# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_mo_SK_15_0m
_database_code_depnum_ccdc_archive 'CCDC 1543526'
_audit_update_record             
;
2017-04-11 deposited with the CCDC.
2017-10-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H49 B N P'
_chemical_formula_sum            'C36 H49 B N P'
_chemical_formula_weight         537.54

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'
B B 0.0013 0.0007 '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                   17.885(9)
_cell_length_b                   10.312(5)
_cell_length_c                   19.369(10)
_cell_angle_alpha                90
_cell_angle_beta                 115.481(11)
_cell_angle_gamma                90
_cell_volume                     3225(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    7920
_cell_measurement_theta_min      2.293
_cell_measurement_theta_max      25.85

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.107
_exptl_crystal_F_000             1168
_exptl_transmission_factor_min   0.6300
_exptl_transmission_factor_max   0.7453
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.109
_shelx_estimated_absorpt_T_min   0.989
_shelx_estimated_absorpt_T_max   0.989
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   
'Sheldrick, G. M. (2012) SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker SMART X2S benchtop diffractometer'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            27848
_diffrn_reflns_av_unetI/netI     0.0511
_diffrn_reflns_av_R_equivalents  0.0646
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.052
_diffrn_reflns_theta_max         26.078
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             6302
_reflns_number_gt                5072
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_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)+(0.0501P)²+0.8495P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6302
_refine_ls_number_parameters     356
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0546
_refine_ls_R_factor_gt           0.0413
_refine_ls_wR_factor_ref         0.1119
_refine_ls_wR_factor_gt          0.1033
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_restrained_S_all      1.022
_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 -0.06904(2) 0.84288(4) 0.75690(2) 0.02178(11) Uani 1 1 d . . . . .
N1 N -0.00147(7) 0.94838(11) 0.73930(6) 0.0184(3) Uani 1 1 d . . . . .
C1 C -0.14422(9) 0.94397(14) 0.77418(9) 0.0254(3) Uani 1 1 d . . . . .
C2 C -0.29119(11) 0.98678(18) 0.73401(12) 0.0424(5) Uani 1 1 d . . . . .
H43 H -0.3461 0.9716 0.7002 0.051 Uiso 1 1 calc R U . . .
C3 C -0.19010(12) 1.09604(17) 0.84435(11) 0.0393(4) Uani 1 1 d . . . . .
H44 H -0.1777 1.1545 0.8843 0.047 Uiso 1 1 calc R U . . .
C4 C 0.27117(10) 0.97154(17) 0.66391(10) 0.0323(4) Uani 1 1 d . . . . .
H35 H 0.3233 1.0087 0.6695 0.039 Uiso 1 1 calc R U . . .
H1 H 0.2604 0.8950 0.6320 0.039 Uiso 1 1 calc R U . . .
C5 C 0.27761(10) 0.93307(18) 0.74300(10) 0.0344(4) Uani 1 1 d . . . . .
H40 H 0.2940 1.0081 0.7765 0.041 Uiso 1 1 calc R U . . .
H34 H 0.3200 0.8671 0.7652 0.041 Uiso 1 1 calc R U . . .
C6 C 0.19441(9) 0.88070(16) 0.73737(9) 0.0288(3) Uani 1 1 d . . . . .
H41 H 0.1998 0.8634 0.7885 0.035 Uiso 1 1 calc R U . . .
H33 H 0.1822 0.7991 0.7097 0.035 Uiso 1 1 calc R U . . .
C7 C 0.12022(9) 0.97573(14) 0.69643(8) 0.0221(3) Uani 1 1 d . . . . .
H42 H 0.1295 1.0533 0.7283 0.027 Uiso 1 1 calc R U . . .
C8 C -0.22750(10) 0.92327(16) 0.72387(10) 0.0332(4) Uani 1 1 d . . . . .
H46 H -0.2407 0.8663 0.6831 0.040 Uiso 1 1 calc R U . . .
C9 C 0.07947(13) 0.63902(18) 0.99275(11) 0.0460(5) Uani 1 1 d . . . . .
H3 H 0.1084 0.5946 1.0384 0.055 Uiso 1 1 calc R U . . .
C10 C 0.11530(11) 0.65875(16) 0.94202(10) 0.0364(4) Uani 1 1 d . . . . .
H49 H 0.1682 0.6273 0.9540 0.044 Uiso 1 1 calc R U . . .
C11 C 0.07194(10) 0.72553(14) 0.87331(9) 0.0271(3) Uani 1 1 d . . . . .
H4 H 0.0960 0.7365 0.8396 0.032 Uiso 1 1 calc R U . . .
C12 C -0.00723(10) 0.77624(14) 0.85447(9) 0.0261(3) Uani 1 1 d . . . . .
C13 C 0.00489(8) 1.08412(13) 0.76413(8) 0.0195(3) Uani 1 1 d . . . . .
C14 C -0.05652(9) 1.17095(14) 0.71543(8) 0.0217(3) Uani 1 1 d . . . . .
C15 C -0.12648(9) 1.13005(15) 0.63830(9) 0.0259(3) Uani 1 1 d . . . . .
H11 H -0.1337 1.0361 0.6402 0.031 Uiso 1 1 calc R U . . .
C16 C -0.10346(11) 1.15745(18) 0.57131(10) 0.0375(4) Uani 1 1 d . . . . .
H5 H -0.0541 1.1104 0.5792 0.056 Uiso 1 1 calc R U . . .
H7 H -0.0940 1.2487 0.5690 0.056 Uiso 1 1 calc R U . . .
H6 H -0.1480 1.1303 0.5241 0.056 Uiso 1 1 calc R U . . .
C17 C -0.21031(10) 1.19427(18) 0.62247(11) 0.0386(4) Uani 1 1 d . . . . .
H8 H -0.2077 1.2851 0.6129 0.058 Uiso 1 1 calc R U . . .
H10 H -0.2219 1.1831 0.6661 0.058 Uiso 1 1 calc R U . . .
H9 H -0.2534 1.1545 0.5786 0.058 Uiso 1 1 calc R U . . .
C18 C -0.05204(10) 1.30063(15) 0.73819(9) 0.0290(4) Uani 1 1 d . . . . .
H21 H -0.0913 1.3593 0.7065 0.035 Uiso 1 1 calc R U . . .
C19 C 0.00975(10) 1.34376(15) 0.80714(10) 0.0319(4) Uani 1 1 d . . . . .
H20 H 0.0109 1.4299 0.8217 0.038 Uiso 1 1 calc R U . . .
C20 C 0.06949(10) 1.25804(15) 0.85390(9) 0.0283(3) Uani 1 1 d . . . . .
H19 H 0.1110 1.2878 0.8997 0.034 Uiso 1 1 calc R U . . .
C21 C 0.06903(9) 1.12736(14) 0.83399(8) 0.0230(3) Uani 1 1 d . . . . .
C22 C 0.13924(10) 1.04089(15) 0.88777(9) 0.0283(3) Uani 1 1 d . . . . .
H12 H 0.1329 0.9557 0.8635 0.034 Uiso 1 1 calc R U . . .
C23 C 0.13555(13) 1.02117(19) 0.96565(10) 0.0448(5) Uani 1 1 d . . . . .
H14 H 0.0837 0.9820 0.9573 0.067 Uiso 1 1 calc R U . . .
H13 H 0.1405 1.1036 0.9903 0.067 Uiso 1 1 calc R U . . .
H15 H 0.1802 0.9657 0.9976 0.067 Uiso 1 1 calc R U . . .
C24 C 0.22487(10) 1.09521(18) 0.90090(10) 0.0374(4) Uani 1 1 d . . . . .
H16 H 0.2367 1.1713 0.9324 0.056 Uiso 1 1 calc R U . . .
H17 H 0.2244 1.1172 0.8526 0.056 Uiso 1 1 calc R U . . .
H18 H 0.2666 1.0308 0.9259 0.056 Uiso 1 1 calc R U . . .
C25 C 0.01280(9) 0.77281(14) 0.64121(8) 0.0234(3) Uani 1 1 d . . . . .
H22 H 0.0493 0.7718 0.6153 0.028 Uiso 1 1 calc R U . . .
C26 C -0.07575(10) 0.78148(15) 0.57497(9) 0.0316(4) Uani 1 1 d . . . . .
H31 H -0.1162 0.7762 0.5958 0.038 Uiso 1 1 calc R U . . .
H32 H -0.0826 0.8646 0.5495 0.038 Uiso 1 1 calc R U . . .
C27 C -0.09162(12) 0.67176(16) 0.51636(9) 0.0389(4) Uani 1 1 d . . . . .
H29 H -0.1483 0.6768 0.4774 0.047 Uiso 1 1 calc R U . . .
H30 H -0.0551 0.6823 0.4915 0.047 Uiso 1 1 calc R U . . .
C28 C -0.07673(11) 0.53888(15) 0.55526(9) 0.0334(4) Uani 1 1 d . . . . .
H28 H -0.0835 0.4718 0.5179 0.040 Uiso 1 1 calc R U . . .
H27 H -0.1175 0.5243 0.5750 0.040 Uiso 1 1 calc R U . . .
C29 C 0.01052(10) 0.52973(15) 0.62103(9) 0.0280(3) Uani 1 1 d . . . . .
H26 H 0.0172 0.4462 0.6460 0.034 Uiso 1 1 calc R U . . .
H25 H 0.0513 0.5359 0.6006 0.034 Uiso 1 1 calc R U . . .
C30 C 0.02560(9) 0.63811(14) 0.67981(8) 0.0243(3) Uani 1 1 d . . . . .
H23 H 0.0817 0.6317 0.7198 0.029 Uiso 1 1 calc R U . . .
H24 H -0.0123 0.6281 0.7032 0.029 Uiso 1 1 calc R U . . .
C31 C 0.20189(10) 1.06969(16) 0.62581(10) 0.0306(4) Uani 1 1 d . . . . .
H37 H 0.1978 1.0908 0.5755 0.037 Uiso 1 1 calc R U . . .
H36 H 0.2151 1.1488 0.6559 0.037 Uiso 1 1 calc R U . . .
C32 C 0.11793(9) 1.01716(16) 0.61800(9) 0.0278(3) Uani 1 1 d . . . . .
H39 H 0.1023 0.9430 0.5839 0.033 Uiso 1 1 calc R U . . .
H38 H 0.0760 1.0835 0.5952 0.033 Uiso 1 1 calc R U . . .
C33 C -0.12616(11) 1.03269(15) 0.83485(9) 0.0307(4) Uani 1 1 d . . . . .
H45 H -0.0714 1.0490 0.8686 0.037 Uiso 1 1 calc R U . . .
C34 C -0.04284(12) 0.75331(17) 0.90616(10) 0.0386(4) Uani 1 1 d . . . . .
H48 H -0.0960 0.7836 0.8943 0.046 Uiso 1 1 calc R U . . .
C35 C 0.00045(14) 0.6861(2) 0.97460(11) 0.0502(5) Uani 1 1 d . . . . .
H47 H -0.0237 0.6729 1.0080 0.060 Uiso 1 1 calc R U . . .
B1 B 0.03997(10) 0.90162(15) 0.69377(9) 0.0201(3) Uani 1 1 d . . . . .
C36 C -0.27244(12) 1.07207(18) 0.79424(12) 0.0442(5) Uani 1 1 d . . . . .
H2 H -0.3148 1.1135 0.8013 0.053 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 N1 1.7648(13) . ?
P1 C1 1.8423(17) . ?
P1 C12 1.8622(18) . ?
N1 B1 1.457(2) . ?
N1 C13 1.4684(19) . ?
C1 C8 1.402(2) . ?
C1 C33 1.413(2) . ?
C2 C36 1.382(3) . ?
C2 C8 1.399(2) . ?
C2 H43 0.9300 . ?
C3 C36 1.394(3) . ?
C3 C33 1.396(2) . ?
C3 H44 0.9300 . ?
C4 C31 1.522(2) . ?
C4 C5 1.538(3) . ?
C4 H35 0.9700 . ?
C4 H1 0.9700 . ?
C5 C6 1.542(2) . ?
C5 H40 0.9700 . ?
C5 H34 0.9700 . ?
C6 C7 1.563(2) . ?
C6 H41 0.9700 . ?
C6 H33 0.9700 . ?
C7 C32 1.562(2) . ?
C7 B1 1.607(2) . ?
C7 H42 0.9800 . ?
C8 H46 0.9300 . ?
C9 C35 1.389(3) . ?
C9 C10 1.400(3) . ?
C9 H3 0.9300 . ?
C10 C11 1.400(2) . ?
C10 H49 0.9300 . ?
C11 C12 1.402(2) . ?
C11 H4 0.9300 . ?
C12 C34 1.419(2) . ?
C13 C14 1.416(2) . ?
C13 C21 1.418(2) . ?
C14 C18 1.399(2) . ?
C14 C15 1.539(2) . ?
C15 C17 1.544(2) . ?
C15 C16 1.547(2) . ?
C15 H11 0.9800 . ?
C16 H5 0.9600 . ?
C16 H7 0.9600 . ?
C16 H6 0.9600 . ?
C17 H8 0.9600 . ?
C17 H10 0.9600 . ?
C17 H9 0.9600 . ?
C18 C19 1.390(2) . ?
C18 H21 0.9300 . ?
C19 C20 1.382(2) . ?
C19 H20 0.9300 . ?
C20 C21 1.401(2) . ?
C20 H19 0.9300 . ?
C21 C22 1.527(2) . ?
C22 C24 1.546(2) . ?
C22 C23 1.551(2) . ?
C22 H12 0.9800 . ?
C23 H14 0.9600 . ?
C23 H13 0.9600 . ?
C23 H15 0.9600 . ?
C24 H16 0.9600 . ?
C24 H17 0.9600 . ?
C24 H18 0.9600 . ?
C25 C30 1.547(2) . ?
C25 C26 1.554(2) . ?
C25 B1 1.616(2) . ?
C25 H22 0.9800 . ?
C26 C27 1.540(2) . ?
C26 H31 0.9700 . ?
C26 H32 0.9700 . ?
C27 C28 1.531(2) . ?
C27 H29 0.9700 . ?
C27 H30 0.9700 . ?
C28 C29 1.535(2) . ?
C28 H28 0.9700 . ?
C28 H27 0.9700 . ?
C29 C30 1.534(2) . ?
C29 H26 0.9700 . ?
C29 H25 0.9700 . ?
C30 H23 0.9700 . ?
C30 H24 0.9700 . ?
C31 C32 1.541(2) . ?
C31 H37 0.9700 . ?
C31 H36 0.9700 . ?
C32 H39 0.9700 . ?
C32 H38 0.9700 . ?
C33 H45 0.9300 . ?
C34 C35 1.398(3) . ?
C34 H48 0.9300 . ?
C35 H47 0.9300 . ?
C36 H2 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 P1 C1 107.47(7) . . ?
N1 P1 C12 105.47(7) . . ?
C1 P1 C12 100.69(8) . . ?
B1 N1 C13 121.73(11) . . ?
B1 N1 P1 118.81(10) . . ?
C13 N1 P1 119.16(9) . . ?
C8 C1 C33 118.11(15) . . ?
C8 C1 P1 115.33(13) . . ?
C33 C1 P1 126.44(12) . . ?
C36 C2 C8 119.99(17) . . ?
C36 C2 H43 120.0 . . ?
C8 C2 H43 120.0 . . ?
C36 C3 C33 120.35(17) . . ?
C36 C3 H44 119.8 . . ?
C33 C3 H44 119.8 . . ?
C31 C4 C5 110.54(14) . . ?
C31 C4 H35 109.5 . . ?
C5 C4 H35 109.5 . . ?
C31 C4 H1 109.5 . . ?
C5 C4 H1 109.5 . . ?
H35 C4 H1 108.1 . . ?
C4 C5 C6 111.31(13) . . ?
C4 C5 H40 109.4 . . ?
C6 C5 H40 109.4 . . ?
C4 C5 H34 109.4 . . ?
C6 C5 H34 109.4 . . ?
H40 C5 H34 108.0 . . ?
C5 C6 C7 113.51(13) . . ?
C5 C6 H41 108.9 . . ?
C7 C6 H41 108.9 . . ?
C5 C6 H33 108.9 . . ?
C7 C6 H33 108.9 . . ?
H41 C6 H33 107.7 . . ?
C32 C7 C6 109.04(12) . . ?
C32 C7 B1 116.71(12) . . ?
C6 C7 B1 105.64(12) . . ?
C32 C7 H42 108.4 . . ?
C6 C7 H42 108.4 . . ?
B1 C7 H42 108.4 . . ?
C2 C8 C1 121.12(17) . . ?
C2 C8 H46 119.4 . . ?
C1 C8 H46 119.4 . . ?
C35 C9 C10 119.65(17) . . ?
C35 C9 H3 120.2 . . ?
C10 C9 H3 120.2 . . ?
C11 C10 C9 120.35(17) . . ?
C11 C10 H49 119.8 . . ?
C9 C10 H49 119.8 . . ?
C10 C11 C12 121.02(15) . . ?
C10 C11 H4 119.5 . . ?
C12 C11 H4 119.5 . . ?
C11 C12 C34 117.63(15) . . ?
C11 C12 P1 119.59(12) . . ?
C34 C12 P1 121.80(13) . . ?
C14 C13 C21 120.92(13) . . ?
C14 C13 N1 117.12(12) . . ?
C21 C13 N1 121.95(12) . . ?
C18 C14 C13 118.12(14) . . ?
C18 C14 C15 118.70(13) . . ?
C13 C14 C15 123.16(13) . . ?
C14 C15 C17 112.94(13) . . ?
C14 C15 C16 111.46(13) . . ?
C17 C15 C16 109.95(13) . . ?
C14 C15 H11 107.4 . . ?
C17 C15 H11 107.4 . . ?
C16 C15 H11 107.4 . . ?
C15 C16 H5 109.5 . . ?
C15 C16 H7 109.5 . . ?
H5 C16 H7 109.5 . . ?
C15 C16 H6 109.5 . . ?
H5 C16 H6 109.5 . . ?
H7 C16 H6 109.5 . . ?
C15 C17 H8 109.5 . . ?
C15 C17 H10 109.5 . . ?
H8 C17 H10 109.5 . . ?
C15 C17 H9 109.5 . . ?
H8 C17 H9 109.5 . . ?
H10 C17 H9 109.5 . . ?
C19 C18 C14 121.49(14) . . ?
C19 C18 H21 119.3 . . ?
C14 C18 H21 119.3 . . ?
C20 C19 C18 119.72(14) . . ?
C20 C19 H20 120.1 . . ?
C18 C19 H20 120.1 . . ?
C19 C20 C21 121.57(14) . . ?
C19 C20 H19 119.2 . . ?
C21 C20 H19 119.2 . . ?
C20 C21 C13 118.15(14) . . ?
C20 C21 C22 117.93(13) . . ?
C13 C21 C22 123.90(13) . . ?
C21 C22 C24 111.49(13) . . ?
C21 C22 C23 111.93(14) . . ?
C24 C22 C23 109.95(13) . . ?
C21 C22 H12 107.8 . . ?
C24 C22 H12 107.8 . . ?
C23 C22 H12 107.8 . . ?
C22 C23 H14 109.5 . . ?
C22 C23 H13 109.5 . . ?
H14 C23 H13 109.5 . . ?
C22 C23 H15 109.5 . . ?
H14 C23 H15 109.5 . . ?
H13 C23 H15 109.5 . . ?
C22 C24 H16 109.5 . . ?
C22 C24 H17 109.5 . . ?
H16 C24 H17 109.5 . . ?
C22 C24 H18 109.5 . . ?
H16 C24 H18 109.5 . . ?
H17 C24 H18 109.5 . . ?
C30 C25 C26 109.70(12) . . ?
C30 C25 B1 119.45(12) . . ?
C26 C25 B1 113.35(12) . . ?
C30 C25 H22 104.2 . . ?
C26 C25 H22 104.2 . . ?
B1 C25 H22 104.2 . . ?
C27 C26 C25 111.45(14) . . ?
C27 C26 H31 109.3 . . ?
C25 C26 H31 109.3 . . ?
C27 C26 H32 109.3 . . ?
C25 C26 H32 109.3 . . ?
H31 C26 H32 108.0 . . ?
C28 C27 C26 110.90(14) . . ?
C28 C27 H29 109.5 . . ?
C26 C27 H29 109.5 . . ?
C28 C27 H30 109.5 . . ?
C26 C27 H30 109.5 . . ?
H29 C27 H30 108.0 . . ?
C27 C28 C29 111.28(13) . . ?
C27 C28 H28 109.4 . . ?
C29 C28 H28 109.4 . . ?
C27 C28 H27 109.4 . . ?
C29 C28 H27 109.4 . . ?
H28 C28 H27 108.0 . . ?
C30 C29 C28 111.25(13) . . ?
C30 C29 H26 109.4 . . ?
C28 C29 H26 109.4 . . ?
C30 C29 H25 109.4 . . ?
C28 C29 H25 109.4 . . ?
H26 C29 H25 108.0 . . ?
C29 C30 C25 110.68(13) . . ?
C29 C30 H23 109.5 . . ?
C25 C30 H23 109.5 . . ?
C29 C30 H24 109.5 . . ?
C25 C30 H24 109.5 . . ?
H23 C30 H24 108.1 . . ?
C4 C31 C32 111.68(13) . . ?
C4 C31 H37 109.3 . . ?
C32 C31 H37 109.3 . . ?
C4 C31 H36 109.3 . . ?
C32 C31 H36 109.3 . . ?
H37 C31 H36 107.9 . . ?
C31 C32 C7 112.58(12) . . ?
C31 C32 H39 109.1 . . ?
C7 C32 H39 109.1 . . ?
C31 C32 H38 109.1 . . ?
C7 C32 H38 109.1 . . ?
H39 C32 H38 107.8 . . ?
C3 C33 C1 120.37(16) . . ?
C3 C33 H45 119.8 . . ?
C1 C33 H45 119.8 . . ?
C35 C34 C12 121.21(17) . . ?
C35 C34 H48 119.4 . . ?
C12 C34 H48 119.4 . . ?
C9 C35 C34 120.10(17) . . ?
C9 C35 H47 120.0 . . ?
C34 C35 H47 120.0 . . ?
N1 B1 C7 120.21(13) . . ?
N1 B1 C25 124.07(13) . . ?
C7 B1 C25 115.68(13) . . ?
C2 C36 C3 120.04(16) . . ?
C2 C36 H2 120.0 . . ?
C3 C36 H2 120.0 . . ?

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 N1 B1 -154.41(11) . . . . ?
C12 P1 N1 B1 98.80(11) . . . . ?
C1 P1 N1 C13 19.45(12) . . . . ?
C12 P1 N1 C13 -87.34(11) . . . . ?
N1 P1 C1 C8 120.86(12) . . . . ?
C12 P1 C1 C8 -129.02(12) . . . . ?
N1 P1 C1 C33 -63.09(15) . . . . ?
C12 P1 C1 C33 47.03(15) . . . . ?
C31 C4 C5 C6 55.96(19) . . . . ?
C4 C5 C6 C7 -54.56(19) . . . . ?
C5 C6 C7 C32 51.76(18) . . . . ?
C5 C6 C7 B1 177.95(13) . . . . ?
C36 C2 C8 C1 0.3(3) . . . . ?
C33 C1 C8 C2 -1.1(2) . . . . ?
P1 C1 C8 C2 175.33(13) . . . . ?
C35 C9 C10 C11 0.0(3) . . . . ?
C9 C10 C11 C12 1.3(3) . . . . ?
C10 C11 C12 C34 -2.2(2) . . . . ?
C10 C11 C12 P1 -171.09(12) . . . . ?
N1 P1 C12 C11 -48.97(14) . . . . ?
C1 P1 C12 C11 -160.64(12) . . . . ?
N1 P1 C12 C34 142.65(13) . . . . ?
C1 P1 C12 C34 30.98(15) . . . . ?
B1 N1 C13 C14 91.29(16) . . . . ?
P1 N1 C13 C14 -82.39(15) . . . . ?
B1 N1 C13 C21 -89.22(17) . . . . ?
P1 N1 C13 C21 97.11(14) . . . . ?
C21 C13 C14 C18 0.1(2) . . . . ?
N1 C13 C14 C18 179.56(13) . . . . ?
C21 C13 C14 C15 178.75(13) . . . . ?
N1 C13 C14 C15 -1.7(2) . . . . ?
C18 C14 C15 C17 -40.39(19) . . . . ?
C13 C14 C15 C17 140.93(15) . . . . ?
C18 C14 C15 C16 83.97(17) . . . . ?
C13 C14 C15 C16 -94.71(17) . . . . ?
C13 C14 C18 C19 -1.1(2) . . . . ?
C15 C14 C18 C19 -179.89(14) . . . . ?
C14 C18 C19 C20 1.5(2) . . . . ?
C18 C19 C20 C21 -0.7(2) . . . . ?
C19 C20 C21 C13 -0.3(2) . . . . ?
C19 C20 C21 C22 177.85(15) . . . . ?
C14 C13 C21 C20 0.7(2) . . . . ?
N1 C13 C21 C20 -178.82(13) . . . . ?
C14 C13 C21 C22 -177.42(14) . . . . ?
N1 C13 C21 C22 3.1(2) . . . . ?
C20 C21 C22 C24 -56.52(19) . . . . ?
C13 C21 C22 C24 121.56(16) . . . . ?
C20 C21 C22 C23 67.11(18) . . . . ?
C13 C21 C22 C23 -114.81(16) . . . . ?
C30 C25 C26 C27 -56.44(18) . . . . ?
B1 C25 C26 C27 167.23(14) . . . . ?
C25 C26 C27 C28 55.9(2) . . . . ?
C26 C27 C28 C29 -55.3(2) . . . . ?
C27 C28 C29 C30 56.41(19) . . . . ?
C28 C29 C30 C25 -57.34(17) . . . . ?
C26 C25 C30 C29 56.88(16) . . . . ?
B1 C25 C30 C29 -169.84(13) . . . . ?
C5 C4 C31 C32 -57.30(18) . . . . ?
C4 C31 C32 C7 56.75(18) . . . . ?
C6 C7 C32 C31 -52.35(17) . . . . ?
B1 C7 C32 C31 -171.88(13) . . . . ?
C36 C3 C33 C1 0.2(2) . . . . ?
C8 C1 C33 C3 0.8(2) . . . . ?
P1 C1 C33 C3 -175.15(12) . . . . ?
C11 C12 C34 C35 2.0(3) . . . . ?
P1 C12 C34 C35 170.55(15) . . . . ?
C10 C9 C35 C34 -0.3(3) . . . . ?
C12 C34 C35 C9 -0.7(3) . . . . ?
C13 N1 B1 C7 24.18(19) . . . . ?
P1 N1 B1 C7 -162.13(10) . . . . ?
C13 N1 B1 C25 -158.42(13) . . . . ?
P1 N1 B1 C25 15.28(18) . . . . ?
C32 C7 B1 N1 -127.05(15) . . . . ?
C6 C7 B1 N1 111.62(15) . . . . ?
C32 C7 B1 C25 55.34(17) . . . . ?
C6 C7 B1 C25 -66.00(16) . . . . ?
C30 C25 B1 N1 -68.64(19) . . . . ?
C26 C25 B1 N1 63.07(19) . . . . ?
C30 C25 B1 C7 108.87(15) . . . . ?
C26 C25 B1 C7 -119.41(15) . . . . ?
C8 C2 C36 C3 0.8(3) . . . . ?
C33 C3 C36 C2 -1.0(3) . . . . ?

_refine_diff_density_max         0.251
_refine_diff_density_min         -0.294
_refine_diff_density_rms         0.042

_shelxl_version_number           2013-4


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

data_Q1_a
_database_code_depnum_ccdc_archive 'CCDC 1543528'
_audit_update_record             
;
2017-04-11 deposited with the CCDC.
2017-10-09 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         'C49 H63 B N O4 P'
_chemical_formula_sum            'C49 H63 B N O4 P'
_chemical_formula_weight         771.78

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'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   10.6838(12)
_cell_length_b                   12.1850(12)
_cell_length_c                   17.8138(18)
_cell_angle_alpha                75.008(4)
_cell_angle_beta                 76.864(4)
_cell_angle_gamma                89.922(3)
_cell_volume                     2177.4(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9840
_cell_measurement_theta_min      2.64
_cell_measurement_theta_max      69.75

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.177
_exptl_crystal_F_000             832
_exptl_transmission_factor_min   0.6830
_exptl_transmission_factor_max   0.7532
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_absorpt_coefficient_mu    0.896
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   
'Sheldrick,G. M.(2012)SADABS. Bruker AXS Inc.,Madison,Wisconsin,USA.'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            30493
_diffrn_reflns_av_unetI/netI     0.0335
_diffrn_reflns_av_R_equivalents  0.0380
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.642
_diffrn_reflns_theta_max         69.743
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             8163
_reflns_number_gt                7080
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_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)+(0.0535P)²+2.0427P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8163
_refine_ls_number_parameters     512
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0545
_refine_ls_R_factor_gt           0.0467
_refine_ls_wR_factor_ref         0.1210
_refine_ls_wR_factor_gt          0.1156
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_restrained_S_all      1.003
_refine_ls_shift/su_max          0.006
_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
C3 C 0.95967(16) 0.71175(14) 0.60653(10) 0.0133(3) Uani 1 1 d . . . . .
C4 C 0.82982(15) 0.47257(14) 0.68103(10) 0.0139(3) Uani 1 1 d . . . . .
C1 C 0.83986(16) 0.68588(13) 0.66218(9) 0.0128(3) Uani 1 1 d . . . . .
C8 C 0.82248(17) 0.92688(15) 0.70561(10) 0.0172(4) Uani 1 1 d . . . . .
H8 H 0.8849 0.8742 0.7117 0.021 Uiso 1 1 calc R U . . .
C5 C 0.38554(16) 0.70654(14) 0.66130(10) 0.0163(3) Uani 1 1 d . . . . .
C27 C 0.46227(16) 0.71727(14) 0.71425(10) 0.0144(3) Uani 1 1 d . . . . .
C7 C 0.53600(16) 0.46546(14) 0.78196(10) 0.0158(3) Uani 1 1 d . . . . .
H7 H 0.4508 0.4958 0.7934 0.019 Uiso 1 1 calc R U . . .
C2 C 0.79244(16) 0.56975(14) 0.71987(10) 0.0133(3) Uani 1 1 d . . . . .
C9 C 0.71766(16) 0.90304(14) 0.67652(10) 0.0148(3) Uani 1 1 d . . . . .
C10 C 0.84268(16) 0.54531(14) 0.79863(10) 0.0150(3) Uani 1 1 d . . . . .
H10 H 0.8176 0.4657 0.8280 0.018 Uiso 1 1 calc R U . . .
C11 C 0.41365(17) 0.76517(14) 0.77869(10) 0.0175(4) Uani 1 1 d . . . . .
C12 C 0.71108(16) 0.81502(15) 0.54062(10) 0.0161(3) Uani 1 1 d . . . . .
C13 C 0.98933(17) 0.55998(16) 0.78091(10) 0.0193(4) Uani 1 1 d . . . . .
H13A H 1.0170 0.6369 0.7487 0.023 Uiso 1 1 calc R U . . .
H13B H 1.0266 0.5081 0.7500 0.023 Uiso 1 1 calc R U . . .
C14 C 0.78198(17) 0.61936(15) 0.85299(10) 0.0182(4) Uani 1 1 d . . . . .
H14A H 0.6893 0.6042 0.8677 0.022 Uiso 1 1 calc R U . . .
H14B H 0.8001 0.6989 0.8238 0.022 Uiso 1 1 calc R U . . .
C15 C 0.74347(17) 0.73364(16) 0.49772(11) 0.0195(4) Uani 1 1 d . . . . .
H15 H 0.7597 0.6606 0.5242 0.023 Uiso 1 1 calc R U . . .
C16 C 0.26339(17) 0.74908(15) 0.67193(11) 0.0201(4) Uani 1 1 d . . . . .
H16 H 0.2119 0.7430 0.6374 0.024 Uiso 1 1 calc R U . . .
C17 C 0.42383(17) 0.64565(15) 0.59559(10) 0.0177(4) Uani 1 1 d . . . . .
H17 H 0.5116 0.6212 0.5942 0.021 Uiso 1 1 calc R U . . .
C18 C 0.53118(16) 0.38773(14) 0.72578(10) 0.0163(3) Uani 1 1 d . . . . .
H18A H 0.5207 0.4337 0.6745 0.020 Uiso 1 1 calc R U . . .
H18B H 0.6116 0.3507 0.7168 0.020 Uiso 1 1 calc R U . . .
C19 C 0.21722(17) 0.80022(15) 0.73286(12) 0.0230(4) Uani 1 1 d . . . . .
H19 H 0.1365 0.8301 0.7380 0.028 Uiso 1 1 calc R U . . .
C20 C 0.8343(2) 1.02877(16) 0.72553(11) 0.0243(4) Uani 1 1 d . . . . .
H20 H 0.9033 1.0432 0.7461 0.029 Uiso 1 1 calc R U . . .
C21 C 0.48395(18) 0.76409(16) 0.84427(10) 0.0209(4) Uani 1 1 d . . . . .
H21 H 0.5750 0.7531 0.8238 0.025 Uiso 1 1 calc R U . . .
C22 C 0.29133(17) 0.80680(15) 0.78613(11) 0.0219(4) Uani 1 1 d . . . . .
H22 H 0.2588 0.8397 0.8277 0.026 Uiso 1 1 calc R U . . .
C23 C 0.68703(19) 0.92417(16) 0.49985(11) 0.0240(4) Uani 1 1 d . . . . .
H23 H 0.6666 0.9795 0.5274 0.029 Uiso 1 1 calc R U . . .
C24 C 0.62439(18) 0.98311(15) 0.66788(11) 0.0213(4) Uani 1 1 d . . . . .
H24 H 0.5528 0.9677 0.6500 0.026 Uiso 1 1 calc R U . . .
C25 C 0.84907(19) 0.41165(16) 0.56371(11) 0.0229(4) Uani 1 1 d . . . . .
H25A H 0.9370 0.3956 0.5639 0.034 Uiso 1 1 calc R U . . .
H25B H 0.8410 0.4400 0.5096 0.034 Uiso 1 1 calc R U . . .
H25C H 0.7949 0.3432 0.5891 0.034 Uiso 1 1 calc R U . . .
C26 C 0.6392(2) 1.08557(16) 0.68611(12) 0.0273(4) Uani 1 1 d . . . . .
H26 H 0.5783 1.1395 0.6789 0.033 Uiso 1 1 calc R U . . .
C6 C 1.06108(18) 0.85701(16) 0.48880(11) 0.0223(4) Uani 1 1 d . . . . .
H6A H 1.1443 0.8319 0.4949 0.033 Uiso 1 1 calc R U . . .
H6B H 1.0667 0.9381 0.4671 0.033 Uiso 1 1 calc R U . . .
H6C H 1.0322 0.8211 0.4532 0.033 Uiso 1 1 calc R U . . .
C28 C 0.42039(19) 0.72222(17) 0.51310(11) 0.0240(4) Uani 1 1 d . . . . .
H28A H 0.3333 0.7409 0.5122 0.036 Uiso 1 1 calc R U . . .
H28B H 0.4527 0.6829 0.4730 0.036 Uiso 1 1 calc R U . . .
H28C H 0.4730 0.7908 0.5024 0.036 Uiso 1 1 calc R U . . .
C29 C 0.33216(18) 0.53953(16) 0.61419(12) 0.0239(4) Uani 1 1 d . . . . .
H29A H 0.3276 0.4944 0.6677 0.036 Uiso 1 1 calc R U . . .
H29B H 0.3639 0.4953 0.5772 0.036 Uiso 1 1 calc R U . . .
H29C H 0.2479 0.5628 0.6092 0.036 Uiso 1 1 calc R U . . .
C30 C 0.55553(19) 0.38823(15) 0.86148(11) 0.0214(4) Uani 1 1 d . . . . .
H30A H 0.6369 0.3528 0.8518 0.026 Uiso 1 1 calc R U . . .
H30B H 0.5590 0.4341 0.8982 0.026 Uiso 1 1 calc R U . . .
C31 C 0.83278(19) 0.59725(17) 0.92925(11) 0.0246(4) Uani 1 1 d . . . . .
H31A H 0.7956 0.6489 0.9603 0.030 Uiso 1 1 calc R U . . .
H31B H 0.8066 0.5201 0.9615 0.030 Uiso 1 1 calc R U . . .
C32 C 0.43343(19) 0.22283(16) 0.84330(11) 0.0244(4) Uani 1 1 d . . . . .
H32A H 0.3589 0.1696 0.8673 0.029 Uiso 1 1 calc R U . . .
H32B H 0.5092 0.1794 0.8353 0.029 Uiso 1 1 calc R U . . .
C33 C 0.7437(2) 1.10867(16) 0.71490(11) 0.0276(4) Uani 1 1 d . . . . .
H33 H 0.7527 1.1776 0.7270 0.033 Uiso 1 1 calc R U . . .
C34 C 0.41901(17) 0.29725(15) 0.76273(11) 0.0205(4) Uani 1 1 d . . . . .
H34A H 0.3384 0.3343 0.7700 0.025 Uiso 1 1 calc R U . . .
H34B H 0.4169 0.2500 0.7267 0.025 Uiso 1 1 calc R U . . .
C35 C 0.9791(2) 0.61390(18) 0.90911(11) 0.0279(4) Uani 1 1 d . . . . .
H35A H 1.0051 0.6928 0.8810 0.033 Uiso 1 1 calc R U . . .
H35B H 1.0092 0.5960 0.9581 0.033 Uiso 1 1 calc R U . . .
C36 C 0.7516(2) 0.76080(17) 0.41607(11) 0.0270(4) Uani 1 1 d . . . . .
H36 H 0.7737 0.7063 0.3880 0.032 Uiso 1 1 calc R U . . .
C37 C 0.4460(2) 0.29572(16) 0.89942(11) 0.0262(4) Uani 1 1 d . . . . .
H37A H 0.4621 0.2474 0.9485 0.031 Uiso 1 1 calc R U . . .
H37B H 0.3657 0.3312 0.9130 0.031 Uiso 1 1 calc R U . . .
C38 C 1.03950(19) 0.53735(18) 0.85718(11) 0.0263(4) Uani 1 1 d . . . . .
H38A H 1.0194 0.4583 0.8871 0.032 Uiso 1 1 calc R U . . .
H38B H 1.1324 0.5511 0.8430 0.032 Uiso 1 1 calc R U . . .
C39 C 0.4294(2) 0.66222(17) 0.91587(11) 0.0275(4) Uani 1 1 d . . . . .
H39A H 0.3421 0.6740 0.9396 0.041 Uiso 1 1 calc R U . . .
H39B H 0.4804 0.6548 0.9547 0.041 Uiso 1 1 calc R U . . .
H39C H 0.4316 0.5941 0.8982 0.041 Uiso 1 1 calc R U . . .
C40 C 0.6935(2) 0.95045(17) 0.41853(12) 0.0316(5) Uani 1 1 d . . . . .
H40 H 0.6756 1.0229 0.3920 0.038 Uiso 1 1 calc R U . . .
C41 C 0.7265(2) 0.86958(18) 0.37640(12) 0.0322(5) Uani 1 1 d . . . . .
H41 H 0.7319 0.8881 0.3217 0.039 Uiso 1 1 calc R U . . .
C42 C 0.4763(2) 0.87351(17) 0.87182(12) 0.0298(4) Uani 1 1 d . . . . .
H42A H 0.5018 0.9379 0.8261 0.045 Uiso 1 1 calc R U . . .
H42B H 0.5328 0.8712 0.9070 0.045 Uiso 1 1 calc R U . . .
H42C H 0.3895 0.8800 0.8995 0.045 Uiso 1 1 calc R U . . .
C43 C 0.9733(2) 0.1246(2) 0.87432(15) 0.0409(6) Uani 1 1 d . . . . .
C44 C 1.0211(4) 0.0156(3) 0.89110(17) 0.0593(8) Uani 1 1 d . . . . .
H44 H 1.1087 0.0058 0.8762 0.071 Uiso 1 1 calc R U . . .
C45 C 0.8467(3) 0.1351(3) 0.89718(19) 0.0646(9) Uani 1 1 d . . . . .
H45 H 0.8160 0.2075 0.8856 0.078 Uiso 1 1 calc R U . . .
C46 C 1.0668(3) 0.2232(3) 0.8315(2) 0.0760(10) Uani 1 1 d . . . . .
H46A H 1.0256 0.2812 0.7995 0.114 Uiso 1 1 calc R U . . .
H46B H 1.1386 0.1991 0.7975 0.114 Uiso 1 1 calc R U . . .
H46C H 1.0965 0.2531 0.8696 0.114 Uiso 1 1 calc R U . . .
C47 C 0.8137(6) -0.0692(4) 0.9528(2) 0.0999(18) Uani 1 1 d . . . . .
H47 H 0.7622 -0.1358 0.9787 0.120 Uiso 1 1 calc R U . . .
C48 C 0.7571(4) 0.0417(6) 0.9381(2) 0.1046(18) Uani 1 1 d . . . . .
H48 H 0.6694 0.0499 0.9543 0.126 Uiso 1 1 calc R U . . .
C49 C 0.9384(6) -0.0723(3) 0.9286(2) 0.0925(15) Uani 1 1 d . . . . .
H49 H 0.9721 -0.1436 0.9388 0.111 Uiso 1 1 calc R U . . .
P1 P 0.71895(4) 0.77305(3) 0.64516(2) 0.01167(11) Uani 1 1 d . . . . .
O1 O 1.04633(11) 0.64934(10) 0.59170(7) 0.0166(3) Uani 1 1 d . . . . .
O2 O 0.97146(11) 0.82700(10) 0.56521(7) 0.0159(3) Uani 1 1 d . . . . .
O4 O 0.81039(12) 0.49610(10) 0.60672(7) 0.0170(3) Uani 1 1 d . . . . .
O3 O 0.86595(12) 0.38236(10) 0.71292(7) 0.0205(3) Uani 1 1 d . . . . .
N1 N 0.59348(13) 0.68016(12) 0.70287(8) 0.0131(3) Uani 1 1 d . . . . .
B1 B 0.63630(18) 0.57071(16) 0.73779(11) 0.0134(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
C3 O1 1.223(2) . ?
C3 O2 1.398(2) . ?
C3 C1 1.408(2) . ?
C4 O3 1.206(2) . ?
C4 O4 1.344(2) . ?
C4 C2 1.529(2) . ?
C1 C2 1.526(2) . ?
C1 P1 1.7019(16) . ?
C8 C20 1.390(2) . ?
C8 C9 1.396(2) . ?
C8 H8 0.9300 . ?
C5 C16 1.394(2) . ?
C5 C27 1.412(2) . ?
C5 C17 1.523(2) . ?
C27 C11 1.415(2) . ?
C27 N1 1.458(2) . ?
C7 C30 1.543(2) . ?
C7 C18 1.554(2) . ?
C7 B1 1.585(2) . ?
C7 H7 0.9800 . ?
C2 C10 1.572(2) . ?
C2 B1 1.626(2) . ?
C9 C24 1.399(2) . ?
C9 P1 1.8098(17) . ?
C10 C13 1.528(2) . ?
C10 C14 1.529(2) . ?
C10 H10 0.9800 . ?
C11 C22 1.392(3) . ?
C11 C21 1.523(2) . ?
C12 C15 1.399(2) . ?
C12 C23 1.395(3) . ?
C12 P1 1.8206(17) . ?
C13 C38 1.532(2) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 C31 1.536(2) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 C36 1.388(3) . ?
C15 H15 0.9300 . ?
C16 C19 1.384(3) . ?
C16 H16 0.9300 . ?
C17 C28 1.532(2) . ?
C17 C29 1.541(2) . ?
C17 H17 0.9800 . ?
C18 C34 1.534(2) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 C22 1.384(3) . ?
C19 H19 0.9300 . ?
C20 C33 1.381(3) . ?
C20 H20 0.9300 . ?
C21 C42 1.531(3) . ?
C21 C39 1.534(3) . ?
C21 H21 0.9800 . ?
C22 H22 0.9300 . ?
C23 C40 1.386(3) . ?
C23 H23 0.9300 . ?
C24 C26 1.387(3) . ?
C24 H24 0.9300 . ?
C25 O4 1.442(2) . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 C33 1.387(3) . ?
C26 H26 0.9300 . ?
C6 O2 1.433(2) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 C37 1.532(2) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C31 C35 1.524(3) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C32 C37 1.526(3) . ?
C32 C34 1.527(3) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C33 H33 0.9300 . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C35 C38 1.522(3) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C36 C41 1.389(3) . ?
C36 H36 0.9300 . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C39 H39A 0.9600 . ?
C39 H39B 0.9600 . ?
C39 H39C 0.9600 . ?
C40 C41 1.386(3) . ?
C40 H40 0.9300 . ?
C41 H41 0.9300 . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C43 C45 1.337(4) . ?
C43 C44 1.406(4) . ?
C43 C46 1.485(4) . ?
C44 C49 1.319(5) . ?
C44 H44 0.9300 . ?
C45 C48 1.414(6) . ?
C45 H45 0.9300 . ?
C46 H46A 0.9600 . ?
C46 H46B 0.9600 . ?
C46 H46C 0.9600 . ?
C47 C49 1.307(7) . ?
C47 C48 1.465(7) . ?
C47 H47 0.9300 . ?
C48 H48 0.9300 . ?
C49 H49 0.9300 . ?
P1 N1 1.7062(14) . ?
N1 B1 1.440(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
O1 C3 O2 120.55(15) . . ?
O1 C3 C1 129.44(16) . . ?
O2 C3 C1 110.01(14) . . ?
O3 C4 O4 122.50(15) . . ?
O3 C4 C2 125.66(15) . . ?
O4 C4 C2 111.73(13) . . ?
C3 C1 C2 125.78(14) . . ?
C3 C1 P1 117.62(12) . . ?
C2 C1 P1 113.42(12) . . ?
C20 C8 C9 120.53(17) . . ?
C20 C8 H8 119.7 . . ?
C9 C8 H8 119.7 . . ?
C16 C5 C27 118.33(16) . . ?
C16 C5 C17 117.10(15) . . ?
C27 C5 C17 124.48(15) . . ?
C5 C27 C11 120.61(15) . . ?
C5 C27 N1 120.46(14) . . ?
C11 C27 N1 118.93(15) . . ?
C30 C7 C18 107.10(14) . . ?
C30 C7 B1 117.53(14) . . ?
C18 C7 B1 110.38(13) . . ?
C30 C7 H7 107.1 . . ?
C18 C7 H7 107.1 . . ?
B1 C7 H7 107.1 . . ?
C1 C2 C4 112.00(13) . . ?
C1 C2 C10 113.63(13) . . ?
C4 C2 C10 107.89(13) . . ?
C1 C2 B1 104.47(13) . . ?
C4 C2 B1 106.52(13) . . ?
C10 C2 B1 112.14(13) . . ?
C8 C9 C24 119.05(16) . . ?
C8 C9 P1 116.60(13) . . ?
C24 C9 P1 124.18(14) . . ?
C13 C10 C14 109.94(14) . . ?
C13 C10 C2 111.88(13) . . ?
C14 C10 C2 112.17(14) . . ?
C13 C10 H10 107.5 . . ?
C14 C10 H10 107.5 . . ?
C2 C10 H10 107.5 . . ?
C22 C11 C27 118.49(16) . . ?
C22 C11 C21 118.28(16) . . ?
C27 C11 C21 123.01(16) . . ?
C15 C12 C23 118.81(16) . . ?
C15 C12 P1 116.38(13) . . ?
C23 C12 P1 124.53(14) . . ?
C10 C13 C38 112.40(15) . . ?
C10 C13 H13A 109.1 . . ?
C38 C13 H13A 109.1 . . ?
C10 C13 H13B 109.1 . . ?
C38 C13 H13B 109.1 . . ?
H13A C13 H13B 107.9 . . ?
C10 C14 C31 112.28(15) . . ?
C10 C14 H14A 109.1 . . ?
C31 C14 H14A 109.1 . . ?
C10 C14 H14B 109.1 . . ?
C31 C14 H14B 109.1 . . ?
H14A C14 H14B 107.9 . . ?
C36 C15 C12 120.70(17) . . ?
C36 C15 H15 119.6 . . ?
C12 C15 H15 119.6 . . ?
C19 C16 C5 121.34(17) . . ?
C19 C16 H16 119.3 . . ?
C5 C16 H16 119.3 . . ?
C5 C17 C28 112.33(15) . . ?
C5 C17 C29 109.68(15) . . ?
C28 C17 C29 108.85(15) . . ?
C5 C17 H17 108.6 . . ?
C28 C17 H17 108.6 . . ?
C29 C17 H17 108.6 . . ?
C34 C18 C7 110.57(14) . . ?
C34 C18 H18A 109.5 . . ?
C7 C18 H18A 109.5 . . ?
C34 C18 H18B 109.5 . . ?
C7 C18 H18B 109.5 . . ?
H18A C18 H18B 108.1 . . ?
C16 C19 C22 119.89(17) . . ?
C16 C19 H19 120.1 . . ?
C22 C19 H19 120.1 . . ?
C33 C20 C8 120.13(18) . . ?
C33 C20 H20 119.9 . . ?
C8 C20 H20 119.9 . . ?
C11 C21 C42 114.27(16) . . ?
C11 C21 C39 108.76(15) . . ?
C42 C21 C39 109.62(15) . . ?
C11 C21 H21 108.0 . . ?
C42 C21 H21 108.0 . . ?
C39 C21 H21 108.0 . . ?
C19 C22 C11 121.23(17) . . ?
C19 C22 H22 119.4 . . ?
C11 C22 H22 119.4 . . ?
C40 C23 C12 120.28(18) . . ?
C40 C23 H23 119.9 . . ?
C12 C23 H23 119.9 . . ?
C26 C24 C9 119.72(18) . . ?
C26 C24 H24 120.1 . . ?
C9 C24 H24 120.1 . . ?
O4 C25 H25A 109.5 . . ?
O4 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
O4 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 C33 120.87(18) . . ?
C24 C26 H26 119.6 . . ?
C33 C26 H26 119.6 . . ?
O2 C6 H6A 109.5 . . ?
O2 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
O2 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C17 C28 H28A 109.5 . . ?
C17 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C17 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C17 C29 H29A 109.5 . . ?
C17 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C17 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C37 C30 C7 111.16(15) . . ?
C37 C30 H30A 109.4 . . ?
C7 C30 H30A 109.4 . . ?
C37 C30 H30B 109.4 . . ?
C7 C30 H30B 109.4 . . ?
H30A C30 H30B 108.0 . . ?
C35 C31 C14 111.05(15) . . ?
C35 C31 H31A 109.4 . . ?
C14 C31 H31A 109.4 . . ?
C35 C31 H31B 109.4 . . ?
C14 C31 H31B 109.4 . . ?
H31A C31 H31B 108.0 . . ?
C37 C32 C34 110.72(15) . . ?
C37 C32 H32A 109.5 . . ?
C34 C32 H32A 109.5 . . ?
C37 C32 H32B 109.5 . . ?
C34 C32 H32B 109.5 . . ?
H32A C32 H32B 108.1 . . ?
C20 C33 C26 119.67(17) . . ?
C20 C33 H33 120.2 . . ?
C26 C33 H33 120.2 . . ?
C32 C34 C18 110.73(15) . . ?
C32 C34 H34A 109.5 . . ?
C18 C34 H34A 109.5 . . ?
C32 C34 H34B 109.5 . . ?
C18 C34 H34B 109.5 . . ?
H34A C34 H34B 108.1 . . ?
C38 C35 C31 110.36(16) . . ?
C38 C35 H35A 109.6 . . ?
C31 C35 H35A 109.6 . . ?
C38 C35 H35B 109.6 . . ?
C31 C35 H35B 109.6 . . ?
H35A C35 H35B 108.1 . . ?
C41 C36 C15 119.83(18) . . ?
C41 C36 H36 120.1 . . ?
C15 C36 H36 120.1 . . ?
C32 C37 C30 111.75(15) . . ?
C32 C37 H37A 109.3 . . ?
C30 C37 H37A 109.3 . . ?
C32 C37 H37B 109.3 . . ?
C30 C37 H37B 109.3 . . ?
H37A C37 H37B 107.9 . . ?
C35 C38 C13 110.86(16) . . ?
C35 C38 H38A 109.5 . . ?
C13 C38 H38A 109.5 . . ?
C35 C38 H38B 109.5 . . ?
C13 C38 H38B 109.5 . . ?
H38A C38 H38B 108.1 . . ?
C21 C39 H39A 109.5 . . ?
C21 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C21 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C23 C40 C41 120.52(19) . . ?
C23 C40 H40 119.7 . . ?
C41 C40 H40 119.7 . . ?
C36 C41 C40 119.84(18) . . ?
C36 C41 H41 120.1 . . ?
C40 C41 H41 120.1 . . ?
C21 C42 H42A 109.5 . . ?
C21 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C21 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C45 C43 C44 119.0(3) . . ?
C45 C43 C46 123.0(3) . . ?
C44 C43 C46 118.0(3) . . ?
C49 C44 C43 118.3(4) . . ?
C49 C44 H44 120.9 . . ?
C43 C44 H44 120.9 . . ?
C43 C45 C48 123.4(4) . . ?
C43 C45 H45 118.3 . . ?
C48 C45 H45 118.3 . . ?
C43 C46 H46A 109.5 . . ?
C43 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C43 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C49 C47 C48 118.3(4) . . ?
C49 C47 H47 120.8 . . ?
C48 C47 H47 120.8 . . ?
C45 C48 C47 114.6(4) . . ?
C45 C48 H48 122.7 . . ?
C47 C48 H48 122.7 . . ?
C44 C49 C47 126.5(5) . . ?
C44 C49 H49 116.8 . . ?
C47 C49 H49 116.8 . . ?
C1 P1 N1 97.51(7) . . ?
C1 P1 C9 116.91(8) . . ?
N1 P1 C9 111.24(7) . . ?
C1 P1 C12 113.11(8) . . ?
N1 P1 C12 111.78(7) . . ?
C9 P1 C12 106.28(8) . . ?
C3 O2 C6 115.89(13) . . ?
C4 O4 C25 115.73(13) . . ?
B1 N1 C27 127.89(14) . . ?
B1 N1 P1 111.94(11) . . ?
C27 N1 P1 120.12(11) . . ?
N1 B1 C7 120.65(15) . . ?
N1 B1 C2 112.29(14) . . ?
C7 B1 C2 126.90(15) . . ?

_refine_diff_density_max         0.776
_refine_diff_density_min         -0.459
_refine_diff_density_rms         0.055


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

data_cu_atndie2_1_0m_a_sqd
_database_code_depnum_ccdc_archive 'CCDC 1543527'
_audit_update_record             
;
2017-04-11 deposited with the CCDC.
2017-10-09 downloaded from the CCDC.
;

#============================================================================
# start Validation Reply Form
#============================================================================


# ALERT LEVEL B

loop_

_vrf_THETM01_cu_atndie2_1_0m_a_sqd
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575
RESPONSE:The crystal was of very poor quality and it was not diffracting 
at higher angles.
;
_vrf_PLAT029_cu_atndie2_1_0m_a_sqd 
;
PROBLEM: diffrn_measured_fraction_theta_full value Low
RESPONSE:Since the crystal was not diffracting at higher angles, 
the 2theta cutoff was set 60.016 during data integration.
;
#============================================================================
# End Validation Reply Form
#============================================================================

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44 H59 B N O4 P'
_chemical_formula_weight         707.70

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'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   18.4589(7)
_cell_length_b                   10.3146(4)
_cell_length_c                   24.4094(9)
_cell_angle_alpha                90
_cell_angle_beta                 104.138(2)
_cell_angle_gamma                90
_cell_volume                     4506.7(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    7693
_cell_measurement_theta_min      2.47
_cell_measurement_theta_max      57.31

_exptl_crystal_description       PLATE
_exptl_crystal_colour            COLORLESS
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.043
_exptl_crystal_F_000             1528
_exptl_transmission_factor_min   0.1486
_exptl_transmission_factor_max   0.2510
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_exptl_absorpt_coefficient_mu    0.826
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   
'Sheldrick, G. M. (2012) SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker SMART X2S benchtop diffractometer'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            54285
_diffrn_reflns_av_unetI/netI     0.1232
_diffrn_reflns_av_R_equivalents  0.1334
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.468
_diffrn_reflns_theta_max         60.015
_diffrn_reflns_theta_full        60.016
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measured_fraction_theta_full 0.954
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_Laue_measured_fraction_full 0.954
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_point_group_measured_fraction_full 0.954
_reflns_number_total             6388
_reflns_number_gt                3553
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ', SQUEEZE'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0756P)²+13.1990P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6388
_refine_ls_number_parameters     466
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1683
_refine_ls_R_factor_gt           0.0922
_refine_ls_wR_factor_ref         0.2323
_refine_ls_wR_factor_gt          0.2031
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_restrained_S_all      1.039
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

# SQUEEZE RESULTS
# 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 -0.024 0.000 502 85 ' '
2 0.000 -0.025 0.500 501 84 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          
;
TITL cu_ATNDIE2_1_0m_a.res in P2(1)/c
CELL   18.4589   10.3146   24.4094     90.00    104.14     90.00
SPGR P21/c
# Solvent Accessible Volume =    1019.8
# Electrons Found in S.A.V. =     168.6
# Note: Atoms in Void as Cxxx and Qxxx all others
C101 0.940 0.660 0.008 !       3.93 eA-3
C102 0.111 0.311 0.019 !       3.89 eA-3
C103 0.048 0.158 0.051 !       3.55 eA-3
C104 0.980 0.188 0.011 !       3.48 eA-3
C105 0.015 0.725 0.017 !       3.36 eA-3
C106 0.107 0.221 0.051 !       3.34 eA-3
C107 0.063 0.063 0.453 !       2.29 eA-3
C108 0.059 0.052 0.090 !       1.86 eA-3
C109 1.002 0.556 0.439 !       0.90 eA-3
C110 0.106 1.005 0.455 !       0.85 eA-3
Q111 0.144 0.278 0.490 !       0.81 eA-3
Q112 0.235 0.276 0.433 !       0.80 eA-3
C113 0.171 0.245 0.086 !       0.80 eA-3
Q114 0.262 0.087 0.080 !       0.78 eA-3
C115 0.924 0.503 0.369 !       0.77 eA-3
Q116 0.114 0.597 0.168 !       0.76 eA-3
C117 0.969 0.096 0.453 !       0.74 eA-3
C118 0.998 0.036 0.399 !       0.72 eA-3
Q119 0.634 0.538 0.225 !       0.72 eA-3
C120 0.948 0.340 0.468 !       0.71 eA-3
Q121 0.280 0.567 0.020 !       0.71 eA-3
C122 0.014 0.058 0.115 !       0.71 eA-3
Q123 0.085 0.351 0.381 !       0.70 eA-3
Q124 0.503 0.681 0.477 !       0.70 eA-3
Q125 0.136 0.885 0.354 !       0.70 eA-3
Q126 0.235 0.474 0.400 !       0.69 eA-3
C127 0.987 0.591 0.111 !       0.69 eA-3
Q128 0.109 0.496 0.196 !       0.69 eA-3
C129 0.943 0.146 0.496 !       0.69 eA-3
Q130 0.889 1.000 0.124 !       0.68 eA-3
Q131 0.704 0.973 0.371 !       0.67 eA-3
Q132 0.293 0.972 0.219 !       0.66 eA-3
Q133 0.652 0.432 0.304 !       0.65 eA-3
C134 0.009 0.621 0.416 !       0.65 eA-3
Q135 0.017 0.279 0.362 !       0.65 eA-3
Q136 0.983 0.721 0.638 !       0.65 eA-3
Q137 0.021 0.301 0.149 !       0.65 eA-3
Q138 0.139 0.561 0.122 !       0.64 eA-3
Q139 0.361 0.943 0.438 !       0.64 eA-3
Q140 0.999 0.186 0.178 !       0.64 eA-3
Q141 0.171 0.186 0.283 !       0.64 eA-3
Q142 0.030 0.880 0.192 !       0.64 eA-3
Q143 0.406 0.162 0.105 !       0.64 eA-3
C144 0.124 0.877 0.062 !       0.64 eA-3
Q145 0.905 0.757 0.074 !       0.63 eA-3
Q146 0.441 0.937 0.468 !       0.63 eA-3
Q147 0.238 0.900 0.052 !       0.62 eA-3
C148 0.896 0.696 0.033 !       0.62 eA-3
Q149 0.015 0.845 0.295 !       0.62 eA-3
Q150 0.880 0.096 0.212 !       0.61 eA-3
Q151 0.844 0.125 0.362 !       0.61 eA-3
Q152 0.278 0.715 0.446 !       0.60 eA-3
Q153 0.338 0.874 0.180 !       0.60 eA-3
C154 0.876 0.467 0.443 !       0.60 eA-3
Q155 0.394 0.695 0.167 !       0.60 eA-3
Q156 0.409 0.435 0.453 !       0.60 eA-3
C157 0.122 0.127 0.015 !       0.60 eA-3
Q158 0.409 0.592 0.140 !       0.60 eA-3
Q159 0.481 0.351 0.303 !       0.60 eA-3
C160 0.172 0.596 0.032 !       0.60 eA-3
Q161 0.154 0.250 0.181 !       0.59 eA-3
Q162 0.053 0.936 0.396 !       0.59 eA-3
Q163 0.565 0.532 0.456 !       0.58 eA-3
Q164 0.572 0.995 0.056 !       0.57 eA-3
Q165 0.635 0.661 0.021 !       0.57 eA-3
Q166 0.596 0.189 0.270 !       0.57 eA-3
C167 0.121 1.002 0.139 !       0.57 eA-3
Q168 0.479 0.064 0.463 !       0.56 eA-3
Q169 0.943 0.723 0.109 !       0.56 eA-3
Q170 0.483 0.075 0.330 !       0.56 eA-3
Q171 0.216 1.000 0.326 !       0.56 eA-3
Q172 0.386 0.810 0.478 !       0.56 eA-3
C173 0.081 0.923 0.020 !       0.55 eA-3
C174 0.147 0.029 0.424 !       0.55 eA-3
Q175 0.993 0.906 0.064 !       0.55 eA-3
Q176 0.120 0.905 0.433 !       0.55 eA-3
Q177 1.007 0.410 0.089 !       0.55 eA-3
Q178 0.635 0.279 0.419 !       0.54 eA-3
Q179 0.956 0.072 0.143 !       0.54 eA-3
Q180 0.686 0.909 0.155 !       0.54 eA-3
Q181 0.626 0.558 0.390 !       0.54 eA-3
Q182 0.783 0.282 0.475 !       0.54 eA-3
Q183 0.355 0.559 0.073 !       0.54 eA-3
Q184 0.467 0.155 0.207 !       0.54 eA-3
Q185 0.845 0.840 0.276 !       0.54 eA-3
Q186 0.745 0.818 0.013 !       0.54 eA-3
Q187 0.779 0.841 0.091 !       0.54 eA-3
Q188 0.812 0.253 0.497 !       0.54 eA-3
Q189 0.857 0.350 0.326 !       0.54 eA-3
C190 0.950 0.433 0.443 !       0.53 eA-3
Q191 0.128 0.736 0.392 !       0.53 eA-3
Q192 0.216 0.316 0.236 !       0.53 eA-3
Q193 0.172 0.655 0.105 !       0.53 eA-3
Q194 0.338 0.630 0.008 !       0.53 eA-3
Q195 0.030 0.726 0.219 !       0.52 eA-3
Q196 0.172 0.124 0.257 !       0.52 eA-3
Q197 0.048 0.279 0.444 !       0.52 eA-3
Q198 0.952 0.659 0.357 !       0.52 eA-3
Q199 0.951 0.869 0.254 !       0.52 eA-3
;


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 0.64156(9) 0.45777(16) 0.65794(7) 0.0322(5) Uani 1 1 d . . . . .
O4 O 0.6865(2) 0.1224(4) 0.70836(17) 0.0385(11) Uani 1 1 d . . . . .
O1 O 0.5451(2) 0.1311(4) 0.60773(17) 0.0368(11) Uani 1 1 d . . . . .
O2 O 0.5024(2) 0.3374(4) 0.61482(17) 0.0357(11) Uani 1 1 d . . . . .
O3 O 0.7344(2) 0.0125(4) 0.64633(17) 0.0376(11) Uani 1 1 d . . . . .
N1 N 0.7359(3) 0.4529(4) 0.68015(19) 0.0280(12) Uani 1 1 d . . . . .
C1 C 0.6290(3) 0.3100(5) 0.6259(2) 0.0284(15) Uani 1 1 d . . . . .
C43 C 0.7787(3) 0.5719(6) 0.7033(3) 0.0304(15) Uani 1 1 d . . . . .
C44 C 0.7168(3) 0.2109(6) 0.5684(2) 0.0306(15) Uani 1 1 d . . . . .
H44 H 0.7611 0.1554 0.5745 0.037 Uiso 1 1 calc R U . . .
C2 C 0.7025(3) 0.2391(5) 0.6280(2) 0.0295(15) Uani 1 1 d . . . . .
C3 C 0.8526(3) 0.2999(6) 0.6881(2) 0.0342(16) Uani 1 1 d . . . . .
H3 H 0.8795 0.3815 0.6990 0.041 Uiso 1 1 calc R U . . .
C4 C 0.5580(4) 0.2466(6) 0.6152(2) 0.0331(16) Uani 1 1 d . . . . .
C5 C 0.7925(4) 0.6324(6) 0.6046(3) 0.0359(16) Uani 1 1 d . . . . .
H5 H 0.7574 0.5601 0.5939 0.043 Uiso 1 1 calc R U . . .
C6 C 0.6527(3) 0.1367(6) 0.5286(2) 0.0359(16) Uani 1 1 d . . . . .
H6A H 0.6437 0.0562 0.5464 0.043 Uiso 1 1 calc R U . . .
H6B H 0.6074 0.1882 0.5220 0.043 Uiso 1 1 calc R U . . .
C7 C 0.6092(3) 0.3656(6) 0.7550(3) 0.0349(16) Uani 1 1 d . . . . .
H7 H 0.6406 0.2980 0.7504 0.042 Uiso 1 1 calc R U . . .
C8 C 0.5752(3) 0.3629(6) 0.7995(3) 0.0354(16) Uani 1 1 d . . . . .
H8 H 0.5831 0.2935 0.8246 0.042 Uiso 1 1 calc R U . . .
C9 C 0.7943(3) 0.5963(6) 0.7617(3) 0.0313(16) Uani 1 1 d . . . . .
C10 C 0.5708(3) 0.5854(6) 0.5611(3) 0.0341(16) Uani 1 1 d . . . . .
H10 H 0.5649 0.5030 0.5452 0.041 Uiso 1 1 calc R U . . .
C11 C 0.5148(4) 0.5641(6) 0.7682(3) 0.0372(17) Uani 1 1 d . . . . .
H11 H 0.4823 0.6299 0.7728 0.045 Uiso 1 1 calc R U . . .
C12 C 0.8361(3) 0.7728(6) 0.6888(3) 0.0364(17) Uani 1 1 d . . . . .
H12 H 0.8509 0.8314 0.6647 0.044 Uiso 1 1 calc R U . . .
C13 C 0.6110(3) 0.6002(5) 0.6168(3) 0.0290(15) Uani 1 1 d . . . . .
C14 C 0.7093(4) 0.1123(7) 0.6589(3) 0.0373(17) Uani 1 1 d . . . . .
C15 C 0.7342(3) 0.3332(6) 0.5392(2) 0.0334(16) Uani 1 1 d . . . . .
H15A H 0.7768 0.3766 0.5634 0.040 Uiso 1 1 calc R U . . .
H15B H 0.6918 0.3916 0.5333 0.040 Uiso 1 1 calc R U . . .
C16 C 0.8300(3) 0.7120(6) 0.7817(3) 0.0343(16) Uani 1 1 d . . . . .
H16 H 0.8408 0.7293 0.8202 0.041 Uiso 1 1 calc R U . . .
C17 C 0.8007(3) 0.6586(6) 0.6669(3) 0.0338(16) Uani 1 1 d . . . . .
C18 C 0.5897(3) 0.8311(6) 0.6080(3) 0.0370(17) Uani 1 1 d . . . . .
H18 H 0.5959 0.9140 0.6234 0.044 Uiso 1 1 calc R U . . .
C19 C 0.5396(4) 0.6906(6) 0.5289(3) 0.0403(18) Uani 1 1 d . . . . .
H19 H 0.5125 0.6790 0.4918 0.048 Uiso 1 1 calc R U . . .
C20 C 0.6210(3) 0.7258(6) 0.6400(3) 0.0343(16) Uani 1 1 d . . . . .
H20 H 0.6487 0.7378 0.6770 0.041 Uiso 1 1 calc R U . . .
C21 C 0.5478(3) 0.5677(6) 0.7234(3) 0.0356(16) Uani 1 1 d . . . . .
H21 H 0.5374 0.6356 0.6976 0.043 Uiso 1 1 calc R U . . .
C22 C 0.8624(3) 0.2161(6) 0.7422(3) 0.0364(17) Uani 1 1 d . . . . .
H22A H 0.8393 0.2604 0.7687 0.044 Uiso 1 1 calc R U . . .
H22B H 0.8366 0.1343 0.7324 0.044 Uiso 1 1 calc R U . . .
C23 C 0.7516(4) 0.3031(6) 0.4820(3) 0.0427(18) Uani 1 1 d . . . . .
H23A H 0.7600 0.3838 0.4641 0.051 Uiso 1 1 calc R U . . .
H23B H 0.7971 0.2523 0.4884 0.051 Uiso 1 1 calc R U . . .
C24 C 0.7771(3) 0.5046(6) 0.8060(2) 0.0330(16) Uani 1 1 d . . . . .
H24 H 0.7519 0.4277 0.7867 0.040 Uiso 1 1 calc R U . . .
C25 C 0.8496(3) 0.8007(6) 0.7465(3) 0.0373(17) Uani 1 1 d . . . . .
H25 H 0.8717 0.8788 0.7607 0.045 Uiso 1 1 calc R U . . .
C26 C 0.5296(4) 0.4636(6) 0.8064(3) 0.0387(17) Uani 1 1 d . . . . .
H26 H 0.5084 0.4638 0.8372 0.046 Uiso 1 1 calc R U . . .
C27 C 0.5489(4) 0.8129(6) 0.5524(3) 0.0388(17) Uani 1 1 d . . . . .
H27 H 0.5277 0.8840 0.5309 0.047 Uiso 1 1 calc R U . . .
C28 C 0.6886(4) 0.2292(6) 0.4428(3) 0.0397(17) Uani 1 1 d . . . . .
H28A H 0.6445 0.2835 0.4327 0.048 Uiso 1 1 calc R U . . .
H28B H 0.7031 0.2064 0.4084 0.048 Uiso 1 1 calc R U . . .
C29 C 0.9732(4) 0.2022(6) 0.6760(3) 0.0449(18) Uani 1 1 d . . . . .
H29A H 0.9958 0.1564 0.6496 0.054 Uiso 1 1 calc R U . . .
H29B H 0.9993 0.2841 0.6851 0.054 Uiso 1 1 calc R U . . .
C30 C 0.7254(4) 0.5684(6) 0.8391(3) 0.0448(19) Uani 1 1 d . . . . .
H30A H 0.7504 0.6413 0.8599 0.067 Uiso 1 1 calc R U . . .
H30B H 0.7132 0.5065 0.8648 0.067 Uiso 1 1 calc R U . . .
H30C H 0.6804 0.5971 0.8132 0.067 Uiso 1 1 calc R U . . .
C31 C 0.5970(3) 0.4691(6) 0.7167(3) 0.0336(16) Uani 1 1 d . . . . .
C32 C 0.9438(3) 0.1895(6) 0.7708(3) 0.0419(18) Uani 1 1 d . . . . .
H32A H 0.9469 0.1349 0.8036 0.050 Uiso 1 1 calc R U . . .
H32B H 0.9691 0.2706 0.7834 0.050 Uiso 1 1 calc R U . . .
C33 C 0.9826(4) 0.1221(6) 0.7296(3) 0.0425(18) Uani 1 1 d . . . . .
H33A H 1.0353 0.1114 0.7474 0.051 Uiso 1 1 calc R U . . .
H33B H 0.9610 0.0367 0.7202 0.051 Uiso 1 1 calc R U . . .
C34 C 0.8911(3) 0.2288(6) 0.6478(3) 0.0415(17) Uani 1 1 d . . . . .
H34A H 0.8656 0.1474 0.6363 0.050 Uiso 1 1 calc R U . . .
H34B H 0.8877 0.2811 0.6142 0.050 Uiso 1 1 calc R U . . .
C35 C 0.6712(4) 0.1070(6) 0.4718(3) 0.0415(18) Uani 1 1 d . . . . .
H35A H 0.7138 0.0491 0.4782 0.050 Uiso 1 1 calc R U . . .
H35B H 0.6291 0.0630 0.4473 0.050 Uiso 1 1 calc R U . . .
C36 C 0.6913(4) 0.0060(6) 0.7428(3) 0.0430(18) Uani 1 1 d . . . . .
H36A H 0.7287 -0.0525 0.7350 0.052 Uiso 1 1 calc R U . . .
H36B H 0.6435 -0.0386 0.7344 0.052 Uiso 1 1 calc R U . . .
C37 C 0.7612(4) 0.7490(6) 0.5656(3) 0.0463(19) Uani 1 1 d . . . . .
H37A H 0.7155 0.7784 0.5735 0.069 Uiso 1 1 calc R U . . .
H37B H 0.7518 0.7222 0.5268 0.069 Uiso 1 1 calc R U . . .
H37C H 0.7971 0.8182 0.5723 0.069 Uiso 1 1 calc R U . . .
C38 C 0.4269(4) 0.2858(7) 0.6102(3) 0.0480(19) Uani 1 1 d . . . . .
H38A H 0.4216 0.2569 0.6469 0.058 Uiso 1 1 calc R U . . .
H38B H 0.4174 0.2128 0.5844 0.058 Uiso 1 1 calc R U . . .
C39 C 0.8671(4) 0.5896(6) 0.5946(3) 0.0413(18) Uani 1 1 d . . . . .
H39A H 0.9031 0.6577 0.6058 0.062 Uiso 1 1 calc R U . . .
H39B H 0.8613 0.5708 0.5553 0.062 Uiso 1 1 calc R U . . .
H39C H 0.8841 0.5132 0.6165 0.062 Uiso 1 1 calc R U . . .
C40 C 0.8497(4) 0.4610(6) 0.8478(3) 0.0483(19) Uani 1 1 d . . . . .
H40A H 0.8839 0.4282 0.8271 0.072 Uiso 1 1 calc R U . . .
H40B H 0.8386 0.3940 0.8718 0.072 Uiso 1 1 calc R U . . .
H40C H 0.8719 0.5335 0.8704 0.072 Uiso 1 1 calc R U . . .
C41 C 0.3739(4) 0.3924(7) 0.5888(3) 0.054(2) Uani 1 1 d . . . . .
H41A H 0.3829 0.4628 0.6153 0.081 Uiso 1 1 calc R U . . .
H41B H 0.3237 0.3617 0.5840 0.081 Uiso 1 1 calc R U . . .
H41C H 0.3808 0.4218 0.5531 0.081 Uiso 1 1 calc R U . . .
C42 C 0.7125(5) 0.0472(7) 0.8043(3) 0.064(2) Uani 1 1 d . . . . .
H42A H 0.7601 0.0901 0.8123 0.096 Uiso 1 1 calc R U . . .
H42B H 0.7155 -0.0278 0.8280 0.096 Uiso 1 1 calc R U . . .
H42C H 0.6754 0.1056 0.8115 0.096 Uiso 1 1 calc R U . . .
B1 B 0.7671(4) 0.3338(7) 0.6655(3) 0.036(2) 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 N1 1.693(5) . ?
P1 C1 1.703(6) . ?
P1 C13 1.791(6) . ?
P1 C31 1.823(6) . ?
O4 C14 1.375(7) . ?
O4 C36 1.457(7) . ?
O1 C4 1.219(7) . ?
O2 C4 1.388(7) . ?
O2 C38 1.470(7) . ?
O3 C14 1.200(7) . ?
N1 B1 1.438(8) . ?
N1 C43 1.494(7) . ?
C1 C4 1.430(8) . ?
C1 C2 1.530(8) . ?
C43 C17 1.389(8) . ?
C43 C9 1.407(8) . ?
C44 C15 1.522(8) . ?
C44 C6 1.539(8) . ?
C44 C2 1.567(8) . ?
C44 H44 0.9800 . ?
C2 C14 1.500(8) . ?
C2 B1 1.639(9) . ?
C3 C34 1.534(8) . ?
C3 C22 1.552(8) . ?
C3 B1 1.578(10) . ?
C3 H3 0.9800 . ?
C5 C17 1.515(8) . ?
C5 C39 1.523(8) . ?
C5 C37 1.556(8) . ?
C5 H5 0.9800 . ?
C6 C35 1.537(8) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C8 1.383(8) . ?
C7 C31 1.400(8) . ?
C7 H7 0.9300 . ?
C8 C26 1.373(8) . ?
C8 H8 0.9300 . ?
C9 C16 1.393(8) . ?
C9 C24 1.527(8) . ?
C10 C19 1.381(8) . ?
C10 C13 1.390(8) . ?
C10 H10 0.9300 . ?
C11 C26 1.375(8) . ?
C11 C21 1.377(8) . ?
C11 H11 0.9300 . ?
C12 C17 1.388(8) . ?
C12 C25 1.401(8) . ?
C12 H12 0.9300 . ?
C13 C20 1.407(8) . ?
C15 C23 1.537(8) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 C25 1.362(8) . ?
C16 H16 0.9300 . ?
C18 C20 1.380(8) . ?
C18 C27 1.394(8) . ?
C18 H18 0.9300 . ?
C19 C27 1.379(8) . ?
C19 H19 0.9300 . ?
C20 H20 0.9300 . ?
C21 C31 1.400(8) . ?
C21 H21 0.9300 . ?
C22 C32 1.520(8) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 C28 1.518(8) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C24 C30 1.539(8) . ?
C24 C40 1.539(8) . ?
C24 H24 0.9800 . ?
C25 H25 0.9300 . ?
C26 H26 0.9300 . ?
C27 H27 0.9300 . ?
C28 C35 1.518(8) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C29 C33 1.523(8) . ?
C29 C34 1.528(8) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C32 C33 1.534(9) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C36 C42 1.515(9) . ?
C36 H36A 0.9700 . ?
C36 H36B 0.9700 . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?
C38 C41 1.480(8) . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C39 H39A 0.9600 . ?
C39 H39B 0.9600 . ?
C39 H39C 0.9600 . ?
C40 H40A 0.9600 . ?
C40 H40B 0.9600 . ?
C40 H40C 0.9600 . ?
C41 H41A 0.9600 . ?
C41 H41B 0.9600 . ?
C41 H41C 0.9600 . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 P1 C1 97.7(3) . . ?
N1 P1 C13 111.2(3) . . ?
C1 P1 C13 119.2(3) . . ?
N1 P1 C31 112.1(3) . . ?
C1 P1 C31 112.4(3) . . ?
C13 P1 C31 104.3(3) . . ?
C14 O4 C36 117.2(5) . . ?
C4 O2 C38 116.2(5) . . ?
B1 N1 C43 126.0(5) . . ?
B1 N1 P1 112.9(4) . . ?
C43 N1 P1 120.3(4) . . ?
C4 C1 C2 123.5(5) . . ?
C4 C1 P1 120.6(5) . . ?
C2 C1 P1 113.1(4) . . ?
C17 C43 C9 120.9(6) . . ?
C17 C43 N1 119.9(5) . . ?
C9 C43 N1 119.2(5) . . ?
C15 C44 C6 109.5(5) . . ?
C15 C44 C2 112.6(5) . . ?
C6 C44 C2 113.6(5) . . ?
C15 C44 H44 106.9 . . ?
C6 C44 H44 106.9 . . ?
C2 C44 H44 106.9 . . ?
C14 C2 C1 113.4(5) . . ?
C14 C2 C44 107.1(5) . . ?
C1 C2 C44 114.0(5) . . ?
C14 C2 B1 106.2(5) . . ?
C1 C2 B1 104.6(5) . . ?
C44 C2 B1 111.4(5) . . ?
C34 C3 C22 107.7(5) . . ?
C34 C3 B1 117.5(5) . . ?
C22 C3 B1 108.6(5) . . ?
C34 C3 H3 107.5 . . ?
C22 C3 H3 107.5 . . ?
B1 C3 H3 107.5 . . ?
O1 C4 O2 122.7(6) . . ?
O1 C4 C1 127.7(6) . . ?
O2 C4 C1 109.6(5) . . ?
C17 C5 C39 109.8(5) . . ?
C17 C5 C37 114.1(5) . . ?
C39 C5 C37 109.9(5) . . ?
C17 C5 H5 107.6 . . ?
C39 C5 H5 107.6 . . ?
C37 C5 H5 107.6 . . ?
C35 C6 C44 111.3(5) . . ?
C35 C6 H6A 109.4 . . ?
C44 C6 H6A 109.4 . . ?
C35 C6 H6B 109.4 . . ?
C44 C6 H6B 109.4 . . ?
H6A C6 H6B 108.0 . . ?
C8 C7 C31 120.6(6) . . ?
C8 C7 H7 119.7 . . ?
C31 C7 H7 119.7 . . ?
C26 C8 C7 119.4(6) . . ?
C26 C8 H8 120.3 . . ?
C7 C8 H8 120.3 . . ?
C16 C9 C43 118.0(6) . . ?
C16 C9 C24 116.5(5) . . ?
C43 C9 C24 125.5(5) . . ?
C19 C10 C13 121.3(6) . . ?
C19 C10 H10 119.3 . . ?
C13 C10 H10 119.3 . . ?
C26 C11 C21 120.3(6) . . ?
C26 C11 H11 119.8 . . ?
C21 C11 H11 119.8 . . ?
C17 C12 C25 120.9(6) . . ?
C17 C12 H12 119.6 . . ?
C25 C12 H12 119.6 . . ?
C10 C13 C20 118.7(6) . . ?
C10 C13 P1 118.5(5) . . ?
C20 C13 P1 122.5(5) . . ?
O3 C14 O4 120.7(6) . . ?
O3 C14 C2 127.5(6) . . ?
O4 C14 C2 111.7(6) . . ?
C44 C15 C23 111.9(5) . . ?
C44 C15 H15A 109.2 . . ?
C23 C15 H15A 109.2 . . ?
C44 C15 H15B 109.2 . . ?
C23 C15 H15B 109.2 . . ?
H15A C15 H15B 107.9 . . ?
C25 C16 C9 122.1(6) . . ?
C25 C16 H16 118.9 . . ?
C9 C16 H16 118.9 . . ?
C12 C17 C43 119.0(6) . . ?
C12 C17 C5 117.4(6) . . ?
C43 C17 C5 123.6(6) . . ?
C20 C18 C27 119.8(6) . . ?
C20 C18 H18 120.1 . . ?
C27 C18 H18 120.1 . . ?
C27 C19 C10 119.3(6) . . ?
C27 C19 H19 120.3 . . ?
C10 C19 H19 120.3 . . ?
C18 C20 C13 120.1(6) . . ?
C18 C20 H20 120.0 . . ?
C13 C20 H20 120.0 . . ?
C11 C21 C31 120.0(6) . . ?
C11 C21 H21 120.0 . . ?
C31 C21 H21 120.0 . . ?
C32 C22 C3 112.7(5) . . ?
C32 C22 H22A 109.0 . . ?
C3 C22 H22A 109.0 . . ?
C32 C22 H22B 109.0 . . ?
C3 C22 H22B 109.0 . . ?
H22A C22 H22B 107.8 . . ?
C28 C23 C15 112.1(5) . . ?
C28 C23 H23A 109.2 . . ?
C15 C23 H23A 109.2 . . ?
C28 C23 H23B 109.2 . . ?
C15 C23 H23B 109.2 . . ?
H23A C23 H23B 107.9 . . ?
C9 C24 C30 111.6(5) . . ?
C9 C24 C40 110.6(5) . . ?
C30 C24 C40 109.2(5) . . ?
C9 C24 H24 108.4 . . ?
C30 C24 H24 108.4 . . ?
C40 C24 H24 108.4 . . ?
C16 C25 C12 119.1(6) . . ?
C16 C25 H25 120.5 . . ?
C12 C25 H25 120.5 . . ?
C8 C26 C11 120.9(6) . . ?
C8 C26 H26 119.5 . . ?
C11 C26 H26 119.5 . . ?
C19 C27 C18 120.7(6) . . ?
C19 C27 H27 119.7 . . ?
C18 C27 H27 119.7 . . ?
C35 C28 C23 109.9(5) . . ?
C35 C28 H28A 109.7 . . ?
C23 C28 H28A 109.7 . . ?
C35 C28 H28B 109.7 . . ?
C23 C28 H28B 109.7 . . ?
H28A C28 H28B 108.2 . . ?
C33 C29 C34 112.1(5) . . ?
C33 C29 H29A 109.2 . . ?
C34 C29 H29A 109.2 . . ?
C33 C29 H29B 109.2 . . ?
C34 C29 H29B 109.2 . . ?
H29A C29 H29B 107.9 . . ?
C24 C30 H30A 109.5 . . ?
C24 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C24 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C21 C31 C7 118.7(6) . . ?
C21 C31 P1 124.7(5) . . ?
C7 C31 P1 116.5(5) . . ?
C22 C32 C33 110.4(5) . . ?
C22 C32 H32A 109.6 . . ?
C33 C32 H32A 109.6 . . ?
C22 C32 H32B 109.6 . . ?
C33 C32 H32B 109.6 . . ?
H32A C32 H32B 108.1 . . ?
C29 C33 C32 110.1(5) . . ?
C29 C33 H33A 109.6 . . ?
C32 C33 H33A 109.6 . . ?
C29 C33 H33B 109.6 . . ?
C32 C33 H33B 109.6 . . ?
H33A C33 H33B 108.2 . . ?
C29 C34 C3 111.2(5) . . ?
C29 C34 H34A 109.4 . . ?
C3 C34 H34A 109.4 . . ?
C29 C34 H34B 109.4 . . ?
C3 C34 H34B 109.4 . . ?
H34A C34 H34B 108.0 . . ?
C28 C35 C6 111.9(5) . . ?
C28 C35 H35A 109.2 . . ?
C6 C35 H35A 109.2 . . ?
C28 C35 H35B 109.2 . . ?
C6 C35 H35B 109.2 . . ?
H35A C35 H35B 107.9 . . ?
O4 C36 C42 107.7(5) . . ?
O4 C36 H36A 110.2 . . ?
C42 C36 H36A 110.2 . . ?
O4 C36 H36B 110.2 . . ?
C42 C36 H36B 110.2 . . ?
H36A C36 H36B 108.5 . . ?
C5 C37 H37A 109.5 . . ?
C5 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C5 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
O2 C38 C41 106.9(5) . . ?
O2 C38 H38A 110.3 . . ?
C41 C38 H38A 110.3 . . ?
O2 C38 H38B 110.3 . . ?
C41 C38 H38B 110.3 . . ?
H38A C38 H38B 108.6 . . ?
C5 C39 H39A 109.5 . . ?
C5 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C5 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C24 C40 H40A 109.5 . . ?
C24 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C24 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C38 C41 H41A 109.5 . . ?
C38 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C38 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 . . ?
N1 B1 C3 122.0(6) . . ?
N1 B1 C2 111.5(6) . . ?
C3 B1 C2 126.3(6) . . ?

_refine_diff_density_max         0.295
_refine_diff_density_min         -0.338
_refine_diff_density_rms         0.067


_chemical_properties_physical    ', Moisture-sensitive'
