H50A 106.8 . . ?
C51A C50 H50A 106.8 . . ?
C40 C50 H50B 106.9 . . ?
C51B C50 H50B 106.9 . . ?
C52B C50 H50B 106.9 . . ?
C50 C51A H51A 109.5 . . ?
C50 C51A H51B 109.5 . . ?
H51A C51A H51B 109.5 . . ?
C50 C51A H51C 109.5 . . ?
H51A C51A H51C 109.5 . . ?
H51B C51A H51C 109.5 . . ?
C50 C52A H52A 109.5 . . ?
C50 C52A H52B 109.5 . . ?
H52A C52A H52B 109.5 . . ?
C50 C52A H52C 109.5 . . ?
H52A C52A H52C 109.5 . . ?
H52B C52A H52C 109.5 . . ?
C50 C51B H51D 109.5 . . ?
C50 C51B H51E 109.5 . . ?
H51D C51B H51E 109.5 . . ?
C50 C51B H51F 109.5 . . ?
H51D C51B H51F 109.5 . . ?
H51E C51B H51F 109.5 . . ?
C50 C52B H52D 109.5 . . ?
C50 C52B H52E 109.5 . . ?
H52D C52B H52E 109.5 . . ?
C50 C52B H52F 109.5 . . ?
H52D C52B H52F 109.5 . . ?
H52E C52B H52F 109.5 . . ?
C55A C53 C42 112.4(5) . . ?
C54B C53 C42 111.4(4) . . ?
C55A C53 C54A 111.2(6) . . ?
C42 C53 C54A 112.2(5) . . ?
C54B C53 C55B 111.0(5) . . ?
C42 C53 C55B 112.0(4) . . ?
C55A C53 H53A 106.9 . . ?
C42 C53 H53A 106.9 . . ?
C54A C53 H53A 106.9 . . ?
C54B C53 H53B 107.4 . . ?
C42 C53 H53B 107.4 . . ?
C55B C53 H53B 107.4 . . ?
C53 C54A H54A 109.5 . . ?
C53 C54A H54B 109.5 . . ?
H54A C54A H54B 109.5 . . ?
C53 C54A H54C 109.5 . . ?
H54A C54A H54C 109.5 . . ?
H54B C54A H54C 109.5 . . ?
C53 C55A H55A 109.5 . . ?
C53 C55A H55B 109.5 . . ?
H55A C55A H55B 109.5 . . ?
C53 C55A H55C 109.5 . . ?
H55A C55A H55C 109.5 . . ?
H55B C55A H55C 109.5 . . ?
C53 C54B H54D 109.5 . . ?
C53 C54B H54E 109.5 . . ?
H54D C54B H54E 109.5 . . ?
C53 C54B H54F 109.5 . . ?
H54D C54B H54F 109.5 . . ?
H54E C54B H54F 109.5 . . ?
C53 C55B H55D 109.5 . . ?
C53 C55B H55E 109.5 . . ?
H55D C55B H55E 109.5 . . ?
C53 C55B H55F 109.5 . . ?
H55D C55B H55F 109.5 . . ?
H55E C55B H55F 109.5 . . ?
C46 C56 C57 110.4(3) . . ?
C46 C56 C58 113.6(3) . . ?
C57 C56 C58 109.4(3) . . ?
C46 C56 H56 107.7 . . ?
C57 C56 H56 107.7 . . ?
C58 C56 H56 107.7 . . ?
C56 C57 H57A 109.5 . . ?
C56 C57 H57B 109.5 . . ?
H57A C57 H57B 109.5 . . ?
C56 C57 H57C 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
C56 C58 H58A 109.5 . . ?
C56 C58 H58B 109.5 . . ?
H58A C58 H58B 109.5 . . ?
C56 C58 H58C 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C3 P1 C1 C2 -174.1(3) . . . . ?
C1 P1 C3 N1 1.4(4) . . . . ?
C1 P1 C3 N2 -178.7(3) . . . . ?
N2 C3 N1 C4 1.3(4) . . . . ?
P1 C3 N1 C4 -178.8(3) . . . . ?
N2 C3 N1 C6 -170.3(3) . . . . ?
P1 C3 N1 C6 9.7(6) . . . . ?
N1 C3 N2 C5 -1.0(4) . . . . ?
P1 C3 N2 C5 179.1(3) . . . . ?
N1 C3 N2 C12 175.1(3) . . . . ?
P1 C3 N2 C12 -4.8(4) . . . . ?
C3 N1 C4 C5 -1.2(4) . . . . ?
C6 N1 C4 C5 170.8(3) . . . . ?
N1 C4 C5 N2 0.5(4) . . . . ?
C3 N2 C5 C4 0.3(4) . . . . ?
C12 N2 C5 C4 -175.7(3) . . . . ?
C3 N1 C6 C11 -107.5(4) . . . . ?
C4 N1 C6 C11 81.9(4) . . . . ?
C3 N1 C6 C7 74.8(5) . . . . ?
C4 N1 C6 C7 -95.8(4) . . . . ?
C11 C6 C7 C8 1.6(6) . . . . ?
N1 C6 C7 C8 179.2(3) . . . . ?
C11 C6 C7 C18 -175.9(4) . . . . ?
N1 C6 C7 C18 1.7(5) . . . . ?
C6 C7 C8 C9 0.3(6) . . . . ?
C18 C7 C8 C9 177.9(4) . . . . ?
C7 C8 C9 C10 -1.3(7) . . . . ?
C8 C9 C10 C11 0.4(7) . . . . ?
C7 C6 C11 C10 -2.5(6) . . . . ?
N1 C6 C11 C10 -180.0(3) . . . . ?
C7 C6 C11 C21 177.2(4) . . . . ?
N1 C6 C11 C21 -0.3(5) . . . . ?
C9 C10 C11 C6 1.4(6) . . . . ?
C9 C10 C11 C21 -178.3(4) . . . . ?
C5 N2 C12 C13 -87.4(4) . . . . ?
C3 N2 C12 C13 97.1(4) . . . . ?
C5 N2 C12 C17 93.8(4) . . . . ?
C3 N2 C12 C17 -81.7(4) . . . . ?
C17 C12 C13 C14 0.6(6) . . . . ?
N2 C12 C13 C14 -178.1(3) . . . . ?
C17 C12 C13 C24 -178.4(3) . . . . ?
N2 C12 C13 C24 2.9(5) . . . . ?
C12 C13 C14 C15 0.8(6) . . . . ?
C24 C13 C14 C15 179.8(3) . . . . ?
C13 C14 C15 C16 -1.4(6) . . . . ?
C14 C15 C16 C17 0.6(6) . . . . ?
C15 C16 C17 C12 0.7(6) . . . . ?
C15 C16 C17 C27 -176.8(4) . . . . ?
C13 C12 C17 C16 -1.3(6) . . . . ?
N2 C12 C17 C16 177.4(3) . . . . ?
C13 C12 C17 C27 176.2(3) . . . . ?
N2 C12 C17 C27 -5.1(5) . . . . ?
C6 C7 C18 C19B 85.4(11) . . . . ?
C8 C7 C18 C19B -92.0(11) . . . . ?
C6 C7 C18 C20A -122.3(6) . . . . ?
C8 C7 C18 C20A 60.2(7) . . . . ?
C6 C7 C18 C20B -144.0(10) . . . . ?
C8 C7 C18 C20B 38.6(10) . . . . ?
C6 C7 C18 C19A 114.2(6) . . . . ?
C8 C7 C18 C19A -63.2(7) . . . . ?
C6 C11 C21 C23 82.4(5) . . . . ?
C10 C11 C21 C23 -97.9(5) . . . . ?
C6 C11 C21 C22 -151.0(4) . . . . ?
C10 C11 C21 C22 28.7(5) . . . . ?
C12 C13 C24 C26 120.2(4) . . . . ?
C14 C13 C24 C26 -58.8(5) . . . . ?
C12 C13 C24 C25 -117.1(4) . . . . ?
C14 C13 C24 C25 64.0(5) . . . . ?
C16 C17 C27 C28 89.2(5) . . . . ?
C12 C17 C27 C28 -88.2(5) . . . . ?
C16 C17 C27 C29 -35.0(6) . . . . ?
C12 C17 C27 C29 147.6(4) . . . . ?
C32 P2 C30 C31 175.3(3) . . . . ?
C30 P2 C32 N4 0.5(4) . . . . ?
C30 P2 C32 N3 179.5(3) . . . . ?
N4 C32 N3 C33 0.5(4) . . . . ?
P2 C32 N3 C33 -178.8(2) . . . . ?
N4 C32 N3 C35 173.4(3) . . . . ?
P2 C32 N3 C35 -5.9(5) . . . . ?
N3 C32 N4 C34 -0.2(4) . . . . ?
P2 C32 N4 C34 178.9(3) . . . . ?
N3 C32 N4 C41 -179.9(3) . . . . ?
P2 C32 N4 C41 -0.7(6) . . . . ?
C32 N3 C33 C34 -0.6(4) . . . . ?
C35 N3 C33 C34 -173.1(4) . . . . ?
N3 C33 C34 N4 0.4(4) . . . . ?
C32 N4 C34 C33 -0.1(4) . . . . ?
C41 N4 C34 C33 179.5(3) . . . . ?
C33 N3 C35 C40 85.8(5) . . . . ?
C32 N3 C35 C40 -85.9(5) . . . . ?
C33 N3 C35 C36 -94.8(5) . . . . ?
C32 N3 C35 C36 93.5(4) . . . . ?
C40 C35 C36 C37 2.4(6) . . . . ?
N3 C35 C36 C37 -176.9(4) . . . . ?
C40 C35 C36 C47 -175.1(4) . . . . ?
N3 C35 C36 C47 5.6(6) . . . . ?
C35 C36 C37 C38 0.4(7) . . . . ?
C47 C36 C37 C38 178.0(4) . . . . ?
C36 C37 C38 C39 -2.5(8) . . . . ?
C37 C38 C39 C40 1.8(8) . . . . ?
C36 C35 C40 C39 -3.1(6) . . . . ?
N3 C35 C40 C39 176.3(4) . . . . ?
C36 C35 C40 C50 176.3(4) . . . . ?
N3 C35 C40 C50 -4.4(6) . . . . ?
C38 C39 C40 C35 0.9(7) . . . . ?
C38 C39 C40 C50 -178.4(4) . . . . ?
C32 N4 C41 C42 -97.3(4) . . . . ?
C34 N4 C41 C42 83.1(4) . . . . ?
C32 N4 C41 C46 83.3(5) . . . . ?
C34 N4 C41 C46 -96.3(4) . . . . ?
C46 C41 C42 C43 -0.9(6) . . . . ?
N4 C41 C42 C43 179.8(3) . . . . ?
C46 C41 C42 C53 -179.1(3) . . . . ?
N4 C41 C42 C53 1.6(5) . . . . ?
C41 C42 C43 C44 1.9(6) . . . . ?
C53 C42 C43 C44 -179.9(3) . . . . ?
C42 C43 C44 C45 -1.6(6) . . . . ?
C43 C44 C45 C46 0.2(6) . . . . ?
C44 C45 C46 C41 0.8(5) . . . . ?
C44 C45 C46 C56 -178.9(3) . . . . ?
C42 C41 C46 C45 -0.5(5) . . . . ?
N4 C41 C46 C45 178.9(3) . . . . ?
C42 C41 C46 C56 179.3(3) . . . . ?
N4 C41 C46 C56 -1.4(5) . . . . ?
C37 C36 C47 C49B 68.5(8) . . . . ?
C35 C36 C47 C49B -114.0(8) . . . . ?
C37 C36 C47 C48B -65.9(8) . . . . ?
C35 C36 C47 C48B 111.5(8) . . . . ?
C37 C36 C47 C48A -75.9(8) . . . . ?
C35 C36 C47 C48A 101.5(7) . . . . ?
C37 C36 C47 C49A 40.6(7) . . . . ?
C35 C36 C47 C49A -142.0(6) . . . . ?
C35 C40 C50 C52A 112.7(8) . . . . ?
C39 C40 C50 C52A -68.0(9) . . . . ?
C35 C40 C50 C51B -105.6(8) . . . . ?
C39 C40 C50 C51B 73.7(8) . . . . ?
C35 C40 C50 C52B 126.3(7) . . . . ?
C39 C40 C50 C52B -54.3(8) . . . . ?
C35 C40 C50 C51A -122.5(8) . . . . ?
C39 C40 C50 C51A 56.9(9) . . . . ?
C43 C42 C53 C55A -86.1(7) . . . . ?
C41 C42 C53 C55A 92.1(7) . . . . ?
C43 C42 C53 C54B 66.0(7) . . . . ?
C41 C42 C53 C54B -115.9(6) . . . . ?
C43 C42 C53 C54A 40.1(7) . . . . ?
C41 C42 C53 C54A -141.8(7) . . . . ?
C43 C42 C53 C55B -59.0(7) . . . . ?
C41 C42 C53 C55B 119.2(6) . . . . ?
C45 C46 C56 C57 -87.3(4) . . . . ?
C41 C46 C56 C57 93.0(4) . . . . ?
C45 C46 C56 C58 36.1(5) . . . . ?
C41 C46 C56 C58 -143.7(4) . . . . ?

_refine_diff_density_max         0.276
_refine_diff_density_min         -0.230
_refine_diff_density_rms         0.039


# start Validation Reply Form
_vrf_PLAT201_g535_mn             
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......          8 Report
RESPONSE: 4 iPr moieties disordered, disordered atoms refined isotropically.
;
# end Validation Reply Form
####################################################################### 
# 
# 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_g539_mn
_database_code_depnum_ccdc_archive 'CCDC 1992149'
loop_
_audit_author_name
_audit_author_address
'Christoph Feil'
;Universitity of Stuttgart
Germany
;
_audit_update_record             
;
2020-03-23 deposited with the CCDC.	2020-11-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H39 N2 P'
_chemical_formula_sum            'C28 H39 N2 P'
_chemical_formula_weight         434.58

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'

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

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   10.3552(6)
_cell_length_b                   7.0047(4)
_cell_length_c                   37.0995(19)
_cell_angle_alpha                90
_cell_angle_beta                 97.948(3)
_cell_angle_gamma                90
_cell_volume                     2665.2(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    135(2)
_cell_measurement_reflns_used    2988
_cell_measurement_theta_min      1.986
_cell_measurement_theta_max      25.376

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.083
_exptl_crystal_F_000             944
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.118
_exptl_crystal_size_mid          0.049
_exptl_crystal_size_min          0.032
_exptl_absorpt_coefficient_mu    0.119
_shelx_estimated_absorpt_T_min   0.986
_shelx_estimated_absorpt_T_max   0.996
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8100
_exptl_absorpt_correction_T_max  0.8620
_exptl_absorpt_process_details   'BLESSING 1995'
_exptl_absorpt_special_details   ?

_diffrn_ambient_temperature      135(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker Kappa ApexII Duo'
_diffrn_measurement_method       'Omega and phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            29169
_diffrn_reflns_av_unetI/netI     0.0751
_diffrn_reflns_av_R_equivalents  0.0940
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_theta_min         1.986
_diffrn_reflns_theta_max         25.376
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_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             4877
_reflns_number_gt                2988
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker ApexII Software Suite, 2008'
_computing_cell_refinement       'Bruker ApexII Software Suite, 2008'
_computing_data_reduction        'Bruker ApexII Software Suite, 2008'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELX plus XP (Sheldrick, 1991)'
_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)+(0.0455P)²+0.7801P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4877
_refine_ls_number_parameters     281
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1087
_refine_ls_R_factor_gt           0.0528
_refine_ls_wR_factor_ref         0.1174
_refine_ls_wR_factor_gt          0.0994
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_restrained_S_all      1.001
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.82530(8) 0.78748(9) 0.09934(2) 0.0294(2) Uani 1 1 d . . . . .
C1 C 0.8331(3) 0.7375(3) 0.05060(6) 0.0341(7) Uani 1 1 d . . . . .
H1A H 0.8379 0.8581 0.0375 0.051 Uiso 1 1 calc R U . . .
H1B H 0.7549 0.6672 0.0402 0.051 Uiso 1 1 calc R U . . .
H1C H 0.9107 0.6606 0.0484 0.051 Uiso 1 1 calc R U . . .
C2 C 0.8160(2) 0.5657(3) 0.12056(6) 0.0195(6) Uani 1 1 d . . . . .
N1 N 0.8046(2) 0.5579(2) 0.15730(5) 0.0211(5) Uani 1 1 d . . . . .
N2 N 0.8169(2) 0.3768(2) 0.11050(5) 0.0199(5) Uani 1 1 d . . . . .
C3 C 0.7984(3) 0.3700(3) 0.16872(6) 0.0250(6) Uani 1 1 d . . . . .
H3 H 0.7899 0.3286 0.1927 0.030 Uiso 1 1 calc R U . . .
C4 C 0.8066(2) 0.2578(3) 0.14014(6) 0.0255(6) Uani 1 1 d . . . . .
H4 H 0.8056 0.1222 0.1400 0.031 Uiso 1 1 calc R U . . .
C5 C 0.7860(2) 0.7192(3) 0.17979(6) 0.0213(6) Uani 1 1 d . . . . .
C6 C 0.6582(3) 0.7766(3) 0.18211(6) 0.0252(6) Uani 1 1 d . . . . .
C7 C 0.6423(3) 0.9193(3) 0.20721(7) 0.0335(7) Uani 1 1 d . . . . .
H7 H 0.5568 0.9607 0.2099 0.040 Uiso 1 1 calc R U . . .
C8 C 0.7472(3) 1.0016(3) 0.22818(7) 0.0349(7) Uani 1 1 d . . . . .
H8 H 0.7336 1.0960 0.2457 0.042 Uiso 1 1 calc R U . . .
C9 C 0.8715(3) 0.9481(3) 0.22398(6) 0.0342(7) Uani 1 1 d . . . . .
H9 H 0.9432 1.0096 0.2380 0.041 Uiso 1 1 calc R U . . .
C10 C 0.8950(3) 0.8049(3) 0.19944(6) 0.0264(6) Uani 1 1 d . . . . .
C11 C 0.8289(2) 0.3096(3) 0.07426(6) 0.0193(5) Uani 1 1 d . . . . .
C12 C 0.9537(2) 0.2884(3) 0.06489(6) 0.0225(6) Uani 1 1 d . . . . .
C13 C 0.9618(3) 0.2433(3) 0.02871(6) 0.0279(6) Uani 1 1 d . . . . .
H13 H 1.0451 0.2293 0.0210 0.033 Uiso 1 1 calc R U . . .
C14 C 0.8517(3) 0.2187(3) 0.00389(6) 0.0273(6) Uani 1 1 d . . . . .
H14 H 0.8596 0.1939 -0.0209 0.033 Uiso 1 1 calc R U . . .
C15 C 0.7298(3) 0.2297(3) 0.01468(6) 0.0278(6) Uani 1 1 d . . . . .
H15 H 0.6547 0.2066 -0.0025 0.033 Uiso 1 1 calc R U . . .
C16 C 0.7154(2) 0.2742(3) 0.05049(6) 0.0238(6) Uani 1 1 d . . . . .
C17 C 0.5421(3) 0.6907(4) 0.15841(6) 0.0331(7) Uani 1 1 d . . . . .
H17 H 0.5763 0.6069 0.1400 0.040 Uiso 1 1 calc R U . . .
C18 C 0.4607(3) 0.5653(5) 0.18055(8) 0.0522(9) Uani 1 1 d . . . . .
H18A H 0.3866 0.5121 0.1644 0.078 Uiso 1 1 calc R U . . .
H18B H 0.5149 0.4611 0.1919 0.078 Uiso 1 1 calc R U . . .
H18C H 0.4287 0.6426 0.1995 0.078 Uiso 1 1 calc R U . . .
C19 C 0.4586(3) 0.8447(4) 0.13772(8) 0.0532(9) Uani 1 1 d . . . . .
H19A H 0.3842 0.7852 0.1226 0.080 Uiso 1 1 calc R U . . .
H19B H 0.4267 0.9325 0.1551 0.080 Uiso 1 1 calc R U . . .
H19C H 0.5109 0.9155 0.1222 0.080 Uiso 1 1 calc R U . . .
C20 C 1.0322(3) 0.7459(4) 0.19488(7) 0.0380(7) Uani 1 1 d . . . . .
H20 H 1.0274 0.6746 0.1714 0.046 Uiso 1 1 calc R U . . .
C21 C 1.1213(3) 0.9172(5) 0.19247(9) 0.0672(11) Uani 1 1 d . . . . .
H21A H 1.2089 0.8726 0.1895 0.101 Uiso 1 1 calc R U . . .
H21B H 1.0868 0.9961 0.1715 0.101 Uiso 1 1 calc R U . . .
H21C H 1.1254 0.9930 0.2148 0.101 Uiso 1 1 calc R U . . .
C22 C 1.0891(3) 0.6108(5) 0.22513(9) 0.0673(11) Uani 1 1 d . . . . .
H22A H 1.1778 0.5749 0.2215 0.101 Uiso 1 1 calc R U . . .
H22B H 1.0912 0.6746 0.2487 0.101 Uiso 1 1 calc R U . . .
H22C H 1.0347 0.4960 0.2246 0.101 Uiso 1 1 calc R U . . .
C23 C 1.0751(3) 0.3094(4) 0.09233(7) 0.0316(6) Uani 1 1 d . . . . .
H23 H 1.0466 0.3285 0.1168 0.038 Uiso 1 1 calc R U . . .
C24 C 1.1558(3) 0.4823(4) 0.08463(8) 0.0519(9) Uani 1 1 d . . . . .
H24A H 1.2333 0.4904 0.1030 0.078 Uiso 1 1 calc R U . . .
H24B H 1.1827 0.4697 0.0604 0.078 Uiso 1 1 calc R U . . .
H24C H 1.1034 0.5983 0.0855 0.078 Uiso 1 1 calc R U . . .
C25 C 1.1569(3) 0.1275(4) 0.09422(8) 0.0505(9) Uani 1 1 d . . . . .
H25A H 1.2350 0.1440 0.1121 0.076 Uiso 1 1 calc R U . . .
H25B H 1.1054 0.0202 0.1015 0.076 Uiso 1 1 calc R U . . .
H25C H 1.1827 0.1014 0.0703 0.076 Uiso 1 1 calc R U . . .
C26 C 0.5817(3) 0.2833(4) 0.06318(7) 0.0341(7) Uani 1 1 d . . . . .
H26 H 0.5948 0.2601 0.0900 0.041 Uiso 1 1 calc R U . . .
C27 C 0.4909(3) 0.1273(5) 0.04573(8) 0.0518(9) Uani 1 1 d . . . . .
H27A H 0.5330 0.0026 0.0502 0.078 Uiso 1 1 calc R U . . .
H27B H 0.4093 0.1296 0.0563 0.078 Uiso 1 1 calc R U . . .
H27C H 0.4722 0.1497 0.0195 0.078 Uiso 1 1 calc R U . . .
C28 C 0.5199(3) 0.4797(4) 0.05682(8) 0.0510(9) Uani 1 1 d . . . . .
H28A H 0.4343 0.4802 0.0653 0.076 Uiso 1 1 calc R U . . .
H28B H 0.5761 0.5757 0.0703 0.076 Uiso 1 1 calc R U . . .
H28C H 0.5094 0.5096 0.0308 0.076 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1 C2 1.750(2) . ?
P1 C1 1.855(2) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 N2 1.375(3) . ?
C2 N1 1.385(3) . ?
N1 C3 1.387(3) . ?
N1 C5 1.433(3) . ?
N2 C4 1.395(3) . ?
N2 C11 1.446(3) . ?
C3 C4 1.332(3) . ?
C3 H3 0.9500 . ?
C4 H4 0.9500 . ?
C5 C10 1.393(3) . ?
C5 C6 1.397(3) . ?
C6 C7 1.391(3) . ?
C6 C17 1.513(4) . ?
C7 C8 1.372(4) . ?
C7 H7 0.9500 . ?
C8 C9 1.370(4) . ?
C8 H8 0.9500 . ?
C9 C10 1.398(3) . ?
C9 H9 0.9500 . ?
C10 C20 1.511(4) . ?
C11 C16 1.391(3) . ?
C11 C12 1.392(3) . ?
C12 C13 1.393(3) . ?
C12 C23 1.511(3) . ?
C13 C14 1.374(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.378(3) . ?
C14 H14 0.9500 . ?
C15 C16 1.393(3) . ?
C15 H15 0.9500 . ?
C16 C26 1.524(3) . ?
C17 C19 1.522(4) . ?
C17 C18 1.532(4) . ?
C17 H17 1.0000 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 C22 1.523(4) . ?
C20 C21 1.523(4) . ?
C20 H20 1.0000 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C24 1.521(4) . ?
C23 C25 1.526(4) . ?
C23 H23 1.0000 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 C28 1.522(4) . ?
C26 C27 1.526(4) . ?
C26 H26 1.0000 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 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
C2 P1 C1 106.47(10) . . ?
P1 C1 H1A 109.5 . . ?
P1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
P1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N2 C2 N1 103.52(18) . . ?
N2 C2 P1 136.81(16) . . ?
N1 C2 P1 119.68(16) . . ?
C2 N1 C3 110.60(18) . . ?
C2 N1 C5 125.32(18) . . ?
C3 N1 C5 123.69(18) . . ?
C2 N2 C4 110.90(17) . . ?
C2 N2 C11 124.76(17) . . ?
C4 N2 C11 124.33(17) . . ?
C4 C3 N1 107.81(19) . . ?
C4 C3 H3 126.1 . . ?
N1 C3 H3 126.1 . . ?
C3 C4 N2 107.17(19) . . ?
C3 C4 H4 126.4 . . ?
N2 C4 H4 126.4 . . ?
C10 C5 C6 123.4(2) . . ?
C10 C5 N1 118.7(2) . . ?
C6 C5 N1 117.9(2) . . ?
C7 C6 C5 116.7(2) . . ?
C7 C6 C17 121.1(2) . . ?
C5 C6 C17 122.2(2) . . ?
C8 C7 C6 121.6(3) . . ?
C8 C7 H7 119.2 . . ?
C6 C7 H7 119.2 . . ?
C9 C8 C7 120.2(2) . . ?
C9 C8 H8 119.9 . . ?
C7 C8 H8 119.9 . . ?
C8 C9 C10 121.4(3) . . ?
C8 C9 H9 119.3 . . ?
C10 C9 H9 119.3 . . ?
C5 C10 C9 116.6(2) . . ?
C5 C10 C20 122.0(2) . . ?
C9 C10 C20 121.4(2) . . ?
C16 C11 C12 123.7(2) . . ?
C16 C11 N2 118.3(2) . . ?
C12 C11 N2 118.0(2) . . ?
C11 C12 C13 116.5(2) . . ?
C11 C12 C23 122.4(2) . . ?
C13 C12 C23 121.1(2) . . ?
C14 C13 C12 121.3(2) . . ?
C14 C13 H13 119.4 . . ?
C12 C13 H13 119.4 . . ?
C13 C14 C15 120.5(2) . . ?
C13 C14 H14 119.8 . . ?
C15 C14 H14 119.8 . . ?
C14 C15 C16 120.9(2) . . ?
C14 C15 H15 119.6 . . ?
C16 C15 H15 119.6 . . ?
C11 C16 C15 116.9(2) . . ?
C11 C16 C26 121.4(2) . . ?
C15 C16 C26 121.7(2) . . ?
C6 C17 C19 111.2(2) . . ?
C6 C17 C18 111.6(2) . . ?
C19 C17 C18 111.1(2) . . ?
C6 C17 H17 107.6 . . ?
C19 C17 H17 107.6 . . ?
C18 C17 H17 107.6 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C10 C20 C22 111.1(2) . . ?
C10 C20 C21 112.2(2) . . ?
C22 C20 C21 110.9(3) . . ?
C10 C20 H20 107.4 . . ?
C22 C20 H20 107.4 . . ?
C21 C20 H20 107.4 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C12 C23 C24 112.2(2) . . ?
C12 C23 C25 110.8(2) . . ?
C24 C23 C25 111.0(2) . . ?
C12 C23 H23 107.6 . . ?
C24 C23 H23 107.6 . . ?
C25 C23 H23 107.6 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C28 C26 C16 111.8(2) . . ?
C28 C26 C27 111.1(2) . . ?
C16 C26 C27 111.8(2) . . ?
C28 C26 H26 107.3 . . ?
C16 C26 H26 107.3 . . ?
C27 C26 H26 107.3 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 P1 C2 N2 2.2(3) . . . . ?
C1 P1 C2 N1 -177.85(19) . . . . ?
N2 C2 N1 C3 -0.2(3) . . . . ?
P1 C2 N1 C3 179.85(18) . . . . ?
N2 C2 N1 C5 -173.2(2) . . . . ?
P1 C2 N1 C5 6.8(3) . . . . ?
N1 C2 N2 C4 -0.1(3) . . . . ?
P1 C2 N2 C4 179.8(2) . . . . ?
N1 C2 N2 C11 -179.2(2) . . . . ?
P1 C2 N2 C11 0.8(4) . . . . ?
C2 N1 C3 C4 0.4(3) . . . . ?
C5 N1 C3 C4 173.6(2) . . . . ?
N1 C3 C4 N2 -0.5(3) . . . . ?
C2 N2 C4 C3 0.4(3) . . . . ?
C11 N2 C4 C3 179.4(2) . . . . ?
C2 N1 C5 C10 -93.8(3) . . . . ?
C3 N1 C5 C10 94.0(3) . . . . ?
C2 N1 C5 C6 89.2(3) . . . . ?
C3 N1 C5 C6 -83.0(3) . . . . ?
C10 C5 C6 C7 -4.0(3) . . . . ?
N1 C5 C6 C7 172.93(19) . . . . ?
C10 C5 C6 C17 175.4(2) . . . . ?
N1 C5 C6 C17 -7.7(3) . . . . ?
C5 C6 C7 C8 1.1(3) . . . . ?
C17 C6 C7 C8 -178.3(2) . . . . ?
C6 C7 C8 C9 1.9(4) . . . . ?
C7 C8 C9 C10 -2.3(4) . . . . ?
C6 C5 C10 C9 3.7(3) . . . . ?
N1 C5 C10 C9 -173.24(19) . . . . ?
C6 C5 C10 C20 -176.8(2) . . . . ?
N1 C5 C10 C20 6.3(3) . . . . ?
C8 C9 C10 C5 -0.4(3) . . . . ?
C8 C9 C10 C20 -179.9(2) . . . . ?
C2 N2 C11 C16 -93.0(3) . . . . ?
C4 N2 C11 C16 88.1(3) . . . . ?
C2 N2 C11 C12 85.5(3) . . . . ?
C4 N2 C11 C12 -93.4(3) . . . . ?
C16 C11 C12 C13 5.1(3) . . . . ?
N2 C11 C12 C13 -173.34(19) . . . . ?
C16 C11 C12 C23 -173.9(2) . . . . ?
N2 C11 C12 C23 7.7(3) . . . . ?
C11 C12 C13 C14 -0.9(3) . . . . ?
C23 C12 C13 C14 178.1(2) . . . . ?
C12 C13 C14 C15 -3.0(4) . . . . ?
C13 C14 C15 C16 2.9(4) . . . . ?
C12 C11 C16 C15 -5.2(3) . . . . ?
N2 C11 C16 C15 173.24(19) . . . . ?
C12 C11 C16 C26 174.7(2) . . . . ?
N2 C11 C16 C26 -6.9(3) . . . . ?
C14 C15 C16 C11 1.1(3) . . . . ?
C14 C15 C16 C26 -178.8(2) . . . . ?
C7 C6 C17 C19 53.9(3) . . . . ?
C5 C6 C17 C19 -125.5(2) . . . . ?
C7 C6 C17 C18 -70.7(3) . . . . ?
C5 C6 C17 C18 109.9(3) . . . . ?
C5 C10 C20 C22 -99.4(3) . . . . ?
C9 C10 C20 C22 80.1(3) . . . . ?
C5 C10 C20 C21 135.7(3) . . . . ?
C9 C10 C20 C21 -44.8(3) . . . . ?
C11 C12 C23 C24 -113.6(3) . . . . ?
C13 C12 C23 C24 67.5(3) . . . . ?
C11 C12 C23 C25 121.8(2) . . . . ?
C13 C12 C23 C25 -57.1(3) . . . . ?
C11 C16 C26 C28 93.2(3) . . . . ?
C15 C16 C26 C28 -86.9(3) . . . . ?
C11 C16 C26 C27 -141.5(2) . . . . ?
C15 C16 C26 C27 38.3(3) . . . . ?

_refine_diff_density_max         0.212
_refine_diff_density_min         -0.250
_refine_diff_density_rms         0.046

####################################################################### 
# 
# 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_g530_mn
_database_code_depnum_ccdc_archive 'CCDC 1992152'
loop_
_audit_author_name
_audit_author_address
'Christoph Feil'
;Universitity of Stuttgart
Germany
;
_audit_update_record             
;
2020-03-23 deposited with the CCDC.	2020-11-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C29 H42 N2 P, B F4'
_chemical_formula_sum            'C29 H42 B F4 N2 P'
_chemical_formula_weight         536.42

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'
B B 0.0013 0.0007 '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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   9.4999(3)
_cell_length_b                   19.6312(7)
_cell_length_c                   16.2528(6)
_cell_angle_alpha                90
_cell_angle_beta                 100.794(2)
_cell_angle_gamma                90
_cell_volume                     2977.43(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    135(2)
_cell_measurement_reflns_used    6734
_cell_measurement_theta_min      2.075
_cell_measurement_theta_max      30.590

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.197
_exptl_crystal_F_000             1144
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.814
_exptl_crystal_size_mid          0.566
_exptl_crystal_size_min          0.418
_exptl_absorpt_coefficient_mu    0.137
_shelx_estimated_absorpt_T_min   0.896
_shelx_estimated_absorpt_T_max   0.945

_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7143
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_process_details   'BLESSING 1995'
_exptl_absorpt_special_details   ?

_diffrn_ambient_temperature      135(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker Kappa ApexII Duo'
_diffrn_measurement_method       'Omega and phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            60555
_diffrn_reflns_av_unetI/netI     0.0261
_diffrn_reflns_av_R_equivalents  0.0353
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.075
_diffrn_reflns_theta_max         30.590
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             9063
_reflns_number_gt                6733
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker ApexII Software Suite, 2008'
_computing_cell_refinement       'Bruker ApexII Software Suite, 2008'
_computing_data_reduction        'Bruker ApexII Software Suite, 2008'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELX plus XP (Sheldrick, 1991)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'

_refine_special_details          
;
The P(H)Et moiety and onr IPr moiety disordered. Use of constraints (EADP)
and restraints (SADI) for the refinement.
Disordered atoms refined isotropically.

Use of restraints (RIGU, SADFI) for the refinement of the BF4 anions
;


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0695P)²+2.8021P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014)'
_refine_ls_extinction_coef       0.0047(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         9063
_refine_ls_number_parameters     335
_refine_ls_number_restraints     70
_refine_ls_R_factor_all          0.0851
_refine_ls_R_factor_gt           0.0594
_refine_ls_wR_factor_ref         0.1690
_refine_ls_wR_factor_gt          0.1450
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.073
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.55810(5) 0.21411(2) 0.41670(3) 0.02436(11) Uani 1 1 d D . . . .
H1A H 0.673(3) 0.2498(16) 0.419(2) 0.029 Uiso 0.612(4) 1 d D U P A 1
C1A C 0.6398(3) 0.13634(15) 0.46389(19) 0.0312(5) Uiso 0.612(4) 1 d D . P A 1
H1A1 H 0.5630 0.1080 0.4798 0.037 Uiso 0.612(4) 1 calc R U P A 1
H1A2 H 0.6783 0.1110 0.4203 0.037 Uiso 0.612(4) 1 calc R U P A 1
C2A C 0.7576(6) 0.1424(3) 0.5392(3) 0.0396(6) Uiso 0.612(4) 1 d D . P A 1
H2A1 H 0.7915 0.0968 0.5579 0.059 Uiso 0.612(4) 1 calc R U P A 1
H2A2 H 0.8370 0.1687 0.5245 0.059 Uiso 0.612(4) 1 calc R U P A 1
H2A3 H 0.7212 0.1656 0.5843 0.059 Uiso 0.612(4) 1 calc R U P A 1
H1B H 0.506(4) 0.1545(17) 0.427(2) 0.047 Uiso 0.388(4) 1 d D U P A 2
C1B C 0.7454(5) 0.1942(3) 0.4664(3) 0.0312(5) Uiso 0.388(4) 1 d D . P A 2
H1B1 H 0.7918 0.1729 0.4231 0.037 Uiso 0.388(4) 1 calc R U P A 2
H1B2 H 0.7950 0.2380 0.4816 0.037 Uiso 0.388(4) 1 calc R U P A 2
C2B C 0.7749(10) 0.1493(5) 0.5423(5) 0.0396(6) Uiso 0.388(4) 1 d D . P A 2
H2B1 H 0.8786 0.1439 0.5606 0.059 Uiso 0.388(4) 1 calc R U P A 2
H2B2 H 0.7342 0.1700 0.5875 0.059 Uiso 0.388(4) 1 calc R U P A 2
H2B3 H 0.7310 0.1045 0.5286 0.059 Uiso 0.388(4) 1 calc R U P A 2
C3 C 0.49692(18) 0.25582(8) 0.50421(9) 0.0202(3) Uani 1 1 d D . . . .
N1 N 0.53668(15) 0.31761(7) 0.53663(8) 0.0217(3) Uani 1 1 d . . . . .
N2 N 0.38899(15) 0.23455(7) 0.54129(8) 0.0222(3) Uani 1 1 d . . . . .
C4 C 0.4545(2) 0.33446(9) 0.59548(10) 0.0270(3) Uani 1 1 d . . . . .
H4 H 0.4617 0.3750 0.6279 0.032 Uiso 1 1 calc R U . . .
C5 C 0.3627(2) 0.28298(9) 0.59833(10) 0.0272(3) Uani 1 1 d . . . . .
H5 H 0.2927 0.2803 0.6330 0.033 Uiso 1 1 calc R U . . .
C6 C 0.64213(19) 0.36163(8) 0.51045(10) 0.0232(3) Uani 1 1 d . . . . .
C7 C 0.77519(19) 0.36929(8) 0.56365(10) 0.0240(3) Uani 1 1 d . . . . .
C8 C 0.8744(2) 0.41185(9) 0.53643(12) 0.0317(4) Uani 1 1 d . . . . .
H8 H 0.9660 0.4183 0.5707 0.038 Uiso 1 1 calc R U . . .
C9 C 0.8409(2) 0.44494(10) 0.45974(12) 0.0362(4) Uani 1 1 d . . . . .
H9 H 0.9104 0.4732 0.4417 0.043 Uiso 1 1 calc R U . . .
C10 C 0.7075(3) 0.43709(10) 0.40938(12) 0.0360(4) Uani 1 1 d . . . . .
H10 H 0.6861 0.4606 0.3575 0.043 Uiso 1 1 calc R U . . .
C11 C 0.6045(2) 0.39549(8) 0.43327(11) 0.0282(4) Uani 1 1 d . . . . .
C12 C 0.29779(18) 0.17657(9) 0.51386(10) 0.0237(3) Uani 1 1 d . . . . .
C13 C 0.32100(19) 0.11554(9) 0.55794(11) 0.0282(4) Uani 1 1 d . . . . .
C14 C 0.2313(2) 0.06112(11) 0.52759(13) 0.0380(4) Uani 1 1 d . . . . .
H14 H 0.2427 0.0186 0.5560 0.046 Uiso 1 1 calc R U . . .
C15 C 0.1262(2) 0.06830(12) 0.45688(14) 0.0432(5) Uani 1 1 d . . . . .
H15 H 0.0682 0.0303 0.4363 0.052 Uiso 1 1 calc R U . . .
C16 C 0.1047(2) 0.12974(12) 0.41591(13) 0.0387(5) Uani 1 1 d . . . . .
H16 H 0.0312 0.1337 0.3677 0.046 Uiso 1 1 calc R U . . .
C17 C 0.18848(19) 0.18626(10) 0.44360(11) 0.0291(4) Uani 1 1 d D . . . .
C18 C 0.81245(19) 0.33582(8) 0.64899(10) 0.0245(3) Uani 1 1 d . . . . .
H18 H 0.7339 0.3032 0.6546 0.029 Uiso 1 1 calc R U . . .
C19 C 0.9530(2) 0.29587(10) 0.66026(12) 0.0316(4) Uani 1 1 d . . . . .
H19A H 0.9726 0.2752 0.7161 0.047 Uiso 1 1 calc R U . . .
H19B H 0.9450 0.2600 0.6177 0.047 Uiso 1 1 calc R U . . .
H19C H 1.0314 0.3268 0.6542 0.047 Uiso 1 1 calc R U . . .
C20 C 0.8198(2) 0.39000(10) 0.71773(11) 0.0334(4) Uani 1 1 d . . . . .
H20A H 0.8439 0.3682 0.7728 0.050 Uiso 1 1 calc R U . . .
H20B H 0.8935 0.4237 0.7119 0.050 Uiso 1 1 calc R U . . .
H20C H 0.7266 0.4127 0.7123 0.050 Uiso 1 1 calc R U . . .
C21 C 0.4548(2) 0.39087(10) 0.37974(12) 0.0363(4) Uani 1 1 d . . . . .
H21 H 0.4122 0.3465 0.3929 0.044 Uiso 1 1 calc R U . . .
C22 C 0.4561(3) 0.39163(15) 0.28573(14) 0.0569(7) Uani 1 1 d . . . . .
H22A H 0.5176 0.3548 0.2722 0.085 Uiso 1 1 calc R U . . .
H22B H 0.3584 0.3851 0.2544 0.085 Uiso 1 1 calc R U . . .
H22C H 0.4932 0.4355 0.2704 0.085 Uiso 1 1 calc R U . . .
C23 C 0.3602(3) 0.44748(15) 0.40321(19) 0.0668(9) Uani 1 1 d . . . . .
H23A H 0.2643 0.4440 0.3684 0.100 Uiso 1 1 calc R U . . .
H23B H 0.3532 0.4431 0.4624 0.100 Uiso 1 1 calc R U . . .
H23C H 0.4021 0.4918 0.3939 0.100 Uiso 1 1 calc R U . . .
C24 C 0.4321(2) 0.10783(11) 0.63725(13) 0.0394(5) Uani 1 1 d . . . . .
H24 H 0.5011 0.1466 0.6399 0.047 Uiso 1 1 calc R U . . .
C25 C 0.5168(3) 0.04156(13) 0.63983(18) 0.0547(7) Uani 1 1 d . . . . .
H25A H 0.5869 0.0392 0.6923 0.082 Uiso 1 1 calc R U . . .
H25B H 0.4511 0.0028 0.6365 0.082 Uiso 1 1 calc R U . . .
H25C H 0.5669 0.0402 0.5923 0.082 Uiso 1 1 calc R U . . .
C26 C 0.3589(4) 0.11299(15) 0.71300(14) 0.0609(8) Uani 1 1 d . . . . .
H26A H 0.4307 0.1080 0.7645 0.091 Uiso 1 1 calc R U . . .
H26B H 0.3121 0.1575 0.7129 0.091 Uiso 1 1 calc R U . . .
H26C H 0.2871 0.0768 0.7103 0.091 Uiso 1 1 calc R U . . .
C27 C 0.1557(2) 0.25486(11) 0.40212(12) 0.0397(5) Uani 1 1 d D . . . .
H27A H 0.2230 0.2894 0.4329 0.048 Uiso 0.665(5) 1 calc R U P B 1
H27B H 0.2484 0.2801 0.4167 0.048 Uiso 0.335(5) 1 calc R U P B 2
C28A C -0.0032(4) 0.2730(2) 0.4131(2) 0.0428(7) Uiso 0.665(5) 1 d D . P B 1
H28A H -0.0307 0.3173 0.3873 0.064 Uiso 0.665(5) 1 calc R U P B 1
H28B H -0.0693 0.2379 0.3860 0.064 Uiso 0.665(5) 1 calc R U P B 1
H28C H -0.0071 0.2750 0.4729 0.064 Uiso 0.665(5) 1 calc R U P B 1
C29A C 0.1646(4) 0.25754(19) 0.31010(19) 0.0337(6) Uiso 0.665(5) 1 d D . P B 1
H29A H 0.1419 0.3037 0.2887 0.051 Uiso 0.665(5) 1 calc R U P B 1
H29B H 0.2618 0.2454 0.3032 0.051 Uiso 0.665(5) 1 calc R U P B 1
H29C H 0.0960 0.2252 0.2789 0.051 Uiso 0.665(5) 1 calc R U P B 1
C28B C 0.0512(8) 0.3012(3) 0.4279(4) 0.0428(7) Uiso 0.335(5) 1 d D . P B 2
H28D H 0.0446 0.3428 0.3941 0.064 Uiso 0.335(5) 1 calc R U P B 2
H28E H -0.0428 0.2790 0.4197 0.064 Uiso 0.335(5) 1 calc R U P B 2
H28F H 0.0818 0.3128 0.4872 0.064 Uiso 0.335(5) 1 calc R U P B 2
C29B C 0.1353(8) 0.2458(4) 0.3075(3) 0.0337(6) Uiso 0.335(5) 1 d D . P B 2
H29D H 0.2080 0.2144 0.2943 0.051 Uiso 0.335(5) 1 calc R U P B 2
H29E H 0.0396 0.2272 0.2863 0.051 Uiso 0.335(5) 1 calc R U P B 2
H29F H 0.1450 0.2900 0.2811 0.051 Uiso 0.335(5) 1 calc R U P B 2
B1 B 0.7897(2) 0.08517(11) 0.25318(13) 0.0307(4) Uani 1 1 d D U . . .
F1 F 0.79539(14) 0.15544(6) 0.26032(8) 0.0413(3) Uani 1 1 d D U . . .
F2 F 0.92112(14) 0.06259(7) 0.23586(9) 0.0478(3) Uani 1 1 d D U . . .
F3 F 0.68284(15) 0.06554(9) 0.18883(11) 0.0667(5) Uani 1 1 d D U . . .
F4 F 0.7730(2) 0.05678(9) 0.32751(11) 0.0768(6) Uani 1 1 d D U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1 C1A 1.816(3) . ?
P1 C3 1.8278(16) . ?
P1 C1B 1.853(4) . ?
P1 H1A 1.29(3) . ?
P1 H1B 1.29(3) . ?
C1A C2A 1.500(5) . ?
C1A H1A1 0.9900 . ?
C1A H1A2 0.9900 . ?
C2A H2A1 0.9800 . ?
C2A H2A2 0.9800 . ?
C2A H2A3 0.9800 . ?
C1B C2B 1.500(7) . ?
C1B H1B1 0.9900 . ?
C1B H1B2 0.9900 . ?
C2B H2B1 0.9800 . ?
C2B H2B2 0.9800 . ?
C2B H2B3 0.9800 . ?
C3 N1 1.348(2) . ?
C3 N2 1.349(2) . ?
N1 C4 1.383(2) . ?
N1 C6 1.446(2) . ?
N2 C5 1.383(2) . ?
N2 C12 1.449(2) . ?
C4 C5 1.341(3) . ?
C4 H4 0.9500 . ?
C5 H5 0.9500 . ?
C6 C7 1.400(2) . ?
C6 C11 1.405(2) . ?
C7 C8 1.392(2) . ?
C7 C18 1.516(2) . ?
C8 C9 1.389(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.383(3) . ?
C9 H9 0.9500 . ?
C10 C11 1.385(3) . ?
C10 H10 0.9500 . ?
C11 C21 1.525(3) . ?
C12 C13 1.392(2) . ?
C12 C17 1.405(2) . ?
C13 C14 1.398(2) . ?
C13 C24 1.513(3) . ?
C14 C15 1.381(3) . ?
C14 H14 0.9500 . ?
C15 C16 1.374(3) . ?
C15 H15 0.9500 . ?
C16 C17 1.390(3) . ?
C16 H16 0.9500 . ?
C17 C27 1.512(3) . ?
C18 C19 1.530(3) . ?
C18 C20 1.535(2) . ?
C18 H18 1.0000 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C23 1.522(3) . ?
C21 C22 1.530(3) . ?
C21 H21 1.0000 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 C26 1.526(4) . ?
C24 C25 1.526(4) . ?
C24 H24 1.0000 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 C28B 1.465(5) . ?
C27 C29A 1.515(4) . ?
C27 C29B 1.524(5) . ?
C27 C28A 1.593(4) . ?
C27 H27A 1.0000 . ?
C27 H27B 1.0000 . ?
C28A H28A 0.9800 . ?
C28A H28B 0.9800 . ?
C28A H28C 0.9800 . ?
C29A H29A 0.9800 . ?
C29A H29B 0.9800 . ?
C29A H29C 0.9800 . ?
C28B H28D 0.9800 . ?
C28B H28E 0.9800 . ?
C28B H28F 0.9800 . ?
C29B H29D 0.9800 . ?
C29B H29E 0.9800 . ?
C29B H29F 0.9800 . ?
B1 F4 1.366(2) . ?
B1 F3 1.369(2) . ?
B1 F1 1.385(2) . ?
B1 F2 1.402(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
C1A P1 C3 102.77(11) . . ?
C3 P1 C1B 100.07(16) . . ?
C1A P1 H1A 98.7(14) . . ?
C3 P1 H1A 96.9(14) . . ?
C3 P1 H1B 96.6(17) . . ?
C1B P1 H1B 96.3(17) . . ?
C2A C1A P1 118.2(3) . . ?
C2A C1A H1A1 107.8 . . ?
P1 C1A H1A1 107.8 . . ?
C2A C1A H1A2 107.8 . . ?
P1 C1A H1A2 107.8 . . ?
H1A1 C1A H1A2 107.1 . . ?
C1A C2A H2A1 109.5 . . ?
C1A C2A H2A2 109.5 . . ?
H2A1 C2A H2A2 109.5 . . ?
C1A C2A H2A3 109.5 . . ?
H2A1 C2A H2A3 109.5 . . ?
H2A2 C2A H2A3 109.5 . . ?
C2B C1B P1 119.9(5) . . ?
C2B C1B H1B1 107.4 . . ?
P1 C1B H1B1 107.4 . . ?
C2B C1B H1B2 107.4 . . ?
P1 C1B H1B2 107.4 . . ?
H1B1 C1B H1B2 106.9 . . ?
C1B C2B H2B1 109.5 . . ?
C1B C2B H2B2 109.5 . . ?
H2B1 C2B H2B2 109.5 . . ?
C1B C2B H2B3 109.5 . . ?
H2B1 C2B H2B3 109.5 . . ?
H2B2 C2B H2B3 109.5 . . ?
N1 C3 N2 106.53(14) . . ?
N1 C3 P1 126.92(12) . . ?
N2 C3 P1 126.01(12) . . ?
C3 N1 C4 109.41(14) . . ?
C3 N1 C6 125.56(14) . . ?
C4 N1 C6 124.92(14) . . ?
C3 N2 C5 109.55(14) . . ?
C3 N2 C12 124.48(13) . . ?
C5 N2 C12 124.99(14) . . ?
C5 C4 N1 107.37(15) . . ?
C5 C4 H4 126.3 . . ?
N1 C4 H4 126.3 . . ?
C4 C5 N2 107.13(15) . . ?
C4 C5 H5 126.4 . . ?
N2 C5 H5 126.4 . . ?
C7 C6 C11 123.38(16) . . ?
C7 C6 N1 118.53(14) . . ?
C11 C6 N1 118.08(15) . . ?
C8 C7 C6 117.06(15) . . ?
C8 C7 C18 119.67(15) . . ?
C6 C7 C18 123.23(15) . . ?
C9 C8 C7 120.73(18) . . ?
C9 C8 H8 119.6 . . ?
C7 C8 H8 119.6 . . ?
C10 C9 C8 120.66(18) . . ?
C10 C9 H9 119.7 . . ?
C8 C9 H9 119.7 . . ?
C9 C10 C11 121.15(17) . . ?
C9 C10 H10 119.4 . . ?
C11 C10 H10 119.4 . . ?
C10 C11 C6 117.00(17) . . ?
C10 C11 C21 120.52(16) . . ?
C6 C11 C21 122.38(17) . . ?
C13 C12 C17 123.81(16) . . ?
C13 C12 N2 119.32(14) . . ?
C17 C12 N2 116.87(15) . . ?
C12 C13 C14 116.66(17) . . ?
C12 C13 C24 122.86(15) . . ?
C14 C13 C24 120.41(17) . . ?
C15 C14 C13 120.9(2) . . ?
C15 C14 H14 119.5 . . ?
C13 C14 H14 119.5 . . ?
C16 C15 C14 120.76(19) . . ?
C16 C15 H15 119.6 . . ?
C14 C15 H15 119.6 . . ?
C15 C16 C17 121.30(18) . . ?
C15 C16 H16 119.4 . . ?
C17 C16 H16 119.4 . . ?
C16 C17 C12 116.49(18) . . ?
C16 C17 C27 120.59(17) . . ?
C12 C17 C27 122.82(17) . . ?
C7 C18 C19 112.39(15) . . ?
C7 C18 C20 109.67(14) . . ?
C19 C18 C20 110.40(15) . . ?
C7 C18 H18 108.1 . . ?
C19 C18 H18 108.1 . . ?
C20 C18 H18 108.1 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C23 C21 C11 110.17(17) . . ?
C23 C21 C22 111.0(2) . . ?
C11 C21 C22 112.8(2) . . ?
C23 C21 H21 107.5 . . ?
C11 C21 H21 107.5 . . ?
C22 C21 H21 107.5 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C13 C24 C26 109.3(2) . . ?
C13 C24 C25 112.88(19) . . ?
C26 C24 C25 110.6(2) . . ?
C13 C24 H24 108.0 . . ?
C26 C24 H24 108.0 . . ?
C25 C24 H24 108.0 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C28B C27 C17 121.3(3) . . ?
C17 C27 C29A 115.2(2) . . ?
C28B C27 C29B 113.3(4) . . ?
C17 C27 C29B 108.8(3) . . ?
C17 C27 C28A 105.6(2) . . ?
C29A C27 C28A 109.4(2) . . ?
C17 C27 H27A 108.8 . . ?
C29A C27 H27A 108.8 . . ?
C28A C27 H27A 108.8 . . ?
C28B C27 H27B 103.7 . . ?
C17 C27 H27B 103.7 . . ?
C29B C27 H27B 103.7 . . ?
C27 C28A H28A 109.5 . . ?
C27 C28A H28B 109.5 . . ?
H28A C28A H28B 109.5 . . ?
C27 C28A H28C 109.5 . . ?
H28A C28A H28C 109.5 . . ?
H28B C28A H28C 109.5 . . ?
C27 C29A H29A 109.5 . . ?
C27 C29A H29B 109.5 . . ?
H29A C29A H29B 109.5 . . ?
C27 C29A H29C 109.5 . . ?
H29A C29A H29C 109.5 . . ?
H29B C29A H29C 109.5 . . ?
C27 C28B H28D 109.5 . . ?
C27 C28B H28E 109.5 . . ?
H28D C28B H28E 109.5 . . ?
C27 C28B H28F 109.5 . . ?
H28D C28B H28F 109.5 . . ?
H28E C28B H28F 109.5 . . ?
C27 C29B H29D 109.5 . . ?
C27 C29B H29E 109.5 . . ?
H29D C29B H29E 109.5 . . ?
C27 C29B H29F 109.5 . . ?
H29D C29B H29F 109.5 . . ?
H29E C29B H29F 109.5 . . ?
F4 B1 F3 111.63(19) . . ?
F4 B1 F1 109.96(17) . . ?
F3 B1 F1 110.87(17) . . ?
F4 B1 F2 107.66(18) . . ?
F3 B1 F2 108.56(17) . . ?
F1 B1 F2 108.03(16) . . ?

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
C3 P1 C1A C2A -56.3(4) . . . . ?
C3 P1 C1B C2B 60.0(6) . . . . ?
C1A P1 C3 N1 120.20(17) . . . . ?
C1B P1 C3 N1 70.6(2) . . . . ?
C1A P1 C3 N2 -69.35(17) . . . . ?
C1B P1 C3 N2 -118.9(2) . . . . ?
N2 C3 N1 C4 1.03(18) . . . . ?
P1 C3 N1 C4 172.98(12) . . . . ?
N2 C3 N1 C6 -175.24(14) . . . . ?
P1 C3 N1 C6 -3.3(2) . . . . ?
N1 C3 N2 C5 -0.97(18) . . . . ?
P1 C3 N2 C5 -173.02(12) . . . . ?
N1 C3 N2 C12 168.19(14) . . . . ?
P1 C3 N2 C12 -3.9(2) . . . . ?
C3 N1 C4 C5 -0.71(19) . . . . ?
C6 N1 C4 C5 175.59(15) . . . . ?
N1 C4 C5 N2 0.10(19) . . . . ?
C3 N2 C5 C4 0.5(2) . . . . ?
C12 N2 C5 C4 -168.55(15) . . . . ?
C3 N1 C6 C7 -107.51(18) . . . . ?
C4 N1 C6 C7 76.8(2) . . . . ?
C3 N1 C6 C11 73.6(2) . . . . ?
C4 N1 C6 C11 -102.13(19) . . . . ?
C11 C6 C7 C8 -1.4(3) . . . . ?
N1 C6 C7 C8 179.79(16) . . . . ?
C11 C6 C7 C18 176.45(16) . . . . ?
N1 C6 C7 C18 -2.4(2) . . . . ?
C6 C7 C8 C9 0.1(3) . . . . ?
C18 C7 C8 C9 -177.78(18) . . . . ?
C7 C8 C9 C10 1.0(3) . . . . ?
C8 C9 C10 C11 -0.9(3) . . . . ?
C9 C10 C11 C6 -0.3(3) . . . . ?
C9 C10 C11 C21 176.10(19) . . . . ?
C7 C6 C11 C10 1.5(3) . . . . ?
N1 C6 C11 C10 -179.69(16) . . . . ?
C7 C6 C11 C21 -174.88(17) . . . . ?
N1 C6 C11 C21 4.0(2) . . . . ?
C3 N2 C12 C13 102.8(2) . . . . ?
C5 N2 C12 C13 -89.7(2) . . . . ?
C3 N2 C12 C17 -78.0(2) . . . . ?
C5 N2 C12 C17 89.5(2) . . . . ?
C17 C12 C13 C14 1.9(3) . . . . ?
N2 C12 C13 C14 -178.89(17) . . . . ?
C17 C12 C13 C24 -175.21(19) . . . . ?
N2 C12 C13 C24 4.0(3) . . . . ?
C12 C13 C14 C15 0.6(3) . . . . ?
C24 C13 C14 C15 177.8(2) . . . . ?
C13 C14 C15 C16 -1.8(4) . . . . ?
C14 C15 C16 C17 0.7(4) . . . . ?
C15 C16 C17 C12 1.6(3) . . . . ?
C15 C16 C17 C27 -175.0(2) . . . . ?
C13 C12 C17 C16 -3.0(3) . . . . ?
N2 C12 C17 C16 177.80(16) . . . . ?
C13 C12 C17 C27 173.56(18) . . . . ?
N2 C12 C17 C27 -5.7(3) . . . . ?
C8 C7 C18 C19 -54.1(2) . . . . ?
C6 C7 C18 C19 128.11(18) . . . . ?
C8 C7 C18 C20 69.1(2) . . . . ?
C6 C7 C18 C20 -108.68(19) . . . . ?
C10 C11 C21 C23 -86.2(3) . . . . ?
C6 C11 C21 C23 90.0(2) . . . . ?
C10 C11 C21 C22 38.5(3) . . . . ?
C6 C11 C21 C22 -145.25(19) . . . . ?
C12 C13 C24 C26 99.2(2) . . . . ?
C14 C13 C24 C26 -77.8(3) . . . . ?
C12 C13 C24 C25 -137.3(2) . . . . ?
C14 C13 C24 C25 45.7(3) . . . . ?
C16 C17 C27 C28B 85.8(4) . . . . ?
C12 C17 C27 C28B -90.6(4) . . . . ?
C16 C17 C27 C29A -61.3(3) . . . . ?
C12 C17 C27 C29A 122.3(2) . . . . ?
C16 C17 C27 C29B -48.4(4) . . . . ?
C12 C17 C27 C29B 135.2(4) . . . . ?
C16 C17 C27 C28A 59.6(3) . . . . ?
C12 C17 C27 C28A -116.8(2) . . . . ?

_refine_diff_density_max         1.144
_refine_diff_density_min         -0.803
_refine_diff_density_rms         0.067


# start Validation Reply Form
_vrf_PLAT201_g530_mn             
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......          4 Report
RESPONSE: P(H)Et moiety and one iPr moiety disordered,
disordered atoms refined isotropically
;
# end Validation Reply Form
####################################################################### 
# 
# 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_g544_mn
_database_code_depnum_ccdc_archive 'CCDC 1992158'
loop_
_audit_author_name
_audit_author_address
'Christoph Feil'
;Universitity of Stuttgart
Germany
;
_audit_update_record             
;
2020-03-23 deposited with the CCDC.	2020-11-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H44 N2 P, B F4'
_chemical_formula_sum            'C30 H44 B F4 N2 P'
_chemical_formula_weight         550.45

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'
B B 0.0013 0.0007 '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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   9.6514(5)
_cell_length_b                   19.5693(9)
_cell_length_c                   16.5413(7)
_cell_angle_alpha                90
_cell_angle_beta                 101.591(2)
_cell_angle_gamma                90
_cell_volume                     3060.5(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    135(2)
_cell_measurement_reflns_used    5433
_cell_measurement_theta_min      1.632
_cell_measurement_theta_max      28.339

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.195
_exptl_crystal_F_000             1176
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.472
_exptl_crystal_size_mid          0.368
_exptl_crystal_size_min          0.287
_exptl_absorpt_coefficient_mu    0.135
_shelx_estimated_absorpt_T_min   0.939
_shelx_estimated_absorpt_T_max   0.962
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7134
_exptl_absorpt_correction_T_max  0.7373
_exptl_absorpt_process_details   'BLESSING 1995'
_exptl_absorpt_special_details   ?

_diffrn_ambient_temperature      135(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker Kappa ApexII Duo'
_diffrn_measurement_method       'Omega and phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            64438
_diffrn_reflns_av_unetI/netI     0.0392
_diffrn_reflns_av_R_equivalents  0.0507
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.632
_diffrn_reflns_theta_max         28.339
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             7592
_reflns_number_gt                5433
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker ApexII Software Suite, 2008'
_computing_cell_refinement       'Bruker ApexII Software Suite, 2008'
_computing_data_reduction        'Bruker ApexII Software Suite, 2008'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
PMeEt moiety disordered, use of constraints (EADP) and restraints (SADI)
for the refinement. Disordered atoms refined isotropically.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0541P)²+2.1846P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7592
_refine_ls_number_parameters     340
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0823
_refine_ls_R_factor_gt           0.0521
_refine_ls_wR_factor_ref         0.1366
_refine_ls_wR_factor_gt          0.1212
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.033
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.94057(6) 0.20548(3) 0.57841(3) 0.02676(13) Uani 1 1 d D . . . .
C1A C 0.7774(3) 0.23818(15) 0.59137(18) 0.0283(6) Uiso 0.678(2) 1 d D . P A 1
H1A1 H 0.7348 0.2068 0.6256 0.042 Uiso 0.678(2) 1 calc R U P A 1
H1A2 H 0.7142 0.2431 0.5373 0.042 Uiso 0.678(2) 1 calc R U P A 1
H1A3 H 0.7917 0.2829 0.6184 0.042 Uiso 0.678(2) 1 calc R U P A 1
C2A C 0.8884(4) 0.12331(17) 0.5234(2) 0.0373(7) Uiso 0.678(2) 1 d D . P A 1
H2A1 H 0.9724 0.1041 0.5057 0.045 Uiso 0.678(2) 1 calc R U P A 1
H2A2 H 0.8604 0.0907 0.5630 0.045 Uiso 0.678(2) 1 calc R U P A 1
C3A C 0.7687(4) 0.1278(2) 0.4484(2) 0.0514(9) Uiso 0.678(2) 1 d D . P A 1
H3A1 H 0.7494 0.0823 0.4240 0.077 Uiso 0.678(2) 1 calc R U P A 1
H3A2 H 0.6835 0.1453 0.4651 0.077 Uiso 0.678(2) 1 calc R U P A 1
H3A3 H 0.7958 0.1587 0.4076 0.077 Uiso 0.678(2) 1 calc R U P A 1
C1B C 0.9929(7) 0.1219(3) 0.5770(4) 0.0283(6) Uiso 0.322(2) 1 d D . P A 2
H1B1 H 0.9367 0.0939 0.6075 0.042 Uiso 0.322(2) 1 calc R U P A 2
H1B2 H 1.0933 0.1182 0.6029 0.042 Uiso 0.322(2) 1 calc R U P A 2
H1B3 H 0.9787 0.1059 0.5198 0.042 Uiso 0.322(2) 1 calc R U P A 2
C2B C 0.7427(7) 0.1946(4) 0.5279(4) 0.0373(7) Uiso 0.322(2) 1 d D . P A 2
H2B1 H 0.6931 0.1759 0.5699 0.045 Uiso 0.322(2) 1 calc R U P A 2
H2B2 H 0.7026 0.2405 0.5125 0.045 Uiso 0.322(2) 1 calc R U P A 2
C3B C 0.7094(10) 0.1488(5) 0.4514(5) 0.0514(9) Uiso 0.322(2) 1 d D . P A 2
H3B1 H 0.6068 0.1470 0.4311 0.077 Uiso 0.322(2) 1 calc R U P A 2
H3B2 H 0.7548 0.1674 0.4083 0.077 Uiso 0.322(2) 1 calc R U P A 2
H3B3 H 0.7452 0.1026 0.4659 0.077 Uiso 0.322(2) 1 calc R U P A 2
C4 C 0.99531(18) 0.25396(8) 0.49460(10) 0.0164(3) Uani 1 1 d D . . . .
N1 N 1.10533(15) 0.23747(7) 0.45930(8) 0.0174(3) Uani 1 1 d . . . . .
N2 N 0.94855(15) 0.31544(7) 0.46280(8) 0.0168(3) Uani 1 1 d . . . . .
C5 C 1.12407(19) 0.28739(9) 0.40361(10) 0.0208(4) Uani 1 1 d . . . . .
H5 H 1.1930 0.2873 0.3699 0.025 Uiso 1 1 calc R U . . .
C6 C 1.02709(19) 0.33590(9) 0.40579(10) 0.0202(4) Uani 1 1 d . . . . .
H6 H 1.0146 0.3767 0.3741 0.024 Uiso 1 1 calc R U . . .
C7 C 1.20299(18) 0.18084(9) 0.48272(10) 0.0205(4) Uani 1 1 d . . . . .
C8 C 1.30251(19) 0.18724(10) 0.55701(11) 0.0234(4) Uani 1 1 d . . . . .
C9 C 1.3932(2) 0.13210(12) 0.57916(13) 0.0358(5) Uani 1 1 d . . . . .
H9 H 1.4609 0.1335 0.6295 0.043 Uiso 1 1 calc R U . . .
C10 C 1.3862(3) 0.07528(12) 0.52893(14) 0.0442(6) Uani 1 1 d . . . . .
H10 H 1.4486 0.0381 0.5456 0.053 Uiso 1 1 calc R U . . .
C11 C 1.2906(2) 0.07153(11) 0.45526(13) 0.0382(5) Uani 1 1 d . . . . .
H11 H 1.2890 0.0323 0.4213 0.046 Uiso 1 1 calc R U . . .
C12 C 1.1956(2) 0.12499(10) 0.42975(11) 0.0277(4) Uani 1 1 d . . . . .
C13 C 0.84738(18) 0.35982(9) 0.49098(10) 0.0187(3) Uani 1 1 d . . . . .
C14 C 0.89510(19) 0.39728(9) 0.56341(10) 0.0210(4) Uani 1 1 d . . . . .
C15 C 0.7968(2) 0.43932(10) 0.59004(11) 0.0255(4) Uani 1 1 d . . . . .
H15 H 0.8244 0.4651 0.6394 0.031 Uiso 1 1 calc R U . . .
C16 C 0.6597(2) 0.44403(10) 0.54553(12) 0.0272(4) Uani 1 1 d . . . . .
H16 H 0.5935 0.4723 0.5652 0.033 Uiso 1 1 calc R U . . .
C17 C 0.6178(2) 0.40818(10) 0.47283(12) 0.0251(4) Uani 1 1 d . . . . .
H17 H 0.5238 0.4130 0.4424 0.030 Uiso 1 1 calc R U . . .
C18 C 0.71140(19) 0.36498(9) 0.44347(11) 0.0211(4) Uani 1 1 d . . . . .
C19 C 1.31462(19) 0.25125(10) 0.60949(11) 0.0242(4) Uani 1 1 d . . . . .
H19 H 1.2165 0.2686 0.6076 0.029 Uiso 1 1 calc R U . . .
C20 C 1.3954(3) 0.30718(12) 0.57528(13) 0.0399(5) Uani 1 1 d . . . . .
H20A H 1.4012 0.3477 0.6106 0.060 Uiso 1 1 calc R U . . .
H20B H 1.4910 0.2910 0.5739 0.060 Uiso 1 1 calc R U . . .
H20C H 1.3461 0.3189 0.5193 0.060 Uiso 1 1 calc R U . . .
C21 C 1.3816(2) 0.23855(12) 0.69978(12) 0.0364(5) Uani 1 1 d . . . . .
H21A H 1.3865 0.2816 0.7304 0.055 Uiso 1 1 calc R U . . .
H21B H 1.3241 0.2056 0.7233 0.055 Uiso 1 1 calc R U . . .
H21C H 1.4772 0.2202 0.7037 0.055 Uiso 1 1 calc R U . . .
C22 C 1.0960(2) 0.12186(11) 0.34680(12) 0.0340(5) Uani 1 1 d . . . . .
H22 H 1.0262 0.1600 0.3442 0.041 Uiso 1 1 calc R U . . .
C23 C 1.1788(3) 0.13301(15) 0.27854(13) 0.0519(7) Uani 1 1 d . . . . .
H23A H 1.1140 0.1310 0.2247 0.078 Uiso 1 1 calc R U . . .
H23B H 1.2246 0.1779 0.2855 0.078 Uiso 1 1 calc R U . . .
H23C H 1.2509 0.0973 0.2815 0.078 Uiso 1 1 calc R U . . .
C24 C 1.0137(3) 0.05465(13) 0.33301(16) 0.0492(7) Uani 1 1 d . . . . .
H24A H 0.9509 0.0553 0.2785 0.074 Uiso 1 1 calc R U . . .
H24B H 1.0802 0.0165 0.3360 0.074 Uiso 1 1 calc R U . . .
H24C H 0.9573 0.0492 0.3757 0.074 Uiso 1 1 calc R U . . .
C25 C 1.0468(2) 0.39567(10) 0.61116(11) 0.0257(4) Uani 1 1 d . . . . .
H25 H 1.0980 0.3595 0.5861 0.031 Uiso 1 1 calc R U . . .
C26 C 1.1202(3) 0.46320(13) 0.60371(16) 0.0446(6) Uani 1 1 d . . . . .
H26A H 1.1130 0.4744 0.5453 0.067 Uiso 1 1 calc R U . . .
H26B H 1.0751 0.4993 0.6304 0.067 Uiso 1 1 calc R U . . .
H26C H 1.2201 0.4596 0.6307 0.067 Uiso 1 1 calc R U . . .
C27 C 1.0573(3) 0.37783(15) 0.70146(14) 0.0494(6) Uani 1 1 d . . . . .
H27A H 1.0096 0.3342 0.7058 0.074 Uiso 1 1 calc R U . . .
H27B H 1.1570 0.3741 0.7286 0.074 Uiso 1 1 calc R U . . .
H27C H 1.0120 0.4137 0.7283 0.074 Uiso 1 1 calc R U . . .
C28 C 0.6647(2) 0.32859(10) 0.36173(12) 0.0297(4) Uani 1 1 d . . . . .
H28 H 0.7396 0.2948 0.3555 0.036 Uiso 1 1 calc R U . . .
C29 C 0.5259(2) 0.28981(13) 0.35710(16) 0.0451(6) Uani 1 1 d . . . . .
H29A H 0.4998 0.2671 0.3034 0.068 Uiso 1 1 calc R U . . .
H29B H 0.5376 0.2555 0.4011 0.068 Uiso 1 1 calc R U . . .
H29C H 0.4512 0.3220 0.3638 0.068 Uiso 1 1 calc R U . . .
C30 C 0.6512(3) 0.38042(13) 0.29115(12) 0.0407(6) Uani 1 1 d . . . . .
H30A H 0.6210 0.3569 0.2383 0.061 Uiso 1 1 calc R U . . .
H30B H 0.5810 0.4152 0.2974 0.061 Uiso 1 1 calc R U . . .
H30C H 0.7429 0.4024 0.2926 0.061 Uiso 1 1 calc R U . . .
B1 B 0.2037(2) 0.41522(12) 0.24795(13) 0.0249(4) Uani 1 1 d . . . . .
F1 F 0.07596(13) 0.43834(7) 0.26395(8) 0.0420(3) Uani 1 1 d . . . . .
F2 F 0.31360(14) 0.44054(7) 0.30624(9) 0.0501(4) Uani 1 1 d . . . . .
F3 F 0.20391(15) 0.34428(6) 0.24963(8) 0.0412(3) Uani 1 1 d . . . . .
F4 F 0.21651(16) 0.43586(7) 0.16979(8) 0.0458(4) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1 C1B 1.713(6) . ?
P1 C1A 1.753(3) . ?
P1 C4 1.8426(17) . ?
P1 C2A 1.867(3) . ?
P1 C2B 1.937(7) . ?
C1A H1A1 0.9800 . ?
C1A H1A2 0.9800 . ?
C1A H1A3 0.9800 . ?
C2A C3A 1.519(5) . ?
C2A H2A1 0.9900 . ?
C2A H2A2 0.9900 . ?
C3A H3A1 0.9800 . ?
C3A H3A2 0.9800 . ?
C3A H3A3 0.9800 . ?
C1B H1B1 0.9800 . ?
C1B H1B2 0.9800 . ?
C1B H1B3 0.9800 . ?
C2B C3B 1.532(9) . ?
C2B H2B1 0.9900 . ?
C2B H2B2 0.9900 . ?
C3B H3B1 0.9800 . ?
C3B H3B2 0.9800 . ?
C3B H3B3 0.9800 . ?
C4 N1 1.350(2) . ?
C4 N2 1.354(2) . ?
N1 C5 1.379(2) . ?
N1 C7 1.456(2) . ?
N2 C6 1.383(2) . ?
N2 C13 1.452(2) . ?
C5 C6 1.339(3) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C12 1.394(3) . ?
C7 C8 1.405(2) . ?
C8 C9 1.392(3) . ?
C8 C19 1.515(3) . ?
C9 C10 1.382(3) . ?
C9 H9 0.9500 . ?
C10 C11 1.375(3) . ?
C10 H10 0.9500 . ?
C11 C12 1.399(3) . ?
C11 H11 0.9500 . ?
C12 C22 1.510(3) . ?
C13 C18 1.391(2) . ?
C13 C14 1.401(2) . ?
C14 C15 1.392(2) . ?
C14 C25 1.517(3) . ?
C15 C16 1.382(3) . ?
C15 H15 0.9500 . ?
C16 C17 1.381(3) . ?
C16 H16 0.9500 . ?
C17 C18 1.394(2) . ?
C17 H17 0.9500 . ?
C18 C28 1.514(3) . ?
C19 C20 1.518(3) . ?
C19 C21 1.524(3) . ?
C19 H19 1.0000 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C23 1.524(3) . ?
C22 C24 1.529(3) . ?
C22 H22 1.0000 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C26 1.517(3) . ?
C25 C27 1.517(3) . ?
C25 H25 1.0000 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 C29 1.529(3) . ?
C28 C30 1.532(3) . ?
C28 H28 1.0000 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
B1 F2 1.374(2) . ?
B1 F4 1.383(2) . ?
B1 F1 1.388(2) . ?
B1 F3 1.389(3) . ?

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
C1B P1 C4 110.6(2) . . ?
C1A P1 C4 107.74(11) . . ?
C1A P1 C2A 102.30(15) . . ?
C4 P1 C2A 99.60(12) . . ?
C1B P1 C2B 99.1(3) . . ?
C4 P1 C2B 98.0(2) . . ?
P1 C1A H1A1 109.5 . . ?
P1 C1A H1A2 109.5 . . ?
H1A1 C1A H1A2 109.5 . . ?
P1 C1A H1A3 109.5 . . ?
H1A1 C1A H1A3 109.5 . . ?
H1A2 C1A H1A3 109.5 . . ?
C3A C2A P1 115.8(3) . . ?
C3A C2A H2A1 108.3 . . ?
P1 C2A H2A1 108.3 . . ?
C3A C2A H2A2 108.3 . . ?
P1 C2A H2A2 108.3 . . ?
H2A1 C2A H2A2 107.4 . . ?
C2A C3A H3A1 109.5 . . ?
C2A C3A H3A2 109.5 . . ?
H3A1 C3A H3A2 109.5 . . ?
C2A C3A H3A3 109.5 . . ?
H3A1 C3A H3A3 109.5 . . ?
H3A2 C3A H3A3 109.5 . . ?
P1 C1B H1B1 109.5 . . ?
P1 C1B H1B2 109.5 . . ?
H1B1 C1B H1B2 109.5 . . ?
P1 C1B H1B3 109.5 . . ?
H1B1 C1B H1B3 109.5 . . ?
H1B2 C1B H1B3 109.5 . . ?
C3B C2B P1 116.5(5) . . ?
C3B C2B H2B1 108.2 . . ?
P1 C2B H2B1 108.2 . . ?
C3B C2B H2B2 108.2 . . ?
P1 C2B H2B2 108.2 . . ?
H2B1 C2B H2B2 107.3 . . ?
C2B C3B H3B1 109.5 . . ?
C2B C3B H3B2 109.5 . . ?
H3B1 C3B H3B2 109.5 . . ?
C2B C3B H3B3 109.5 . . ?
H3B1 C3B H3B3 109.5 . . ?
H3B2 C3B H3B3 109.5 . . ?
N1 C4 N2 105.92(14) . . ?
N1 C4 P1 124.87(12) . . ?
N2 C4 P1 128.78(12) . . ?
C4 N1 C5 109.86(14) . . ?
C4 N1 C7 126.19(14) . . ?
C5 N1 C7 123.51(14) . . ?
C4 N2 C6 109.68(14) . . ?
C4 N2 C13 126.89(14) . . ?
C6 N2 C13 122.82(14) . . ?
C6 C5 N1 107.34(15) . . ?
C6 C5 H5 126.3 . . ?
N1 C5 H5 126.3 . . ?
C5 C6 N2 107.17(15) . . ?
C5 C6 H6 126.4 . . ?
N2 C6 H6 126.4 . . ?
C12 C7 C8 124.01(16) . . ?
C12 C7 N1 118.75(15) . . ?
C8 C7 N1 117.20(15) . . ?
C9 C8 C7 116.40(17) . . ?
C9 C8 C19 121.21(17) . . ?
C7 C8 C19 122.36(16) . . ?
C10 C9 C8 120.90(19) . . ?
C10 C9 H9 119.6 . . ?
C8 C9 H9 119.6 . . ?
C11 C10 C9 121.3(2) . . ?
C11 C10 H10 119.4 . . ?
C9 C10 H10 119.4 . . ?
C10 C11 C12 120.66(19) . . ?
C10 C11 H11 119.7 . . ?
C12 C11 H11 119.7 . . ?
C7 C12 C11 116.69(17) . . ?
C7 C12 C22 123.08(17) . . ?
C11 C12 C22 120.17(17) . . ?
C18 C13 C14 123.76(16) . . ?
C18 C13 N2 118.75(15) . . ?
C14 C13 N2 117.44(15) . . ?
C15 C14 C13 116.87(17) . . ?
C15 C14 C25 119.65(16) . . ?
C13 C14 C25 123.45(16) . . ?
C16 C15 C14 120.74(17) . . ?
C16 C15 H15 119.6 . . ?
C14 C15 H15 119.6 . . ?
C17 C16 C15 120.75(17) . . ?
C17 C16 H16 119.6 . . ?
C15 C16 H16 119.6 . . ?
C16 C17 C18 120.99(18) . . ?
C16 C17 H17 119.5 . . ?
C18 C17 H17 119.5 . . ?
C13 C18 C17 116.81(16) . . ?
C13 C18 C28 123.21(16) . . ?
C17 C18 C28 119.94(17) . . ?
C8 C19 C20 111.64(16) . . ?
C8 C19 C21 113.29(16) . . ?
C20 C19 C21 109.56(17) . . ?
C8 C19 H19 107.4 . . ?
C20 C19 H19 107.4 . . ?
C21 C19 H19 107.4 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C12 C22 C23 109.53(19) . . ?
C12 C22 C24 112.77(19) . . ?
C23 C22 C24 110.27(19) . . ?
C12 C22 H22 108.0 . . ?
C23 C22 H22 108.0 . . ?
C24 C22 H22 108.0 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C26 C25 C27 109.92(19) . . ?
C26 C25 C14 110.95(16) . . ?
C27 C25 C14 112.58(17) . . ?
C26 C25 H25 107.7 . . ?
C27 C25 H25 107.7 . . ?
C14 C25 H25 107.7 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C18 C28 C29 112.25(18) . . ?
C18 C28 C30 109.48(17) . . ?
C29 C28 C30 110.53(18) . . ?
C18 C28 H28 108.2 . . ?
C29 C28 H28 108.2 . . ?
C30 C28 H28 108.2 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C28 C30 H30A 109.5 . . ?
C28 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C28 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
F2 B1 F4 110.45(17) . . ?
F2 B1 F1 109.78(16) . . ?
F4 B1 F1 109.41(17) . . ?
F2 B1 F3 110.42(18) . . ?
F4 B1 F3 108.10(16) . . ?
F1 B1 F3 108.64(17) . . ?

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
C1A P1 C2A C3A 49.7(3) . . . . ?
C4 P1 C2A C3A -61.0(3) . . . . ?
C1B P1 C4 N1 -25.2(3) . . . . ?
C1A P1 C4 N1 -170.39(17) . . . . ?
C2A P1 C4 N1 -64.08(18) . . . . ?
C2B P1 C4 N1 -128.1(2) . . . . ?
C1B P1 C4 N2 163.4(3) . . . . ?
C1A P1 C4 N2 18.2(2) . . . . ?
C2A P1 C4 N2 124.52(18) . . . . ?
C2B P1 C4 N2 60.5(3) . . . . ?
N2 C4 N1 C5 -2.02(19) . . . . ?
P1 C4 N1 C5 -175.06(13) . . . . ?
N2 C4 N1 C7 170.45(15) . . . . ?
P1 C4 N1 C7 -2.6(2) . . . . ?
N1 C4 N2 C6 1.90(19) . . . . ?
P1 C4 N2 C6 174.57(13) . . . . ?
N1 C4 N2 C13 -169.21(15) . . . . ?
P1 C4 N2 C13 3.5(3) . . . . ?
C4 N1 C5 C6 1.4(2) . . . . ?
C7 N1 C5 C6 -171.31(15) . . . . ?
N1 C5 C6 N2 -0.2(2) . . . . ?
C4 N2 C6 C5 -1.1(2) . . . . ?
C13 N2 C6 C5 170.47(15) . . . . ?
C4 N1 C7 C12 109.0(2) . . . . ?
C5 N1 C7 C12 -79.5(2) . . . . ?
C4 N1 C7 C8 -72.9(2) . . . . ?
C5 N1 C7 C8 98.6(2) . . . . ?
C12 C7 C8 C9 -3.2(3) . . . . ?
N1 C7 C8 C9 178.85(17) . . . . ?
C12 C7 C8 C19 175.00(18) . . . . ?
N1 C7 C8 C19 -3.0(3) . . . . ?
C7 C8 C9 C10 1.5(3) . . . . ?
C19 C8 C9 C10 -176.7(2) . . . . ?
C8 C9 C10 C11 0.6(4) . . . . ?
C9 C10 C11 C12 -1.1(4) . . . . ?
C8 C7 C12 C11 2.7(3) . . . . ?
N1 C7 C12 C11 -179.37(18) . . . . ?
C8 C7 C12 C22 -174.64(19) . . . . ?
N1 C7 C12 C22 3.3(3) . . . . ?
C10 C11 C12 C7 -0.4(3) . . . . ?
C10 C11 C12 C22 177.0(2) . . . . ?
C4 N2 C13 C18 -106.4(2) . . . . ?
C6 N2 C13 C18 83.5(2) . . . . ?
C4 N2 C13 C14 76.1(2) . . . . ?
C6 N2 C13 C14 -93.9(2) . . . . ?
C18 C13 C14 C15 3.1(3) . . . . ?
N2 C13 C14 C15 -179.61(15) . . . . ?
C18 C13 C14 C25 -174.92(17) . . . . ?
N2 C13 C14 C25 2.4(3) . . . . ?
C13 C14 C15 C16 -1.0(3) . . . . ?
C25 C14 C15 C16 177.06(17) . . . . ?
C14 C15 C16 C17 -1.3(3) . . . . ?
C15 C16 C17 C18 1.7(3) . . . . ?
C14 C13 C18 C17 -2.7(3) . . . . ?
N2 C13 C18 C17 -179.98(16) . . . . ?
C14 C13 C18 C28 174.86(18) . . . . ?
N2 C13 C18 C28 -2.4(3) . . . . ?
C16 C17 C18 C13 0.3(3) . . . . ?
C16 C17 C18 C28 -177.38(18) . . . . ?
C9 C8 C19 C20 98.9(2) . . . . ?
C7 C8 C19 C20 -79.2(2) . . . . ?
C9 C8 C19 C21 -25.4(3) . . . . ?
C7 C8 C19 C21 156.55(18) . . . . ?
C7 C12 C22 C23 104.9(2) . . . . ?
C11 C12 C22 C23 -72.4(3) . . . . ?
C7 C12 C22 C24 -131.9(2) . . . . ?
C11 C12 C22 C24 50.8(3) . . . . ?
C15 C14 C25 C26 -67.8(2) . . . . ?
C13 C14 C25 C26 110.1(2) . . . . ?
C15 C14 C25 C27 55.9(2) . . . . ?
C13 C14 C25 C27 -126.2(2) . . . . ?
C13 C18 C28 C29 130.5(2) . . . . ?
C17 C18 C28 C29 -52.0(2) . . . . ?
C13 C18 C28 C30 -106.4(2) . . . . ?
C17 C18 C28 C30 71.1(2) . . . . ?

_refine_diff_density_max         0.545
_refine_diff_density_min         -0.456
_refine_diff_density_rms         0.054


# start Validation Reply Form

_vrf_PLAT201_g544_mn             
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......          3 Report
RESPONSE: disorder of Me(P) vs. Et(P), disordered atome refined isotropically
;
# end Validation Reply Form
####################################################################### 
# 
# 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_g563_mn
_database_code_depnum_ccdc_archive 'CCDC 1992157'
loop_
_audit_author_name
_audit_author_address
'Christoph Feil'
;Universitity of Stuttgart
Germany
;
_audit_update_record             
;
2020-03-23 deposited with the CCDC.	2020-11-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C27 H38 N2 P, B F4, C H2 Cl2'
_chemical_formula_sum            'C28 H40 B Cl2 F4 N2 P'
_chemical_formula_weight         593.30

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'
B B 0.0013 0.0007 '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'
F F 0.0171 0.0103 '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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           64
_space_group_name_H-M_alt        'C m c a'
_space_group_name_Hall           '-C 2bc 2'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   16.2797(11)
_cell_length_b                   19.2139(11)
_cell_length_c                   20.2982(14)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6349.2(7)
_cell_formula_units_Z            8
_cell_measurement_temperature    135(2)
_cell_measurement_reflns_used    2523
_cell_measurement_theta_min      1.922
_cell_measurement_theta_max      26.423

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.241
_exptl_crystal_F_000             2496
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.506
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.124
_exptl_absorpt_coefficient_mu    0.298
_shelx_estimated_absorpt_T_min   0.864
_shelx_estimated_absorpt_T_max   0.964
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7253
_exptl_absorpt_correction_T_max  0.7433
_exptl_absorpt_process_details   'BLESSING 1995'
_exptl_absorpt_special_details   ?

_diffrn_ambient_temperature      135(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker Kappa ApexII Duo'
_diffrn_measurement_method       'Omega and phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            42948
_diffrn_reflns_av_unetI/netI     0.0277
_diffrn_reflns_av_R_equivalents  0.0466
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.922
_diffrn_reflns_theta_max         26.423
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             3384
_reflns_number_gt                2523
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker ApexII Software Suite, 2008'
_computing_cell_refinement       'Bruker ApexII Software Suite, 2008'
_computing_data_reduction        'Bruker ApexII Software Suite, 2008'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELX plus XP (Sheldrick, 1991)'
_computing_publication_material  ?

_refine_special_details          
;
Solvent CH2Cl2 disordered about the m.. mirror plane (s.o.f.= 0.50), 
use of restraints (SADI, RIGU) for the refinement.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1180P)²+19.3776P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3384
_refine_ls_number_parameters     196
_refine_ls_number_restraints     14
_refine_ls_R_factor_all          0.0936
_refine_ls_R_factor_gt           0.0699
_refine_ls_wR_factor_ref         0.2139
_refine_ls_wR_factor_gt          0.1937
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.049
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.0000 0.22589(6) 0.72498(5) 0.0253(3) Uani 1 2 d DS T P . .
H1P H 0.0553(17) 0.2708(14) 0.7250(17) 0.038 Uiso 1 1 d D U . . .
C1 C 0.0000 0.22039(18) 0.63568(18) 0.0178(7) Uani 1 2 d S T P . .
N1 N 0.06625(14) 0.21415(11) 0.59665(11) 0.0195(5) Uani 1 1 d . . . . .
C2 C 0.04130(19) 0.20444(15) 0.53197(13) 0.0249(6) Uani 1 1 d . . . . .
H2 H 0.0760 0.1988 0.4947 0.030 Uiso 1 1 calc R U . . .
C3 C 0.15016(16) 0.20907(14) 0.62024(13) 0.0220(6) Uani 1 1 d . . . . .
C4 C 0.17820(17) 0.14335(15) 0.63922(13) 0.0239(6) Uani 1 1 d . . . . .
C5 C 0.26000(19) 0.13908(18) 0.65938(16) 0.0345(7) Uani 1 1 d . . . . .
H5 H 0.2819 0.0953 0.6722 0.041 Uiso 1 1 calc R U . . .
C6 C 0.3097(2) 0.1974(2) 0.66099(18) 0.0408(8) Uani 1 1 d . . . . .
H6 H 0.3653 0.1932 0.6745 0.049 Uiso 1 1 calc R U . . .
C7 C 0.2794(2) 0.26126(19) 0.64331(18) 0.0402(9) Uani 1 1 d . . . . .
H7 H 0.3143 0.3008 0.6456 0.048 Uiso 1 1 calc R U . . .
C8 C 0.19832(19) 0.26961(16) 0.62192(15) 0.0305(7) Uani 1 1 d . . . . .
C9 C 0.12516(18) 0.07886(14) 0.63661(15) 0.0262(6) Uani 1 1 d . . . . .
H9 H 0.0671 0.0942 0.6298 0.031 Uiso 1 1 calc R U . . .
C10 C 0.1282(3) 0.03665(19) 0.70019(18) 0.0453(9) Uani 1 1 d . . . . .
H10A H 0.0928 -0.0044 0.6959 0.068 Uiso 1 1 calc R U . . .
H10B H 0.1848 0.0218 0.7087 0.068 Uiso 1 1 calc R U . . .
H10C H 0.1088 0.0654 0.7369 0.068 Uiso 1 1 calc R U . . .
C11 C 0.1494(3) 0.0340(2) 0.57808(19) 0.0594(12) Uani 1 1 d . . . . .
H11A H 0.1146 -0.0076 0.5768 0.089 Uiso 1 1 calc R U . . .
H11B H 0.1420 0.0606 0.5373 0.089 Uiso 1 1 calc R U . . .
H11C H 0.2070 0.0202 0.5823 0.089 Uiso 1 1 calc R U . . .
C12 C 0.1667(2) 0.33950(17) 0.60129(19) 0.0416(9) Uani 1 1 d . . . . .
H12 H 0.1073 0.3344 0.5897 0.050 Uiso 1 1 calc R U . . .
C13 C 0.1736(3) 0.3928(2) 0.6574(2) 0.0630(12) Uani 1 1 d . . . . .
H13A H 0.1525 0.4378 0.6424 0.095 Uiso 1 1 calc R U . . .
H13B H 0.1414 0.3768 0.6952 0.095 Uiso 1 1 calc R U . . .
H13C H 0.2313 0.3977 0.6703 0.095 Uiso 1 1 calc R U . . .
C14 C 0.2126(3) 0.3650(2) 0.5398(2) 0.0574(11) Uani 1 1 d . . . . .
H14A H 0.1913 0.4107 0.5268 0.086 Uiso 1 1 calc R U . . .
H14B H 0.2713 0.3688 0.5495 0.086 Uiso 1 1 calc R U . . .
H14C H 0.2043 0.3319 0.5037 0.086 Uiso 1 1 calc R U . . .
B1 B 0.0000 0.3504(2) 0.8629(2) 0.0264(10) Uani 1 2 d S T P . .
F1 F 0.0000 0.27796(13) 0.85978(14) 0.0388(7) Uani 1 2 d S T P . .
F2 F -0.06900(13) 0.37132(11) 0.89822(12) 0.0489(6) Uani 1 1 d . . . . .
F3 F 0.0000 0.37926(15) 0.80151(15) 0.0577(9) Uani 1 2 d S T P . .
C1C C 0.0220(6) 0.3782(4) 0.4229(3) 0.074(3) Uani 0.5 1 d D U P A -1
H1C1 H -0.0075 0.3346 0.4125 0.089 Uiso 0.5 1 calc R U P A -1
H1C2 H 0.0813 0.3674 0.4256 0.089 Uiso 0.5 1 calc R U P A -1
Cl1 Cl 0.0059(7) 0.43734(16) 0.36051(11) 0.1012(15) Uani 0.5 1 d D U P A -1
Cl2 Cl -0.0107(4) 0.4085(2) 0.49782(17) 0.145(2) Uani 0.5 1 d D U P A -1


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1 C1 1.816(4) . ?
P1 H1P 1.248(18) . ?
C1 N1 1.344(3) . ?
C1 N1 1.344(3) 12 ?
N1 C2 1.387(3) . ?
N1 C3 1.451(3) . ?
C2 C2 1.345(6) 12 ?
C2 H2 0.9500 . ?
C3 C4 1.397(4) . ?
C3 C8 1.403(4) . ?
C4 C5 1.396(4) . ?
C4 C9 1.511(4) . ?
C5 C6 1.382(5) . ?
C5 H5 0.9500 . ?
C6 C7 1.370(5) . ?
C6 H6 0.9500 . ?
C7 C8 1.399(5) . ?
C7 H7 0.9500 . ?
C8 C12 1.498(5) . ?
C9 C11 1.519(5) . ?
C9 C10 1.525(4) . ?
C9 H9 1.0000 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C13 1.535(5) . ?
C12 C14 1.536(5) . ?
C12 H12 1.0000 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
B1 F3 1.363(6) . ?
B1 F2 1.392(3) . ?
B1 F2 1.392(3) 12 ?
B1 F1 1.393(5) . ?
C1C Cl2 1.713(6) . ?
C1C Cl1 1.721(6) . ?
C1C H1C1 0.9900 . ?
C1C H1C2 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 P1 H1P 92.3(16) . . ?
N1 C1 N1 106.8(3) . 12 ?
N1 C1 P1 126.43(16) . . ?
N1 C1 P1 126.43(16) 12 . ?
C1 N1 C2 109.6(2) . . ?
C1 N1 C3 124.6(2) . . ?
C2 N1 C3 125.4(2) . . ?
C2 C2 N1 107.04(15) 12 . ?
C2 C2 H2 126.5 12 . ?
N1 C2 H2 126.5 . . ?
C4 C3 C8 124.1(3) . . ?
C4 C3 N1 117.4(2) . . ?
C8 C3 N1 118.6(3) . . ?
C5 C4 C3 116.5(3) . . ?
C5 C4 C9 120.5(3) . . ?
C3 C4 C9 123.0(2) . . ?
C6 C5 C4 121.2(3) . . ?
C6 C5 H5 119.4 . . ?
C4 C5 H5 119.4 . . ?
C7 C6 C5 120.6(3) . . ?
C7 C6 H6 119.7 . . ?
C5 C6 H6 119.7 . . ?
C6 C7 C8 121.6(3) . . ?
C6 C7 H7 119.2 . . ?
C8 C7 H7 119.2 . . ?
C7 C8 C3 116.1(3) . . ?
C7 C8 C12 120.9(3) . . ?
C3 C8 C12 123.0(3) . . ?
C4 C9 C11 110.1(3) . . ?
C4 C9 C10 112.8(3) . . ?
C11 C9 C10 110.6(3) . . ?
C4 C9 H9 107.7 . . ?
C11 C9 H9 107.7 . . ?
C10 C9 H9 107.7 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C8 C12 C13 111.4(3) . . ?
C8 C12 C14 110.3(3) . . ?
C13 C12 C14 110.8(3) . . ?
C8 C12 H12 108.1 . . ?
C13 C12 H12 108.1 . . ?
C14 C12 H12 108.1 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
F3 B1 F2 110.7(3) . . ?
F3 B1 F2 110.7(3) . 12 ?
F2 B1 F2 107.6(4) . 12 ?
F3 B1 F1 111.4(4) . . ?
F2 B1 F1 108.2(3) . . ?
F2 B1 F1 108.2(3) 12 . ?
Cl2 C1C Cl1 112.5(5) . . ?
Cl2 C1C H1C1 109.1 . . ?
Cl1 C1C H1C1 109.1 . . ?
Cl2 C1C H1C2 109.1 . . ?
Cl1 C1C H1C2 109.1 . . ?
H1C1 C1C H1C2 107.8 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 N1 C2 0.5(4) 12 . . . ?
P1 C1 N1 C2 174.0(2) . . . . ?
N1 C1 N1 C3 -171.91(17) 12 . . . ?
P1 C1 N1 C3 1.5(4) . . . . ?
C1 N1 C2 C2 -0.3(2) . . . 12 ?
C3 N1 C2 C2 172.0(2) . . . 12 ?
C1 N1 C3 C4 83.7(3) . . . . ?
C2 N1 C3 C4 -87.5(3) . . . . ?
C1 N1 C3 C8 -97.1(3) . . . . ?
C2 N1 C3 C8 91.7(3) . . . . ?
C8 C3 C4 C5 -1.5(4) . . . . ?
N1 C3 C4 C5 177.6(2) . . . . ?
C8 C3 C4 C9 -179.7(3) . . . . ?
N1 C3 C4 C9 -0.5(4) . . . . ?
C3 C4 C5 C6 0.7(4) . . . . ?
C9 C4 C5 C6 178.9(3) . . . . ?
C4 C5 C6 C7 0.6(5) . . . . ?
C5 C6 C7 C8 -1.3(5) . . . . ?
C6 C7 C8 C3 0.5(5) . . . . ?
C6 C7 C8 C12 -178.6(3) . . . . ?
C4 C3 C8 C7 0.9(4) . . . . ?
N1 C3 C8 C7 -178.2(3) . . . . ?
C4 C3 C8 C12 -180.0(3) . . . . ?
N1 C3 C8 C12 0.8(4) . . . . ?
C5 C4 C9 C11 -73.8(4) . . . . ?
C3 C4 C9 C11 104.3(4) . . . . ?
C5 C4 C9 C10 50.3(4) . . . . ?
C3 C4 C9 C10 -131.6(3) . . . . ?
C7 C8 C12 C13 -59.0(4) . . . . ?
C3 C8 C12 C13 121.9(4) . . . . ?
C7 C8 C12 C14 64.4(4) . . . . ?
C3 C8 C12 C14 -114.6(4) . . . . ?

_refine_diff_density_max         1.077
_refine_diff_density_min         -0.976
_refine_diff_density_rms         0.080

####################################################################### 
# 
# 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_g579_mn_1
_database_code_depnum_ccdc_archive 'CCDC 1992156'
loop_
_audit_author_name
_audit_author_address
'Christoph Feil'
;Universitity of Stuttgart
Germany
;
_audit_update_record             
;
2020-03-23 deposited with the CCDC.	2020-11-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H28 N2 P, B F4'
_chemical_formula_sum            'C22 H28 B F4 N2 P'
_chemical_formula_weight         438.24

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'
B B 0.0013 0.0007 '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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   10.6034(5)
_cell_length_b                   27.3731(13)
_cell_length_c                   16.1467(7)
_cell_angle_alpha                90
_cell_angle_beta                 91.181(2)
_cell_angle_gamma                90
_cell_volume                     4685.6(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    135(2)
_cell_measurement_reflns_used    7252
_cell_measurement_theta_min      1.464
_cell_measurement_theta_max      28.334

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.242
_exptl_crystal_F_000             1840
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.639
_exptl_crystal_size_mid          0.503
_exptl_crystal_size_min          0.194
_exptl_absorpt_coefficient_mu    0.159
_shelx_estimated_absorpt_T_min   0.905
_shelx_estimated_absorpt_T_max   0.970
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6995
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   'BLESSING 1995'
_exptl_absorpt_special_details   ?

_diffrn_ambient_temperature      135(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker Kappa ApexII Duo'
_diffrn_measurement_method       'Omega and phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            41082
_diffrn_reflns_av_unetI/netI     0.0525
_diffrn_reflns_av_R_equivalents  0.0377
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.464
_diffrn_reflns_theta_max         28.334
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             11552
_reflns_number_gt                7251
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker ApexII Software Suite, 2008'
_computing_cell_refinement       'Bruker ApexII Software Suite, 2008'
_computing_data_reduction        'Bruker ApexII Software Suite, 2008'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELX plus XP (Sheldrick, 1991)'
_computing_publication_material  ?

_refine_special_details          
;
Both P(H)Me moieties and one BF4 anion disordered, disordered C and F atoms
refined isotropically. Use of constraints (EADP) and restraints (SIMU, SADI)
for the refinement of the disordered moieties. Use of a general RIGU restraint
in the refinement.
A common occupancy factor was calculated for the 3 different disordered moieties
and afterwards fixed to 10.75.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1130P)²+9.5711P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         11552
_refine_ls_number_parameters     562
_refine_ls_number_restraints     721
_refine_ls_R_factor_all          0.1427
_refine_ls_R_factor_gt           0.0944
_refine_ls_wR_factor_ref         0.2697
_refine_ls_wR_factor_gt          0.2370
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.204
_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
C1A C 0.8030(7) 0.1294(3) 0.0362(4) 0.0626(16) Uiso 0.75 1 d D . P A 1
H1A1 H 0.7522 0.1515 0.0015 0.094 Uiso 0.75 1 calc R U P A 1
H1A2 H 0.8915 0.1397 0.0359 0.094 Uiso 0.75 1 calc R U P A 1
H1A3 H 0.7959 0.0960 0.0145 0.094 Uiso 0.75 1 calc R U P A 1
C1B C 0.737(2) 0.1076(7) 0.0384(7) 0.0626(16) Uiso 0.25 1 d D . P A 2
H1B1 H 0.6794 0.1279 0.0049 0.094 Uiso 0.25 1 calc R U P A 2
H1B2 H 0.8212 0.1082 0.0145 0.094 Uiso 0.25 1 calc R U P A 2
H1B3 H 0.7058 0.0739 0.0392 0.094 Uiso 0.25 1 calc R U P A 2
P1 P 0.74565(10) 0.13100(4) 0.14299(7) 0.0413(3) Uani 1 1 d D U . . .
H1PA H 0.650(2) 0.1045(12) 0.135(2) 0.050 Uiso 0.75 1 d D U P B 1
H1PB H 0.817(4) 0.1670(11) 0.135(3) 0.050 Uiso 0.25 1 d D U P C 2
C2 C 0.8562(3) 0.08742(12) 0.1901(2) 0.0296(7) Uani 1 1 d D U . . .
N1 N 0.9705(3) 0.09851(11) 0.22251(17) 0.0314(6) Uani 1 1 d . U . . .
N2 N 0.8372(3) 0.03970(11) 0.20548(18) 0.0330(6) Uani 1 1 d . U . . .
C3 C 1.0228(4) 0.05730(15) 0.2584(3) 0.0431(9) Uani 1 1 d . U . . .
H3 H 1.1031 0.0552 0.2854 0.052 Uiso 1 1 calc R U . . .
C4 C 0.9403(4) 0.02098(15) 0.2483(3) 0.0422(9) Uani 1 1 d . U . . .
H4 H 0.9506 -0.0117 0.2671 0.051 Uiso 1 1 calc R U . . .
C5 C 1.0276(3) 0.14619(13) 0.2235(2) 0.0314(7) Uani 1 1 d . U . . .
C6 C 1.1152(3) 0.15747(13) 0.1628(2) 0.0329(7) Uani 1 1 d . U . . .
C7 C 1.1739(4) 0.20253(14) 0.1687(2) 0.0385(8) Uani 1 1 d . U . . .
H7 H 1.2331 0.2115 0.1280 0.046 Uiso 1 1 calc R U . . .
C8 C 1.1490(4) 0.23498(14) 0.2323(2) 0.0405(9) Uani 1 1 d . U . . .
C9 C 1.0611(4) 0.22234(15) 0.2908(2) 0.0425(9) Uani 1 1 d . U . . .
H9 H 1.0425 0.2448 0.3337 0.051 Uiso 1 1 calc R U . . .
C10 C 0.9995(3) 0.17757(14) 0.2884(2) 0.0365(8) Uani 1 1 d . U . . .
C11 C 0.7230(4) 0.01315(13) 0.1849(2) 0.0379(8) Uani 1 1 d . U . . .
C12 C 0.6237(4) 0.01682(14) 0.2387(3) 0.0423(9) Uani 1 1 d . U . . .
C13 C 0.5129(4) -0.00786(16) 0.2170(4) 0.0593(12) Uani 1 1 d . U . . .
H13 H 0.4423 -0.0057 0.2521 0.071 Uiso 1 1 calc R U . . .
C14 C 0.5039(5) -0.03533(17) 0.1455(4) 0.0721(14) Uani 1 1 d . U . . .
C15 C 0.6057(6) -0.03848(18) 0.0949(4) 0.0724(14) Uani 1 1 d . U . . .
H15 H 0.5987 -0.0578 0.0461 0.087 Uiso 1 1 calc R U . . .
C16 C 0.7186(5) -0.01452(15) 0.1121(3) 0.0546(11) Uani 1 1 d . U . . .
C17 C 1.1484(4) 0.12188(16) 0.0958(2) 0.0460(10) Uani 1 1 d . U . . .
H17A H 1.1947 0.1389 0.0525 0.069 Uiso 1 1 calc R U . . .
H17B H 1.0709 0.1078 0.0718 0.069 Uiso 1 1 calc R U . . .
H17C H 1.2011 0.0958 0.1194 0.069 Uiso 1 1 calc R U . . .
C18 C 1.2205(5) 0.28274(16) 0.2400(3) 0.0582(12) Uani 1 1 d . U . . .
H18A H 1.3037 0.2767 0.2656 0.087 Uiso 1 1 calc R U . . .
H18B H 1.1733 0.3054 0.2747 0.087 Uiso 1 1 calc R U . . .
H18C H 1.2308 0.2970 0.1849 0.087 Uiso 1 1 calc R U . . .
C19 C 0.9080(4) 0.16301(18) 0.3542(3) 0.0516(11) Uani 1 1 d . U . . .
H19A H 0.8235 0.1594 0.3293 0.077 Uiso 1 1 calc R U . . .
H19B H 0.9063 0.1883 0.3972 0.077 Uiso 1 1 calc R U . . .
H19C H 0.9346 0.1319 0.3791 0.077 Uiso 1 1 calc R U . . .
C20 C 0.6336(4) 0.04644(16) 0.3169(3) 0.0482(10) Uani 1 1 d . U . . .
H20A H 0.7122 0.0382 0.3468 0.072 Uiso 1 1 calc R U . . .
H20B H 0.5616 0.0391 0.3519 0.072 Uiso 1 1 calc R U . . .
H20C H 0.6335 0.0813 0.3030 0.072 Uiso 1 1 calc R U . . .
C21 C 0.3814(7) -0.0615(2) 0.1246(6) 0.118(3) Uani 1 1 d . U . . .
H21A H 0.3709 -0.0891 0.1624 0.177 Uiso 1 1 calc R U . . .
H21B H 0.3833 -0.0734 0.0674 0.177 Uiso 1 1 calc R U . . .
H21C H 0.3106 -0.0388 0.1305 0.177 Uiso 1 1 calc R U . . .
C22 C 0.8293(6) -0.0187(2) 0.0572(3) 0.0737(15) Uani 1 1 d . U . . .
H22A H 0.8639 0.0138 0.0469 0.111 Uiso 1 1 calc R U . . .
H22B H 0.8029 -0.0337 0.0045 0.111 Uiso 1 1 calc R U . . .
H22C H 0.8941 -0.0391 0.0842 0.111 Uiso 1 1 calc R U . . .
B1 B 0.4536(4) 0.19179(15) 0.9932(2) 0.0416(10) Uani 1 1 d D U . . .
F1 F 0.5480(3) 0.18486(12) 0.93746(18) 0.0750(9) Uani 1 1 d D U . . .
F2 F 0.3392(3) 0.18514(14) 0.95515(18) 0.0800(10) Uani 1 1 d D U . . .
F3 F 0.4702(3) 0.16071(13) 1.05911(17) 0.0830(10) Uani 1 1 d D U . . .
F4 F 0.4578(4) 0.23943(13) 1.0213(3) 0.1072(13) Uani 1 1 d D U . . .
C23A C 0.3082(7) 0.2493(3) 0.5165(5) 0.0655(17) Uiso 0.75 1 d D . P D 1
H23A H 0.2553 0.2775 0.5019 0.098 Uiso 0.75 1 calc R U P D 1
H23B H 0.3325 0.2510 0.5753 0.098 Uiso 0.75 1 calc R U P D 1
H23C H 0.3841 0.2496 0.4829 0.098 Uiso 0.75 1 calc R U P D 1
P2A P 0.22067(13) 0.19362(5) 0.49692(8) 0.0368(3) Uani 0.75 1 d D U P D 1
H2PA H 0.151(3) 0.1923(14) 0.5588(17) 0.044 Uiso 0.75 1 d D U P E 1
C23B C 0.267(2) 0.2330(7) 0.4377(8) 0.0655(17) Uiso 0.25 1 d D . P D 2
H23D H 0.2431 0.2675 0.4370 0.098 Uiso 0.25 1 calc R U P D 2
H23E H 0.3447 0.2286 0.4064 0.098 Uiso 0.25 1 calc R U P D 2
H23F H 0.1994 0.2134 0.4122 0.098 Uiso 0.25 1 calc R U P D 2
P2B P 0.2936(6) 0.21342(16) 0.5425(3) 0.0582(13) Uani 0.25 1 d D U P D 2
H2PB H 0.402(2) 0.2296(15) 0.559(3) 0.070 Uiso 0.25 1 d D U P F 2
C24 C 0.3377(3) 0.14763(12) 0.52850(19) 0.0277(7) Uani 1 1 d D U . . .
N3 N 0.4391(2) 0.13477(10) 0.48461(16) 0.0259(6) Uani 1 1 d . U . . .
N4 N 0.3255(3) 0.11346(10) 0.58748(16) 0.0278(6) Uani 1 1 d . U . . .
C25 C 0.4899(4) 0.09289(15) 0.5162(2) 0.0418(9) Uani 1 1 d . U . . .
H25 H 0.5619 0.0762 0.4965 0.050 Uiso 1 1 calc R U . . .
C26 C 0.4195(4) 0.07956(15) 0.5804(2) 0.0415(9) Uani 1 1 d . U . . .
H26 H 0.4325 0.0517 0.6146 0.050 Uiso 1 1 calc R U . . .
C27 C 0.4857(3) 0.16243(12) 0.41556(19) 0.0264(6) Uani 1 1 d . U . . .
C28 C 0.4320(3) 0.15457(12) 0.33735(19) 0.0254(6) Uani 1 1 d . U . . .
C29 C 0.4759(3) 0.18321(12) 0.2726(2) 0.0302(7) Uani 1 1 d . U . . .
H29 H 0.4419 0.1782 0.2183 0.036 Uiso 1 1 calc R U . . .
C30 C 0.5673(4) 0.21860(13) 0.2850(2) 0.0337(8) Uani 1 1 d . U . . .
C31 C 0.6192(3) 0.22458(13) 0.3640(2) 0.0355(8) Uani 1 1 d . U . . .
H31 H 0.6824 0.2488 0.3729 0.043 Uiso 1 1 calc R U . . .
C32 C 0.5815(3) 0.19623(14) 0.4305(2) 0.0338(8) Uani 1 1 d . U . . .
C33 C 0.2329(3) 0.11424(13) 0.65218(19) 0.0292(7) Uani 1 1 d . U . . .
C34 C 0.2727(3) 0.13007(13) 0.7302(2) 0.0309(7) Uani 1 1 d . U . . .
C35 C 0.1821(4) 0.13127(14) 0.7920(2) 0.0366(8) Uani 1 1 d . U . . .
H35 H 0.2067 0.1409 0.8466 0.044 Uiso 1 1 calc R U . . .
C36 C 0.0583(4) 0.11878(14) 0.7756(2) 0.0400(9) Uani 1 1 d . U . . .
C37 C 0.0228(4) 0.10358(15) 0.6965(3) 0.0417(9) Uani 1 1 d . U . . .
H37 H -0.0629 0.0954 0.6851 0.050 Uiso 1 1 calc R U . . .
C38 C 0.1105(3) 0.09998(15) 0.6332(2) 0.0383(8) Uani 1 1 d . U . . .
C39 C 0.3307(3) 0.11719(13) 0.3221(2) 0.0324(7) Uani 1 1 d . U . . .
H39A H 0.3468 0.0887 0.3574 0.049 Uiso 1 1 calc R U . . .
H39B H 0.3308 0.1072 0.2638 0.049 Uiso 1 1 calc R U . . .
H39C H 0.2485 0.1313 0.3351 0.049 Uiso 1 1 calc R U . . .
C40 C 0.6106(5) 0.24962(14) 0.2139(3) 0.0464(10) Uani 1 1 d . U . . .
H40A H 0.5852 0.2342 0.1614 0.070 Uiso 1 1 calc R U . . .
H40B H 0.7027 0.2528 0.2167 0.070 Uiso 1 1 calc R U . . .
H40C H 0.5721 0.2821 0.2174 0.070 Uiso 1 1 calc R U . . .
C41 C 0.6428(4) 0.20155(19) 0.5154(2) 0.0538(12) Uani 1 1 d . U . . .
H41A H 0.5789 0.2111 0.5554 0.081 Uiso 1 1 calc R U . . .
H41B H 0.7085 0.2267 0.5137 0.081 Uiso 1 1 calc R U . . .
H41C H 0.6806 0.1703 0.5323 0.081 Uiso 1 1 calc R U . . .
C42 C 0.4046(4) 0.14744(16) 0.7472(2) 0.0427(9) Uani 1 1 d . U . . .
H42A H 0.4641 0.1211 0.7353 0.064 Uiso 1 1 calc R U . . .
H42B H 0.4136 0.1570 0.8055 0.064 Uiso 1 1 calc R U . . .
H42C H 0.4223 0.1756 0.7119 0.064 Uiso 1 1 calc R U . . .
C43 C -0.0386(5) 0.1233(2) 0.8426(3) 0.0606(13) Uani 1 1 d . U . . .
H43A H 0.0025 0.1185 0.8969 0.091 Uiso 1 1 calc R U . . .
H43B H -0.1041 0.0984 0.8340 0.091 Uiso 1 1 calc R U . . .
H43C H -0.0770 0.1558 0.8402 0.091 Uiso 1 1 calc R U . . .
C44 C 0.0719(5) 0.0813(2) 0.5485(3) 0.0649(14) Uani 1 1 d . U . . .
H44A H 0.0690 0.1086 0.5092 0.097 Uiso 1 1 calc R U . . .
H44B H -0.0117 0.0662 0.5511 0.097 Uiso 1 1 calc R U . . .
H44C H 0.1333 0.0571 0.5302 0.097 Uiso 1 1 calc R U . . .
B2 B -0.2607(4) 0.02464(15) 0.5978(3) 0.0599(15) Uani 1 1 d D . . . .
F5A F -0.3734(3) 0.00042(16) 0.5954(2) 0.0519(9) Uiso 0.75 1 d D U P G 1
F6A F -0.2383(4) 0.04452(14) 0.5163(2) 0.0649(9) Uiso 0.75 1 d D U P G 1
F7A F -0.1603(3) -0.00095(14) 0.6199(2) 0.0657(10) Uiso 0.75 1 d D U P G 1
F8A F -0.2802(4) 0.06658(16) 0.6438(3) 0.0831(12) Uiso 0.75 1 d D U P G 1
F5B F -0.2415(9) 0.0314(3) 0.6856(4) 0.0519(9) Uiso 0.25 1 d D U P G 2
F6B F -0.2340(10) 0.0655(3) 0.5599(6) 0.0649(9) Uiso 0.25 1 d D U P G 2
F7B F -0.1761(9) -0.0157(3) 0.5885(7) 0.0657(10) Uiso 0.25 1 d D U P G 2
F8B F -0.3744(9) 0.0027(6) 0.5793(10) 0.0831(12) Uiso 0.25 1 d D U P G 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1A P1 1.840(6) . ?
C1A H1A1 0.9800 . ?
C1A H1A2 0.9800 . ?
C1A H1A3 0.9800 . ?
C1B P1 1.807(10) . ?
C1B H1B1 0.9800 . ?
C1B H1B2 0.9800 . ?
C1B H1B3 0.9800 . ?
P1 C2 1.828(3) . ?
P1 H1PA 1.251(11) . ?
P1 H1PB 1.251(12) . ?
C2 N1 1.344(4) . ?
C2 N2 1.345(4) . ?
N1 C3 1.379(5) . ?
N1 C5 1.439(5) . ?
N2 C4 1.380(5) . ?
N2 C11 1.446(5) . ?
C3 C4 1.331(6) . ?
C3 H3 0.9500 . ?
C4 H4 0.9500 . ?
C5 C10 1.392(5) . ?
C5 C6 1.398(5) . ?
C6 C7 1.385(5) . ?
C6 C17 1.503(5) . ?
C7 C8 1.387(6) . ?
C7 H7 0.9500 . ?
C8 C9 1.385(6) . ?
C8 C18 1.515(6) . ?
C9 C10 1.389(6) . ?
C9 H9 0.9500 . ?
C10 C19 1.508(6) . ?
C11 C12 1.382(6) . ?
C11 C16 1.399(6) . ?
C12 C13 1.394(6) . ?
C12 C20 1.502(6) . ?
C13 C14 1.380(8) . ?
C13 H13 0.9500 . ?
C14 C15 1.370(9) . ?
C14 C21 1.515(7) . ?
C15 C16 1.389(7) . ?
C15 H15 0.9500 . ?
C16 C22 1.489(7) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
B1 F2 1.361(4) . ?
B1 F3 1.371(4) . ?
B1 F1 1.373(4) . ?
B1 F4 1.381(4) . ?
C23A P2A 1.809(7) . ?
C23A H23A 0.9800 . ?
C23A H23B 0.9800 . ?
C23A H23C 0.9800 . ?
P2A C24 1.833(3) . ?
P2A H2PA 1.253(11) . ?
C23B P2B 1.792(10) . ?
C23B H23D 0.9800 . ?
C23B H23E 0.9800 . ?
C23B H23F 0.9800 . ?
P2B C24 1.876(5) . ?
P2B H2PB 1.251(12) . ?
C24 N4 1.343(4) . ?
C24 N3 1.346(4) . ?
N3 C25 1.362(5) . ?
N3 C27 1.444(4) . ?
N4 C26 1.368(5) . ?
N4 C33 1.449(4) . ?
C25 C26 1.340(5) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C27 C32 1.391(5) . ?
C27 C28 1.392(4) . ?
C28 C29 1.395(5) . ?
C28 C39 1.500(5) . ?
C29 C30 1.382(5) . ?
C29 H29 0.9500 . ?
C30 C31 1.388(5) . ?
C30 C40 1.507(5) . ?
C31 C32 1.390(5) . ?
C31 H31 0.9500 . ?
C32 C41 1.513(5) . ?
C33 C38 1.383(5) . ?
C33 C34 1.389(5) . ?
C34 C35 1.400(5) . ?
C34 C42 1.497(5) . ?
C35 C36 1.378(6) . ?
C35 H35 0.9500 . ?
C36 C37 1.387(6) . ?
C36 C43 1.512(5) . ?
C37 C38 1.399(5) . ?
C37 H37 0.9500 . ?
C38 C44 1.508(6) . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
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 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
B2 F6B 1.310(6) . ?
B2 F7A 1.317(5) . ?
B2 F5A 1.367(5) . ?
B2 F8B 1.375(6) . ?
B2 F8A 1.385(5) . ?
B2 F7B 1.432(6) . ?
B2 F5B 1.439(6) . ?
B2 F6A 1.449(5) . ?

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 C1A H1A1 109.5 . . ?
P1 C1A H1A2 109.5 . . ?
H1A1 C1A H1A2 109.5 . . ?
P1 C1A H1A3 109.5 . . ?
H1A1 C1A H1A3 109.5 . . ?
H1A2 C1A H1A3 109.5 . . ?
P1 C1B H1B1 109.5 . . ?
P1 C1B H1B2 109.5 . . ?
H1B1 C1B H1B2 109.5 . . ?
P1 C1B H1B3 109.5 . . ?
H1B1 C1B H1B3 109.5 . . ?
H1B2 C1B H1B3 109.5 . . ?
C1B P1 C2 100.2(6) . . ?
C2 P1 C1A 98.8(2) . . ?
C2 P1 H1PA 100.1(19) . . ?
C1A P1 H1PA 100.0(18) . . ?
C1B P1 H1PB 102(2) . . ?
C2 P1 H1PB 100(2) . . ?
N1 C2 N2 106.5(3) . . ?
N1 C2 P1 125.4(3) . . ?
N2 C2 P1 127.8(3) . . ?
C2 N1 C3 109.3(3) . . ?
C2 N1 C5 125.8(3) . . ?
C3 N1 C5 124.9(3) . . ?
C2 N2 C4 109.4(3) . . ?
C2 N2 C11 125.0(3) . . ?
C4 N2 C11 125.4(3) . . ?
C4 C3 N1 107.6(3) . . ?
C4 C3 H3 126.2 . . ?
N1 C3 H3 126.2 . . ?
C3 C4 N2 107.2(3) . . ?
C3 C4 H4 126.4 . . ?
N2 C4 H4 126.4 . . ?
C10 C5 C6 123.2(3) . . ?
C10 C5 N1 118.1(3) . . ?
C6 C5 N1 118.5(3) . . ?
C7 C6 C5 116.9(3) . . ?
C7 C6 C17 121.0(3) . . ?
C5 C6 C17 122.0(3) . . ?
C6 C7 C8 122.0(4) . . ?
C6 C7 H7 119.0 . . ?
C8 C7 H7 119.0 . . ?
C9 C8 C7 119.1(4) . . ?
C9 C8 C18 120.1(4) . . ?
C7 C8 C18 120.8(4) . . ?
C8 C9 C10 121.6(4) . . ?
C8 C9 H9 119.2 . . ?
C10 C9 H9 119.2 . . ?
C9 C10 C5 117.2(4) . . ?
C9 C10 C19 121.5(4) . . ?
C5 C10 C19 121.2(4) . . ?
C12 C11 C16 123.7(4) . . ?
C12 C11 N2 117.7(3) . . ?
C16 C11 N2 118.6(4) . . ?
C11 C12 C13 117.1(4) . . ?
C11 C12 C20 121.8(3) . . ?
C13 C12 C20 121.1(4) . . ?
C14 C13 C12 121.2(5) . . ?
C14 C13 H13 119.4 . . ?
C12 C13 H13 119.4 . . ?
C15 C14 C13 119.4(5) . . ?
C15 C14 C21 121.3(6) . . ?
C13 C14 C21 119.3(7) . . ?
C14 C15 C16 122.5(5) . . ?
C14 C15 H15 118.7 . . ?
C16 C15 H15 118.7 . . ?
C15 C16 C11 115.9(5) . . ?
C15 C16 C22 122.1(5) . . ?
C11 C16 C22 121.9(4) . . ?
C6 C17 H17A 109.5 . . ?
C6 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C6 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C8 C18 H18A 109.5 . . ?
C8 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C8 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C10 C19 H19A 109.5 . . ?
C10 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C10 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C12 C20 H20A 109.5 . . ?
C12 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C12 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C14 C21 H21A 109.5 . . ?
C14 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C14 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C16 C22 H22A 109.5 . . ?
C16 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C16 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
F2 B1 F3 111.5(3) . . ?
F2 B1 F1 109.9(3) . . ?
F3 B1 F1 109.9(3) . . ?
F2 B1 F4 107.3(3) . . ?
F3 B1 F4 109.2(3) . . ?
F1 B1 F4 109.1(4) . . ?
P2A C23A H23A 109.5 . . ?
P2A C23A H23B 109.5 . . ?
H23A C23A H23B 109.5 . . ?
P2A C23A H23C 109.5 . . ?
H23A C23A H23C 109.5 . . ?
H23B C23A H23C 109.5 . . ?
C23A P2A C24 100.9(3) . . ?
C23A P2A H2PA 101.1(18) . . ?
C24 P2A H2PA 99.4(18) . . ?
P2B C23B H23D 109.5 . . ?
P2B C23B H23E 109.5 . . ?
H23D C23B H23E 109.5 . . ?
P2B C23B H23F 109.5 . . ?
H23D C23B H23F 109.5 . . ?
H23E C23B H23F 109.5 . . ?
C23B P2B C24 101.9(6) . . ?
C23B P2B H2PB 102(2) . . ?
C24 P2B H2PB 98(2) . . ?
N4 C24 N3 106.3(3) . . ?
N4 C24 P2A 127.0(2) . . ?
N3 C24 P2A 125.2(2) . . ?
N4 C24 P2B 123.7(3) . . ?
N3 C24 P2B 121.2(3) . . ?
C24 N3 C25 109.7(3) . . ?
C24 N3 C27 124.0(3) . . ?
C25 N3 C27 126.3(3) . . ?
C24 N4 C26 109.4(3) . . ?
C24 N4 C33 125.3(3) . . ?
C26 N4 C33 125.2(3) . . ?
C26 C25 N3 107.3(3) . . ?
C26 C25 H25 126.4 . . ?
N3 C25 H25 126.4 . . ?
C25 C26 N4 107.4(3) . . ?
C25 C26 H26 126.3 . . ?
N4 C26 H26 126.3 . . ?
C32 C27 C28 122.9(3) . . ?
C32 C27 N3 118.4(3) . . ?
C28 C27 N3 118.6(3) . . ?
C27 C28 C29 117.2(3) . . ?
C27 C28 C39 122.2(3) . . ?
C29 C28 C39 120.6(3) . . ?
C30 C29 C28 121.9(3) . . ?
C30 C29 H29 119.0 . . ?
C28 C29 H29 119.0 . . ?
C29 C30 C31 118.7(3) . . ?
C29 C30 C40 120.5(3) . . ?
C31 C30 C40 120.8(3) . . ?
C30 C31 C32 121.9(3) . . ?
C30 C31 H31 119.1 . . ?
C32 C31 H31 119.1 . . ?
C31 C32 C27 117.3(3) . . ?
C31 C32 C41 121.4(3) . . ?
C27 C32 C41 121.3(3) . . ?
C38 C33 C34 123.7(3) . . ?
C38 C33 N4 118.9(3) . . ?
C34 C33 N4 117.4(3) . . ?
C33 C34 C35 117.0(3) . . ?
C33 C34 C42 122.0(3) . . ?
C35 C34 C42 120.9(3) . . ?
C36 C35 C34 121.4(3) . . ?
C36 C35 H35 119.3 . . ?
C34 C35 H35 119.3 . . ?
C35 C36 C37 119.4(3) . . ?
C35 C36 C43 120.1(4) . . ?
C37 C36 C43 120.5(4) . . ?
C36 C37 C38 121.4(4) . . ?
C36 C37 H37 119.3 . . ?
C38 C37 H37 119.3 . . ?
C33 C38 C37 116.9(3) . . ?
C33 C38 C44 122.1(4) . . ?
C37 C38 C44 120.9(4) . . ?
C28 C39 H39A 109.5 . . ?
C28 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C28 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C30 C40 H40A 109.5 . . ?
C30 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C30 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C32 C41 H41A 109.5 . . ?
C32 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C32 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C34 C42 H42A 109.5 . . ?
C34 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C34 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C36 C43 H43A 109.5 . . ?
C36 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C36 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C38 C44 H44A 109.5 . . ?
C38 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C38 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
F7A B2 F5A 116.8(4) . . ?
F6B B2 F8B 117.9(8) . . ?
F7A B2 F8A 115.2(4) . . ?
F5A B2 F8A 106.1(4) . . ?
F6B B2 F7B 117.9(7) . . ?
F8B B2 F7B 100.8(7) . . ?
F6B B2 F5B 108.8(6) . . ?
F8B B2 F5B 112.2(7) . . ?
F7B B2 F5B 97.3(6) . . ?
F7A B2 F6A 107.4(4) . . ?
F5A B2 F6A 108.4(4) . . ?
F8A B2 F6A 101.8(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1B P1 C2 N1 117.4(8) . . . . ?
C1A P1 C2 N1 87.8(4) . . . . ?
C1B P1 C2 N2 -68.5(8) . . . . ?
C1A P1 C2 N2 -98.1(4) . . . . ?
N2 C2 N1 C3 0.0(4) . . . . ?
P1 C2 N1 C3 175.1(3) . . . . ?
N2 C2 N1 C5 -177.3(3) . . . . ?
P1 C2 N1 C5 -2.1(5) . . . . ?
N1 C2 N2 C4 0.3(4) . . . . ?
P1 C2 N2 C4 -174.7(3) . . . . ?
N1 C2 N2 C11 176.7(3) . . . . ?
P1 C2 N2 C11 1.7(5) . . . . ?
C2 N1 C3 C4 -0.3(4) . . . . ?
C5 N1 C3 C4 177.0(3) . . . . ?
N1 C3 C4 N2 0.5(5) . . . . ?
C2 N2 C4 C3 -0.5(4) . . . . ?
C11 N2 C4 C3 -176.8(4) . . . . ?
C2 N1 C5 C10 86.1(4) . . . . ?
C3 N1 C5 C10 -90.8(4) . . . . ?
C2 N1 C5 C6 -98.3(4) . . . . ?
C3 N1 C5 C6 84.8(4) . . . . ?
C10 C5 C6 C7 -0.8(5) . . . . ?
N1 C5 C6 C7 -176.1(3) . . . . ?
C10 C5 C6 C17 177.0(3) . . . . ?
N1 C5 C6 C17 1.6(5) . . . . ?
C5 C6 C7 C8 0.8(5) . . . . ?
C17 C6 C7 C8 -177.0(4) . . . . ?
C6 C7 C8 C9 -1.1(5) . . . . ?
C6 C7 C8 C18 176.3(4) . . . . ?
C7 C8 C9 C10 1.4(6) . . . . ?
C18 C8 C9 C10 -176.0(4) . . . . ?
C8 C9 C10 C5 -1.4(5) . . . . ?
C8 C9 C10 C19 177.4(4) . . . . ?
C6 C5 C10 C9 1.1(5) . . . . ?
N1 C5 C10 C9 176.4(3) . . . . ?
C6 C5 C10 C19 -177.7(3) . . . . ?
N1 C5 C10 C19 -2.3(5) . . . . ?
C2 N2 C11 C12 -81.9(5) . . . . ?
C4 N2 C11 C12 93.8(4) . . . . ?
C2 N2 C11 C16 97.9(4) . . . . ?
C4 N2 C11 C16 -86.4(5) . . . . ?
C16 C11 C12 C13 -1.5(6) . . . . ?
N2 C11 C12 C13 178.3(3) . . . . ?
C16 C11 C12 C20 179.1(4) . . . . ?
N2 C11 C12 C20 -1.1(5) . . . . ?
C11 C12 C13 C14 1.0(6) . . . . ?
C20 C12 C13 C14 -179.6(4) . . . . ?
C12 C13 C14 C15 0.1(7) . . . . ?
C12 C13 C14 C21 -180.0(5) . . . . ?
C13 C14 C15 C16 -0.7(8) . . . . ?
C21 C14 C15 C16 179.3(5) . . . . ?
C14 C15 C16 C11 0.3(7) . . . . ?
C14 C15 C16 C22 179.1(5) . . . . ?
C12 C11 C16 C15 0.9(6) . . . . ?
N2 C11 C16 C15 -178.9(4) . . . . ?
C12 C11 C16 C22 -178.0(4) . . . . ?
N2 C11 C16 C22 2.3(6) . . . . ?
C23A P2A C24 N4 121.2(4) . . . . ?
C23A P2A C24 N3 -74.9(4) . . . . ?
C23B P2B C24 N4 -156.7(8) . . . . ?
C23B P2B C24 N3 60.2(8) . . . . ?
N4 C24 N3 C25 -0.2(4) . . . . ?
P2A C24 N3 C25 -166.8(3) . . . . ?
P2B C24 N3 C25 148.5(4) . . . . ?
N4 C24 N3 C27 -179.2(3) . . . . ?
P2A C24 N3 C27 14.1(5) . . . . ?
P2B C24 N3 C27 -30.6(5) . . . . ?
N3 C24 N4 C26 0.3(4) . . . . ?
P2A C24 N4 C26 166.6(3) . . . . ?
P2B C24 N4 C26 -147.4(4) . . . . ?
N3 C24 N4 C33 176.2(3) . . . . ?
P2A C24 N4 C33 -17.5(5) . . . . ?
P2B C24 N4 C33 28.6(5) . . . . ?
C24 N3 C25 C26 0.0(5) . . . . ?
C27 N3 C25 C26 179.0(3) . . . . ?
N3 C25 C26 N4 0.2(5) . . . . ?
C24 N4 C26 C25 -0.3(4) . . . . ?
C33 N4 C26 C25 -176.2(3) . . . . ?
C24 N3 C27 C32 94.5(4) . . . . ?
C25 N3 C27 C32 -84.5(4) . . . . ?
C24 N3 C27 C28 -84.8(4) . . . . ?
C25 N3 C27 C28 96.3(4) . . . . ?
C32 C27 C28 C29 -1.6(5) . . . . ?
N3 C27 C28 C29 177.6(3) . . . . ?
C32 C27 C28 C39 178.6(3) . . . . ?
N3 C27 C28 C39 -2.2(5) . . . . ?
C27 C28 C29 C30 -1.1(5) . . . . ?
C39 C28 C29 C30 178.7(3) . . . . ?
C28 C29 C30 C31 2.0(5) . . . . ?
C28 C29 C30 C40 -178.7(3) . . . . ?
C29 C30 C31 C32 -0.3(5) . . . . ?
C40 C30 C31 C32 -179.6(4) . . . . ?
C30 C31 C32 C27 -2.2(5) . . . . ?
C30 C31 C32 C41 177.3(4) . . . . ?
C28 C27 C32 C31 3.2(5) . . . . ?
N3 C27 C32 C31 -176.0(3) . . . . ?
C28 C27 C32 C41 -176.3(4) . . . . ?
N3 C27 C32 C41 4.5(5) . . . . ?
C24 N4 C33 C38 79.0(4) . . . . ?
C26 N4 C33 C38 -105.7(4) . . . . ?
C24 N4 C33 C34 -100.2(4) . . . . ?
C26 N4 C33 C34 75.1(5) . . . . ?
C38 C33 C34 C35 0.1(5) . . . . ?
N4 C33 C34 C35 179.3(3) . . . . ?
C38 C33 C34 C42 -177.1(4) . . . . ?
N4 C33 C34 C42 2.1(5) . . . . ?
C33 C34 C35 C36 -2.0(5) . . . . ?
C42 C34 C35 C36 175.2(4) . . . . ?
C34 C35 C36 C37 1.5(6) . . . . ?
C34 C35 C36 C43 -176.5(4) . . . . ?
C35 C36 C37 C38 0.9(6) . . . . ?
C43 C36 C37 C38 178.9(4) . . . . ?
C34 C33 C38 C37 2.2(6) . . . . ?
N4 C33 C38 C37 -177.0(3) . . . . ?
C34 C33 C38 C44 -177.8(4) . . . . ?
N4 C33 C38 C44 3.0(6) . . . . ?
C36 C37 C38 C33 -2.7(6) . . . . ?
C36 C37 C38 C44 177.3(4) . . . . ?

_refine_diff_density_max         1.173
_refine_diff_density_min         -1.030
_refine_diff_density_rms         0.080


# start Validation Reply Form
_vrf_PLAT201_g579_mn_1           
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......          2 Report
RESPONSE: both P(H)Me moieties and one BF4 anion are disordered.
Disordered C and F atoms refined isotropically.
;
# end Validation Reply Form
####################################################################### 
# 
# 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_g540_mn
_database_code_depnum_ccdc_archive 'CCDC 1992153'
loop_
_audit_author_name
_audit_author_address
'Christoph Feil'
;Universitity of Stuttgart
Germany
;
_audit_update_record             
;
2020-03-23 deposited with the CCDC.	2020-11-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C29 H42 N2 P, B F4'
_chemical_formula_sum            'C29 H42 B F4 N2 P'
_chemical_formula_weight         536.42

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'
B B 0.0013 0.0007 '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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   18.5540(5)
_cell_length_b                   19.0734(6)
_cell_length_c                   8.1713(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2891.72(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    135(2)
_cell_measurement_reflns_used    3607
_cell_measurement_theta_min      2.136
_cell_measurement_theta_max      30.659

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.232
_exptl_crystal_F_000             1144
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.591
_exptl_crystal_size_mid          0.430
_exptl_crystal_size_min          0.422
_exptl_absorpt_coefficient_mu    0.141
_shelx_estimated_absorpt_T_min   0.921
_shelx_estimated_absorpt_T_max   0.943
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7100
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_process_details   'BLESSING 1995'
_exptl_absorpt_special_details   ?

_diffrn_ambient_temperature      135(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker Kappa ApexII Duo'
_diffrn_measurement_method       'Omega and phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            37631
_diffrn_reflns_av_unetI/netI     0.0237
_diffrn_reflns_av_R_equivalents  0.0327
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.136
_diffrn_reflns_theta_max         30.659
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             4562
_reflns_number_gt                3607
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker ApexII Software Suite, 2008'
_computing_cell_refinement       'Bruker ApexII Software Suite, 2008'
_computing_data_reduction        'Bruker ApexII Software Suite, 2008'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_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)+(0.0566P)²+1.3806P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4562
_refine_ls_number_parameters     176
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_gt           0.0430
_refine_ls_wR_factor_ref         0.1223
_refine_ls_wR_factor_gt          0.1100
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_restrained_S_all      1.049
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.64646(2) 0.2500 0.82497(5) 0.01826(11) Uani 1 2 d S T P . .
C1 C 0.71018(9) 0.32222(9) 0.8048(2) 0.0429(4) Uani 1 1 d . . . . .
H1A H 0.6841 0.3669 0.8077 0.064 Uiso 1 1 calc R U . . .
H1B H 0.7359 0.3180 0.7005 0.064 Uiso 1 1 calc R U . . .
H1C H 0.7448 0.3206 0.8952 0.064 Uiso 1 1 calc R U . . .
C2 C 0.60229(8) 0.2500 0.62264(19) 0.0149(3) Uani 1 2 d S T P . .
N1 N 0.57633(5) 0.30655(5) 0.54222(12) 0.01557(19) Uani 1 1 d . . . . .
C3 C 0.53410(6) 0.28525(6) 0.41160(14) 0.0202(2) Uani 1 1 d . . . . .
H3 H 0.5097 0.3149 0.3362 0.024 Uiso 1 1 calc R U . . .
C4 C 0.57975(6) 0.37951(6) 0.59215(14) 0.0168(2) Uani 1 1 d . . . . .
C5 C 0.63116(6) 0.42317(6) 0.51909(15) 0.0187(2) Uani 1 1 d . . . . .
C6 C 0.62956(7) 0.49358(6) 0.56404(16) 0.0235(3) Uani 1 1 d . . . . .
H6 H 0.6639 0.5250 0.5185 0.028 Uiso 1 1 calc R U . . .
C7 C 0.57897(7) 0.51869(7) 0.67378(17) 0.0267(3) Uani 1 1 d . . . . .
H7 H 0.5782 0.5672 0.7005 0.032 Uiso 1 1 calc R U . . .
C8 C 0.52955(7) 0.47378(6) 0.74491(17) 0.0251(3) Uani 1 1 d . . . . .
H8 H 0.4955 0.4917 0.8209 0.030 Uiso 1 1 calc R U . . .
C9 C 0.52893(6) 0.40241(6) 0.70667(14) 0.0191(2) Uani 1 1 d . . . . .
C10 C 0.68637(7) 0.39631(7) 0.39757(16) 0.0238(3) Uani 1 1 d . . . . .
H10 H 0.6908 0.3445 0.4132 0.029 Uiso 1 1 calc R U . . .
C11 C 0.76090(8) 0.42875(8) 0.4242(2) 0.0363(3) Uani 1 1 d . . . . .
H11A H 0.7947 0.4099 0.3431 0.055 Uiso 1 1 calc R U . . .
H11B H 0.7578 0.4798 0.4119 0.055 Uiso 1 1 calc R U . . .
H11C H 0.7780 0.4173 0.5345 0.055 Uiso 1 1 calc R U . . .
C12 C 0.66164(10) 0.40938(10) 0.22190(19) 0.0407(4) Uani 1 1 d . . . . .
H12A H 0.6981 0.3916 0.1457 0.061 Uiso 1 1 calc R U . . .
H12B H 0.6159 0.3851 0.2027 0.061 Uiso 1 1 calc R U . . .
H12C H 0.6551 0.4598 0.2046 0.061 Uiso 1 1 calc R U . . .
C13 C 0.47533(7) 0.35333(6) 0.78730(16) 0.0230(2) Uani 1 1 d . . . . .
H13 H 0.4925 0.3043 0.7684 0.028 Uiso 1 1 calc R U . . .
C14 C 0.40059(8) 0.35941(10) 0.7126(2) 0.0428(4) Uani 1 1 d . . . . .
H14A H 0.4037 0.3523 0.5940 0.064 Uiso 1 1 calc R U . . .
H14B H 0.3690 0.3237 0.7605 0.064 Uiso 1 1 calc R U . . .
H14C H 0.3809 0.4061 0.7351 0.064 Uiso 1 1 calc R U . . .
C15 C 0.47052(11) 0.36436(13) 0.9706(2) 0.0571(6) Uani 1 1 d . . . . .
H15A H 0.4354 0.3316 1.0171 0.086 Uiso 1 1 calc R U . . .
H15B H 0.5179 0.3560 1.0202 0.086 Uiso 1 1 calc R U . . .
H15C H 0.4553 0.4126 0.9932 0.086 Uiso 1 1 calc R U . . .
B1 B 0.32632(12) 0.2500 0.2548(3) 0.0251(4) Uani 1 2 d S T P . .
F1 F 0.31393(8) 0.2500 0.08728(15) 0.0408(3) Uani 1 2 d S T P . .
F2 F 0.26116(8) 0.2500 0.33397(19) 0.0546(4) Uani 1 2 d S T P . .
F3 F 0.36512(6) 0.30912(6) 0.29850(14) 0.0539(3) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1 C1 1.8227(15) 7_565 ?
P1 C1 1.8227(15) . ?
P1 C2 1.8453(16) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 N1 1.3517(13) 7_565 ?
C2 N1 1.3517(13) . ?
N1 C3 1.3851(14) . ?
N1 C4 1.4515(14) . ?
C3 C3 1.345(2) 7_565 ?
C3 H3 0.9500 . ?
C4 C9 1.3984(16) . ?
C4 C5 1.4000(16) . ?
C5 C6 1.3927(16) . ?
C5 C10 1.5159(17) . ?
C6 C7 1.3837(18) . ?
C6 H6 0.9500 . ?
C7 C8 1.3829(19) . ?
C7 H7 0.9500 . ?
C8 C9 1.3966(16) . ?
C8 H8 0.9500 . ?
C9 C13 1.5164(17) . ?
C10 C12 1.528(2) . ?
C10 C11 1.5304(19) . ?
C10 H10 1.0000 . ?
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 C15 1.515(2) . ?
C13 C14 1.520(2) . ?
C13 H13 1.0000 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
B1 F2 1.371(3) . ?
B1 F3 1.3846(15) 7_565 ?
B1 F3 1.3847(15) . ?
B1 F1 1.388(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
C1 P1 C1 98.18(13) 7_565 . ?
C1 P1 C2 101.94(6) 7_565 . ?
C1 P1 C2 101.94(6) . . ?
P1 C1 H1A 109.5 . . ?
P1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
P1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 N1 105.87(13) 7_565 . ?
N1 C2 P1 126.43(7) 7_565 . ?
N1 C2 P1 126.43(7) . . ?
C2 N1 C3 110.01(10) . . ?
C2 N1 C4 127.80(10) . . ?
C3 N1 C4 121.50(9) . . ?
C3 C3 N1 107.05(6) 7_565 . ?
C3 C3 H3 126.5 7_565 . ?
N1 C3 H3 126.5 . . ?
C9 C4 C5 123.98(10) . . ?
C9 C4 N1 117.27(10) . . ?
C5 C4 N1 118.70(10) . . ?
C6 C5 C4 116.53(11) . . ?
C6 C5 C10 120.87(11) . . ?
C4 C5 C10 122.60(10) . . ?
C7 C6 C5 121.27(12) . . ?
C7 C6 H6 119.4 . . ?
C5 C6 H6 119.4 . . ?
C8 C7 C6 120.51(12) . . ?
C8 C7 H7 119.7 . . ?
C6 C7 H7 119.7 . . ?
C7 C8 C9 121.01(12) . . ?
C7 C8 H8 119.5 . . ?
C9 C8 H8 119.5 . . ?
C8 C9 C4 116.66(11) . . ?
C8 C9 C13 120.66(11) . . ?
C4 C9 C13 122.69(10) . . ?
C5 C10 C12 110.94(11) . . ?
C5 C10 C11 112.39(11) . . ?
C12 C10 C11 109.81(12) . . ?
C5 C10 H10 107.8 . . ?
C12 C10 H10 107.8 . . ?
C11 C10 H10 107.8 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C15 C13 C9 112.49(12) . . ?
C15 C13 C14 109.44(13) . . ?
C9 C13 C14 112.14(11) . . ?
C15 C13 H13 107.5 . . ?
C9 C13 H13 107.5 . . ?
C14 C13 H13 107.5 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
F2 B1 F3 109.68(12) . 7_565 ?
F2 B1 F3 109.68(12) . . ?
F3 B1 F3 109.05(17) 7_565 . ?
F2 B1 F1 108.62(17) . . ?
F3 B1 F1 109.90(12) 7_565 . ?
F3 B1 F1 109.90(12) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 P1 C2 N1 46.80(15) 7_565 . . 7_565 ?
C1 P1 C2 N1 147.95(13) . . . 7_565 ?
C1 P1 C2 N1 -147.95(13) 7_565 . . . ?
C1 P1 C2 N1 -46.80(15) . . . . ?
N1 C2 N1 C3 0.05(16) 7_565 . . . ?
P1 C2 N1 C3 -167.66(10) . . . . ?
N1 C2 N1 C4 170.46(7) 7_565 . . . ?
P1 C2 N1 C4 2.8(2) . . . . ?
C2 N1 C3 C3 -0.03(10) . . . 7_565 ?
C4 N1 C3 C3 -171.15(8) . . . 7_565 ?
C2 N1 C4 C9 -80.44(15) . . . . ?
C3 N1 C4 C9 88.98(13) . . . . ?
C2 N1 C4 C5 102.07(15) . . . . ?
C3 N1 C4 C5 -88.51(13) . . . . ?
C9 C4 C5 C6 -0.92(18) . . . . ?
N1 C4 C5 C6 176.39(10) . . . . ?
C9 C4 C5 C10 178.86(11) . . . . ?
N1 C4 C5 C10 -3.83(17) . . . . ?
C4 C5 C6 C7 -0.78(19) . . . . ?
C10 C5 C6 C7 179.43(12) . . . . ?
C5 C6 C7 C8 1.6(2) . . . . ?
C6 C7 C8 C9 -0.7(2) . . . . ?
C7 C8 C9 C4 -0.90(19) . . . . ?
C7 C8 C9 C13 179.01(12) . . . . ?
C5 C4 C9 C8 1.74(18) . . . . ?
N1 C4 C9 C8 -175.60(10) . . . . ?
C5 C4 C9 C13 -178.17(11) . . . . ?
N1 C4 C9 C13 4.49(17) . . . . ?
C6 C5 C10 C12 -82.88(15) . . . . ?
C4 C5 C10 C12 97.34(15) . . . . ?
C6 C5 C10 C11 40.50(17) . . . . ?
C4 C5 C10 C11 -139.28(12) . . . . ?
C8 C9 C13 C15 -46.13(18) . . . . ?
C4 C9 C13 C15 133.78(15) . . . . ?
C8 C9 C13 C14 77.74(16) . . . . ?
C4 C9 C13 C14 -102.35(15) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C1 H1C F2 0.98 2.61 3.392(2) 137.1 6_657

_refine_diff_density_max         0.390
_refine_diff_density_min         -0.403
_refine_diff_density_rms         0.057

####################################################################### 
# 
# 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_g481_mn_sq
_database_code_depnum_ccdc_archive 'CCDC 1992155'
loop_
_audit_author_name
_audit_author_address
'Christoph Feil'
;Universitity of Stuttgart
Germany
;
_audit_update_record             
;
2020-03-23 deposited with the CCDC.	2020-11-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C27 H38 N2 P, I, 0.5 (C2 H3 N), 0.5 (H2 O)'
_chemical_formula_sum            'C28 H40.50 I N2.50 O0.50 P'
_chemical_formula_weight         578.00

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'
I I -0.4742 1.8119 '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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_H-M_alt        'F d d 2'
_space_group_name_Hall           'F 2 -2d'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'x+1/4, -y+1/4, z+1/4'
'-x+1/4, y+1/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'x+1/4, -y+3/4, z+3/4'
'-x+1/4, y+3/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'x+3/4, -y+1/4, z+3/4'
'-x+3/4, y+1/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'x+3/4, -y+3/4, z+1/4'
'-x+3/4, y+3/4, z+1/4'

_cell_length_a                   30.490(2)
_cell_length_b                   32.625(2)
_cell_length_c                   12.8127(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     12745.1(14)
_cell_formula_units_Z            16
_cell_measurement_temperature    130(2)
_cell_measurement_reflns_used    7381
_cell_measurement_theta_min      1.834
_cell_measurement_theta_max      28.308

_exptl_crystal_description       prism
_exptl_crystal_colour            light-yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.205
_exptl_crystal_F_000             4768
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.376
_exptl_crystal_size_mid          0.146
_exptl_crystal_size_min          0.130
_exptl_absorpt_coefficient_mu    1.074
_shelx_estimated_absorpt_T_min   0.688
_shelx_estimated_absorpt_T_max   0.873
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6459
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   'BLESSING 1995'
_exptl_absorpt_special_details   ?

_diffrn_ambient_temperature      130(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker Kappa ApexII Duo'
_diffrn_measurement_method       'Omega and phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            63973
_diffrn_reflns_av_unetI/netI     0.0185
_diffrn_reflns_av_R_equivalents  0.0264
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.834
_diffrn_reflns_theta_max         28.308
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             7918
_reflns_number_gt                7380
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.917
_reflns_Friedel_fraction_max     0.998
_reflns_Friedel_fraction_full    0.999

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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       'Bruker ApexII Software Suite, 2008'
_computing_cell_refinement       'Bruker ApexII Software Suite, 2008'
_computing_data_reduction        'Bruker ApexII Software Suite, 2008'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXS plus XP (Sheldrick, 1991)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'

_refine_special_details          
;
One iPr group disordered and the I-anion disordered. Use of restraints
(ASDI) and constrtaints (EADP) for the refinement of the disordered 
iPr-moiety. Use of general RIGU restraint.

Refinement with the listed atoms show residual electron density in 8 voids due to
a heavily disordered acetonitril and water solvent (one CH3CN and one H2O per void)
which could not be refined with split atoms.
Therefore the option "SQUEEZE" of the program package PLATON
(Spek, A.L. (2009). Acta Cryst. D65, 148-155. Spek, A.L. (2015). Acta Cryst. C71, 9-18.) 
was used to create a hkl file taking into account the residual electron density
in the void areas.
Therefore the atoms list and unit card do not agree.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1376P)²+31.7700P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 3308 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.053(6)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         7918
_refine_ls_number_parameters     287
_refine_ls_number_restraints     236
_refine_ls_R_factor_all          0.0688
_refine_ls_R_factor_gt           0.0647
_refine_ls_wR_factor_ref         0.1944
_refine_ls_wR_factor_gt          0.1886
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_restrained_S_all      1.109
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.76043(7) 0.46611(6) 0.62983(17) 0.0484(4) Uani 1 1 d . U . . .
H1P H 0.7544 0.4759 0.5366 0.073 Uiso 1 1 d R U . . .
H2P H 0.7857 0.4379 0.6027 0.073 Uiso 1 1 d R U . . .
C1 C 0.7119(2) 0.43236(19) 0.6341(5) 0.0359(11) Uani 1 1 d . U . . .
N1 N 0.67439(18) 0.44008(18) 0.5817(4) 0.0400(11) Uani 1 1 d . U . . .
N2 N 0.70666(18) 0.39819(16) 0.6863(4) 0.0365(10) Uani 1 1 d . U . . .
C2 C 0.6456(2) 0.4087(2) 0.5996(5) 0.0423(13) Uani 1 1 d . U . . .
H2 H 0.6171 0.4061 0.5702 0.051 Uiso 1 1 calc R U . . .
C3 C 0.6647(2) 0.3823(2) 0.6664(5) 0.0415(13) Uani 1 1 d . U . . .
H3 H 0.6524 0.3579 0.6942 0.050 Uiso 1 1 calc R U . . .
C4 C 0.6674(2) 0.4742(2) 0.5102(6) 0.0451(14) Uani 1 1 d . U . . .
C5 C 0.6549(3) 0.5130(3) 0.5536(7) 0.0531(16) Uani 1 1 d . U . . .
C6 C 0.6471(3) 0.5436(3) 0.4815(8) 0.062(2) Uani 1 1 d . U . . .
H6 H 0.6381 0.5698 0.5056 0.074 Uiso 1 1 calc R U . . .
C7 C 0.6520(3) 0.5375(3) 0.3773(8) 0.063(2) Uani 1 1 d . U . . .
H7 H 0.6471 0.5596 0.3305 0.076 Uiso 1 1 calc R U . . .
C8 C 0.6638(3) 0.5001(3) 0.3388(7) 0.0595(18) Uani 1 1 d . U . . .
H8 H 0.6661 0.4965 0.2654 0.071 Uiso 1 1 calc R U . . .
C9 C 0.6726(3) 0.4668(3) 0.4050(6) 0.0496(15) Uani 1 1 d . U . . .
C10 C 0.7392(2) 0.3787(2) 0.7520(5) 0.0380(12) Uani 1 1 d . U . . .
C11 C 0.7374(3) 0.3854(2) 0.8578(6) 0.0483(15) Uani 1 1 d D U . . .
C12 C 0.7700(3) 0.3664(3) 0.9194(8) 0.063(2) Uani 1 1 d . U . . .
H12 H 0.7703 0.3700 0.9929 0.076 Uiso 1 1 calc R U . . .
C13 C 0.8020(3) 0.3420(3) 0.8707(9) 0.064(2) Uani 1 1 d . U . . .
H13 H 0.8242 0.3295 0.9119 0.077 Uiso 1 1 calc R U . . .
C14 C 0.8019(3) 0.3360(3) 0.7646(9) 0.063(2) Uani 1 1 d . U . . .
H14 H 0.8237 0.3190 0.7341 0.076 Uiso 1 1 calc R U . . .
C15 C 0.7710(2) 0.3538(2) 0.7020(7) 0.0480(15) Uani 1 1 d . U . . .
C16 C 0.6464(4) 0.5176(3) 0.6687(8) 0.069(2) Uani 1 1 d . U . . .
H16 H 0.6670 0.4990 0.7062 0.083 Uiso 1 1 calc R U . . .
C17 C 0.6020(5) 0.5066(5) 0.6999(13) 0.105(4) Uani 1 1 d . U . . .
H17A H 0.5988 0.5103 0.7754 0.157 Uiso 1 1 calc R U . . .
H17B H 0.5809 0.5241 0.6634 0.157 Uiso 1 1 calc R U . . .
H17C H 0.5965 0.4778 0.6819 0.157 Uiso 1 1 calc R U . . .
C18 C 0.6570(5) 0.5624(3) 0.7035(10) 0.081(3) Uani 1 1 d . U . . .
H18A H 0.6869 0.5695 0.6820 0.122 Uiso 1 1 calc R U . . .
H18B H 0.6362 0.5814 0.6707 0.122 Uiso 1 1 calc R U . . .
H18C H 0.6546 0.5645 0.7795 0.122 Uiso 1 1 calc R U . . .
C19 C 0.6883(3) 0.4259(3) 0.3625(6) 0.0561(17) Uani 1 1 d . U . . .
H19 H 0.6916 0.4065 0.4223 0.067 Uiso 1 1 calc R U . . .
C20 C 0.6533(4) 0.4081(4) 0.2866(9) 0.084(3) Uani 1 1 d . U . . .
H20A H 0.6251 0.4057 0.3229 0.126 Uiso 1 1 calc R U . . .
H20B H 0.6500 0.4265 0.2265 0.126 Uiso 1 1 calc R U . . .
H20C H 0.6627 0.3810 0.2625 0.126 Uiso 1 1 calc R U . . .
C21 C 0.7317(3) 0.4300(3) 0.3097(8) 0.064(2) Uani 1 1 d . U . . .
H21A H 0.7410 0.4032 0.2831 0.096 Uiso 1 1 calc R U . . .
H21B H 0.7292 0.4494 0.2516 0.096 Uiso 1 1 calc R U . . .
H21C H 0.7534 0.4401 0.3599 0.096 Uiso 1 1 calc R U . . .
C22 C 0.7032(3) 0.4127(3) 0.9081(6) 0.0564(18) Uani 1 1 d D U . . .
H22A H 0.6845 0.4257 0.8532 0.068 Uiso 0.54(2) 1 calc R U P A 1
H22B H 0.6794 0.4146 0.8546 0.068 Uiso 0.46(2) 1 calc R U P A 2
C23A C 0.7281(6) 0.4466(6) 0.9716(17) 0.074(4) Uiso 0.54(2) 1 d D . P A 1
H23A H 0.7067 0.4648 1.0051 0.112 Uiso 0.54(2) 1 calc R U P A 1
H23B H 0.7464 0.4336 1.0251 0.112 Uiso 0.54(2) 1 calc R U P A 1
H23C H 0.7467 0.4626 0.9243 0.112 Uiso 0.54(2) 1 calc R U P A 1
C24A C 0.6743(7) 0.3839(7) 0.980(2) 0.087(5) Uiso 0.54(2) 1 d D . P A 1
H24A H 0.6516 0.4002 1.0148 0.130 Uiso 0.54(2) 1 calc R U P A 1
H24B H 0.6605 0.3626 0.9375 0.130 Uiso 0.54(2) 1 calc R U P A 1
H24C H 0.6930 0.3710 1.0331 0.130 Uiso 0.54(2) 1 calc R U P A 1
C23B C 0.7215(8) 0.4576(5) 0.915(2) 0.074(4) Uiso 0.46(2) 1 d D . P A 2
H23D H 0.6995 0.4754 0.9479 0.112 Uiso 0.46(2) 1 calc R U P A 2
H23E H 0.7483 0.4577 0.9578 0.112 Uiso 0.46(2) 1 calc R U P A 2
H23F H 0.7282 0.4677 0.8452 0.112 Uiso 0.46(2) 1 calc R U P A 2
C24B C 0.6804(9) 0.3944(9) 1.0046(18) 0.087(5) Uiso 0.46(2) 1 d D . P A 2
H24D H 0.6589 0.4140 1.0318 0.130 Uiso 0.46(2) 1 calc R U P A 2
H24E H 0.6653 0.3689 0.9848 0.130 Uiso 0.46(2) 1 calc R U P A 2
H24F H 0.7023 0.3884 1.0584 0.130 Uiso 0.46(2) 1 calc R U P A 2
C25 C 0.7703(3) 0.3465(3) 0.5855(8) 0.0598(19) Uani 1 1 d . U . . .
H25 H 0.7489 0.3661 0.5536 0.072 Uiso 1 1 calc R U . . .
C26 C 0.8152(4) 0.3539(4) 0.5357(11) 0.083(3) Uani 1 1 d . U . . .
H26A H 0.8133 0.3489 0.4604 0.125 Uiso 1 1 calc R U . . .
H26B H 0.8242 0.3824 0.5481 0.125 Uiso 1 1 calc R U . . .
H26C H 0.8368 0.3353 0.5666 0.125 Uiso 1 1 calc R U . . .
C27 C 0.7543(4) 0.3025(4) 0.5638(10) 0.081(3) Uani 1 1 d . U . . .
H27A H 0.7538 0.2976 0.4883 0.122 Uiso 1 1 calc R U . . .
H27B H 0.7742 0.2829 0.5970 0.122 Uiso 1 1 calc R U . . .
H27C H 0.7247 0.2990 0.5922 0.122 Uiso 1 1 calc R U . . .
I1A I 0.63059(2) 0.27414(2) 0.79042(5) 0.0452(2) Uani 0.6781(19) 1 d . . P B 1
I1B I 0.53555(5) 0.43609(4) 0.46670(12) 0.0488(5) Uani 0.3219(19) 1 d . . P B 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1 C1 1.845(7) . ?
P1 H1P 1.2500 . ?
P1 H2P 1.2500 . ?
C1 N2 1.310(8) . ?
C1 N1 1.350(8) . ?
N1 C2 1.369(9) . ?
N1 C4 1.458(9) . ?
N2 C3 1.404(8) . ?
N2 C10 1.448(8) . ?
C2 C3 1.348(10) . ?
C2 H2 0.9500 . ?
C3 H3 0.9500 . ?
C4 C9 1.379(11) . ?
C4 C5 1.434(11) . ?
C5 C6 1.379(12) . ?
C5 C16 1.504(13) . ?
C6 C7 1.358(14) . ?
C6 H6 0.9500 . ?
C7 C8 1.364(15) . ?
C7 H7 0.9500 . ?
C8 C9 1.406(11) . ?
C8 H8 0.9500 . ?
C9 C19 1.518(13) . ?
C10 C11 1.375(10) . ?
C10 C15 1.420(10) . ?
C11 C12 1.413(11) . ?
C11 C22 1.515(12) . ?
C12 C13 1.405(15) . ?
C12 H12 0.9500 . ?
C13 C14 1.374(16) . ?
C13 H13 0.9500 . ?
C14 C15 1.365(12) . ?
C14 H14 0.9500 . ?
C15 C25 1.512(13) . ?
C16 C17 1.455(19) . ?
C16 C18 1.562(16) . ?
C16 H16 1.0000 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 C21 1.493(13) . ?
C19 C20 1.555(12) . ?
C19 H19 1.0000 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C24B 1.541(14) . ?
C22 C23A 1.568(14) . ?
C22 C23B 1.570(14) . ?
C22 C24A 1.587(14) . ?
C22 H22A 1.0000 . ?
C22 H22B 1.0000 . ?
C23A H23A 0.9800 . ?
C23A H23B 0.9800 . ?
C23A H23C 0.9800 . ?
C24A H24A 0.9800 . ?
C24A H24B 0.9800 . ?
C24A H24C 0.9800 . ?
C23B H23D 0.9800 . ?
C23B H23E 0.9800 . ?
C23B H23F 0.9800 . ?
C24B H24D 0.9800 . ?
C24B H24E 0.9800 . ?
C24B H24F 0.9800 . ?
C25 C26 1.528(13) . ?
C25 C27 1.542(13) . ?
C25 H25 1.0000 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 P1 H1P 93.5 . . ?
C1 P1 H2P 93.6 . . ?
H1P P1 H2P 90.8 . . ?
N2 C1 N1 108.0(6) . . ?
N2 C1 P1 128.4(5) . . ?
N1 C1 P1 123.6(5) . . ?
C1 N1 C2 108.7(5) . . ?
C1 N1 C4 125.4(6) . . ?
C2 N1 C4 125.7(6) . . ?
C1 N2 C3 109.5(6) . . ?
C1 N2 C10 126.0(6) . . ?
C3 N2 C10 124.5(5) . . ?
C3 C2 N1 107.9(6) . . ?
C3 C2 H2 126.1 . . ?
N1 C2 H2 126.1 . . ?
C2 C3 N2 105.8(6) . . ?
C2 C3 H3 127.1 . . ?
N2 C3 H3 127.1 . . ?
C9 C4 C5 124.5(7) . . ?
C9 C4 N1 117.5(7) . . ?
C5 C4 N1 118.0(6) . . ?
C6 C5 C4 115.0(8) . . ?
C6 C5 C16 123.7(8) . . ?
C4 C5 C16 120.9(7) . . ?
C7 C6 C5 122.4(9) . . ?
C7 C6 H6 118.8 . . ?
C5 C6 H6 118.8 . . ?
C6 C7 C8 120.9(9) . . ?
C6 C7 H7 119.5 . . ?
C8 C7 H7 119.5 . . ?
C7 C8 C9 121.6(8) . . ?
C7 C8 H8 119.2 . . ?
C9 C8 H8 119.2 . . ?
C4 C9 C8 115.5(8) . . ?
C4 C9 C19 122.9(7) . . ?
C8 C9 C19 121.5(7) . . ?
C11 C10 C15 124.3(7) . . ?
C11 C10 N2 118.4(6) . . ?
C15 C10 N2 117.3(6) . . ?
C10 C11 C12 116.9(8) . . ?
C10 C11 C22 122.7(7) . . ?
C12 C11 C22 120.4(8) . . ?
C13 C12 C11 119.4(9) . . ?
C13 C12 H12 120.3 . . ?
C11 C12 H12 120.3 . . ?
C14 C13 C12 121.1(8) . . ?
C14 C13 H13 119.4 . . ?
C12 C13 H13 119.4 . . ?
C15 C14 C13 121.6(9) . . ?
C15 C14 H14 119.2 . . ?
C13 C14 H14 119.2 . . ?
C14 C15 C10 116.7(8) . . ?
C14 C15 C25 121.6(8) . . ?
C10 C15 C25 121.7(7) . . ?
C17 C16 C5 113.9(12) . . ?
C17 C16 C18 110.3(10) . . ?
C5 C16 C18 109.7(9) . . ?
C17 C16 H16 107.6 . . ?
C5 C16 H16 107.6 . . ?
C18 C16 H16 107.6 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C21 C19 C9 111.3(7) . . ?
C21 C19 C20 111.0(8) . . ?
C9 C19 C20 109.7(9) . . ?
C21 C19 H19 108.3 . . ?
C9 C19 H19 108.3 . . ?
C20 C19 H19 108.3 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C11 C22 C24B 115.0(11) . . ?
C11 C22 C23A 107.6(9) . . ?
C11 C22 C23B 109.2(9) . . ?
C24B C22 C23B 118.4(15) . . ?
C11 C22 C24A 106.3(10) . . ?
C23A C22 C24A 112.6(14) . . ?
C11 C22 H22A 110.1 . . ?
C23A C22 H22A 110.1 . . ?
C24A C22 H22A 110.1 . . ?
C11 C22 H22B 104.1 . . ?
C24B C22 H22B 104.1 . . ?
C23B C22 H22B 104.1 . . ?
C22 C23A H23A 109.5 . . ?
C22 C23A H23B 109.5 . . ?
H23A C23A H23B 109.5 . . ?
C22 C23A H23C 109.5 . . ?
H23A C23A H23C 109.5 . . ?
H23B C23A H23C 109.5 . . ?
C22 C24A H24A 109.5 . . ?
C22 C24A H24B 109.5 . . ?
H24A C24A H24B 109.5 . . ?
C22 C24A H24C 109.5 . . ?
H24A C24A H24C 109.5 . . ?
H24B C24A H24C 109.5 . . ?
C22 C23B H23D 109.5 . . ?
C22 C23B H23E 109.5 . . ?
H23D C23B H23E 109.5 . . ?
C22 C23B H23F 109.5 . . ?
H23D C23B H23F 109.5 . . ?
H23E C23B H23F 109.5 . . ?
C22 C24B H24D 109.5 . . ?
C22 C24B H24E 109.5 . . ?
H24D C24B H24E 109.5 . . ?
C22 C24B H24F 109.5 . . ?
H24D C24B H24F 109.5 . . ?
H24E C24B H24F 109.5 . . ?
C15 C25 C26 112.0(9) . . ?
C15 C25 C27 109.1(8) . . ?
C26 C25 C27 110.9(8) . . ?
C15 C25 H25 108.2 . . ?
C26 C25 H25 108.2 . . ?
C27 C25 H25 108.2 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 C1 N1 C2 -2.1(7) . . . . ?
P1 C1 N1 C2 178.5(5) . . . . ?
N2 C1 N1 C4 -176.9(6) . . . . ?
P1 C1 N1 C4 3.7(9) . . . . ?
N1 C1 N2 C3 1.2(7) . . . . ?
P1 C1 N2 C3 -179.5(5) . . . . ?
N1 C1 N2 C10 179.3(6) . . . . ?
P1 C1 N2 C10 -1.4(9) . . . . ?
C1 N1 C2 C3 2.2(8) . . . . ?
C4 N1 C2 C3 177.0(6) . . . . ?
N1 C2 C3 N2 -1.4(8) . . . . ?
C1 N2 C3 C2 0.2(7) . . . . ?
C10 N2 C3 C2 -178.0(6) . . . . ?
C1 N1 C4 C9 97.1(9) . . . . ?
C2 N1 C4 C9 -76.9(9) . . . . ?
C1 N1 C4 C5 -84.0(9) . . . . ?
C2 N1 C4 C5 102.1(8) . . . . ?
C9 C4 C5 C6 1.3(12) . . . . ?
N1 C4 C5 C6 -177.6(7) . . . . ?
C9 C4 C5 C16 174.9(9) . . . . ?
N1 C4 C5 C16 -3.9(12) . . . . ?
C4 C5 C6 C7 -1.4(14) . . . . ?
C16 C5 C6 C7 -174.9(10) . . . . ?
C5 C6 C7 C8 1.7(15) . . . . ?
C6 C7 C8 C9 -1.8(14) . . . . ?
C5 C4 C9 C8 -1.3(12) . . . . ?
N1 C4 C9 C8 177.5(6) . . . . ?
C5 C4 C9 C19 176.6(7) . . . . ?
N1 C4 C9 C19 -4.6(11) . . . . ?
C7 C8 C9 C4 1.6(12) . . . . ?
C7 C8 C9 C19 -176.4(8) . . . . ?
C1 N2 C10 C11 97.4(8) . . . . ?
C3 N2 C10 C11 -84.7(8) . . . . ?
C1 N2 C10 C15 -82.3(8) . . . . ?
C3 N2 C10 C15 95.5(8) . . . . ?
C15 C10 C11 C12 0.6(11) . . . . ?
N2 C10 C11 C12 -179.1(7) . . . . ?
C15 C10 C11 C22 179.1(6) . . . . ?
N2 C10 C11 C22 -0.7(10) . . . . ?
C10 C11 C12 C13 0.1(12) . . . . ?
C22 C11 C12 C13 -178.3(7) . . . . ?
C11 C12 C13 C14 -0.9(14) . . . . ?
C12 C13 C14 C15 0.9(15) . . . . ?
C13 C14 C15 C10 -0.1(13) . . . . ?
C13 C14 C15 C25 -178.9(9) . . . . ?
C11 C10 C15 C14 -0.6(11) . . . . ?
N2 C10 C15 C14 179.1(7) . . . . ?
C11 C10 C15 C25 178.1(7) . . . . ?
N2 C10 C15 C25 -2.2(10) . . . . ?
C6 C5 C16 C17 88.5(14) . . . . ?
C4 C5 C16 C17 -84.6(12) . . . . ?
C6 C5 C16 C18 -35.7(14) . . . . ?
C4 C5 C16 C18 151.2(9) . . . . ?
C4 C9 C19 C21 -115.0(9) . . . . ?
C8 C9 C19 C21 62.8(10) . . . . ?
C4 C9 C19 C20 121.7(9) . . . . ?
C8 C9 C19 C20 -60.5(10) . . . . ?
C10 C11 C22 C24B 132.8(16) . . . . ?
C12 C11 C22 C24B -48.8(17) . . . . ?
C10 C11 C22 C23A -123.5(12) . . . . ?
C12 C11 C22 C23A 54.9(13) . . . . ?
C10 C11 C22 C23B -91.2(14) . . . . ?
C12 C11 C22 C23B 87.2(14) . . . . ?
C10 C11 C22 C24A 115.7(14) . . . . ?
C12 C11 C22 C24A -65.9(14) . . . . ?
C14 C15 C25 C26 -50.8(12) . . . . ?
C10 C15 C25 C26 130.6(9) . . . . ?
C14 C15 C25 C27 72.4(11) . . . . ?
C10 C15 C25 C27 -106.2(9) . . . . ?

_refine_diff_density_max         1.555
_refine_diff_density_min         -0.821
_refine_diff_density_rms         0.136



# SQUEEZE RESULTS (Version =  30118)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.217 104 29 'CH3CN, H2O'
2 0.000 0.500 0.717 104 29 'CH3CN, H2O'
3 0.250 0.250 0.467 104 29 'CH3CN, H2O'
4 0.250 0.750 -0.033 104 29 'CH3CN, H2O'
5 0.500 0.000 0.717 104 29 'CH3CN, H2O'
6 0.500 0.500 0.217 104 29 'CH3CN, H2O'
7 0.750 0.250 -0.033 104 29 'CH3CN, H2O'
8 0.750 0.750 0.467 104 29 'CH3CN, H2O'
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?

# start Validation Reply Form
_vrf_PLAT201_g481_mn_sq          
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PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......          2 Report
RESPONSE: one iPr disordered, disordered atoms refined isotropically.
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# end Validation Reply Form
