# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2015

 
data_pbts150113
 
_audit_creation_method            SHELXL-2013
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          'C33 H48 N3 P, C H2 Cl2, 2(Br)'
_chemical_formula_sum
 'C34 H50 Br2 Cl2 N3 P' 
_chemical_formula_weight          762.46

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'
 'Br'  'Br'  -0.2901   2.4595
 '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       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                    12.1055(4)
_cell_length_b                    25.0614(9)
_cell_length_c                    14.6620(4)
_cell_angle_alpha                 90
_cell_angle_beta                  123.958(2)
_cell_angle_gamma                 90
_cell_volume                      3689.5(2)
_cell_formula_units_Z             4
_cell_measurement_temperature     173(2)
_cell_measurement_reflns_used     7390 
_cell_measurement_theta_min       2.33
_cell_measurement_theta_max       26.76
 
_exptl_crystal_description        'prism' 
_exptl_crystal_colour             'colourless'
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_method     ?              
_exptl_crystal_density_diffrn     1.373          
_exptl_crystal_F_000              1576
_exptl_transmission_factor_min    ?                                             
_exptl_transmission_factor_max    ?                                             
_exptl_crystal_size_max           0.350
_exptl_crystal_size_mid           0.250
_exptl_crystal_size_min           0.200
_exptl_absorpt_coefficient_mu     2.412
_shelx_estimated_absorpt_T_min    0.486
_shelx_estimated_absorpt_T_max    0.644
_exptl_absorpt_correction_type    'multi-scan' 
_exptl_absorpt_correction_T_min   0.6625  
_exptl_absorpt_correction_T_max   0.7456
_exptl_absorpt_process_details    'sadabs'
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       173(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_source                    'fine focus sealed tube'                       
_diffrn_measurement_device_type   'Bruker APEX-II CCD'
_diffrn_measurement_method        'φ and ω scans'
_diffrn_detector_area_resol_mean  ? 
_diffrn_reflns_number             36844
_diffrn_reflns_av_unetI/netI      0.0399
_diffrn_reflns_av_R_equivalents   0.0413
_diffrn_reflns_limit_h_min        -15
_diffrn_reflns_limit_h_max        15
_diffrn_reflns_limit_k_min        -33
_diffrn_reflns_limit_k_max        32
_diffrn_reflns_limit_l_min        -19
_diffrn_reflns_limit_l_max        19
_diffrn_reflns_theta_min          1.625
_diffrn_reflns_theta_max          28.005
_diffrn_reflns_theta_full         25.242
_diffrn_measured_fraction_theta_max   1.000
_diffrn_measured_fraction_theta_full  1.000
_diffrn_reflns_Laue_measured_fraction_max    1.000
_diffrn_reflns_Laue_measured_fraction_full   1.000
_diffrn_reflns_point_group_measured_fraction_max   1.000
_diffrn_reflns_point_group_measured_fraction_full  1.000
_reflns_number_total              8912
_reflns_number_gt                 6146
_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 APEX2'
_computing_cell_refinement        'Bruker SAINT'
_computing_data_reduction         'Bruker SAINT'
_computing_structure_solution     'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement   'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics     'Bruker SHELXTL'
_computing_publication_material   'Bruker SHELXTL'
 
_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)+(0.0581P)²+8.2172P] 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          8912
_refine_ls_number_parameters      372
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0934
_refine_ls_R_factor_gt            0.0585
_refine_ls_wR_factor_ref          0.1487
_refine_ls_wR_factor_gt           0.1313
_refine_ls_goodness_of_fit_ref    1.021
_refine_ls_restrained_S_all       1.021
_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
C1 C 0.6033(3) 0.73527(15) 0.3774(3) 0.0291(7) Uani 1 1 d . . . . .
H1 H 0.5719 0.7597 0.4075 0.035 Uiso 1 1 calc R U . . .
C2 C 0.7289(4) 0.67729(16) 0.3606(3) 0.0342(8) Uani 1 1 d . . . . .
H2 H 0.8009 0.6545 0.3781 0.041 Uiso 1 1 calc R U . . .
C3 C 0.6161(4) 0.68457(16) 0.2603(3) 0.0354(8) Uani 1 1 d . . . . .
H3 H 0.5938 0.6680 0.1938 0.043 Uiso 1 1 calc R U . . .
C4 C 0.4080(4) 0.74119(16) 0.1868(3) 0.0324(8) Uani 1 1 d . . . . .
C5 C 0.2965(4) 0.71335(18) 0.1648(3) 0.0412(9) Uani 1 1 d . . . . .
C6 C 0.1730(4) 0.7360(2) 0.0874(4) 0.0503(11) Uani 1 1 d . . . . .
H6 H 0.0939 0.7187 0.0708 0.060 Uiso 1 1 calc R U . . .
C7 C 0.1637(4) 0.7828(2) 0.0347(4) 0.0518(12) Uani 1 1 d . . . . .
H7 H 0.0785 0.7976 -0.0171 0.062 Uiso 1 1 calc R U . . .
C8 C 0.2761(5) 0.8084(2) 0.0559(4) 0.0490(11) Uani 1 1 d . . . . .
H8 H 0.2676 0.8404 0.0177 0.059 Uiso 1 1 calc R U . . .
C9 C 0.4032(4) 0.78799(17) 0.1333(3) 0.0413(9) Uani 1 1 d . . . . .
C10 C 0.3041(5) 0.6599(2) 0.2162(5) 0.0579(13) Uani 1 1 d . . . . .
H10 H 0.3987 0.6535 0.2780 0.069 Uiso 1 1 calc R U . . .
C11 C 0.2626(7) 0.6158(2) 0.1302(7) 0.090(2) Uani 1 1 d . . . . .
H11A H 0.1678 0.6196 0.0718 0.135 Uiso 1 1 calc R U . . .
H11B H 0.2782 0.5808 0.1653 0.135 Uiso 1 1 calc R U . . .
H11C H 0.3152 0.6189 0.0984 0.135 Uiso 1 1 calc R U . . .
C12 C 0.2177(6) 0.6580(3) 0.2628(5) 0.0761(18) Uani 1 1 d . . . . .
H12A H 0.2397 0.6884 0.3122 0.114 Uiso 1 1 calc R U . . .
H12B H 0.2350 0.6247 0.3037 0.114 Uiso 1 1 calc R U . . .
H12C H 0.1235 0.6597 0.2023 0.114 Uiso 1 1 calc R U . . .
C13 C 0.5276(5) 0.8169(2) 0.1591(5) 0.0629(14) Uani 1 1 d . . . . .
H13 H 0.6064 0.7937 0.2082 0.075 Uiso 1 1 calc R U . . .
C14 C 0.5457(9) 0.8695(3) 0.2186(6) 0.109(3) Uani 1 1 d . . . . .
H14A H 0.4761 0.8947 0.1678 0.164 Uiso 1 1 calc R U . . .
H14B H 0.6333 0.8846 0.2447 0.164 Uiso 1 1 calc R U . . .
H14C H 0.5392 0.8631 0.2814 0.164 Uiso 1 1 calc R U . . .
C15 C 0.5221(7) 0.8279(3) 0.0534(5) 0.0777(18) Uani 1 1 d . . . . .
H15A H 0.4977 0.7951 0.0099 0.116 Uiso 1 1 calc R U . . .
H15B H 0.6096 0.8401 0.0727 0.116 Uiso 1 1 calc R U . . .
H15C H 0.4555 0.8555 0.0102 0.116 Uiso 1 1 calc R U . . .
C16 C 0.8197(4) 0.71453(16) 0.5492(3) 0.0327(8) Uani 1 1 d . . . . .
C17 C 0.8104(5) 0.75256(19) 0.6121(3) 0.0485(11) Uani 1 1 d . . . . .
H17 H 0.7364 0.7761 0.5815 0.058 Uiso 1 1 calc R U . . .
C18 C 0.9137(5) 0.7550(2) 0.7221(4) 0.0644(14) Uani 1 1 d . . . . .
H18 H 0.9132 0.7812 0.7687 0.077 Uiso 1 1 calc R U . . .
C19 C 1.0171(5) 0.7192(2) 0.7632(4) 0.0616(14) Uani 1 1 d . . . . .
H19 H 1.0882 0.7201 0.8387 0.074 Uiso 1 1 calc R U . . .
C20 C 1.0162(4) 0.68228(19) 0.6940(3) 0.0477(11) Uani 1 1 d . . . . .
C21 C 1.1292(5) 0.6428(2) 0.7345(5) 0.0751(17) Uani 1 1 d . . . . .
H21A H 1.1705 0.6363 0.8138 0.090 Uiso 1 1 calc R U . . .
H21B H 1.1979 0.6590 0.7263 0.090 Uiso 1 1 calc R U . . .
C22 C 0.9536(7) 0.5447(2) 0.6687(5) 0.0717(17) Uani 1 1 d . . . . .
H22 H 0.9841 0.5068 0.6853 0.086 Uiso 1 1 calc R U . A 1
C23 C 0.8125(17) 0.5442(6) 0.5450(14) 0.0873(15) Uani 0.5 1 d . . P B 1
H23A H 0.7733 0.5804 0.5267 0.105 Uiso 0.5 1 calc R U P B 1
H23B H 0.8308 0.5338 0.4895 0.105 Uiso 0.5 1 calc R U P B 1
C24 C 0.7145(16) 0.5052(6) 0.5419(14) 0.0873(15) Uani 0.5 1 d . . P B 1
H24A H 0.7481 0.4683 0.5489 0.105 Uiso 0.5 1 calc R U P B 1
H24B H 0.6280 0.5081 0.4700 0.105 Uiso 0.5 1 calc R U P B 1
C25 C 0.6935(16) 0.5158(6) 0.6348(14) 0.0873(15) Uani 0.5 1 d . . P B 1
H25A H 0.6459 0.5500 0.6206 0.105 Uiso 0.5 1 calc R U P B 1
H25B H 0.6368 0.4872 0.6345 0.105 Uiso 0.5 1 calc R U P B 1
C26 C 0.8196(16) 0.5179(7) 0.7439(15) 0.0873(15) Uani 0.5 1 d . . P B 1
H26A H 0.8617 0.4822 0.7631 0.105 Uiso 0.5 1 calc R U P B 1
H26B H 0.8016 0.5279 0.7997 0.105 Uiso 0.5 1 calc R U P B 1
C27 C 0.9153(15) 0.5587(6) 0.7452(14) 0.0873(15) Uani 0.5 1 d . . P B 1
H27A H 0.8722 0.5943 0.7252 0.105 Uiso 0.5 1 calc R U P B 1
H27B H 0.9966 0.5612 0.8207 0.105 Uiso 0.5 1 calc R U P B 1
C23B C 0.8215(17) 0.5584(6) 0.5899(14) 0.0873(15) Uani 0.5 1 d . . P B 2
H23C H 0.8022 0.5556 0.5149 0.105 Uiso 0.5 1 calc R U P B 2
H23D H 0.8030 0.5954 0.6014 0.105 Uiso 0.5 1 calc R U P B 2
C24B C 0.7359(16) 0.5181(6) 0.6052(14) 0.0873(15) Uani 0.5 1 d . . P B 2
H24C H 0.6402 0.5253 0.5505 0.105 Uiso 0.5 1 calc R U P B 2
H24D H 0.7554 0.4813 0.5935 0.105 Uiso 0.5 1 calc R U P B 2
C25B C 0.7675(16) 0.5234(8) 0.7209(16) 0.0873(15) Uani 0.5 1 d . . P B 2
H25C H 0.7442 0.5599 0.7307 0.105 Uiso 0.5 1 calc R U P B 2
H25D H 0.7121 0.4978 0.7301 0.105 Uiso 0.5 1 calc R U P B 2
C26B C 0.9108(15) 0.5131(6) 0.8068(14) 0.0873(15) Uani 0.5 1 d . . P B 2
H26C H 0.9341 0.4761 0.7999 0.105 Uiso 0.5 1 calc R U P B 2
H26D H 0.9277 0.5172 0.8808 0.105 Uiso 0.5 1 calc R U P B 2
C27B C 0.9953(15) 0.5523(6) 0.7929(13) 0.0873(15) Uani 0.5 1 d . . P B 2
H27C H 1.0912 0.5445 0.8457 0.105 Uiso 0.5 1 calc R U P B 2
H27D H 0.9776 0.5893 0.8051 0.105 Uiso 0.5 1 calc R U P B 2
C28 C 1.2017(11) 0.5271(4) 0.7064(11) 0.063(2) Uani 0.5 1 d . . P C 1
H28 H 1.1643 0.4940 0.6610 0.075 Uiso 0.5 1 calc R U P C 1
C29 C 1.261(2) 0.5176(12) 0.839(2) 0.129(3) Uani 0.5 1 d . . P C 1
H29A H 1.3017 0.5507 0.8816 0.155 Uiso 0.5 1 calc R U P C 1
H29B H 1.1890 0.5061 0.8475 0.155 Uiso 0.5 1 calc R U P C 1
C30 C 1.3681(17) 0.4723(8) 0.8753(16) 0.129(3) Uani 0.5 1 d . . P C 1
H30A H 1.4023 0.4623 0.9521 0.155 Uiso 0.5 1 calc R U P C 1
H30B H 1.3231 0.4405 0.8289 0.155 Uiso 0.5 1 calc R U P C 1
C31 C 1.4631(18) 0.4832(9) 0.8704(17) 0.129(3) Uani 0.5 1 d . . P C 1
H31A H 1.5239 0.4521 0.8956 0.155 Uiso 0.5 1 calc R U P C 1
H31B H 1.5128 0.5134 0.9205 0.155 Uiso 0.5 1 calc R U P C 1
C32 C 1.418(2) 0.4989(10) 0.7482(16) 0.129(3) Uani 0.5 1 d . . P C 1
H32A H 1.3699 0.4687 0.6978 0.155 Uiso 0.5 1 calc R U P C 1
H32B H 1.4978 0.5066 0.7473 0.155 Uiso 0.5 1 calc R U P C 1
C33 C 1.3221(17) 0.5512(9) 0.7067(17) 0.129(3) Uani 0.5 1 d . . P C 1
H33A H 1.3642 0.5814 0.7587 0.155 Uiso 0.5 1 calc R U P C 1
H33B H 1.2951 0.5627 0.6324 0.155 Uiso 0.5 1 calc R U P C 1
C28B C 1.2512(11) 0.5523(4) 0.7351(11) 0.063(2) Uani 0.5 1 d . . P C 2
H28B H 1.3173 0.5822 0.7658 0.075 Uiso 0.5 1 calc R U P C 2
C29B C 1.287(2) 0.5125(11) 0.822(2) 0.129(3) Uani 0.5 1 d . . P C 2
H29C H 1.2061 0.4953 0.8091 0.155 Uiso 0.5 1 calc R U P C 2
H29D H 1.3338 0.5304 0.8950 0.155 Uiso 0.5 1 calc R U P C 2
C30B C 1.3934(19) 0.4640(9) 0.8214(17) 0.129(3) Uani 0.5 1 d . . P C 2
H30C H 1.4542 0.4501 0.8971 0.155 Uiso 0.5 1 calc R U P C 2
H30D H 1.3381 0.4338 0.7743 0.155 Uiso 0.5 1 calc R U P C 2
C31B C 1.4571(19) 0.4798(9) 0.7898(18) 0.129(3) Uani 0.5 1 d . . P C 2
H31C H 1.5149 0.4504 0.7950 0.155 Uiso 0.5 1 calc R U P C 2
H31D H 1.5161 0.5084 0.8402 0.155 Uiso 0.5 1 calc R U P C 2
C32B C 1.3915(18) 0.4985(9) 0.6895(16) 0.129(3) Uani 0.5 1 d . . P C 2
H32C H 1.3722 0.4688 0.6380 0.155 Uiso 0.5 1 calc R U P C 2
H32D H 1.4481 0.5246 0.6831 0.155 Uiso 0.5 1 calc R U P C 2
C33B C 1.2553(18) 0.5265(9) 0.6547(16) 0.129(3) Uani 0.5 1 d . . P C 2
H33C H 1.2323 0.5526 0.5960 0.155 Uiso 0.5 1 calc R U P C 2
H33D H 1.1847 0.4989 0.6223 0.155 Uiso 0.5 1 calc R U P C 2
C34 C 0.8098(8) 0.8922(3) 0.5325(6) 0.092(2) Uani 1 1 d . . . . .
H34A H 0.7199 0.8825 0.5133 0.111 Uiso 1 1 calc R U . . .
H34B H 0.8726 0.8895 0.6133 0.111 Uiso 1 1 calc R U . . .
N1 N 0.7201(3) 0.70945(12) 0.4336(2) 0.0291(6) Uani 1 1 d . . . . .
N2 N 0.5390(3) 0.72083(13) 0.2726(2) 0.0294(6) Uani 1 1 d . . . . .
N3 N 0.9185(3) 0.67968(14) 0.5865(3) 0.0403(8) Uani 1 1 d . . . . .
P1 P 1.07899(14) 0.58007(6) 0.66333(11) 0.0618(4) Uani 1 1 d . . . . .
Br1 Br 0.98232(4) 0.89902(2) 0.85555(4) 0.04471(13) Uani 1 1 d . . . . .
Br2 Br 0.47916(4) 0.83449(2) 0.46548(3) 0.04640(14) Uani 1 1 d . . . . .
Cl1 Cl 0.8083(5) 0.95707(11) 0.4909(2) 0.207(2) Uani 1 1 d . . . . .
Cl2 Cl 0.85916(18) 0.84729(9) 0.46662(17) 0.0984(6) Uani 1 1 d . . . . .
H1P H 1.022(4) 0.5823(17) 0.552(3) 0.045(12) Uiso 1 1 d . . . . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
C1 N2 1.327(5) . ?
C1 N1 1.340(4) . ?
C1 H1 0.9500 . ?
C2 C3 1.348(5) . ?
C2 N1 1.391(5) . ?
C2 H2 0.9500 . ?
C3 N2 1.385(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.388(6) . ?
C4 C9 1.394(6) . ?
C4 N2 1.459(4) . ?
C5 C6 1.397(6) . ?
C5 C10 1.515(6) . ?
C6 C7 1.373(7) . ?
C6 H6 0.9500 . ?
C7 C8 1.374(7) . ?
C7 H7 0.9500 . ?
C8 C9 1.402(6) . ?
C8 H8 0.9500 . ?
C9 C13 1.516(7) . ?
C10 C11 1.535(9) . ?
C10 C12 1.536(7) . ?
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 C14 1.528(9) . ?
C13 C15 1.539(8) . ?
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 . ?
C16 N3 1.328(5) . ?
C16 C17 1.374(6) . ?
C16 N1 1.435(4) . ?
C17 C18 1.384(6) . ?
C17 H17 0.9500 . ?
C18 C19 1.375(8) . ?
C18 H18 0.9500 . ?
C19 C20 1.369(7) . ?
C19 H19 0.9500 . ?
C20 N3 1.344(5) . ?
C20 C21 1.515(7) . ?
C21 P1 1.796(6) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 C23B 1.396(18) . ?
C22 C27 1.475(14) . ?
C22 C27B 1.605(16) . ?
C22 C23 1.657(19) . ?
C22 P1 1.797(6) . ?
C22 H22 1.0000 . ?
C23 C24 1.52(2) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 C25 1.542(19) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 C26 1.47(2) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 C27 1.54(2) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C23B C24B 1.55(2) . ?
C23B H23C 0.9900 . ?
C23B H23D 0.9900 . ?
C24B C25B 1.52(2) . ?
C24B H24C 0.9900 . ?
C24B H24D 0.9900 . ?
C25B C26B 1.49(2) . ?
C25B H25C 0.9900 . ?
C25B H25D 0.9900 . ?
C26B C27B 1.512(19) . ?
C26B H26C 0.9900 . ?
C26B H26D 0.9900 . ?
C27B H27C 0.9900 . ?
C27B H27D 0.9900 . ?
C28 C33 1.57(2) . ?
C28 C29 1.67(3) . ?
C28 P1 1.822(11) . ?
C28 H28 1.0000 . ?
C29 C30 1.58(2) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 C31 1.22(3) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C32 1.60(3) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 C33 1.63(2) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C28B C33B 1.37(2) . ?
C28B C29B 1.48(3) . ?
C28B P1 1.866(11) . ?
C28B H28B 1.0000 . ?
C29B C30B 1.77(2) . ?
C29B H29C 0.9900 . ?
C29B H29D 0.9900 . ?
C30B C31B 1.17(3) . ?
C30B H30C 0.9900 . ?
C30B H30D 0.9900 . ?
C31B C32B 1.31(2) . ?
C31B H31C 0.9900 . ?
C31B H31D 0.9900 . ?
C32B C33B 1.59(2) . ?
C32B H32C 0.9900 . ?
C32B H32D 0.9900 . ?
C33B H33C 0.9900 . ?
C33B H33D 0.9900 . ?
C34 Cl1 1.732(7) . ?
C34 Cl2 1.790(8) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
P1 H1P 1.38(4) . ?
 
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
N2 C1 N1 108.4(3) . . ?
N2 C1 H1 125.8 . . ?
N1 C1 H1 125.8 . . ?
C3 C2 N1 107.2(3) . . ?
C3 C2 H2 126.4 . . ?
N1 C2 H2 126.4 . . ?
C2 C3 N2 107.0(3) . . ?
C2 C3 H3 126.5 . . ?
N2 C3 H3 126.5 . . ?
C5 C4 C9 124.2(4) . . ?
C5 C4 N2 118.2(3) . . ?
C9 C4 N2 117.6(3) . . ?
C4 C5 C6 116.5(4) . . ?
C4 C5 C10 123.3(4) . . ?
C6 C5 C10 120.2(4) . . ?
C7 C6 C5 121.2(4) . . ?
C7 C6 H6 119.4 . . ?
C5 C6 H6 119.4 . . ?
C6 C7 C8 120.8(4) . . ?
C6 C7 H7 119.6 . . ?
C8 C7 H7 119.6 . . ?
C7 C8 C9 120.9(4) . . ?
C7 C8 H8 119.6 . . ?
C9 C8 H8 119.6 . . ?
C4 C9 C8 116.4(4) . . ?
C4 C9 C13 122.6(4) . . ?
C8 C9 C13 121.0(4) . . ?
C5 C10 C11 109.0(5) . . ?
C5 C10 C12 112.5(4) . . ?
C11 C10 C12 110.6(5) . . ?
C5 C10 H10 108.2 . . ?
C11 C10 H10 108.2 . . ?
C12 C10 H10 108.2 . . ?
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 . . ?
C9 C13 C14 111.2(5) . . ?
C9 C13 C15 110.9(5) . . ?
C14 C13 C15 109.4(5) . . ?
C9 C13 H13 108.4 . . ?
C14 C13 H13 108.4 . . ?
C15 C13 H13 108.4 . . ?
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 . . ?
N3 C16 C17 125.0(4) . . ?
N3 C16 N1 113.4(3) . . ?
C17 C16 N1 121.6(3) . . ?
C16 C17 C18 116.9(4) . . ?
C16 C17 H17 121.5 . . ?
C18 C17 H17 121.5 . . ?
C19 C18 C17 119.4(5) . . ?
C19 C18 H18 120.3 . . ?
C17 C18 H18 120.3 . . ?
C20 C19 C18 119.1(4) . . ?
C20 C19 H19 120.4 . . ?
C18 C19 H19 120.4 . . ?
N3 C20 C19 122.7(4) . . ?
N3 C20 C21 116.0(4) . . ?
C19 C20 C21 121.3(4) . . ?
C20 C21 P1 113.9(3) . . ?
C20 C21 H21A 108.8 . . ?
P1 C21 H21A 108.8 . . ?
C20 C21 H21B 108.8 . . ?
P1 C21 H21B 108.8 . . ?
H21A C21 H21B 107.7 . . ?
C23B C22 C27B 113.6(9) . . ?
C27 C22 C23 105.3(9) . . ?
C23B C22 P1 116.6(7) . . ?
C27 C22 P1 123.2(8) . . ?
C27B C22 P1 104.7(6) . . ?
C23 C22 P1 109.6(6) . . ?
C27 C22 H22 105.8 . . ?
C23 C22 H22 105.8 . . ?
P1 C22 H22 105.8 . . ?
C24 C23 C22 110.4(11) . . ?
C24 C23 H23A 109.6 . . ?
C22 C23 H23A 109.6 . . ?
C24 C23 H23B 109.6 . . ?
C22 C23 H23B 109.6 . . ?
H23A C23 H23B 108.1 . . ?
C23 C24 C25 111.9(14) . . ?
C23 C24 H24A 109.2 . . ?
C25 C24 H24A 109.2 . . ?
C23 C24 H24B 109.2 . . ?
C25 C24 H24B 109.2 . . ?
H24A C24 H24B 107.9 . . ?
C26 C25 C24 112.6(13) . . ?
C26 C25 H25A 109.1 . . ?
C24 C25 H25A 109.1 . . ?
C26 C25 H25B 109.1 . . ?
C24 C25 H25B 109.1 . . ?
H25A C25 H25B 107.8 . . ?
C25 C26 C27 110.7(14) . . ?
C25 C26 H26A 109.5 . . ?
C27 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
C27 C26 H26B 109.5 . . ?
H26A C26 H26B 108.1 . . ?
C22 C27 C26 112.7(13) . . ?
C22 C27 H27A 109.0 . . ?
C26 C27 H27A 109.0 . . ?
C22 C27 H27B 109.0 . . ?
C26 C27 H27B 109.0 . . ?
H27A C27 H27B 107.8 . . ?
C22 C23B C24B 105.6(12) . . ?
C22 C23B H23C 110.6 . . ?
C24B C23B H23C 110.6 . . ?
C22 C23B H23D 110.6 . . ?
C24B C23B H23D 110.6 . . ?
H23C C23B H23D 108.8 . . ?
C25B C24B C23B 109.5(14) . . ?
C25B C24B H24C 109.8 . . ?
C23B C24B H24C 109.8 . . ?
C25B C24B H24D 109.8 . . ?
C23B C24B H24D 109.8 . . ?
H24C C24B H24D 108.2 . . ?
C26B C25B C24B 112.1(12) . . ?
C26B C25B H25C 109.2 . . ?
C24B C25B H25C 109.2 . . ?
C26B C25B H25D 109.2 . . ?
C24B C25B H25D 109.2 . . ?
H25C C25B H25D 107.9 . . ?
C25B C26B C27B 109.2(13) . . ?
C25B C26B H26C 109.8 . . ?
C27B C26B H26C 109.8 . . ?
C25B C26B H26D 109.8 . . ?
C27B C26B H26D 109.8 . . ?
H26C C26B H26D 108.3 . . ?
C26B C27B C22 105.6(12) . . ?
C26B C27B H27C 110.6 . . ?
C22 C27B H27C 110.6 . . ?
C26B C27B H27D 110.6 . . ?
C22 C27B H27D 110.6 . . ?
H27C C27B H27D 108.8 . . ?
C33 C28 C29 104.9(14) . . ?
C33 C28 P1 107.2(9) . . ?
C29 C28 P1 104.0(9) . . ?
C33 C28 H28 113.3 . . ?
C29 C28 H28 113.3 . . ?
P1 C28 H28 113.3 . . ?
C30 C29 C28 103.6(14) . . ?
C30 C29 H29A 111.0 . . ?
C28 C29 H29A 111.0 . . ?
C30 C29 H29B 111.0 . . ?
C28 C29 H29B 111.0 . . ?
H29A C29 H29B 109.0 . . ?
C31 C30 C29 116(2) . . ?
C31 C30 H30A 108.2 . . ?
C29 C30 H30A 108.2 . . ?
C31 C30 H30B 108.2 . . ?
C29 C30 H30B 108.2 . . ?
H30A C30 H30B 107.4 . . ?
C30 C31 C32 112.2(18) . . ?
C30 C31 H31A 109.2 . . ?
C32 C31 H31A 109.2 . . ?
C30 C31 H31B 109.2 . . ?
C32 C31 H31B 109.2 . . ?
H31A C31 H31B 107.9 . . ?
C31 C32 C33 109.9(16) . . ?
C31 C32 H32A 109.7 . . ?
C33 C32 H32A 109.7 . . ?
C31 C32 H32B 109.7 . . ?
C33 C32 H32B 109.7 . . ?
H32A C32 H32B 108.2 . . ?
C28 C33 C32 99.2(15) . . ?
C28 C33 H33A 111.9 . . ?
C32 C33 H33A 111.9 . . ?
C28 C33 H33B 111.9 . . ?
C32 C33 H33B 111.9 . . ?
H33A C33 H33B 109.6 . . ?
C33B C28B C29B 106.8(14) . . ?
C33B C28B P1 104.9(10) . . ?
C29B C28B P1 115.9(11) . . ?
C33B C28B H28B 109.7 . . ?
C29B C28B H28B 109.7 . . ?
P1 C28B H28B 109.7 . . ?
C28B C29B C30B 108.7(15) . . ?
C28B C29B H29C 109.9 . . ?
C30B C29B H29C 109.9 . . ?
C28B C29B H29D 109.9 . . ?
C30B C29B H29D 109.9 . . ?
H29C C29B H29D 108.3 . . ?
C31B C30B C29B 114(2) . . ?
C31B C30B H30C 108.7 . . ?
C29B C30B H30C 108.7 . . ?
C31B C30B H30D 108.7 . . ?
C29B C30B H30D 108.7 . . ?
H30C C30B H30D 107.6 . . ?
C30B C31B C32B 117(2) . . ?
C30B C31B H31C 108.1 . . ?
C32B C31B H31C 108.1 . . ?
C30B C31B H31D 108.1 . . ?
C32B C31B H31D 108.1 . . ?
H31C C31B H31D 107.3 . . ?
C31B C32B C33B 112.8(18) . . ?
C31B C32B H32C 109.0 . . ?
C33B C32B H32C 109.0 . . ?
C31B C32B H32D 109.0 . . ?
C33B C32B H32D 109.0 . . ?
H32C C32B H32D 107.8 . . ?
C28B C33B C32B 117.5(15) . . ?
C28B C33B H33C 107.9 . . ?
C32B C33B H33C 107.9 . . ?
C28B C33B H33D 107.9 . . ?
C32B C33B H33D 107.9 . . ?
H33C C33B H33D 107.2 . . ?
Cl1 C34 Cl2 109.9(4) . . ?
Cl1 C34 H34A 109.7 . . ?
Cl2 C34 H34A 109.7 . . ?
Cl1 C34 H34B 109.7 . . ?
Cl2 C34 H34B 109.7 . . ?
H34A C34 H34B 108.2 . . ?
C1 N1 C2 108.3(3) . . ?
C1 N1 C16 125.8(3) . . ?
C2 N1 C16 125.9(3) . . ?
C1 N2 C3 109.1(3) . . ?
C1 N2 C4 123.7(3) . . ?
C3 N2 C4 127.1(3) . . ?
C16 N3 C20 116.8(4) . . ?
C21 P1 C22 115.2(3) . . ?
C21 P1 C28 119.4(4) . . ?
C22 P1 C28 99.9(4) . . ?
C21 P1 C28B 95.1(4) . . ?
C22 P1 C28B 119.8(4) . . ?
C21 P1 H1P 115.9(18) . . ?
C22 P1 H1P 101.5(18) . . ?
C28 P1 H1P 102.2(18) . . ?
C28B P1 H1P 110.2(18) . . ?
 
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 C2 C3 N2 -0.3(4) . . . . ?
C9 C4 C5 C6 -3.1(6) . . . . ?
N2 C4 C5 C6 175.9(4) . . . . ?
C9 C4 C5 C10 174.0(4) . . . . ?
N2 C4 C5 C10 -7.0(6) . . . . ?
C4 C5 C6 C7 1.3(7) . . . . ?
C10 C5 C6 C7 -175.9(5) . . . . ?
C5 C6 C7 C8 0.7(7) . . . . ?
C6 C7 C8 C9 -1.1(7) . . . . ?
C5 C4 C9 C8 2.7(6) . . . . ?
N2 C4 C9 C8 -176.3(4) . . . . ?
C5 C4 C9 C13 -179.4(4) . . . . ?
N2 C4 C9 C13 1.6(6) . . . . ?
C7 C8 C9 C4 -0.5(7) . . . . ?
C7 C8 C9 C13 -178.4(5) . . . . ?
C4 C5 C10 C11 -104.9(5) . . . . ?
C6 C5 C10 C11 72.2(6) . . . . ?
C4 C5 C10 C12 132.1(5) . . . . ?
C6 C5 C10 C12 -50.9(7) . . . . ?
C4 C9 C13 C14 -109.5(6) . . . . ?
C8 C9 C13 C14 68.2(6) . . . . ?
C4 C9 C13 C15 128.5(5) . . . . ?
C8 C9 C13 C15 -53.7(7) . . . . ?
N3 C16 C17 C18 1.2(7) . . . . ?
N1 C16 C17 C18 -178.2(4) . . . . ?
C16 C17 C18 C19 -1.6(8) . . . . ?
C17 C18 C19 C20 0.7(9) . . . . ?
C18 C19 C20 N3 0.6(8) . . . . ?
C18 C19 C20 C21 178.5(5) . . . . ?
N3 C20 C21 P1 -32.6(6) . . . . ?
C19 C20 C21 P1 149.4(5) . . . . ?
C23B C22 C23 C24 -81(2) . . . . ?
C27 C22 C23 C24 -57.4(12) . . . . ?
C27B C22 C23 C24 -52.5(17) . . . . ?
P1 C22 C23 C24 168.2(8) . . . . ?
C22 C23 C24 C25 53.2(14) . . . . ?
C23 C24 C25 C26 -52.8(17) . . . . ?
C24 C25 C26 C27 54.2(18) . . . . ?
C23B C22 C27 C26 70.7(14) . . . . ?
C27B C22 C27 C26 -112(2) . . . . ?
C23 C22 C27 C26 61.1(14) . . . . ?
P1 C22 C27 C26 -172.3(9) . . . . ?
C25 C26 C27 C22 -62.7(17) . . . . ?
C27 C22 C23B C24B -62.6(12) . . . . ?
C27B C22 C23B C24B -64.3(14) . . . . ?
C23 C22 C23B C24B 95(3) . . . . ?
P1 C22 C23B C24B 173.8(8) . . . . ?
C22 C23B C24B C25B 60.3(14) . . . . ?
C23B C24B C25B C26B -59.3(17) . . . . ?
C24B C25B C26B C27B 59.0(18) . . . . ?
C25B C26B C27B C22 -56.1(14) . . . . ?
C23B C22 C27B C26B 64.2(13) . . . . ?
C27 C22 C27B C26B 60.9(17) . . . . ?
C23 C22 C27B C26B 51.8(16) . . . . ?
P1 C22 C27B C26B -167.6(8) . . . . ?
C33 C28 C29 C30 -67(2) . . . . ?
P1 C28 C29 C30 -179.3(15) . . . . ?
C28 C29 C30 C31 63(3) . . . . ?
C29 C30 C31 C32 -59(3) . . . . ?
C30 C31 C32 C33 61(3) . . . . ?
C29 C28 C33 C32 69.0(17) . . . . ?
P1 C28 C33 C32 179.2(11) . . . . ?
C31 C32 C33 C28 -64(2) . . . . ?
C33B C28B C29B C30B 28(2) . . . . ?
P1 C28B C29B C30B 144.7(14) . . . . ?
C28B C29B C30B C31B 28(3) . . . . ?
C29B C30B C31B C32B -60(3) . . . . ?
C30B C31B C32B C33B 33(3) . . . . ?
C29B C28B C33B C32B -57(2) . . . . ?
P1 C28B C33B C32B 179.4(16) . . . . ?
C31B C32B C33B C28B 33(3) . . . . ?
N2 C1 N1 C2 -0.2(4) . . . . ?
N2 C1 N1 C16 179.3(3) . . . . ?
C3 C2 N1 C1 0.3(4) . . . . ?
C3 C2 N1 C16 -179.1(4) . . . . ?
N3 C16 N1 C1 172.2(3) . . . . ?
C17 C16 N1 C1 -8.3(6) . . . . ?
N3 C16 N1 C2 -8.5(5) . . . . ?
C17 C16 N1 C2 171.1(4) . . . . ?
N1 C1 N2 C3 0.0(4) . . . . ?
N1 C1 N2 C4 -179.8(3) . . . . ?
C2 C3 N2 C1 0.2(4) . . . . ?
C2 C3 N2 C4 179.9(3) . . . . ?
C5 C4 N2 C1 -90.8(5) . . . . ?
C9 C4 N2 C1 88.3(5) . . . . ?
C5 C4 N2 C3 89.5(5) . . . . ?
C9 C4 N2 C3 -91.5(5) . . . . ?
C17 C16 N3 C20 0.0(6) . . . . ?
N1 C16 N3 C20 179.5(4) . . . . ?
C19 C20 N3 C16 -1.0(7) . . . . ?
C21 C20 N3 C16 -179.0(4) . . . . ?
C20 C21 P1 C22 -58.3(5) . . . . ?
C20 C21 P1 C28 -177.2(6) . . . . ?
C20 C21 P1 C28B 175.3(6) . . . . ?
C23B C22 P1 C21 85.4(9) . . . . ?
C27 C22 P1 C21 -13.5(9) . . . . ?
C27B C22 P1 C21 -41.0(7) . . . . ?
C23 C22 P1 C21 111.2(6) . . . . ?
C23B C22 P1 C28 -145.4(9) . . . . ?
C27 C22 P1 C28 115.8(9) . . . . ?
C27B C22 P1 C28 88.2(7) . . . . ?
C23 C22 P1 C28 -119.6(8) . . . . ?
C23B C22 P1 C28B -162.1(9) . . . . ?
C27 C22 P1 C28B 99.1(10) . . . . ?
C27B C22 P1 C28B 71.5(8) . . . . ?
C23 C22 P1 C28B -136.3(8) . . . . ?
C33 C28 P1 C21 -53.5(13) . . . . ?
C29 C28 P1 C21 57.3(13) . . . . ?
C33 C28 P1 C22 -179.9(11) . . . . ?
C29 C28 P1 C22 -69.2(13) . . . . ?
C33 C28 P1 C28B -35.7(14) . . . . ?
C29 C28 P1 C28B 75.1(19) . . . . ?
C33B C28B P1 C21 -139.2(13) . . . . ?
C29B C28B P1 C21 103.4(15) . . . . ?
C33B C28B P1 C22 97.8(13) . . . . ?
C29B C28B P1 C22 -19.6(16) . . . . ?
C33B C28B P1 C28 56.3(16) . . . . ?
C29B C28B P1 C28 -61.1(19) . . . . ?
 
_refine_diff_density_max    1.113
_refine_diff_density_min   -1.015
_refine_diff_density_rms    0.086

_shelxl_version_number 2013-4



 
data_pbts150130_02
 
_audit_creation_method            SHELXL-2013
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          
 'C74 H110 K2 N6 O2 P2, 2(C37 H55 K N3 O P)'
_chemical_formula_sum
 'C148 H220 K4 N12 O4 P4' 
_chemical_formula_weight          2511.63

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0033   0.0016
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 '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'
 'K'  'K'   0.2009   0.2494
 '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       triclinic
_space_group_IT_number            2
_space_group_name_H-M_alt         'P -1'
_space_group_name_Hall            '-P 1'
 
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-x, -y, -z'
 
_cell_length_a                    12.9906(12)
_cell_length_b                    14.5542(13)
_cell_length_c                    21.8297(19)
_cell_angle_alpha                 72.803(2)
_cell_angle_beta                  78.663(2)
_cell_angle_gamma                 70.389(2)
_cell_volume                      3692.3(6)
_cell_formula_units_Z             1
_cell_measurement_temperature     173(2)
_cell_measurement_reflns_used     5875
_cell_measurement_theta_min       2.30
_cell_measurement_theta_max       27.80
 
_exptl_crystal_description        'block'
_exptl_crystal_colour             'orange'
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_method     ?              
_exptl_crystal_density_diffrn     1.130          
_exptl_crystal_F_000              1360
_exptl_transmission_factor_min    ?                                             
_exptl_transmission_factor_max    ?                                             
_exptl_crystal_size_max           0.200
_exptl_crystal_size_mid           0.120
_exptl_crystal_size_min           0.080
_exptl_absorpt_coefficient_mu     0.218
_shelx_estimated_absorpt_T_min    0.958
_shelx_estimated_absorpt_T_max    0.983
_exptl_absorpt_correction_type    'multi-scan'
_exptl_absorpt_correction_T_min   0.5787 
_exptl_absorpt_correction_T_max   0.7456
_exptl_absorpt_process_details    'sadabs'
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       173(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_monochromator   'triumph'
_diffrn_source                    'sealed tube'            
_diffrn_measurement_device_type   'Bruker APEX-II CCD'
_diffrn_measurement_method        'φ and ω scans'
_diffrn_detector_area_resol_mean  ? 
_diffrn_reflns_number             65782
_diffrn_reflns_av_unetI/netI      0.2149
_diffrn_reflns_av_R_equivalents   0.1848
_diffrn_reflns_limit_h_min        -17
_diffrn_reflns_limit_h_max        17
_diffrn_reflns_limit_k_min        -19
_diffrn_reflns_limit_k_max        19
_diffrn_reflns_limit_l_min        -28
_diffrn_reflns_limit_l_max        28
_diffrn_reflns_theta_min          1.533
_diffrn_reflns_theta_max          28.160
_diffrn_reflns_theta_full         25.242
_diffrn_measured_fraction_theta_max   0.982
_diffrn_measured_fraction_theta_full  0.998
_diffrn_reflns_Laue_measured_fraction_max    0.982
_diffrn_reflns_Laue_measured_fraction_full   0.998
_diffrn_reflns_point_group_measured_fraction_max   0.982
_diffrn_reflns_point_group_measured_fraction_full  0.998
_reflns_number_total              17796
_reflns_number_gt                 6627
_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 APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
 
_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)+(0.1094P)²] 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          17796
_refine_ls_number_parameters      693
_refine_ls_number_restraints      6
_refine_ls_R_factor_all           0.2459
_refine_ls_R_factor_gt            0.0896
_refine_ls_wR_factor_ref          0.2458
_refine_ls_wR_factor_gt           0.1884
_refine_ls_goodness_of_fit_ref    0.944
_refine_ls_restrained_S_all       0.948
_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
C1 C 1.1154(3) -0.0419(3) 0.64761(19) 0.0349(10) Uani 1 1 d . . . . .
C2 C 1.2059(4) -0.1754(3) 0.7240(2) 0.0407(11) Uani 1 1 d . . . . .
H2 H 1.2545 -0.2133 0.7560 0.049 Uiso 1 1 calc R U . . .
C3 C 1.1387(4) -0.2080(3) 0.7026(2) 0.0408(11) Uani 1 1 d . . . . .
H3 H 1.1299 -0.2735 0.7161 0.049 Uiso 1 1 calc R U . . .
C4 C 1.2452(4) -0.0108(3) 0.70210(19) 0.0372(11) Uani 1 1 d . . . . .
C5 C 1.1880(4) 0.0536(4) 0.7417(2) 0.0482(12) Uani 1 1 d . . . . .
C6 C 1.2407(5) 0.1174(4) 0.7500(2) 0.0564(14) Uani 1 1 d . . . . .
H6 H 1.2038 0.1631 0.7762 0.068 Uiso 1 1 calc R U . . .
C7 C 1.3448(5) 0.1156(4) 0.7212(3) 0.0583(14) Uani 1 1 d . . . . .
H7 H 1.3792 0.1596 0.7277 0.070 Uiso 1 1 calc R U . . .
C8 C 1.3994(4) 0.0508(4) 0.6829(2) 0.0513(13) Uani 1 1 d . . . . .
H8 H 1.4714 0.0505 0.6630 0.062 Uiso 1 1 calc R U . . .
C9 C 1.3514(4) -0.0145(3) 0.6726(2) 0.0396(11) Uani 1 1 d . . . . .
C10 C 1.0744(5) 0.0547(4) 0.7754(3) 0.0669(16) Uani 1 1 d . . . . .
H10 H 1.0545 -0.0005 0.7665 0.080 Uiso 1 1 calc R U . . .
C11 C 0.9896(6) 0.1541(5) 0.7490(3) 0.0997(16) Uani 1 1 d . . . . .
H11A H 1.0034 0.2087 0.7606 0.150 Uiso 1 1 calc R U . . .
H11B H 0.9157 0.1500 0.7675 0.150 Uiso 1 1 calc R U . . .
H11C H 0.9953 0.1674 0.7019 0.150 Uiso 1 1 calc R U . . .
C12 C 1.0713(6) 0.0349(6) 0.8478(3) 0.0997(16) Uani 1 1 d . . . . .
H12A H 1.1329 -0.0240 0.8631 0.150 Uiso 1 1 calc R U . . .
H12B H 1.0019 0.0219 0.8689 0.150 Uiso 1 1 calc R U . . .
H12C H 1.0773 0.0938 0.8583 0.150 Uiso 1 1 calc R U . . .
C13 C 1.4098(4) -0.0842(4) 0.6284(2) 0.0464(12) Uani 1 1 d . . . . .
H13 H 1.3754 -0.1399 0.6400 0.056 Uiso 1 1 calc R U . . .
C14 C 1.5321(4) -0.1315(4) 0.6353(3) 0.0658(15) Uani 1 1 d . . . . .
H14A H 1.5683 -0.0785 0.6233 0.099 Uiso 1 1 calc R U . . .
H14B H 1.5645 -0.1774 0.6069 0.099 Uiso 1 1 calc R U . . .
H14C H 1.5423 -0.1692 0.6801 0.099 Uiso 1 1 calc R U . . .
C15 C 1.3894(5) -0.0258(5) 0.5592(2) 0.0814(19) Uani 1 1 d . . . . .
H15A H 1.3101 -0.0005 0.5559 0.122 Uiso 1 1 calc R U . . .
H15B H 1.4249 -0.0704 0.5303 0.122 Uiso 1 1 calc R U . . .
H15C H 1.4199 0.0310 0.5471 0.122 Uiso 1 1 calc R U . . .
C16 C 0.9965(3) -0.1285(3) 0.62537(19) 0.0319(10) Uani 1 1 d . . . . .
C17 C 1.0016(4) -0.2170(3) 0.61218(19) 0.0361(10) Uani 1 1 d . . . . .
H17 H 1.0631 -0.2754 0.6201 0.043 Uiso 1 1 calc R U . . .
C18 C 0.9102(4) -0.2155(3) 0.5863(2) 0.0385(11) Uani 1 1 d . . . . .
H18 H 0.9089 -0.2743 0.5764 0.046 Uiso 1 1 calc R U . . .
C19 C 0.8237(4) -0.1308(3) 0.57523(18) 0.0342(10) Uani 1 1 d . . . . .
H19 H 0.7623 -0.1313 0.5580 0.041 Uiso 1 1 calc R U . . .
C20 C 0.8236(3) -0.0395(3) 0.58943(18) 0.0321(10) Uani 1 1 d . . . . .
C21 C 0.7357(4) 0.0473(3) 0.5797(2) 0.0370(11) Uani 1 1 d . . . . .
H21 H 0.6729 0.0446 0.5651 0.044 Uiso 1 1 calc R U . . .
C22 C 0.6398(11) 0.2604(10) 0.5402(7) 0.0552(10) Uani 0.55 1 d . . P A 1
H22 H 0.5910 0.2172 0.5465 0.066 Uiso 0.55 1 calc R U P A 1
C23 C 0.6676(15) 0.2627(17) 0.4659(10) 0.0552(10) Uani 0.55 1 d D . P A 1
H23A H 0.7304 0.2906 0.4494 0.066 Uiso 0.55 1 calc R U P A 1
H23B H 0.6938 0.1920 0.4625 0.066 Uiso 0.55 1 calc R U P A 1
C24 C 0.5771(9) 0.3217(7) 0.4188(5) 0.0552(10) Uani 0.55 1 d D . P A 1
H24A H 0.6125 0.3337 0.3738 0.066 Uiso 0.55 1 calc R U P A 1
H24B H 0.5279 0.2805 0.4227 0.066 Uiso 0.55 1 calc R U P A 1
C25 C 0.5146(8) 0.4145(7) 0.4325(4) 0.0552(10) Uani 0.55 1 d . . P A 1
H25A H 0.4563 0.4487 0.4031 0.066 Uiso 0.55 1 calc R U P A 1
H25B H 0.5626 0.4581 0.4246 0.066 Uiso 0.55 1 calc R U P A 1
C26 C 0.4613(8) 0.3999(7) 0.5034(5) 0.0552(10) Uani 0.55 1 d . . P A 1
H26A H 0.4199 0.4664 0.5120 0.066 Uiso 0.55 1 calc R U P A 1
H26B H 0.4087 0.3609 0.5103 0.066 Uiso 0.55 1 calc R U P A 1
C27 C 0.5467(8) 0.3456(7) 0.5494(4) 0.0552(10) Uani 0.55 1 d . . P A 1
H27A H 0.5771 0.3969 0.5539 0.066 Uiso 0.55 1 calc R U P A 1
H27B H 0.5068 0.3229 0.5918 0.066 Uiso 0.55 1 calc R U P A 1
C22B C 0.6158(14) 0.2463(13) 0.5353(8) 0.0552(10) Uani 0.45 1 d . . P A 2
H22B H 0.6169 0.3118 0.5407 0.066 Uiso 0.45 1 calc R U P A 2
C23B C 0.6845(18) 0.257(2) 0.4683(12) 0.0552(10) Uani 0.45 1 d . . P A 2
H23C H 0.7565 0.2632 0.4716 0.066 Uiso 0.45 1 calc R U P A 2
H23D H 0.6977 0.1961 0.4525 0.066 Uiso 0.45 1 calc R U P A 2
C24B C 0.6220(10) 0.3480(9) 0.4228(6) 0.0552(10) Uani 0.45 1 d . . P A 2
H24C H 0.6514 0.3455 0.3777 0.066 Uiso 0.45 1 calc R U P A 2
H24D H 0.6294 0.4093 0.4302 0.066 Uiso 0.45 1 calc R U P A 2
C25B C 0.4948(10) 0.3508(10) 0.4352(5) 0.0552(10) Uani 0.45 1 d . . P A 2
H25C H 0.4517 0.4128 0.4067 0.066 Uiso 0.45 1 calc R U P A 2
H25D H 0.4878 0.2923 0.4238 0.066 Uiso 0.45 1 calc R U P A 2
C26B C 0.4481(11) 0.3484(9) 0.5043(6) 0.0552(10) Uani 0.45 1 d . . P A 2
H26C H 0.3728 0.3425 0.5107 0.066 Uiso 0.45 1 calc R U P A 2
H26D H 0.4430 0.4127 0.5134 0.066 Uiso 0.45 1 calc R U P A 2
C27B C 0.5177(9) 0.2613(8) 0.5518(5) 0.0552(10) Uani 0.45 1 d . . P A 2
H27C H 0.5006 0.2761 0.5948 0.066 Uiso 0.45 1 calc R U P A 2
H27D H 0.4982 0.1995 0.5559 0.066 Uiso 0.45 1 calc R U P A 2
C28 C 0.6568(5) 0.1688(4) 0.6739(2) 0.0632(6) Uani 1 1 d . . . . .
H28 H 0.5789 0.1725 0.6728 0.076 Uiso 1 1 calc R U . . .
C29 C 0.6564(5) 0.2602(4) 0.6937(2) 0.0632(6) Uani 1 1 d . . . . .
H29A H 0.6177 0.3219 0.6631 0.076 Uiso 1 1 calc R U . . .
H29B H 0.7330 0.2608 0.6914 0.076 Uiso 1 1 calc R U . . .
C30 C 0.6002(5) 0.2613(4) 0.7621(2) 0.0632(6) Uani 1 1 d . . . . .
H30A H 0.6055 0.3202 0.7737 0.076 Uiso 1 1 calc R U . . .
H30B H 0.5213 0.2688 0.7631 0.076 Uiso 1 1 calc R U . . .
C31 C 0.6503(5) 0.1673(4) 0.8111(2) 0.0632(6) Uani 1 1 d . . . . .
H31A H 0.6082 0.1692 0.8539 0.076 Uiso 1 1 calc R U . . .
H31B H 0.7268 0.1634 0.8140 0.076 Uiso 1 1 calc R U . . .
C32 C 0.6499(5) 0.0760(4) 0.7924(2) 0.0632(6) Uani 1 1 d . . . . .
H32A H 0.5731 0.0759 0.7947 0.076 Uiso 1 1 calc R U . . .
H32B H 0.6881 0.0146 0.8235 0.076 Uiso 1 1 calc R U . . .
C33 C 0.7073(5) 0.0739(4) 0.7236(2) 0.0632(6) Uani 1 1 d . . . . .
H33A H 0.7862 0.0662 0.7226 0.076 Uiso 1 1 calc R U . . .
H33B H 0.7018 0.0149 0.7121 0.076 Uiso 1 1 calc R U . . .
C34 C 0.8564(6) 0.4038(5) 0.5181(4) 0.102(2) Uani 1 1 d . . . . .
H34A H 0.8922 0.4081 0.4738 0.152 Uiso 1 1 calc R U . . .
H34B H 0.7989 0.4672 0.5200 0.152 Uiso 1 1 calc R U . . .
H34C H 0.8235 0.3484 0.5313 0.152 Uiso 1 1 calc R U . . .
C35 C 0.9366(8) 0.3856(6) 0.5607(4) 0.112(3) Uani 1 1 d . . . . .
H35A H 0.9615 0.4460 0.5517 0.135 Uiso 1 1 calc R U . . .
H35B H 0.9025 0.3729 0.6059 0.135 Uiso 1 1 calc R U . . .
C36 C 1.1140(8) 0.3015(8) 0.5811(4) 0.138(3) Uani 1 1 d D . . . .
H36A H 1.0996 0.2776 0.6285 0.165 Uiso 1 1 calc R U . . .
H36B H 1.1181 0.3711 0.5716 0.165 Uiso 1 1 calc R U . . .
C37 C 1.2177(7) 0.2392(8) 0.5600(5) 0.156(4) Uani 1 1 d D . . . .
H37A H 1.2209 0.1682 0.5782 0.234 Uiso 1 1 calc R U . . .
H37B H 1.2767 0.2528 0.5744 0.234 Uiso 1 1 calc R U . . .
H37C H 1.2266 0.2537 0.5128 0.234 Uiso 1 1 calc R U . . .
C38 C 0.8067(4) 0.6556(3) 0.84062(19) 0.0338(10) Uani 1 1 d . . . . .
C39 C 0.7543(4) 0.7911(3) 0.7546(2) 0.0408(11) Uani 1 1 d . . . . .
H39 H 0.7144 0.8359 0.7199 0.049 Uiso 1 1 calc R U . . .
C40 C 0.8421(4) 0.7982(3) 0.77339(19) 0.0390(11) Uani 1 1 d . . . . .
H40 H 0.8765 0.8499 0.7550 0.047 Uiso 1 1 calc R U . . .
C41 C 0.6430(4) 0.6700(3) 0.79176(19) 0.0363(10) Uani 1 1 d . . . . .
C42 C 0.6612(4) 0.6043(3) 0.7528(2) 0.0421(11) Uani 1 1 d . . . . .
C43 C 0.5727(4) 0.5741(4) 0.7483(2) 0.0537(13) Uani 1 1 d . . . . .
H43 H 0.5825 0.5291 0.7223 0.064 Uiso 1 1 calc R U . . .
C44 C 0.4715(5) 0.6085(4) 0.7807(3) 0.0608(15) Uani 1 1 d . . . . .
H44 H 0.4120 0.5873 0.7768 0.073 Uiso 1 1 calc R U . . .
C45 C 0.4555(4) 0.6731(4) 0.8187(2) 0.0540(14) Uani 1 1 d . . . . .
H45 H 0.3849 0.6955 0.8411 0.065 Uiso 1 1 calc R U . . .
C46 C 0.5403(4) 0.7063(3) 0.8252(2) 0.0423(11) Uani 1 1 d . . . . .
C47 C 0.7723(4) 0.5642(4) 0.7171(2) 0.0504(13) Uani 1 1 d . . . . .
H47 H 0.8235 0.5971 0.7244 0.060 Uiso 1 1 calc R U . . .
C48 C 0.7660(5) 0.5910(4) 0.6442(2) 0.0694(16) Uani 1 1 d . . . . .
H48A H 0.7262 0.5509 0.6349 0.104 Uiso 1 1 calc R U . . .
H48B H 0.8405 0.5764 0.6217 0.104 Uiso 1 1 calc R U . . .
H48C H 0.7272 0.6627 0.6294 0.104 Uiso 1 1 calc R U . . .
C49 C 0.8201(5) 0.4508(4) 0.7424(3) 0.0720(17) Uani 1 1 d . . . . .
H49A H 0.8295 0.4353 0.7882 0.108 Uiso 1 1 calc R U . . .
H49B H 0.8916 0.4275 0.7181 0.108 Uiso 1 1 calc R U . . .
H49C H 0.7700 0.4167 0.7373 0.108 Uiso 1 1 calc R U . . .
C50 C 0.5221(4) 0.7778(4) 0.8675(2) 0.0540(13) Uani 1 1 d . . . . .
H50 H 0.5966 0.7744 0.8757 0.065 Uiso 1 1 calc R U . B 1
C51 C 0.4600(10) 0.7491(8) 0.9323(5) 0.081(2) Uani 0.6 1 d . . P C 1
H51A H 0.3844 0.7564 0.9267 0.121 Uiso 0.6 1 calc R U P C 1
H51B H 0.4592 0.7932 0.9588 0.121 Uiso 0.6 1 calc R U P C 1
H51C H 0.4960 0.6790 0.9536 0.121 Uiso 0.6 1 calc R U P C 1
C52 C 0.4679(11) 0.8880(8) 0.8319(5) 0.081(2) Uani 0.6 1 d . . P C 1
H52A H 0.3940 0.8949 0.8234 0.121 Uiso 0.6 1 calc R U P C 1
H52B H 0.5124 0.9058 0.7910 0.121 Uiso 0.6 1 calc R U P C 1
H52C H 0.4628 0.9329 0.8588 0.121 Uiso 0.6 1 calc R U P C 1
C51B C 0.5237(16) 0.7099(12) 0.9385(8) 0.081(2) Uani 0.4 1 d . . P C 2
H51D H 0.4751 0.6680 0.9454 0.121 Uiso 0.4 1 calc R U P C 2
H51E H 0.4982 0.7527 0.9690 0.121 Uiso 0.4 1 calc R U P C 2
H51F H 0.5988 0.6665 0.9454 0.121 Uiso 0.4 1 calc R U P C 2
C52B C 0.4172(16) 0.8613(12) 0.8578(7) 0.081(2) Uani 0.4 1 d . . P C 2
H52D H 0.4126 0.8915 0.8116 0.121 Uiso 0.4 1 calc R U P C 2
H52E H 0.4152 0.9125 0.8791 0.121 Uiso 0.4 1 calc R U P C 2
H52F H 0.3549 0.8345 0.8765 0.121 Uiso 0.4 1 calc R U P C 2
C53 C 0.9696(4) 0.6965(3) 0.85649(18) 0.0354(10) Uani 1 1 d . . . . .
C54 C 0.9985(4) 0.7747(4) 0.8628(2) 0.0476(12) Uani 1 1 d . . . . .
H54 H 0.9549 0.8425 0.8488 0.057 Uiso 1 1 calc R U . . .
C55 C 1.0945(5) 0.7509(4) 0.8906(2) 0.0535(14) Uani 1 1 d . . . . .
H55 H 1.1175 0.8030 0.8963 0.064 Uiso 1 1 calc R U . . .
C56 C 1.1559(4) 0.6529(4) 0.9098(2) 0.0486(13) Uani 1 1 d . . . . .
H56 H 1.2214 0.6370 0.9290 0.058 Uiso 1 1 calc R U . . .
C57 C 1.1220(4) 0.5735(3) 0.90122(18) 0.0377(11) Uani 1 1 d . . . . .
C58 C 1.1836(4) 0.4723(3) 0.9180(2) 0.0416(11) Uani 1 1 d . . . . .
H58 H 1.2466 0.4537 0.9400 0.050 Uiso 1 1 calc R U . . .
C59 C 1.1938(5) 0.3857(5) 0.8109(2) 0.0710(7) Uani 1 1 d . . . . .
H59 H 1.2172 0.3156 0.8054 0.085 Uiso 1 1 calc R U . . .
C60 C 1.0991(5) 0.4447(5) 0.7719(2) 0.0710(7) Uani 1 1 d . . . . .
H60A H 1.0711 0.5140 0.7779 0.085 Uiso 1 1 calc R U . . .
H60B H 1.0389 0.4132 0.7878 0.085 Uiso 1 1 calc R U . . .
C61 C 1.1323(5) 0.4493(5) 0.6991(2) 0.0710(7) Uani 1 1 d . . . . .
H61A H 1.1499 0.3810 0.6925 0.085 Uiso 1 1 calc R U . . .
H61B H 1.0691 0.4934 0.6749 0.085 Uiso 1 1 calc R U . . .
C62 C 1.2276(5) 0.4875(5) 0.6732(2) 0.0710(7) Uani 1 1 d . . . . .
H62A H 1.2063 0.5596 0.6731 0.085 Uiso 1 1 calc R U . . .
H62B H 1.2504 0.4821 0.6281 0.085 Uiso 1 1 calc R U . . .
C63 C 1.3226(5) 0.4301(5) 0.7123(2) 0.0710(7) Uani 1 1 d . . . . .
H63A H 1.3822 0.4622 0.6959 0.085 Uiso 1 1 calc R U . . .
H63B H 1.3513 0.3605 0.7068 0.085 Uiso 1 1 calc R U . . .
C64 C 1.2903(5) 0.4263(5) 0.7846(2) 0.0710(7) Uani 1 1 d . . . . .
H64A H 1.3537 0.3831 0.8088 0.085 Uiso 1 1 calc R U . . .
H64B H 1.2715 0.4950 0.7909 0.085 Uiso 1 1 calc R U . . .
C65 C 1.2507(6) 0.2611(4) 0.9380(3) 0.0738(11) Uani 1 1 d . . . . .
H65 H 1.3254 0.2683 0.9203 0.089 Uiso 1 1 calc R U . D 1
C66 C 1.2414(17) 0.2419(17) 1.0079(11) 0.0738(11) Uani 0.5 1 d . . P E 1
H66A H 1.1660 0.2394 1.0259 0.089 Uiso 0.5 1 calc R U P E 1
H66B H 1.2534 0.2984 1.0191 0.089 Uiso 0.5 1 calc R U P E 1
C67 C 1.3261(11) 0.1405(10) 1.0399(7) 0.0738(11) Uani 0.5 1 d D . P E 1
H67A H 1.4004 0.1315 1.0159 0.089 Uiso 0.5 1 calc R U P E 1
H67B H 1.3302 0.1355 1.0856 0.089 Uiso 0.5 1 calc R U P E 1
C68 C 1.2702(12) 0.0645(10) 1.0329(6) 0.0738(11) Uani 0.5 1 d D . P E 1
H68A H 1.3015 -0.0037 1.0602 0.089 Uiso 0.5 1 calc R U P E 1
H68B H 1.1899 0.0869 1.0452 0.089 Uiso 0.5 1 calc R U P E 1
C69 C 1.2953(12) 0.0650(9) 0.9621(6) 0.0738(11) Uani 0.5 1 d D . P E 1
H69A H 1.2677 0.0145 0.9540 0.089 Uiso 0.5 1 calc R U P E 1
H69B H 1.3759 0.0466 0.9502 0.089 Uiso 0.5 1 calc R U P E 1
C66B C 1.2169(17) 0.2515(17) 1.0105(11) 0.0738(11) Uani 0.5 1 d . . P E 2
H66C H 1.1374 0.2583 1.0202 0.089 Uiso 0.5 1 calc R U P E 2
H66D H 1.2301 0.3066 1.0227 0.089 Uiso 0.5 1 calc R U P E 2
C67B C 1.2825(12) 0.1492(10) 1.0505(7) 0.0738(11) Uani 0.5 1 d . . P E 2
H67C H 1.2393 0.1329 1.0929 0.089 Uiso 0.5 1 calc R U P E 2
H67D H 1.3517 0.1558 1.0586 0.089 Uiso 0.5 1 calc R U P E 2
C68B C 1.3123(12) 0.0566(10) 1.0176(6) 0.0738(11) Uani 0.5 1 d . . P E 2
H68C H 1.3751 0.0031 1.0379 0.089 Uiso 0.5 1 calc R U P E 2
H68D H 1.2489 0.0293 1.0289 0.089 Uiso 0.5 1 calc R U P E 2
C69B C 1.3392(12) 0.0742(10) 0.9501(6) 0.0738(11) Uani 0.5 1 d . . P E 2
H69C H 1.3437 0.0149 0.9352 0.089 Uiso 0.5 1 calc R U P E 2
H69D H 1.4105 0.0890 0.9372 0.089 Uiso 0.5 1 calc R U P E 2
C70 C 1.2408(6) 0.1699(4) 0.9206(3) 0.0738(11) Uani 1 1 d D . . . .
H70A H 1.2726 0.1723 0.8753 0.089 Uiso 1 1 calc R U . E 1
H70B H 1.1617 0.1774 0.9227 0.089 Uiso 1 1 calc R U . E 1
C71 C 0.8567(10) 0.1567(6) 0.9708(4) 0.170(5) Uani 1 1 d D . . . .
H71A H 0.8486 0.1691 1.0135 0.255 Uiso 1 1 calc R U . . .
H71B H 0.9213 0.0989 0.9669 0.255 Uiso 1 1 calc R U . . .
H71C H 0.7909 0.1425 0.9653 0.255 Uiso 1 1 calc R U . . .
C72 C 0.8704(7) 0.2449(6) 0.9215(4) 0.122(3) Uani 1 1 d D . . . .
H72A H 0.9454 0.2489 0.9205 0.146 Uiso 1 1 calc R U . . .
H72B H 0.8641 0.2369 0.8790 0.146 Uiso 1 1 calc R U . . .
C73 C 0.6873(7) 0.3542(7) 0.9172(3) 0.102(2) Uani 1 1 d . . . . .
H73A H 0.6576 0.2991 0.9444 0.122 Uiso 1 1 calc R U . . .
H73B H 0.6883 0.3562 0.8714 0.122 Uiso 1 1 calc R U . . .
C74 C 0.6183(6) 0.4507(6) 0.9304(4) 0.130(3) Uani 1 1 d . . . . .
H74A H 0.6168 0.4476 0.9760 0.195 Uiso 1 1 calc R U . . .
H74B H 0.5434 0.4642 0.9205 0.195 Uiso 1 1 calc R U . . .
H74C H 0.6486 0.5046 0.9035 0.195 Uiso 1 1 calc R U . . .
N1 N 1.1909(3) -0.0750(2) 0.69033(15) 0.0332(8) Uani 1 1 d . . . . .
N2 N 1.0837(3) -0.1262(2) 0.65633(15) 0.0321(8) Uani 1 1 d . . . . .
N3 N 0.9155(3) -0.0422(2) 0.61462(15) 0.0317(8) Uani 1 1 d . . . . .
N4 N 0.7328(3) 0.7043(3) 0.79615(15) 0.0349(9) Uani 1 1 d . . . . .
N5 N 0.8740(3) 0.7161(2) 0.82479(15) 0.0338(8) Uani 1 1 d . . . . .
N6 N 1.0249(3) 0.5992(3) 0.87471(15) 0.0342(8) Uani 1 1 d . . . . .
P1 P 0.73163(10) 0.16366(9) 0.59240(6) 0.0413(3) Uani 1 1 d . . . . .
P2 P 1.14681(10) 0.37744(9) 0.89916(5) 0.0419(3) Uani 1 1 d . . . . .
K1 K 0.99529(9) 0.12122(7) 0.55136(5) 0.0463(3) Uani 1 1 d . . . . .
K2 K 0.88683(8) 0.47789(7) 0.94249(4) 0.0418(3) Uani 1 1 d . . . . .
O1 O 1.0268(3) 0.3031(3) 0.55292(18) 0.0758(12) Uani 1 1 d . . . . .
O2 O 0.7926(4) 0.3374(3) 0.9308(2) 0.0779(12) Uani 1 1 d . . . . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
C1 N1 1.357(5) . ?
C1 N2 1.372(5) . ?
C1 K1 2.887(4) . ?
C2 C3 1.332(6) . ?
C2 N1 1.394(5) . ?
C2 H2 0.9500 . ?
C3 N2 1.396(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.392(6) . ?
C4 C9 1.393(6) . ?
C4 N1 1.447(5) . ?
C5 C6 1.392(7) . ?
C5 C10 1.512(7) . ?
C6 C7 1.369(7) . ?
C6 H6 0.9500 . ?
C7 C8 1.370(7) . ?
C7 H7 0.9500 . ?
C8 C9 1.386(6) . ?
C8 H8 0.9500 . ?
C9 C13 1.520(6) . ?
C10 C12 1.516(8) . ?
C10 C11 1.525(8) . ?
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 C14 1.523(6) . ?
C13 C15 1.523(7) . ?
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 . ?
C16 N3 1.333(5) . ?
C16 C17 1.379(6) . ?
C16 N2 1.443(5) . ?
C16 K1 3.510(4) . ?
C17 C18 1.403(6) . ?
C17 K1 3.425(4) 2_756 ?
C17 H17 0.9500 . ?
C18 C19 1.357(6) . ?
C18 K1 3.108(4) 2_756 ?
C18 H18 0.9500 . ?
C19 C20 1.451(6) . ?
C19 K1 3.259(4) 2_756 ?
C19 H19 0.9500 . ?
C20 C21 1.383(6) . ?
C20 N3 1.393(5) . ?
C21 P1 1.777(4) . ?
C21 H21 0.9500 . ?
C22 C27 1.444(16) . ?
C22 C23 1.58(3) . ?
C22 P1 1.778(12) . ?
C22 H22 1.0000 . ?
C23 C24 1.567(13) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 C25 1.407(13) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 C26 1.552(12) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 C27 1.498(12) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C22B C27B 1.216(18) . ?
C22B C23B 1.55(4) . ?
C22B P1 1.976(15) . ?
C22B H22B 1.0000 . ?
C23B C24B 1.49(2) . ?
C23B H23C 0.9900 . ?
C23B H23D 0.9900 . ?
C24B C25B 1.610(17) . ?
C24B H24C 0.9900 . ?
C24B H24D 0.9900 . ?
C25B C26B 1.506(16) . ?
C25B H25C 0.9900 . ?
C25B H25D 0.9900 . ?
C26B C27B 1.524(14) . ?
C26B H26C 0.9900 . ?
C26B H26D 0.9900 . ?
C27B H27C 0.9900 . ?
C27B H27D 0.9900 . ?
C28 C29 1.513(7) . ?
C28 C33 1.516(7) . ?
C28 P1 1.861(5) . ?
C28 H28 1.0000 . ?
C29 C30 1.530(7) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 C31 1.500(7) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C32 1.501(7) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 C33 1.545(7) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 C35 1.440(9) . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 O1 1.392(8) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 O1 1.383(9) . ?
C36 C37 1.426(8) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 N4 1.367(5) . ?
C38 N5 1.370(5) . ?
C38 K2 2.901(4) . ?
C39 C40 1.330(6) . ?
C39 N4 1.400(5) . ?
C39 H39 0.9500 . ?
C40 N5 1.384(5) . ?
C40 H40 0.9500 . ?
C41 C42 1.394(6) . ?
C41 C46 1.401(6) . ?
C41 N4 1.443(5) . ?
C42 C43 1.391(6) . ?
C42 C47 1.514(6) . ?
C43 C44 1.371(7) . ?
C43 H43 0.9500 . ?
C44 C45 1.371(7) . ?
C44 H44 0.9500 . ?
C45 C46 1.389(7) . ?
C45 H45 0.9500 . ?
C46 C50 1.520(6) . ?
C47 C49 1.524(7) . ?
C47 C48 1.533(7) . ?
C47 H47 1.0000 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C50 C52B 1.493(18) . ?
C50 C51 1.500(12) . ?
C50 C52 1.547(11) . ?
C50 C51B 1.572(17) . ?
C50 H50 1.0000 . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 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 N6 1.333(5) . ?
C53 C54 1.363(6) . ?
C53 N5 1.444(5) . ?
C54 C55 1.388(7) . ?
C54 H54 0.9500 . ?
C55 C56 1.365(7) . ?
C55 H55 0.9500 . ?
C56 C57 1.437(6) . ?
C56 K2 3.271(5) 2_767 ?
C56 H56 0.9500 . ?
C57 N6 1.382(5) . ?
C57 C58 1.396(6) . ?
C57 K2 3.257(4) 2_767 ?
C58 P2 1.778(5) . ?
C58 K2 3.225(4) 2_767 ?
C58 H58 0.9500 . ?
C59 C60 1.499(7) . ?
C59 C64 1.504(8) . ?
C59 P2 1.884(5) . ?
C59 H59 1.0000 . ?
C60 C61 1.551(7) . ?
C60 H60A 0.9900 . ?
C60 H60B 0.9900 . ?
C61 C62 1.471(8) . ?
C61 H61A 0.9900 . ?
C61 H61B 0.9900 . ?
C62 C63 1.500(7) . ?
C62 H62A 0.9900 . ?
C62 H62B 0.9900 . ?
C63 C64 1.541(7) . ?
C63 H63A 0.9900 . ?
C63 H63B 0.9900 . ?
C64 H64A 0.9900 . ?
C64 H64B 0.9900 . ?
C65 C66 1.46(2) . ?
C65 C70 1.533(8) . ?
C65 C66B 1.53(2) . ?
C65 P2 1.864(5) . ?
C65 H65 1.0000 . ?
C66 C67 1.57(2) . ?
C66 H66A 0.9900 . ?
C66 H66B 0.9900 . ?
C67 C68 1.568(15) . ?
C67 H67A 0.9900 . ?
C67 H67B 0.9900 . ?
C68 C69 1.513(14) . ?
C68 H68A 0.9900 . ?
C68 H68B 0.9900 . ?
C69 C70 1.537(12) . ?
C69 H69A 0.9900 . ?
C69 H69B 0.9900 . ?
C66B C67B 1.54(2) . ?
C66B H66C 0.9900 . ?
C66B H66D 0.9900 . ?
C67B C68B 1.611(17) . ?
C67B H67C 0.9900 . ?
C67B H67D 0.9900 . ?
C68B C69B 1.412(16) . ?
C68B H68C 0.9900 . ?
C68B H68D 0.9900 . ?
C69B C70 1.609(14) . ?
C69B H69C 0.9900 . ?
C69B H69D 0.9900 . ?
C70 H70A 0.9900 . ?
C70 H70B 0.9900 . ?
C71 C72 1.449(9) . ?
C71 H71A 0.9800 . ?
C71 H71B 0.9800 . ?
C71 H71C 0.9800 . ?
C72 O2 1.429(8) . ?
C72 H72A 0.9900 . ?
C72 H72B 0.9900 . ?
C73 O2 1.382(8) . ?
C73 C74 1.466(10) . ?
C73 H73A 0.9900 . ?
C73 H73B 0.9900 . ?
C74 H74A 0.9800 . ?
C74 H74B 0.9800 . ?
C74 H74C 0.9800 . ?
N3 K1 2.792(3) . ?
N6 K2 2.838(4) . ?
P1 K1 3.2582(17) . ?
P2 K2 3.2690(16) . ?
K1 O1 2.822(4) . ?
K1 C18 3.108(4) 2_756 ?
K1 C19 3.259(4) 2_756 ?
K1 C17 3.425(4) 2_756 ?
K2 O2 2.803(4) . ?
K2 C58 3.225(4) 2_767 ?
K2 C57 3.257(4) 2_767 ?
K2 C56 3.271(5) 2_767 ?
 
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 101.6(3) . . ?
N1 C1 K1 148.5(3) . . ?
N2 C1 K1 109.9(3) . . ?
C3 C2 N1 106.6(4) . . ?
C3 C2 H2 126.7 . . ?
N1 C2 H2 126.7 . . ?
C2 C3 N2 106.0(4) . . ?
C2 C3 H3 127.0 . . ?
N2 C3 H3 127.0 . . ?
C5 C4 C9 122.7(4) . . ?
C5 C4 N1 118.4(4) . . ?
C9 C4 N1 118.9(4) . . ?
C4 C5 C6 117.0(4) . . ?
C4 C5 C10 122.4(4) . . ?
C6 C5 C10 120.6(4) . . ?
C7 C6 C5 121.4(5) . . ?
C7 C6 H6 119.3 . . ?
C5 C6 H6 119.3 . . ?
C6 C7 C8 120.3(5) . . ?
C6 C7 H7 119.8 . . ?
C8 C7 H7 119.8 . . ?
C7 C8 C9 121.1(5) . . ?
C7 C8 H8 119.4 . . ?
C9 C8 H8 119.4 . . ?
C8 C9 C4 117.5(4) . . ?
C8 C9 C13 121.5(4) . . ?
C4 C9 C13 121.0(4) . . ?
C5 C10 C12 111.5(5) . . ?
C5 C10 C11 110.8(5) . . ?
C12 C10 C11 110.5(5) . . ?
C5 C10 H10 107.9 . . ?
C12 C10 H10 107.9 . . ?
C11 C10 H10 107.9 . . ?
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 . . ?
C9 C13 C14 113.3(4) . . ?
C9 C13 C15 108.5(4) . . ?
C14 C13 C15 111.6(4) . . ?
C9 C13 H13 107.7 . . ?
C14 C13 H13 107.7 . . ?
C15 C13 H13 107.7 . . ?
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 . . ?
N3 C16 C17 126.7(4) . . ?
N3 C16 N2 114.2(3) . . ?
C17 C16 N2 119.1(4) . . ?
N3 C16 K1 47.6(2) . . ?
C17 C16 K1 142.6(3) . . ?
N2 C16 K1 81.6(2) . . ?
C16 C17 C18 115.8(4) . . ?
C16 C17 K1 95.3(3) . 2_756 ?
C18 C17 K1 65.2(2) . 2_756 ?
C16 C17 H17 122.1 . . ?
C18 C17 H17 122.1 . . ?
K1 C17 H17 107.9 2_756 . ?
C19 C18 C17 120.7(4) . . ?
C19 C18 K1 84.0(3) . 2_756 ?
C17 C18 K1 90.7(3) . 2_756 ?
C19 C18 H18 119.6 . . ?
C17 C18 H18 119.6 . . ?
K1 C18 H18 95.4 2_756 . ?
C18 C19 C20 120.9(4) . . ?
C18 C19 K1 71.5(2) . 2_756 ?
C20 C19 K1 96.7(2) . 2_756 ?
C18 C19 H19 119.5 . . ?
C20 C19 H19 119.5 . . ?
K1 C19 H19 101.7 2_756 . ?
C21 C20 N3 120.4(4) . . ?
C21 C20 C19 122.1(4) . . ?
N3 C20 C19 117.5(4) . . ?
C20 C21 P1 124.9(3) . . ?
C20 C21 H21 117.5 . . ?
P1 C21 H21 117.5 . . ?
C27 C22 C23 109.9(10) . . ?
C27 C22 P1 133.9(10) . . ?
C23 C22 P1 116.0(10) . . ?
C27 C22 H22 91.5 . . ?
C23 C22 H22 91.5 . . ?
P1 C22 H22 91.5 . . ?
C24 C23 C22 120.1(14) . . ?
C24 C23 H23A 107.3 . . ?
C22 C23 H23A 107.3 . . ?
C24 C23 H23B 107.3 . . ?
C22 C23 H23B 107.3 . . ?
H23A C23 H23B 106.9 . . ?
C25 C24 C23 111.3(11) . . ?
C25 C24 H24A 109.4 . . ?
C23 C24 H24A 109.4 . . ?
C25 C24 H24B 109.4 . . ?
C23 C24 H24B 109.4 . . ?
H24A C24 H24B 108.0 . . ?
C24 C25 C26 111.3(8) . . ?
C24 C25 H25A 109.4 . . ?
C26 C25 H25A 109.4 . . ?
C24 C25 H25B 109.4 . . ?
C26 C25 H25B 109.4 . . ?
H25A C25 H25B 108.0 . . ?
C27 C26 C25 111.1(8) . . ?
C27 C26 H26A 109.4 . . ?
C25 C26 H26A 109.4 . . ?
C27 C26 H26B 109.4 . . ?
C25 C26 H26B 109.4 . . ?
H26A C26 H26B 108.0 . . ?
C22 C27 C26 124.1(9) . . ?
C22 C27 H27A 106.3 . . ?
C26 C27 H27A 106.3 . . ?
C22 C27 H27B 106.3 . . ?
C26 C27 H27B 106.3 . . ?
H27A C27 H27B 106.4 . . ?
C27B C22B C23B 132.7(15) . . ?
C27B C22B P1 124.4(12) . . ?
C23B C22B P1 101.0(12) . . ?
C27B C22B H22B 94.4 . . ?
C23B C22B H22B 94.4 . . ?
P1 C22B H22B 94.4 . . ?
C24B C23B C22B 108.3(16) . . ?
C24B C23B H23C 110.0 . . ?
C22B C23B H23C 110.0 . . ?
C24B C23B H23D 110.0 . . ?
C22B C23B H23D 110.0 . . ?
H23C C23B H23D 108.4 . . ?
C23B C24B C25B 108.3(14) . . ?
C23B C24B H24C 110.0 . . ?
C25B C24B H24C 110.0 . . ?
C23B C24B H24D 110.0 . . ?
C25B C24B H24D 110.0 . . ?
H24C C24B H24D 108.4 . . ?
C26B C25B C24B 112.1(10) . . ?
C26B C25B H25C 109.2 . . ?
C24B C25B H25C 109.2 . . ?
C26B C25B H25D 109.2 . . ?
C24B C25B H25D 109.2 . . ?
H25C C25B H25D 107.9 . . ?
C25B C26B C27B 112.4(10) . . ?
C25B C26B H26C 109.1 . . ?
C27B C26B H26C 109.1 . . ?
C25B C26B H26D 109.1 . . ?
C27B C26B H26D 109.1 . . ?
H26C C26B H26D 107.8 . . ?
C22B C27B C26B 112.5(12) . . ?
C22B C27B H27C 109.1 . . ?
C26B C27B H27C 109.1 . . ?
C22B C27B H27D 109.1 . . ?
C26B C27B H27D 109.1 . . ?
H27C C27B H27D 107.8 . . ?
C29 C28 C33 109.7(4) . . ?
C29 C28 P1 112.3(4) . . ?
C33 C28 P1 110.2(4) . . ?
C29 C28 H28 108.2 . . ?
C33 C28 H28 108.2 . . ?
P1 C28 H28 108.2 . . ?
C28 C29 C30 112.1(4) . . ?
C28 C29 H29A 109.2 . . ?
C30 C29 H29A 109.2 . . ?
C28 C29 H29B 109.2 . . ?
C30 C29 H29B 109.2 . . ?
H29A C29 H29B 107.9 . . ?
C31 C30 C29 112.4(4) . . ?
C31 C30 H30A 109.1 . . ?
C29 C30 H30A 109.1 . . ?
C31 C30 H30B 109.1 . . ?
C29 C30 H30B 109.1 . . ?
H30A C30 H30B 107.8 . . ?
C30 C31 C32 110.4(4) . . ?
C30 C31 H31A 109.6 . . ?
C32 C31 H31A 109.6 . . ?
C30 C31 H31B 109.6 . . ?
C32 C31 H31B 109.6 . . ?
H31A C31 H31B 108.1 . . ?
C31 C32 C33 111.5(5) . . ?
C31 C32 H32A 109.3 . . ?
C33 C32 H32A 109.3 . . ?
C31 C32 H32B 109.3 . . ?
C33 C32 H32B 109.3 . . ?
H32A C32 H32B 108.0 . . ?
C28 C33 C32 112.2(4) . . ?
C28 C33 H33A 109.2 . . ?
C32 C33 H33A 109.2 . . ?
C28 C33 H33B 109.2 . . ?
C32 C33 H33B 109.2 . . ?
H33A C33 H33B 107.9 . . ?
C35 C34 H34A 109.5 . . ?
C35 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C35 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
O1 C35 C34 111.0(6) . . ?
O1 C35 H35A 109.4 . . ?
C34 C35 H35A 109.4 . . ?
O1 C35 H35B 109.4 . . ?
C34 C35 H35B 109.4 . . ?
H35A C35 H35B 108.0 . . ?
O1 C36 C37 114.1(7) . . ?
O1 C36 H36A 108.7 . . ?
C37 C36 H36A 108.7 . . ?
O1 C36 H36B 108.7 . . ?
C37 C36 H36B 108.7 . . ?
H36A C36 H36B 107.6 . . ?
C36 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C36 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
N4 C38 N5 101.7(3) . . ?
N4 C38 K2 146.8(3) . . ?
N5 C38 K2 111.2(3) . . ?
C40 C39 N4 106.0(4) . . ?
C40 C39 H39 127.0 . . ?
N4 C39 H39 127.0 . . ?
C39 C40 N5 107.1(4) . . ?
C39 C40 H40 126.5 . . ?
N5 C40 H40 126.5 . . ?
C42 C41 C46 122.6(4) . . ?
C42 C41 N4 118.5(4) . . ?
C46 C41 N4 118.8(4) . . ?
C43 C42 C41 117.4(4) . . ?
C43 C42 C47 119.8(4) . . ?
C41 C42 C47 122.8(4) . . ?
C44 C43 C42 121.0(5) . . ?
C44 C43 H43 119.5 . . ?
C42 C43 H43 119.5 . . ?
C45 C44 C43 120.6(5) . . ?
C45 C44 H44 119.7 . . ?
C43 C44 H44 119.7 . . ?
C44 C45 C46 121.3(5) . . ?
C44 C45 H45 119.4 . . ?
C46 C45 H45 119.4 . . ?
C45 C46 C41 117.1(4) . . ?
C45 C46 C50 121.1(4) . . ?
C41 C46 C50 121.8(4) . . ?
C42 C47 C49 111.7(4) . . ?
C42 C47 C48 111.4(4) . . ?
C49 C47 C48 110.3(4) . . ?
C42 C47 H47 107.7 . . ?
C49 C47 H47 107.7 . . ?
C48 C47 H47 107.7 . . ?
C47 C48 H48A 109.5 . . ?
C47 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C47 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C47 C49 H49A 109.5 . . ?
C47 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
C47 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C52B C50 C46 111.9(7) . . ?
C51 C50 C46 113.9(6) . . ?
C51 C50 C52 111.2(6) . . ?
C46 C50 C52 111.2(5) . . ?
C52B C50 C51B 112.4(9) . . ?
C46 C50 C51B 105.1(7) . . ?
C51 C50 H50 106.7 . . ?
C46 C50 H50 106.7 . . ?
C52 C50 H50 106.7 . . ?
C50 C51 H51A 109.5 . . ?
C50 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
C50 C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
C50 C52 H52A 109.5 . . ?
C50 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C50 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 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 . . ?
N6 C53 C54 126.0(4) . . ?
N6 C53 N5 114.1(4) . . ?
C54 C53 N5 119.9(4) . . ?
C53 C54 C55 117.0(4) . . ?
C53 C54 H54 121.5 . . ?
C55 C54 H54 121.5 . . ?
C56 C55 C54 120.2(4) . . ?
C56 C55 H55 119.9 . . ?
C54 C55 H55 119.9 . . ?
C55 C56 C57 120.3(4) . . ?
C55 C56 K2 120.2(3) . 2_767 ?
C57 C56 K2 76.7(2) . 2_767 ?
C55 C56 H56 119.8 . . ?
C57 C56 H56 119.8 . . ?
K2 C56 H56 74.1 2_767 . ?
N6 C57 C58 119.1(4) . . ?
N6 C57 C56 118.3(4) . . ?
C58 C57 C56 122.6(4) . . ?
N6 C57 K2 118.3(3) . 2_767 ?
C58 C57 K2 76.3(2) . 2_767 ?
C56 C57 K2 77.8(2) . 2_767 ?
C57 C58 P2 121.5(3) . . ?
C57 C58 K2 78.8(2) . 2_767 ?
P2 C58 K2 122.2(2) . 2_767 ?
C57 C58 H58 119.3 . . ?
P2 C58 H58 119.3 . . ?
K2 C58 H58 69.7 2_767 . ?
C60 C59 C64 110.6(5) . . ?
C60 C59 P2 109.9(4) . . ?
C64 C59 P2 115.4(4) . . ?
C60 C59 H59 106.8 . . ?
C64 C59 H59 106.8 . . ?
P2 C59 H59 106.8 . . ?
C59 C60 C61 111.9(5) . . ?
C59 C60 H60A 109.2 . . ?
C61 C60 H60A 109.2 . . ?
C59 C60 H60B 109.2 . . ?
C61 C60 H60B 109.2 . . ?
H60A C60 H60B 107.9 . . ?
C62 C61 C60 112.4(5) . . ?
C62 C61 H61A 109.1 . . ?
C60 C61 H61A 109.1 . . ?
C62 C61 H61B 109.1 . . ?
C60 C61 H61B 109.1 . . ?
H61A C61 H61B 107.9 . . ?
C61 C62 C63 111.7(5) . . ?
C61 C62 H62A 109.3 . . ?
C63 C62 H62A 109.3 . . ?
C61 C62 H62B 109.3 . . ?
C63 C62 H62B 109.3 . . ?
H62A C62 H62B 107.9 . . ?
C62 C63 C64 112.3(5) . . ?
C62 C63 H63A 109.1 . . ?
C64 C63 H63A 109.1 . . ?
C62 C63 H63B 109.1 . . ?
C64 C63 H63B 109.1 . . ?
H63A C63 H63B 107.9 . . ?
C59 C64 C63 111.5(5) . . ?
C59 C64 H64A 109.3 . . ?
C63 C64 H64A 109.3 . . ?
C59 C64 H64B 109.3 . . ?
C63 C64 H64B 109.3 . . ?
H64A C64 H64B 108.0 . . ?
C66 C65 C70 108.9(11) . . ?
C70 C65 C66B 109.1(11) . . ?
C66 C65 P2 113.8(8) . . ?
C70 C65 P2 109.7(4) . . ?
C66B C65 P2 104.0(7) . . ?
C66 C65 H65 108.1 . . ?
C70 C65 H65 108.1 . . ?
P2 C65 H65 108.1 . . ?
C65 C66 C67 113.0(13) . . ?
C65 C66 H66A 109.0 . . ?
C67 C66 H66A 109.0 . . ?
C65 C66 H66B 109.0 . . ?
C67 C66 H66B 109.0 . . ?
H66A C66 H66B 107.8 . . ?
C68 C67 C66 98.9(14) . . ?
C68 C67 H67A 112.0 . . ?
C66 C67 H67A 112.0 . . ?
C68 C67 H67B 112.0 . . ?
C66 C67 H67B 112.0 . . ?
H67A C67 H67B 109.7 . . ?
C69 C68 C67 104.2(11) . . ?
C69 C68 H68A 110.9 . . ?
C67 C68 H68A 110.9 . . ?
C69 C68 H68B 110.9 . . ?
C67 C68 H68B 110.9 . . ?
H68A C68 H68B 108.9 . . ?
C68 C69 C70 110.2(10) . . ?
C68 C69 H69A 109.6 . . ?
C70 C69 H69A 109.6 . . ?
C68 C69 H69B 109.6 . . ?
C70 C69 H69B 109.6 . . ?
H69A C69 H69B 108.1 . . ?
C65 C66B C67B 111.1(12) . . ?
C65 C66B H66C 109.4 . . ?
C67B C66B H66C 109.4 . . ?
C65 C66B H66D 109.4 . . ?
C67B C66B H66D 109.4 . . ?
H66C C66B H66D 108.0 . . ?
C66B C67B C68B 114.8(13) . . ?
C66B C67B H67C 108.6 . . ?
C68B C67B H67C 108.6 . . ?
C66B C67B H67D 108.6 . . ?
C68B C67B H67D 108.6 . . ?
H67C C67B H67D 107.5 . . ?
C69B C68B C67B 118.8(12) . . ?
C69B C68B H68C 107.6 . . ?
C67B C68B H68C 107.6 . . ?
C69B C68B H68D 107.6 . . ?
C67B C68B H68D 107.6 . . ?
H68C C68B H68D 107.0 . . ?
C68B C69B C70 104.8(10) . . ?
C68B C69B H69C 110.8 . . ?
C70 C69B H69C 110.8 . . ?
C68B C69B H69D 110.8 . . ?
C70 C69B H69D 110.8 . . ?
H69C C69B H69D 108.9 . . ?
C65 C70 C69 117.3(7) . . ?
C65 C70 C69B 107.1(7) . . ?
C65 C70 H70A 108.0 . . ?
C69 C70 H70A 108.0 . . ?
C65 C70 H70B 108.0 . . ?
C69 C70 H70B 108.0 . . ?
H70A C70 H70B 107.2 . . ?
C72 C71 H71A 109.5 . . ?
C72 C71 H71B 109.5 . . ?
H71A C71 H71B 109.5 . . ?
C72 C71 H71C 109.5 . . ?
H71A C71 H71C 109.5 . . ?
H71B C71 H71C 109.5 . . ?
O2 C72 C71 114.1(7) . . ?
O2 C72 H72A 108.7 . . ?
C71 C72 H72A 108.7 . . ?
O2 C72 H72B 108.7 . . ?
C71 C72 H72B 108.7 . . ?
H72A C72 H72B 107.6 . . ?
O2 C73 C74 108.4(7) . . ?
O2 C73 H73A 110.0 . . ?
C74 C73 H73A 110.0 . . ?
O2 C73 H73B 110.0 . . ?
C74 C73 H73B 110.0 . . ?
H73A C73 H73B 108.4 . . ?
C73 C74 H74A 109.5 . . ?
C73 C74 H74B 109.5 . . ?
H74A C74 H74B 109.5 . . ?
C73 C74 H74C 109.5 . . ?
H74A C74 H74C 109.5 . . ?
H74B C74 H74C 109.5 . . ?
C1 N1 C2 113.0(3) . . ?
C1 N1 C4 123.2(3) . . ?
C2 N1 C4 123.7(3) . . ?
C1 N2 C3 112.7(3) . . ?
C1 N2 C16 124.0(3) . . ?
C3 N2 C16 123.1(4) . . ?
C16 N3 C20 118.3(3) . . ?
C16 N3 K1 111.7(3) . . ?
C20 N3 K1 112.9(2) . . ?
C38 N4 C39 112.5(4) . . ?
C38 N4 C41 124.1(3) . . ?
C39 N4 C41 123.3(3) . . ?
C38 N5 C40 112.6(4) . . ?
C38 N5 C53 124.5(3) . . ?
C40 N5 C53 122.9(4) . . ?
C53 N6 C57 118.2(4) . . ?
C53 N6 K2 112.8(3) . . ?
C57 N6 K2 113.6(2) . . ?
C21 P1 C22 106.9(4) . . ?
C21 P1 C28 106.6(2) . . ?
C22 P1 C28 102.9(5) . . ?
C21 P1 C22B 94.9(5) . . ?
C28 P1 C22B 102.2(6) . . ?
C21 P1 K1 91.75(15) . . ?
C22 P1 K1 118.8(5) . . ?
C28 P1 K1 127.07(19) . . ?
C22B P1 K1 125.7(5) . . ?
C58 P2 C65 101.5(2) . . ?
C58 P2 C59 106.2(3) . . ?
C65 P2 C59 101.8(3) . . ?
C58 P2 K2 91.56(16) . . ?
C65 P2 K2 131.9(2) . . ?
C59 P2 K2 118.65(18) . . ?
N3 K1 O1 149.14(11) . . ?
N3 K1 C1 59.76(11) . . ?
O1 K1 C1 109.45(12) . . ?
N3 K1 C18 138.76(11) . 2_756 ?
O1 K1 C18 71.80(11) . 2_756 ?
C1 K1 C18 126.73(12) . 2_756 ?
N3 K1 P1 61.44(7) . . ?
O1 K1 P1 102.16(9) . . ?
C1 K1 P1 110.28(9) . . ?
C18 K1 P1 121.68(9) 2_756 . ?
N3 K1 C19 125.71(10) . 2_756 ?
O1 K1 C19 83.91(11) . 2_756 ?
C1 K1 C19 103.01(12) . 2_756 ?
C18 K1 C19 24.46(11) 2_756 2_756 ?
P1 K1 C19 141.49(8) . 2_756 ?
N3 K1 C17 121.45(10) . 2_756 ?
O1 K1 C17 85.57(11) . 2_756 ?
C1 K1 C17 141.67(11) . 2_756 ?
C18 K1 C17 24.18(10) 2_756 2_756 ?
P1 K1 C17 100.02(8) . 2_756 ?
C19 K1 C17 41.98(10) 2_756 2_756 ?
N3 K1 C16 20.65(9) . . ?
O1 K1 C16 151.30(11) . . ?
C1 K1 C16 44.40(11) . . ?
C18 K1 C16 130.24(10) 2_756 . ?
P1 K1 C16 82.07(7) . . ?
C19 K1 C16 110.61(10) 2_756 . ?
C17 K1 C16 122.02(10) 2_756 . ?
N3 K1 K1 57.87(7) . 2_756 ?
O1 K1 K1 152.82(9) . 2_756 ?
C1 K1 K1 87.22(9) . 2_756 ?
C18 K1 K1 81.03(8) 2_756 2_756 ?
P1 K1 K1 91.28(4) . 2_756 ?
C19 K1 K1 71.20(7) 2_756 2_756 ?
C17 K1 K1 68.74(7) 2_756 2_756 ?
C16 K1 K1 53.28(7) . 2_756 ?
O2 K2 N6 143.01(11) . . ?
O2 K2 C38 104.66(12) . . ?
N6 K2 C38 59.69(11) . . ?
O2 K2 C58 112.03(12) . 2_767 ?
N6 K2 C58 104.96(11) . 2_767 ?
C38 K2 C58 111.07(12) . 2_767 ?
O2 K2 C57 100.32(12) . 2_767 ?
N6 K2 C57 113.92(10) . 2_767 ?
C38 K2 C57 135.92(12) . 2_767 ?
C58 K2 C57 24.87(11) 2_767 2_767 ?
O2 K2 P2 101.84(10) . . ?
N6 K2 P2 58.66(8) . . ?
C38 K2 P2 107.13(9) . . ?
C58 K2 P2 118.86(9) 2_767 . ?
C57 K2 P2 102.43(9) 2_767 . ?
O2 K2 C56 75.10(12) . 2_767 ?
N6 K2 C56 136.96(11) . 2_767 ?
C38 K2 C56 147.80(13) . 2_767 ?
C58 K2 C56 44.99(12) 2_767 2_767 ?
C57 K2 C56 25.43(11) 2_767 2_767 ?
P2 K2 C56 104.32(10) . 2_767 ?
O2 K2 K2 143.17(10) . 2_767 ?
N6 K2 K2 62.77(7) . 2_767 ?
C38 K2 K2 112.16(9) . 2_767 ?
C58 K2 K2 55.04(8) 2_767 2_767 ?
C57 K2 K2 52.41(8) 2_767 2_767 ?
P2 K2 K2 67.11(3) . 2_767 ?
C56 K2 K2 74.21(8) 2_767 2_767 ?
C36 O1 C35 110.4(6) . . ?
C36 O1 K1 120.2(5) . . ?
C35 O1 K1 120.2(4) . . ?
C73 O2 C72 115.6(6) . . ?
C73 O2 K2 128.1(4) . . ?
C72 O2 K2 114.3(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
N1 C2 C3 N2 -0.2(5) . . . . ?
C9 C4 C5 C6 1.3(7) . . . . ?
N1 C4 C5 C6 -177.5(4) . . . . ?
C9 C4 C5 C10 -177.8(5) . . . . ?
N1 C4 C5 C10 3.4(7) . . . . ?
C4 C5 C6 C7 -0.9(8) . . . . ?
C10 C5 C6 C7 178.3(5) . . . . ?
C5 C6 C7 C8 0.3(8) . . . . ?
C6 C7 C8 C9 -0.2(8) . . . . ?
C7 C8 C9 C4 0.7(7) . . . . ?
C7 C8 C9 C13 177.9(4) . . . . ?
C5 C4 C9 C8 -1.2(7) . . . . ?
N1 C4 C9 C8 177.6(4) . . . . ?
C5 C4 C9 C13 -178.5(4) . . . . ?
N1 C4 C9 C13 0.3(6) . . . . ?
C4 C5 C10 C12 122.8(5) . . . . ?
C6 C5 C10 C12 -56.4(7) . . . . ?
C4 C5 C10 C11 -113.6(6) . . . . ?
C6 C5 C10 C11 67.3(7) . . . . ?
C8 C9 C13 C14 40.7(6) . . . . ?
C4 C9 C13 C14 -142.2(4) . . . . ?
C8 C9 C13 C15 -83.9(5) . . . . ?
C4 C9 C13 C15 93.2(5) . . . . ?
N3 C16 C17 C18 -1.7(6) . . . . ?
N2 C16 C17 C18 175.6(3) . . . . ?
K1 C16 C17 C18 -67.5(6) . . . . ?
N3 C16 C17 K1 63.3(4) . . . 2_756 ?
N2 C16 C17 K1 -119.4(3) . . . 2_756 ?
K1 C16 C17 K1 -2.6(5) . . . 2_756 ?
C16 C17 C18 C19 0.3(6) . . . . ?
K1 C17 C18 C19 -83.4(4) 2_756 . . . ?
C16 C17 C18 K1 83.7(4) . . . 2_756 ?
C17 C18 C19 C20 0.4(6) . . . . ?
K1 C18 C19 C20 -86.8(4) 2_756 . . . ?
C17 C18 C19 K1 87.2(4) . . . 2_756 ?
C18 C19 C20 C21 -178.9(4) . . . . ?
K1 C19 C20 C21 108.7(4) 2_756 . . . ?
C18 C19 C20 N3 0.1(6) . . . . ?
K1 C19 C20 N3 -72.4(3) 2_756 . . . ?
N3 C20 C21 P1 4.0(6) . . . . ?
C19 C20 C21 P1 -177.1(3) . . . . ?
C27 C22 C23 C24 -23(2) . . . . ?
P1 C22 C23 C24 161.9(13) . . . . ?
C22 C23 C24 C25 41(2) . . . . ?
C23 C24 C25 C26 -56.7(15) . . . . ?
C24 C25 C26 C27 57.3(12) . . . . ?
C23 C22 C27 C26 24.4(18) . . . . ?
P1 C22 C27 C26 -161.2(9) . . . . ?
C25 C26 C27 C22 -41.6(14) . . . . ?
C27B C22B C23B C24B 38(3) . . . . ?
P1 C22B C23B C24B -157.2(16) . . . . ?
C22B C23B C24B C25B -42(2) . . . . ?
C23B C24B C25B C26B 56.3(18) . . . . ?
C24B C25B C26B C27B -52.5(14) . . . . ?
C23B C22B C27B C26B -34(3) . . . . ?
P1 C22B C27B C26B 164.8(10) . . . . ?
C25B C26B C27B C22B 38.7(17) . . . . ?
C33 C28 C29 C30 -54.1(6) . . . . ?
P1 C28 C29 C30 -177.0(4) . . . . ?
C28 C29 C30 C31 55.7(7) . . . . ?
C29 C30 C31 C32 -55.2(7) . . . . ?
C30 C31 C32 C33 54.9(6) . . . . ?
C29 C28 C33 C32 54.3(7) . . . . ?
P1 C28 C33 C32 178.4(4) . . . . ?
C31 C32 C33 C28 -55.8(7) . . . . ?
N4 C39 C40 N5 0.9(5) . . . . ?
C46 C41 C42 C43 -0.5(6) . . . . ?
N4 C41 C42 C43 -178.6(4) . . . . ?
C46 C41 C42 C47 -179.5(4) . . . . ?
N4 C41 C42 C47 2.5(6) . . . . ?
C41 C42 C43 C44 0.3(7) . . . . ?
C47 C42 C43 C44 179.3(5) . . . . ?
C42 C43 C44 C45 -0.3(8) . . . . ?
C43 C44 C45 C46 0.6(8) . . . . ?
C44 C45 C46 C41 -0.7(7) . . . . ?
C44 C45 C46 C50 -179.9(4) . . . . ?
C42 C41 C46 C45 0.7(6) . . . . ?
N4 C41 C46 C45 178.8(4) . . . . ?
C42 C41 C46 C50 179.9(4) . . . . ?
N4 C41 C46 C50 -2.1(6) . . . . ?
C43 C42 C47 C49 -64.8(6) . . . . ?
C41 C42 C47 C49 114.1(5) . . . . ?
C43 C42 C47 C48 59.1(6) . . . . ?
C41 C42 C47 C48 -122.0(5) . . . . ?
C45 C46 C50 C52B -44.3(9) . . . . ?
C41 C46 C50 C52B 136.6(8) . . . . ?
C45 C46 C50 C51 45.5(8) . . . . ?
C41 C46 C50 C51 -133.6(6) . . . . ?
C45 C46 C50 C52 -81.1(7) . . . . ?
C41 C46 C50 C52 99.8(7) . . . . ?
C45 C46 C50 C51B 77.9(9) . . . . ?
C41 C46 C50 C51B -101.2(9) . . . . ?
N6 C53 C54 C55 0.2(7) . . . . ?
N5 C53 C54 C55 -176.6(4) . . . . ?
C53 C54 C55 C56 0.5(7) . . . . ?
C54 C55 C56 C57 0.2(7) . . . . ?
C54 C55 C56 K2 -91.6(5) . . . 2_767 ?
C55 C56 C57 N6 -1.6(6) . . . . ?
K2 C56 C57 N6 115.8(3) 2_767 . . . ?
C55 C56 C57 C58 177.8(4) . . . . ?
K2 C56 C57 C58 -64.8(4) 2_767 . . . ?
C55 C56 C57 K2 -117.4(5) . . . 2_767 ?
N6 C57 C58 P2 6.0(6) . . . . ?
C56 C57 C58 P2 -173.4(3) . . . . ?
K2 C57 C58 P2 121.0(3) 2_767 . . . ?
N6 C57 C58 K2 -115.0(3) . . . 2_767 ?
C56 C57 C58 K2 65.6(4) . . . 2_767 ?
C64 C59 C60 C61 54.2(7) . . . . ?
P2 C59 C60 C61 -177.2(4) . . . . ?
C59 C60 C61 C62 -54.2(7) . . . . ?
C60 C61 C62 C63 52.9(7) . . . . ?
C61 C62 C63 C64 -53.4(7) . . . . ?
C60 C59 C64 C63 -54.5(7) . . . . ?
P2 C59 C64 C63 179.9(4) . . . . ?
C62 C63 C64 C59 54.3(7) . . . . ?
C70 C65 C66 C67 54.5(19) . . . . ?
C66B C65 C66 C67 147(12) . . . . ?
P2 C65 C66 C67 177.2(12) . . . . ?
C65 C66 C67 C68 -74.3(19) . . . . ?
C66 C67 C68 C69 74.9(13) . . . . ?
C67 C68 C69 C70 -63.7(13) . . . . ?
C66 C65 C66B C67B -37(9) . . . . ?
C70 C65 C66B C67B 53.6(18) . . . . ?
P2 C65 C66B C67B 170.5(14) . . . . ?
C65 C66B C67B C68B -34(2) . . . . ?
C66B C67B C68B C69B 37(2) . . . . ?
C67B C68B C69B C70 -51.1(16) . . . . ?
C66 C65 C70 C69 -38.1(12) . . . . ?
C66B C65 C70 C69 -50.0(11) . . . . ?
P2 C65 C70 C69 -163.3(7) . . . . ?
C66 C65 C70 C69B -59.9(11) . . . . ?
C66B C65 C70 C69B -71.8(11) . . . . ?
P2 C65 C70 C69B 175.0(6) . . . . ?
C68 C69 C70 C65 44.7(13) . . . . ?
C68 C69 C70 C69B 112(3) . . . . ?
C68B C69B C70 C65 68.6(11) . . . . ?
C68B C69B C70 C69 -52(2) . . . . ?
N2 C1 N1 C2 0.1(4) . . . . ?
K1 C1 N1 C2 179.2(4) . . . . ?
N2 C1 N1 C4 -176.5(3) . . . . ?
K1 C1 N1 C4 2.6(8) . . . . ?
C3 C2 N1 C1 0.1(5) . . . . ?
C3 C2 N1 C4 176.7(4) . . . . ?
C5 C4 N1 C1 78.8(5) . . . . ?
C9 C4 N1 C1 -100.1(5) . . . . ?
C5 C4 N1 C2 -97.5(5) . . . . ?
C9 C4 N1 C2 83.7(5) . . . . ?
N1 C1 N2 C3 -0.3(4) . . . . ?
K1 C1 N2 C3 -179.8(3) . . . . ?
N1 C1 N2 C16 174.7(3) . . . . ?
K1 C1 N2 C16 -4.8(4) . . . . ?
C2 C3 N2 C1 0.3(5) . . . . ?
C2 C3 N2 C16 -174.7(4) . . . . ?
N3 C16 N2 C1 -31.8(5) . . . . ?
C17 C16 N2 C1 150.5(4) . . . . ?
K1 C16 N2 C1 3.8(3) . . . . ?
N3 C16 N2 C3 142.6(4) . . . . ?
C17 C16 N2 C3 -35.0(6) . . . . ?
K1 C16 N2 C3 178.2(3) . . . . ?
C17 C16 N3 C20 2.3(6) . . . . ?
N2 C16 N3 C20 -175.2(3) . . . . ?
K1 C16 N3 C20 133.7(4) . . . . ?
C17 C16 N3 K1 -131.4(4) . . . . ?
N2 C16 N3 K1 51.2(4) . . . . ?
C21 C20 N3 C16 177.6(4) . . . . ?
C19 C20 N3 C16 -1.3(5) . . . . ?
C21 C20 N3 K1 -49.2(4) . . . . ?
C19 C20 N3 K1 131.8(3) . . . . ?
N5 C38 N4 C39 0.3(4) . . . . ?
K2 C38 N4 C39 -172.3(4) . . . . ?
N5 C38 N4 C41 179.6(4) . . . . ?
K2 C38 N4 C41 7.1(7) . . . . ?
C40 C39 N4 C38 -0.8(5) . . . . ?
C40 C39 N4 C41 179.8(4) . . . . ?
C42 C41 N4 C38 -89.4(5) . . . . ?
C46 C41 N4 C38 92.5(5) . . . . ?
C42 C41 N4 C39 89.9(5) . . . . ?
C46 C41 N4 C39 -88.2(5) . . . . ?
N4 C38 N5 C40 0.4(4) . . . . ?
K2 C38 N5 C40 176.0(3) . . . . ?
N4 C38 N5 C53 -178.1(3) . . . . ?
K2 C38 N5 C53 -2.5(5) . . . . ?
C39 C40 N5 C38 -0.9(5) . . . . ?
C39 C40 N5 C53 177.6(4) . . . . ?
N6 C53 N5 C38 35.7(5) . . . . ?
C54 C53 N5 C38 -147.1(4) . . . . ?
N6 C53 N5 C40 -142.5(4) . . . . ?
C54 C53 N5 C40 34.6(6) . . . . ?
C54 C53 N6 C57 -1.6(6) . . . . ?
N5 C53 N6 C57 175.4(3) . . . . ?
C54 C53 N6 K2 134.4(4) . . . . ?
N5 C53 N6 K2 -48.6(4) . . . . ?
C58 C57 N6 C53 -177.2(4) . . . . ?
C56 C57 N6 C53 2.2(5) . . . . ?
K2 C57 N6 C53 93.3(4) 2_767 . . . ?
C58 C57 N6 K2 47.1(4) . . . . ?
C56 C57 N6 K2 -133.4(3) . . . . ?
K2 C57 N6 K2 -42.4(3) 2_767 . . . ?
C20 C21 P1 C22 153.0(6) . . . . ?
C20 C21 P1 C28 -97.5(4) . . . . ?
C20 C21 P1 C22B 158.2(6) . . . . ?
C20 C21 P1 K1 32.1(4) . . . . ?
C27 C22 P1 C21 129.5(11) . . . . ?
C23 C22 P1 C21 -56.3(14) . . . . ?
C27 C22 P1 C28 17.4(13) . . . . ?
C23 C22 P1 C28 -168.4(13) . . . . ?
C27 C22 P1 C22B 106(5) . . . . ?
C23 C22 P1 C22B -80(4) . . . . ?
C27 C22 P1 K1 -128.8(11) . . . . ?
C23 C22 P1 K1 45.4(14) . . . . ?
C29 C28 P1 C21 174.7(4) . . . . ?
C33 C28 P1 C21 52.1(5) . . . . ?
C29 C28 P1 C22 -73.0(6) . . . . ?
C33 C28 P1 C22 164.5(5) . . . . ?
C29 C28 P1 C22B -86.4(6) . . . . ?
C33 C28 P1 C22B 151.1(6) . . . . ?
C29 C28 P1 K1 69.3(4) . . . . ?
C33 C28 P1 K1 -53.2(5) . . . . ?
C57 C58 P2 C65 -176.1(4) . . . . ?
K2 C58 P2 C65 -79.4(3) 2_767 . . . ?
C57 C58 P2 C59 77.8(4) . . . . ?
K2 C58 P2 C59 174.5(2) 2_767 . . . ?
C57 C58 P2 K2 -42.7(4) . . . . ?
K2 C58 P2 K2 54.0(2) 2_767 . . . ?
C66 C65 P2 C58 64.0(13) . . . . ?
C70 C65 P2 C58 -173.7(4) . . . . ?
C66B C65 P2 C58 69.7(12) . . . . ?
C66 C65 P2 C59 173.5(13) . . . . ?
C70 C65 P2 C59 -64.2(5) . . . . ?
C66B C65 P2 C59 179.2(11) . . . . ?
C66 C65 P2 K2 -38.7(13) . . . . ?
C70 C65 P2 K2 83.6(4) . . . . ?
C66B C65 P2 K2 -33.0(12) . . . . ?
C60 C59 P2 C58 -98.5(5) . . . . ?
C64 C59 P2 C58 27.4(5) . . . . ?
C60 C59 P2 C65 155.6(5) . . . . ?
C64 C59 P2 C65 -78.4(5) . . . . ?
C60 C59 P2 K2 2.5(5) . . . . ?
C64 C59 P2 K2 128.4(4) . . . . ?
C37 C36 O1 C35 -162.6(9) . . . . ?
C37 C36 O1 K1 50.4(10) . . . . ?
C34 C35 O1 C36 164.9(7) . . . . ?
C34 C35 O1 K1 -48.1(8) . . . . ?
C74 C73 O2 C72 179.0(6) . . . . ?
C74 C73 O2 K2 -18.6(7) . . . . ?
C71 C72 O2 C73 -74.2(10) . . . . ?
C71 C72 O2 K2 120.9(7) . . . . ?
 
_refine_diff_density_max    0.844
_refine_diff_density_min   -0.620
_refine_diff_density_rms    0.065

_shelxl_version_number 2013-4



 
data_pbad150303
 
_audit_creation_method            SHELXL-2013
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          'C29 H41 Cl Cr N3 P'
_chemical_formula_sum
 'C29 H41 Cl Cr N3 P' 
_chemical_formula_weight          550.07

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'
 'Cl'  'Cl'   0.1484   0.1585
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Cr'  'Cr'   0.3209   0.6236
 '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                    8.370(2)
_cell_length_b                    23.052(6)
_cell_length_c                    17.180(4)
_cell_angle_alpha                 90
_cell_angle_beta                  116.249(10)
_cell_angle_gamma                 90
_cell_volume                      2972.9(13)
_cell_formula_units_Z             4
_cell_measurement_temperature     173(2)
_cell_measurement_reflns_used     3897 
_cell_measurement_theta_min       2.59
_cell_measurement_theta_max       27.69
 
_exptl_crystal_description        'plate' 
_exptl_crystal_colour             'red'
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_method     ?              
_exptl_crystal_density_diffrn     1.229          
_exptl_crystal_F_000              1168
_exptl_transmission_factor_min    ?                                             
_exptl_transmission_factor_max    ?                                             
_exptl_crystal_size_max           0.350
_exptl_crystal_size_mid           0.250
_exptl_crystal_size_min           0.120
_exptl_absorpt_coefficient_mu     0.550
_shelx_estimated_absorpt_T_min    0.831
_shelx_estimated_absorpt_T_max    0.937
_exptl_absorpt_correction_type    'multi-scan' 
_exptl_absorpt_correction_T_min   0.6528  
_exptl_absorpt_correction_T_max   0.7456
_exptl_absorpt_process_details    'sadabs'
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       173(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_source                    'fine focus sealed tube'                       
_diffrn_measurement_device_type   'Bruker APEX-II CCD'
_diffrn_measurement_method        'φ and ω scans'
_diffrn_detector_area_resol_mean  ? 
_diffrn_reflns_number             29169
_diffrn_reflns_av_unetI/netI      0.0968
_diffrn_reflns_av_R_equivalents   0.0971
_diffrn_reflns_limit_h_min        -11
_diffrn_reflns_limit_h_max        11
_diffrn_reflns_limit_k_min        -30
_diffrn_reflns_limit_k_max        30
_diffrn_reflns_limit_l_min        -15
_diffrn_reflns_limit_l_max        22
_diffrn_reflns_theta_min          1.590
_diffrn_reflns_theta_max          28.113
_diffrn_reflns_theta_full         25.242
_diffrn_measured_fraction_theta_max   0.991
_diffrn_measured_fraction_theta_full  1.000
_diffrn_reflns_Laue_measured_fraction_max    0.991
_diffrn_reflns_Laue_measured_fraction_full   1.000
_diffrn_reflns_point_group_measured_fraction_max   0.991
_diffrn_reflns_point_group_measured_fraction_full  1.000
_reflns_number_total              7188
_reflns_number_gt                 4181
_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 APEX2'
_computing_cell_refinement        'Bruker SAINT'
_computing_data_reduction         'Bruker SAINT'
_computing_structure_solution     'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement   'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics     'Bruker SHELXTL'
_computing_publication_material   'Bruker SHELXTL'
 
_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)+(0.0636P)²+0.5470P] 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          7188
_refine_ls_number_parameters      326
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.1320
_refine_ls_R_factor_gt            0.0636
_refine_ls_wR_factor_ref          0.1452
_refine_ls_wR_factor_gt           0.1246
_refine_ls_goodness_of_fit_ref    1.015
_refine_ls_restrained_S_all       1.015
_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
C1 C 0.6164(4) 0.75950(14) 0.34984(18) 0.0260(7) Uani 1 1 d . . . . .
C2 C 0.8381(4) 0.69491(15) 0.4147(2) 0.0360(8) Uani 1 1 d . . . . .
H2 H 0.9033 0.6596 0.4271 0.043 Uiso 1 1 calc R U . . .
C3 C 0.8922(4) 0.74480(16) 0.4576(2) 0.0365(8) Uani 1 1 d . . . . .
H3 H 1.0034 0.7519 0.5061 0.044 Uiso 1 1 calc R U . . .
C4 C 0.5564(4) 0.65999(14) 0.29101(19) 0.0297(7) Uani 1 1 d . . . . .
C5 C 0.5517(5) 0.65440(15) 0.2094(2) 0.0381(8) Uani 1 1 d . . . . .
C6 C 0.4423(5) 0.61120(17) 0.1560(2) 0.0489(10) Uani 1 1 d . . . . .
H6 H 0.4362 0.6057 0.1000 0.059 Uiso 1 1 calc R U . . .
C7 C 0.3434(5) 0.57653(18) 0.1822(3) 0.0546(11) Uani 1 1 d . . . . .
H7 H 0.2699 0.5472 0.1446 0.065 Uiso 1 1 calc R U . . .
C8 C 0.3494(5) 0.58377(17) 0.2627(3) 0.0545(11) Uani 1 1 d . . . . .
H8 H 0.2786 0.5595 0.2797 0.065 Uiso 1 1 calc R U . . .
C9 C 0.4565(4) 0.62565(15) 0.3199(2) 0.0384(8) Uani 1 1 d . . . . .
C10 C 0.6632(6) 0.69276(19) 0.1811(2) 0.0596(12) Uani 1 1 d . . . . .
H10 H 0.6904 0.7292 0.2163 0.071 Uiso 1 1 calc R U . . .
C11 C 0.8388(6) 0.6633(3) 0.2005(3) 0.0953(19) Uani 1 1 d . . . . .
H11A H 0.9002 0.6536 0.2623 0.143 Uiso 1 1 calc R U . . .
H11B H 0.9134 0.6896 0.1857 0.143 Uiso 1 1 calc R U . . .
H11C H 0.8163 0.6278 0.1660 0.143 Uiso 1 1 calc R U . . .
C12 C 0.5688(8) 0.7098(3) 0.0861(3) 0.0901(17) Uani 1 1 d . . . . .
H12A H 0.5487 0.6752 0.0498 0.135 Uiso 1 1 calc R U . . .
H12B H 0.6425 0.7375 0.0730 0.135 Uiso 1 1 calc R U . . .
H12C H 0.4540 0.7278 0.0740 0.135 Uiso 1 1 calc R U . . .
C13 C 0.4583(5) 0.63443(18) 0.4077(2) 0.0502(10) Uani 1 1 d . . . . .
H13 H 0.5631 0.6596 0.4427 0.060 Uiso 1 1 calc R U . . .
C14 C 0.2939(7) 0.6661(3) 0.4000(3) 0.0944(18) Uani 1 1 d . . . . .
H14A H 0.2861 0.7038 0.3722 0.142 Uiso 1 1 calc R U . . .
H14B H 0.3010 0.6719 0.4579 0.142 Uiso 1 1 calc R U . . .
H14C H 0.1879 0.6430 0.3648 0.142 Uiso 1 1 calc R U . . .
C15 C 0.4821(7) 0.5781(2) 0.4572(3) 0.0866(16) Uani 1 1 d . . . . .
H15A H 0.3805 0.5525 0.4251 0.130 Uiso 1 1 calc R U . . .
H15B H 0.4889 0.5863 0.5146 0.130 Uiso 1 1 calc R U . . .
H15C H 0.5922 0.5591 0.4640 0.130 Uiso 1 1 calc R U . . .
C16 C 0.7435(4) 0.84325(15) 0.43950(19) 0.0292(7) Uani 1 1 d . . . . .
C17 C 0.8762(5) 0.87038(17) 0.5063(2) 0.0432(9) Uani 1 1 d . . . . .
H17 H 0.9856 0.8516 0.5416 0.052 Uiso 1 1 calc R U . . .
C18 C 0.8422(5) 0.92885(18) 0.5208(2) 0.0509(10) Uani 1 1 d . . . . .
H18 H 0.9326 0.9504 0.5659 0.061 Uiso 1 1 calc R U . . .
C19 C 0.6855(5) 0.95399(17) 0.4721(2) 0.0447(9) Uani 1 1 d . . . . .
H19 H 0.6656 0.9927 0.4844 0.054 Uiso 1 1 calc R U . . .
C20 C 0.5463(4) 0.92369(14) 0.40134(19) 0.0320(7) Uani 1 1 d . . . . .
C21 C 0.3835(5) 0.94756(15) 0.3499(2) 0.0384(8) Uani 1 1 d . . . . .
H21 H 0.3556 0.9859 0.3603 0.046 Uiso 1 1 calc R U . . .
C22 C 0.1710(7) 0.94932(17) 0.1638(2) 0.0620(12) Uani 1 1 d . . . . .
C23 C 0.3422(10) 0.9478(3) 0.1531(4) 0.122(2) Uani 1 1 d . . . . .
H23A H 0.3702 0.9076 0.1452 0.183 Uiso 1 1 calc R U . . .
H23B H 0.4400 0.9641 0.2050 0.183 Uiso 1 1 calc R U . . .
H23C H 0.3265 0.9708 0.1022 0.183 Uiso 1 1 calc R U . . .
C24 C 0.1264(9) 1.0125(2) 0.1708(3) 0.110(2) Uani 1 1 d . . . . .
H24A H 0.1247 1.0343 0.1215 0.165 Uiso 1 1 calc R U . . .
H24B H 0.2167 1.0290 0.2251 0.165 Uiso 1 1 calc R U . . .
H24C H 0.0092 1.0149 0.1704 0.165 Uiso 1 1 calc R U . . .
C25 C 0.0273(10) 0.9196(2) 0.0858(3) 0.142(3) Uani 1 1 d . . . . .
H25A H -0.0858 0.9214 0.0899 0.213 Uiso 1 1 calc R U . . .
H25B H 0.0603 0.8790 0.0842 0.213 Uiso 1 1 calc R U . . .
H25C H 0.0141 0.9393 0.0327 0.213 Uiso 1 1 calc R U . . .
C26 C 0.0335(5) 0.89269(19) 0.2892(3) 0.0606(12) Uani 1 1 d . . . . .
C27 C 0.1183(9) 0.8572(3) 0.3738(5) 0.145(3) Uani 1 1 d . . . . .
H27A H 0.2224 0.8779 0.4165 0.217 Uiso 1 1 calc R U . . .
H27B H 0.1554 0.8192 0.3618 0.217 Uiso 1 1 calc R U . . .
H27C H 0.0311 0.8518 0.3968 0.217 Uiso 1 1 calc R U . . .
C28 C -0.0463(7) 0.9471(2) 0.3074(4) 0.102(2) Uani 1 1 d . . . . .
H28A H -0.1055 0.9697 0.2538 0.154 Uiso 1 1 calc R U . . .
H28B H 0.0484 0.9704 0.3514 0.154 Uiso 1 1 calc R U . . .
H28C H -0.1334 0.9363 0.3285 0.154 Uiso 1 1 calc R U . . .
C29 C -0.1113(7) 0.8572(3) 0.2189(5) 0.132(3) Uani 1 1 d . . . . .
H29A H -0.2046 0.8480 0.2368 0.198 Uiso 1 1 calc R U . . .
H29B H -0.0600 0.8211 0.2098 0.198 Uiso 1 1 calc R U . . .
H29C H -0.1629 0.8795 0.1648 0.198 Uiso 1 1 calc R U . . .
N1 N 0.6687(3) 0.70422(11) 0.34851(15) 0.0279(6) Uani 1 1 d . . . . .
N2 N 0.7559(3) 0.78404(12) 0.41803(15) 0.0280(6) Uani 1 1 d . . . . .
N3 N 0.5836(3) 0.86654(11) 0.38650(15) 0.0273(6) Uani 1 1 d . . . . .
P1 P 0.22697(11) 0.90609(4) 0.26431(5) 0.0312(2) Uani 1 1 d . . . . .
Cl1 Cl 0.22014(13) 0.76276(5) 0.17040(6) 0.0658(3) Uani 1 1 d . . . . .
Cr1 Cr 0.40619(6) 0.81754(2) 0.28608(3) 0.02761(15) Uani 1 1 d . . . . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
C1 N1 1.351(4) . ?
C1 N2 1.359(4) . ?
C1 Cr1 2.093(3) . ?
C2 C3 1.332(5) . ?
C2 N1 1.386(4) . ?
C2 H2 0.9500 . ?
C3 N2 1.377(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.391(4) . ?
C4 C9 1.392(5) . ?
C4 N1 1.442(4) . ?
C5 C6 1.389(5) . ?
C5 C10 1.514(5) . ?
C6 C7 1.363(5) . ?
C6 H6 0.9500 . ?
C7 C8 1.371(5) . ?
C7 H7 0.9500 . ?
C8 C9 1.386(5) . ?
C8 H8 0.9500 . ?
C9 C13 1.516(5) . ?
C10 C11 1.516(7) . ?
C10 C12 1.518(6) . ?
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 C14 1.511(6) . ?
C13 C15 1.517(6) . ?
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 . ?
C16 C17 1.347(4) . ?
C16 N3 1.353(4) . ?
C16 N2 1.429(4) . ?
C17 C18 1.422(5) . ?
C17 H17 0.9500 . ?
C18 C19 1.336(5) . ?
C18 H18 0.9500 . ?
C19 C20 1.439(4) . ?
C19 H19 0.9500 . ?
C20 C21 1.370(4) . ?
C20 N3 1.403(4) . ?
C21 P1 1.757(3) . ?
C21 H21 0.9500 . ?
C22 C25 1.512(6) . ?
C22 C24 1.521(6) . ?
C22 C23 1.523(8) . ?
C22 P1 1.866(4) . ?
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 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 C28 1.517(6) . ?
C26 C29 1.518(7) . ?
C26 C27 1.540(7) . ?
C26 P1 1.875(4) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
N3 Cr1 2.047(2) . ?
P1 Cr1 2.4616(11) . ?
Cl1 Cr1 2.2874(11) . ?
 
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
N1 C1 N2 104.2(2) . . ?
N1 C1 Cr1 142.9(2) . . ?
N2 C1 Cr1 112.8(2) . . ?
C3 C2 N1 107.1(3) . . ?
C3 C2 H2 126.4 . . ?
N1 C2 H2 126.4 . . ?
C2 C3 N2 106.8(3) . . ?
C2 C3 H3 126.6 . . ?
N2 C3 H3 126.6 . . ?
C5 C4 C9 123.6(3) . . ?
C5 C4 N1 118.4(3) . . ?
C9 C4 N1 118.1(3) . . ?
C6 C5 C4 116.6(3) . . ?
C6 C5 C10 121.8(3) . . ?
C4 C5 C10 121.6(3) . . ?
C7 C6 C5 121.4(4) . . ?
C7 C6 H6 119.3 . . ?
C5 C6 H6 119.3 . . ?
C6 C7 C8 120.3(4) . . ?
C6 C7 H7 119.8 . . ?
C8 C7 H7 119.8 . . ?
C7 C8 C9 121.5(4) . . ?
C7 C8 H8 119.2 . . ?
C9 C8 H8 119.2 . . ?
C8 C9 C4 116.5(3) . . ?
C8 C9 C13 121.1(3) . . ?
C4 C9 C13 122.4(3) . . ?
C5 C10 C11 110.1(4) . . ?
C5 C10 C12 113.3(4) . . ?
C11 C10 C12 110.2(4) . . ?
C5 C10 H10 107.7 . . ?
C11 C10 H10 107.7 . . ?
C12 C10 H10 107.7 . . ?
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 . . ?
C14 C13 C9 111.7(3) . . ?
C14 C13 C15 110.5(4) . . ?
C9 C13 C15 112.6(4) . . ?
C14 C13 H13 107.2 . . ?
C9 C13 H13 107.2 . . ?
C15 C13 H13 107.2 . . ?
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 . . ?
C17 C16 N3 125.9(3) . . ?
C17 C16 N2 122.5(3) . . ?
N3 C16 N2 111.6(2) . . ?
C16 C17 C18 115.8(3) . . ?
C16 C17 H17 122.1 . . ?
C18 C17 H17 122.1 . . ?
C19 C18 C17 121.2(3) . . ?
C19 C18 H18 119.4 . . ?
C17 C18 H18 119.4 . . ?
C18 C19 C20 121.5(3) . . ?
C18 C19 H19 119.3 . . ?
C20 C19 H19 119.3 . . ?
C21 C20 N3 119.9(3) . . ?
C21 C20 C19 123.6(3) . . ?
N3 C20 C19 116.6(3) . . ?
C20 C21 P1 118.8(3) . . ?
C20 C21 H21 120.6 . . ?
P1 C21 H21 120.6 . . ?
C25 C22 C24 112.1(4) . . ?
C25 C22 C23 107.8(5) . . ?
C24 C22 C23 108.0(5) . . ?
C25 C22 P1 110.7(3) . . ?
C24 C22 P1 114.0(3) . . ?
C23 C22 P1 103.6(3) . . ?
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 . . ?
C22 C25 H25A 109.5 . . ?
C22 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C22 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C28 C26 C29 109.9(4) . . ?
C28 C26 C27 107.9(5) . . ?
C29 C26 C27 109.7(5) . . ?
C28 C26 P1 114.5(3) . . ?
C29 C26 P1 111.9(3) . . ?
C27 C26 P1 102.6(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 . . ?
C26 C29 H29A 109.5 . . ?
C26 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C26 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C1 N1 C2 110.7(3) . . ?
C1 N1 C4 124.1(2) . . ?
C2 N1 C4 125.0(3) . . ?
C1 N2 C3 111.1(3) . . ?
C1 N2 C16 119.2(2) . . ?
C3 N2 C16 129.7(3) . . ?
C16 N3 C20 118.9(3) . . ?
C16 N3 Cr1 118.8(2) . . ?
C20 N3 Cr1 122.3(2) . . ?
C21 P1 C22 105.84(18) . . ?
C21 P1 C26 107.34(18) . . ?
C22 P1 C26 114.3(2) . . ?
C21 P1 Cr1 98.36(12) . . ?
C22 P1 Cr1 118.04(15) . . ?
C26 P1 Cr1 111.01(14) . . ?
N3 Cr1 C1 77.48(11) . . ?
N3 Cr1 Cl1 176.52(8) . . ?
C1 Cr1 Cl1 101.15(9) . . ?
N3 Cr1 P1 80.60(8) . . ?
C1 Cr1 P1 157.55(9) . . ?
Cl1 Cr1 P1 101.00(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
N1 C2 C3 N2 0.4(4) . . . . ?
C9 C4 C5 C6 -1.0(5) . . . . ?
N1 C4 C5 C6 179.8(3) . . . . ?
C9 C4 C5 C10 -179.9(3) . . . . ?
N1 C4 C5 C10 1.0(5) . . . . ?
C4 C5 C6 C7 0.6(5) . . . . ?
C10 C5 C6 C7 179.5(4) . . . . ?
C5 C6 C7 C8 0.2(6) . . . . ?
C6 C7 C8 C9 -0.7(6) . . . . ?
C7 C8 C9 C4 0.3(6) . . . . ?
C7 C8 C9 C13 178.2(4) . . . . ?
C5 C4 C9 C8 0.6(5) . . . . ?
N1 C4 C9 C8 179.7(3) . . . . ?
C5 C4 C9 C13 -177.3(3) . . . . ?
N1 C4 C9 C13 1.8(5) . . . . ?
C6 C5 C10 C11 -85.4(4) . . . . ?
C4 C5 C10 C11 93.4(4) . . . . ?
C6 C5 C10 C12 38.6(6) . . . . ?
C4 C5 C10 C12 -142.6(4) . . . . ?
C8 C9 C13 C14 -75.8(5) . . . . ?
C4 C9 C13 C14 102.0(4) . . . . ?
C8 C9 C13 C15 49.3(5) . . . . ?
C4 C9 C13 C15 -132.9(4) . . . . ?
N3 C16 C17 C18 -0.4(5) . . . . ?
N2 C16 C17 C18 -178.5(3) . . . . ?
C16 C17 C18 C19 2.0(5) . . . . ?
C17 C18 C19 C20 -1.9(6) . . . . ?
C18 C19 C20 C21 179.7(3) . . . . ?
C18 C19 C20 N3 0.2(5) . . . . ?
N3 C20 C21 P1 -1.7(4) . . . . ?
C19 C20 C21 P1 178.8(3) . . . . ?
N2 C1 N1 C2 -0.2(3) . . . . ?
Cr1 C1 N1 C2 179.3(3) . . . . ?
N2 C1 N1 C4 174.5(3) . . . . ?
Cr1 C1 N1 C4 -6.0(5) . . . . ?
C3 C2 N1 C1 -0.2(4) . . . . ?
C3 C2 N1 C4 -174.8(3) . . . . ?
C5 C4 N1 C1 87.9(4) . . . . ?
C9 C4 N1 C1 -91.3(4) . . . . ?
C5 C4 N1 C2 -98.2(4) . . . . ?
C9 C4 N1 C2 82.6(4) . . . . ?
N1 C1 N2 C3 0.5(3) . . . . ?
Cr1 C1 N2 C3 -179.2(2) . . . . ?
N1 C1 N2 C16 -178.7(2) . . . . ?
Cr1 C1 N2 C16 1.6(3) . . . . ?
C2 C3 N2 C1 -0.6(4) . . . . ?
C2 C3 N2 C16 178.5(3) . . . . ?
C17 C16 N2 C1 179.8(3) . . . . ?
N3 C16 N2 C1 1.5(4) . . . . ?
C17 C16 N2 C3 0.8(5) . . . . ?
N3 C16 N2 C3 -177.5(3) . . . . ?
C17 C16 N3 C20 -1.2(5) . . . . ?
N2 C16 N3 C20 177.1(2) . . . . ?
C17 C16 N3 Cr1 177.7(3) . . . . ?
N2 C16 N3 Cr1 -4.0(3) . . . . ?
C21 C20 N3 C16 -178.3(3) . . . . ?
C19 C20 N3 C16 1.3(4) . . . . ?
C21 C20 N3 Cr1 2.9(4) . . . . ?
C19 C20 N3 Cr1 -177.6(2) . . . . ?
C20 C21 P1 C22 -122.4(3) . . . . ?
C20 C21 P1 C26 115.2(3) . . . . ?
C20 C21 P1 Cr1 0.0(3) . . . . ?
C25 C22 P1 C21 -176.3(4) . . . . ?
C24 C22 P1 C21 -48.7(4) . . . . ?
C23 C22 P1 C21 68.4(4) . . . . ?
C25 C22 P1 C26 -58.4(5) . . . . ?
C24 C22 P1 C26 69.2(4) . . . . ?
C23 C22 P1 C26 -173.7(3) . . . . ?
C25 C22 P1 Cr1 74.9(5) . . . . ?
C24 C22 P1 Cr1 -157.5(4) . . . . ?
C23 C22 P1 Cr1 -40.4(4) . . . . ?
C28 C26 P1 C21 53.9(4) . . . . ?
C29 C26 P1 C21 179.8(4) . . . . ?
C27 C26 P1 C21 -62.7(4) . . . . ?
C28 C26 P1 C22 -63.1(4) . . . . ?
C29 C26 P1 C22 62.7(4) . . . . ?
C27 C26 P1 C22 -179.7(4) . . . . ?
C28 C26 P1 Cr1 160.3(4) . . . . ?
C29 C26 P1 Cr1 -73.8(4) . . . . ?
C27 C26 P1 Cr1 43.8(4) . . . . ?
 
_refine_diff_density_max    0.777
_refine_diff_density_min   -0.518
_refine_diff_density_rms    0.066

_shelxl_version_number 2013-4



