# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2018

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

data_compound_2-Cy
_database_code_depnum_ccdc_archive 'CCDC 1579154'
_audit_update_record             
;
2017-10-10 deposited with the CCDC.
2018-02-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C50 H82 B Cl N6 Ni O2 Si2'
_chemical_formula_sum            'C50 H82 B Cl N6 Ni O2 Si2'
_chemical_formula_weight         960.36

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

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

_cell_length_a                   27.8322(3)
_cell_length_b                   21.4898(2)
_cell_length_c                   26.4066(3)
_cell_angle_alpha                90
_cell_angle_beta                 116.468(2)
_cell_angle_gamma                90
_cell_volume                     14138.5(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    10927
_cell_measurement_theta_min      2.6940
_cell_measurement_theta_max      73.4920

_exptl_crystal_description       rod
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    0.902
_exptl_crystal_F_000             4144
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.130
_exptl_absorpt_coefficient_mu    1.311
_shelx_estimated_absorpt_T_min   0.727
_shelx_estimated_absorpt_T_max   0.848
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7267
_exptl_absorpt_correction_T_max  0.8480
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43c (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.5435
_diffrn_reflns_number            27061
_diffrn_reflns_av_unetI/netI     0.0364
_diffrn_reflns_av_R_equivalents  0.0272
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         6.430
_diffrn_reflns_theta_max         69.988
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             13278
_reflns_number_gt                10450
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'CrysAlisPro 1.171.38.43c (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43c (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43c (Rigaku OD, 2015)'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0791P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         13278
_refine_ls_number_parameters     591
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0415
_refine_ls_wR_factor_ref         0.1268
_refine_ls_wR_factor_gt          0.1177
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_restrained_S_all      1.023
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_platon_squeeze_void_nr
1
_platon_squeeze_void_average_x   0.218
_platon_squeeze_void_average_y   0.653
_platon_squeeze_void_average_z   -0.018
_platon_squeeze_void_volume      4624
_platon_squeeze_void_count_electrons 1028
_platon_squeeze_void_content     ' '
_platon_squeeze_details          ?

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
Ni1 Ni 0.00990(2) 0.72327(2) 0.50536(2) 0.03744(9) Uani 1 1 d . . . . .
Cl1 Cl -0.05064(2) 0.68119(2) 0.52881(2) 0.05119(12) Uani 1 1 d . . . . .
Si1 Si -0.04976(2) 0.76305(2) 0.42612(2) 0.03632(11) Uani 1 1 d . . . . .
Si2 Si -0.06043(2) 0.87915(2) 0.48902(2) 0.04429(12) Uani 1 1 d . . . . .
O1 O -0.03517(5) 0.77395(6) 0.36957(5) 0.0417(3) Uani 1 1 d . . . . .
N6 N 0.10384(5) 0.76995(7) 0.48961(6) 0.0442(3) Uani 1 1 d . . . . .
O2 O -0.09853(4) 0.70883(6) 0.38875(5) 0.0431(3) Uani 1 1 d . . . . .
N1 N -0.08391(5) 0.82941(7) 0.43012(6) 0.0401(3) Uani 1 1 d . . . . .
N5 N 0.09896(6) 0.58748(7) 0.49527(6) 0.0454(3) Uani 1 1 d . . . . .
C22 C 0.14455(7) 0.71400(9) 0.60902(8) 0.0440(4) Uani 1 1 d . . . . .
N3 N 0.19631(6) 0.70521(8) 0.61983(7) 0.0485(4) Uani 1 1 d . . . . .
C16 C -0.06230(7) 0.73227(8) 0.32759(7) 0.0426(4) Uani 1 1 d . . . . .
N4 N 0.10053(6) 0.56678(7) 0.57593(7) 0.0463(3) Uani 1 1 d . . . . .
C45 C 0.08414(6) 0.81724(8) 0.44519(7) 0.0406(4) Uani 1 1 d . . . . .
H45 H 0.046123 0.827661 0.436003 0.049 Uiso 1 1 calc R U . . .
C15 C 0.00769(8) 0.90917(10) 0.50480(9) 0.0559(5) Uani 1 1 d . . . . .
H15A H 0.033206 0.874489 0.515776 0.084 Uiso 1 1 calc R U . . .
H15B H 0.019098 0.939309 0.535849 0.084 Uiso 1 1 calc R U . . .
H15C H 0.006558 0.929496 0.471060 0.084 Uiso 1 1 calc R U . . .
N2 N 0.14539(6) 0.74870(8) 0.65187(7) 0.0520(4) Uani 1 1 d . . . . .
C21 C -0.09807(7) 0.69562(8) 0.33860(7) 0.0432(4) Uani 1 1 d . . . . .
C27 C 0.21201(7) 0.67646(11) 0.57882(9) 0.0559(5) Uani 1 1 d . . . . .
H27 H 0.177985 0.669870 0.543471 0.067 Uiso 1 1 calc R U . . .
C1 C -0.13609(7) 0.84254(9) 0.38404(8) 0.0442(4) Uani 1 1 d . . . . .
C33 C 0.09856(6) 0.61453(8) 0.54142(8) 0.0428(4) Uani 1 1 d . . . . .
C46 C 0.11854(7) 0.87593(9) 0.46587(8) 0.0454(4) Uani 1 1 d . . . . .
H46A H 0.115328 0.892956 0.499065 0.055 Uiso 1 1 calc R U . . .
H46B H 0.156667 0.865103 0.477930 0.055 Uiso 1 1 calc R U . . .
C50 C 0.08639(7) 0.79217(9) 0.39257(8) 0.0460(4) Uani 1 1 d . . . . .
H50A H 0.062365 0.755638 0.378479 0.055 Uiso 1 1 calc R U . . .
H50B H 0.123402 0.778201 0.402441 0.055 Uiso 1 1 calc R U . . .
C17 C -0.05565(8) 0.72460(10) 0.27952(8) 0.0522(4) Uani 1 1 d . . . . .
H17 H -0.031210 0.749830 0.272524 0.063 Uiso 1 1 calc R U . . .
C34 C 0.10065(7) 0.52251(9) 0.50056(8) 0.0509(4) Uani 1 1 d . . . . .
C47 C 0.10124(9) 0.92521(9) 0.41962(9) 0.0529(4) Uani 1 1 d . . . . .
H47A H 0.064260 0.939005 0.410136 0.064 Uiso 1 1 calc R U . . .
H47B H 0.125250 0.961763 0.433625 0.064 Uiso 1 1 calc R U . . .
C35 C 0.10141(8) 0.50978(9) 0.55129(8) 0.0524(4) Uani 1 1 d . . . . .
C2 C -0.18225(7) 0.81647(10) 0.38509(9) 0.0513(4) Uani 1 1 d . . . . .
C36 C 0.09311(8) 0.62266(9) 0.44470(8) 0.0519(4) Uani 1 1 d . . . . .
H36 H 0.097528 0.667592 0.455695 0.062 Uiso 1 1 calc R U . . .
C6 C -0.14080(8) 0.88097(9) 0.33892(8) 0.0497(4) Uani 1 1 d . . . . .
C24 C 0.19861(9) 0.76011(12) 0.69120(9) 0.0657(6) Uani 1 1 d . . . . .
B1 B 0.09303(7) 0.68714(10) 0.55504(8) 0.0413(4) Uani 1 1 d . . . . .
C30 C 0.09621(9) 0.77408(12) 0.65306(11) 0.0671(6) Uani 1 1 d . . . . .
H30 H 0.065733 0.764249 0.615435 0.080 Uiso 1 1 calc R U . . .
C37 C 0.03621(10) 0.61551(12) 0.39808(10) 0.0667(6) Uani 1 1 d . . . . .
H37A H 0.029430 0.571712 0.386782 0.100 Uiso 1 1 calc R U . . .
H37B H 0.031802 0.640813 0.365413 0.100 Uiso 1 1 calc R U . . .
H37C H 0.010693 0.629407 0.411976 0.100 Uiso 1 1 calc R U . . .
C20 C -0.12800(9) 0.65016(10) 0.30068(8) 0.0585(5) Uani 1 1 d . . . . .
H20 H -0.152571 0.625078 0.307580 0.070 Uiso 1 1 calc R U . . .
C48 C 0.10315(9) 0.89992(10) 0.36682(9) 0.0569(5) Uani 1 1 d . . . . .
H48A H 0.140832 0.890731 0.375263 0.068 Uiso 1 1 calc R U . . .
H48B H 0.089457 0.931870 0.336669 0.068 Uiso 1 1 calc R U . . .
C49 C 0.06962(8) 0.84091(10) 0.34594(8) 0.0534(4) Uani 1 1 d . . . . .
H49A H 0.031234 0.851215 0.332751 0.064 Uiso 1 1 calc R U . . .
H49B H 0.074008 0.823714 0.313468 0.064 Uiso 1 1 calc R U . . .
C42 C 0.10360(10) 0.47768(10) 0.45927(10) 0.0627(5) Uani 1 1 d . . . . .
H42A H 0.139374 0.479479 0.460724 0.094 Uiso 1 1 calc R U . . .
H42B H 0.076512 0.488433 0.421101 0.094 Uiso 1 1 calc R U . . .
H42C H 0.096853 0.435514 0.468733 0.094 Uiso 1 1 calc R U . . .
C12 C -0.09067(10) 0.89367(11) 0.28017(10) 0.0616(5) Uani 1 1 d . . . . .
H12A H -0.092485 0.848356 0.275507 0.092 Uiso 1 1 calc R U . . .
H12B H -0.057073 0.909021 0.281232 0.092 Uiso 1 1 calc R U . . .
H12C H -0.121152 0.912834 0.248334 0.092 Uiso 1 1 calc R U . . .
C10 C -0.09268(9) 0.91051(10) 0.33544(9) 0.0558(5) Uani 1 1 d . . . . .
H10 H -0.059449 0.893861 0.367407 0.067 Uiso 1 1 calc R U . . .
C7 C -0.17984(8) 0.77646(12) 0.43333(9) 0.0597(5) Uani 1 1 d . . . . .
H7 H -0.141163 0.769865 0.460078 0.072 Uiso 1 1 calc R U . . .
C29 C 0.23639(10) 0.61279(12) 0.59757(13) 0.0742(7) Uani 1 1 d . . . . .
H29A H 0.270032 0.616627 0.632354 0.111 Uiso 1 1 calc R U . . .
H29B H 0.243646 0.594024 0.567856 0.111 Uiso 1 1 calc R U . . .
H29C H 0.211333 0.586388 0.604683 0.111 Uiso 1 1 calc R U . . .
C39 C 0.09796(8) 0.57621(10) 0.63021(9) 0.0540(5) Uani 1 1 d . . . . .
H39 H 0.103383 0.621726 0.638732 0.065 Uiso 1 1 calc R U . . .
C23 C 0.23015(8) 0.73263(11) 0.67119(9) 0.0626(6) Uani 1 1 d . . . . .
C3 C -0.23250(8) 0.83009(13) 0.34081(10) 0.0667(6) Uani 1 1 d . . . . .
H3 H -0.263829 0.813158 0.341288 0.080 Uiso 1 1 calc R U . . .
C41 C 0.14302(9) 0.54280(12) 0.67947(9) 0.0644(5) Uani 1 1 d . . . . .
H41A H 0.135196 0.498140 0.677230 0.097 Uiso 1 1 calc R U . . .
H41B H 0.145808 0.559338 0.715263 0.097 Uiso 1 1 calc R U . . .
H41C H 0.177014 0.549445 0.677567 0.097 Uiso 1 1 calc R U . . .
C18 C -0.08586(10) 0.67863(12) 0.24119(9) 0.0669(6) Uani 1 1 d . . . . .
H18 H -0.082058 0.672509 0.207524 0.080 Uiso 1 1 calc R U . . .
C13 C -0.10782(9) 0.94612(11) 0.47365(10) 0.0617(5) Uani 1 1 d . . . . .
H13A H -0.113078 0.966001 0.438156 0.092 Uiso 1 1 calc R U . . .
H13B H -0.092832 0.976417 0.504553 0.092 Uiso 1 1 calc R U . . .
H13C H -0.142374 0.931016 0.470200 0.092 Uiso 1 1 calc R U . . .
C5 C -0.19225(9) 0.89300(12) 0.29568(10) 0.0668(6) Uani 1 1 d . . . . .
H5 H -0.196104 0.919208 0.265125 0.080 Uiso 1 1 calc R U . . .
C14 C -0.05563(9) 0.84267(12) 0.55519(9) 0.0604(5) Uani 1 1 d . . . . .
H14A H -0.091270 0.828575 0.549170 0.091 Uiso 1 1 calc R U . . .
H14B H -0.041942 0.873254 0.585932 0.091 Uiso 1 1 calc R U . . .
H14C H -0.031156 0.807017 0.565239 0.091 Uiso 1 1 calc R U . . .
C28 C 0.24632(10) 0.71921(14) 0.56283(13) 0.0772(7) Uani 1 1 d . . . . .
H28A H 0.229557 0.760407 0.553240 0.116 Uiso 1 1 calc R U . . .
H28B H 0.249534 0.701983 0.530113 0.116 Uiso 1 1 calc R U . . .
H28C H 0.282076 0.722892 0.594802 0.116 Uiso 1 1 calc R U . . .
C4 C -0.23744(9) 0.86761(13) 0.29650(11) 0.0741(7) Uani 1 1 d . . . . .
H4 H -0.271906 0.876017 0.266527 0.089 Uiso 1 1 calc R U . . .
C19 C -0.12099(11) 0.64215(12) 0.25157(9) 0.0724(7) Uani 1 1 d . . . . .
H19 H -0.140937 0.610912 0.225059 0.087 Uiso 1 1 calc R U . . .
C43 C 0.10378(11) 0.44685(11) 0.57692(10) 0.0683(6) Uani 1 1 d . . . . .
H43A H 0.092023 0.415127 0.547148 0.102 Uiso 1 1 calc R U . . .
H43B H 0.080160 0.446226 0.595491 0.102 Uiso 1 1 calc R U . . .
H43C H 0.140717 0.438079 0.604853 0.102 Uiso 1 1 calc R U . . .
C40 C 0.04253(10) 0.56057(15) 0.62434(13) 0.0787(7) Uani 1 1 d . . . . .
H40A H 0.015454 0.584111 0.592708 0.118 Uiso 1 1 calc R U . . .
H40B H 0.040504 0.571603 0.659344 0.118 Uiso 1 1 calc R U . . .
H40C H 0.035850 0.515905 0.617171 0.118 Uiso 1 1 calc R U . . .
C9 C -0.20526(10) 0.71237(13) 0.41251(12) 0.0738(7) Uani 1 1 d . . . . .
H9A H -0.243867 0.717245 0.388507 0.111 Uiso 1 1 calc R U . . .
H9B H -0.199463 0.686110 0.445081 0.111 Uiso 1 1 calc R U . . .
H9C H -0.188677 0.692798 0.390653 0.111 Uiso 1 1 calc R U . . .
C38 C 0.13677(10) 0.60777(12) 0.42677(11) 0.0663(6) Uani 1 1 d . . . . .
H38A H 0.171644 0.606215 0.460268 0.099 Uiso 1 1 calc R U . . .
H38B H 0.137463 0.640126 0.400954 0.099 Uiso 1 1 calc R U . . .
H38C H 0.129309 0.567377 0.407543 0.099 Uiso 1 1 calc R U . . .
C26 C 0.21497(12) 0.79665(16) 0.74486(11) 0.0927(9) Uani 1 1 d . . . . .
H26A H 0.253306 0.790283 0.769382 0.139 Uiso 1 1 calc R U . . .
H26B H 0.194178 0.782536 0.764424 0.139 Uiso 1 1 calc R U . . .
H26C H 0.208117 0.840978 0.735790 0.139 Uiso 1 1 calc R U . . .
C8 C -0.20630(10) 0.80876(16) 0.46579(12) 0.0801(8) Uani 1 1 d . . . . .
H8A H -0.188806 0.848954 0.479938 0.120 Uiso 1 1 calc R U . . .
H8B H -0.202676 0.782662 0.497733 0.120 Uiso 1 1 calc R U . . .
H8C H -0.244432 0.815450 0.440586 0.120 Uiso 1 1 calc R U . . .
C25 C 0.29054(9) 0.73011(16) 0.69843(13) 0.0891(9) Uani 1 1 d . . . . .
H25A H 0.304124 0.761118 0.680798 0.134 Uiso 1 1 calc R U . . .
H25B H 0.302154 0.688530 0.693282 0.134 Uiso 1 1 calc R U . . .
H25C H 0.304655 0.739043 0.738925 0.134 Uiso 1 1 calc R U . . .
C31 C 0.08423(17) 0.74139(18) 0.69679(18) 0.1082(12) Uani 1 1 d . . . . .
H31A H 0.082451 0.696393 0.690174 0.162 Uiso 1 1 calc R U . . .
H31B H 0.049753 0.756041 0.693911 0.162 Uiso 1 1 calc R U . . .
H31C H 0.112702 0.750532 0.734668 0.162 Uiso 1 1 calc R U . . .
C44 C 0.07379(6) 0.73929(8) 0.50464(7) 0.0400(4) Uani 1 1 d . . . . .
C32 C 0.09842(12) 0.84485(14) 0.65828(13) 0.0866(8) Uani 1 1 d . . . . .
H32A H 0.122671 0.856614 0.697281 0.130 Uiso 1 1 calc R U . . .
H32B H 0.062390 0.860991 0.648342 0.130 Uiso 1 1 calc R U . . .
H32C H 0.111633 0.862392 0.632579 0.130 Uiso 1 1 calc R U . . .
C11 C -0.09224(15) 0.98183(12) 0.34141(14) 0.0856(8) Uani 1 1 d . . . . .
H11A H -0.122788 0.999598 0.308684 0.128 Uiso 1 1 calc R U . . .
H11B H -0.058737 0.998527 0.343235 0.128 Uiso 1 1 calc R U . . .
H11C H -0.094918 0.992746 0.376092 0.128 Uiso 1 1 calc R U . . .
H1 H 0.0589(9) 0.6844(11) 0.5704(9) 0.054(6) 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
Ni1 C44 1.8195(17) . ?
Ni1 Si1 2.1839(5) . ?
Ni1 B1 2.2296(18) . ?
Ni1 Cl1 2.2295(5) . ?
Si1 O2 1.7262(12) . ?
Si1 O1 1.7292(13) . ?
Si1 N1 1.7429(15) . ?
Si2 N1 1.7559(15) . ?
Si2 C14 1.865(2) . ?
Si2 C15 1.866(2) . ?
Si2 C13 1.870(2) . ?
O1 C16 1.362(2) . ?
N6 C44 1.260(2) . ?
N6 C45 1.461(2) . ?
O2 C21 1.360(2) . ?
N1 C1 1.447(2) . ?
N5 C33 1.355(3) . ?
N5 C34 1.402(2) . ?
N5 C36 1.479(2) . ?
C22 N2 1.346(3) . ?
C22 N3 1.351(2) . ?
C22 B1 1.612(3) . ?
N3 C23 1.391(3) . ?
N3 C27 1.472(3) . ?
C16 C17 1.372(3) . ?
C16 C21 1.398(3) . ?
N4 C33 1.357(2) . ?
N4 C35 1.392(3) . ?
N4 C39 1.480(3) . ?
C45 C50 1.517(3) . ?
C45 C46 1.529(2) . ?
N2 C24 1.400(3) . ?
N2 C30 1.487(3) . ?
C21 C20 1.381(3) . ?
C27 C29 1.509(3) . ?
C27 C28 1.514(3) . ?
C1 C6 1.407(3) . ?
C1 C2 1.413(3) . ?
C33 B1 1.624(3) . ?
C46 C47 1.523(3) . ?
C50 C49 1.523(3) . ?
C17 C18 1.396(3) . ?
C34 C35 1.358(3) . ?
C34 C42 1.484(3) . ?
C47 C48 1.519(3) . ?
C35 C43 1.501(3) . ?
C2 C3 1.397(3) . ?
C2 C7 1.513(3) . ?
C36 C37 1.520(3) . ?
C36 C38 1.522(3) . ?
C6 C5 1.401(3) . ?
C6 C10 1.522(3) . ?
C24 C23 1.346(4) . ?
C24 C26 1.502(4) . ?
B1 C44 1.637(3) . ?
C30 C31 1.511(4) . ?
C30 C32 1.526(4) . ?
C20 C19 1.405(4) . ?
C48 C49 1.525(3) . ?
C12 C10 1.529(3) . ?
C10 C11 1.540(3) . ?
C7 C8 1.524(4) . ?
C7 C9 1.534(3) . ?
C39 C40 1.518(3) . ?
C39 C41 1.525(3) . ?
C23 C25 1.506(3) . ?
C3 C4 1.377(4) . ?
C18 C19 1.373(4) . ?
C5 C4 1.380(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
C44 Ni1 Si1 104.19(5) . . ?
C44 Ni1 B1 46.32(7) . . ?
Si1 Ni1 B1 147.83(6) . . ?
C44 Ni1 Cl1 160.51(6) . . ?
Si1 Ni1 Cl1 94.527(19) . . ?
B1 Ni1 Cl1 114.19(5) . . ?
O2 Si1 O1 91.45(6) . . ?
O2 Si1 N1 106.01(7) . . ?
O1 Si1 N1 106.60(7) . . ?
O2 Si1 Ni1 110.60(5) . . ?
O1 Si1 Ni1 120.64(4) . . ?
N1 Si1 Ni1 117.67(5) . . ?
N1 Si2 C14 114.65(9) . . ?
N1 Si2 C15 110.38(8) . . ?
C14 Si2 C15 107.15(10) . . ?
N1 Si2 C13 109.16(9) . . ?
C14 Si2 C13 106.02(11) . . ?
C15 Si2 C13 109.30(11) . . ?
C16 O1 Si1 110.81(11) . . ?
C44 N6 C45 123.52(14) . . ?
C21 O2 Si1 110.56(11) . . ?
C1 N1 Si1 118.59(12) . . ?
C1 N1 Si2 117.64(12) . . ?
Si1 N1 Si2 123.65(8) . . ?
C33 N5 C34 110.56(16) . . ?
C33 N5 C36 123.45(16) . . ?
C34 N5 C36 125.75(17) . . ?
N2 C22 N3 106.40(16) . . ?
N2 C22 B1 128.09(16) . . ?
N3 C22 B1 125.51(17) . . ?
C22 N3 C23 109.97(18) . . ?
C22 N3 C27 122.77(16) . . ?
C23 N3 C27 126.95(17) . . ?
O1 C16 C17 125.27(18) . . ?
O1 C16 C21 112.90(15) . . ?
C17 C16 C21 121.82(17) . . ?
C33 N4 C35 110.80(16) . . ?
C33 N4 C39 122.80(17) . . ?
C35 N4 C39 126.25(16) . . ?
N6 C45 C50 109.52(14) . . ?
N6 C45 C46 109.61(14) . . ?
C50 C45 C46 110.19(14) . . ?
C22 N2 C24 109.69(18) . . ?
C22 N2 C30 123.33(16) . . ?
C24 N2 C30 126.8(2) . . ?
O2 C21 C20 126.10(18) . . ?
O2 C21 C16 113.68(15) . . ?
C20 C21 C16 120.20(18) . . ?
N3 C27 C29 112.12(19) . . ?
N3 C27 C28 112.4(2) . . ?
C29 C27 C28 113.21(19) . . ?
C6 C1 C2 120.46(16) . . ?
C6 C1 N1 120.41(16) . . ?
C2 C1 N1 119.13(16) . . ?
N5 C33 N4 105.40(16) . . ?
N5 C33 B1 130.63(16) . . ?
N4 C33 B1 123.86(17) . . ?
C47 C46 C45 111.29(15) . . ?
C45 C50 C49 111.93(15) . . ?
C16 C17 C18 118.0(2) . . ?
C35 C34 N5 106.49(18) . . ?
C35 C34 C42 127.74(19) . . ?
N5 C34 C42 125.72(19) . . ?
C48 C47 C46 111.05(17) . . ?
C34 C35 N4 106.74(17) . . ?
C34 C35 C43 127.2(2) . . ?
N4 C35 C43 126.06(19) . . ?
C3 C2 C1 118.7(2) . . ?
C3 C2 C7 118.42(18) . . ?
C1 C2 C7 122.82(16) . . ?
N5 C36 C37 109.59(17) . . ?
N5 C36 C38 113.06(17) . . ?
C37 C36 C38 114.52(19) . . ?
C5 C6 C1 118.3(2) . . ?
C5 C6 C10 118.76(19) . . ?
C1 C6 C10 122.94(16) . . ?
C23 C24 N2 106.9(2) . . ?
C23 C24 C26 128.5(2) . . ?
N2 C24 C26 124.5(2) . . ?
C22 B1 C33 113.90(14) . . ?
C22 B1 C44 108.28(14) . . ?
C33 B1 C44 120.46(16) . . ?
C22 B1 Ni1 132.55(13) . . ?
C33 B1 Ni1 112.35(11) . . ?
C44 B1 Ni1 53.52(8) . . ?
N2 C30 C31 111.4(2) . . ?
N2 C30 C32 111.5(2) . . ?
C31 C30 C32 114.1(3) . . ?
C21 C20 C19 118.0(2) . . ?
C47 C48 C49 111.30(16) . . ?
C50 C49 C48 111.23(16) . . ?
C6 C10 C12 111.50(19) . . ?
C6 C10 C11 112.1(2) . . ?
C12 C10 C11 109.34(19) . . ?
C2 C7 C8 111.3(2) . . ?
C2 C7 C9 111.60(19) . . ?
C8 C7 C9 110.4(2) . . ?
N4 C39 C40 110.87(19) . . ?
N4 C39 C41 112.65(18) . . ?
C40 C39 C41 113.26(19) . . ?
C24 C23 N3 106.97(17) . . ?
C24 C23 C25 127.8(2) . . ?
N3 C23 C25 125.2(2) . . ?
C4 C3 C2 121.2(2) . . ?
C19 C18 C17 120.8(2) . . ?
C4 C5 C6 121.5(2) . . ?
C3 C4 C5 119.91(19) . . ?
C18 C19 C20 121.2(2) . . ?
N6 C44 B1 126.27(14) . . ?
N6 C44 Ni1 153.05(14) . . ?
B1 C44 Ni1 80.16(10) . . ?

_refine_diff_density_max         0.215
_refine_diff_density_min         -0.354
_refine_diff_density_rms         0.044

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

data_compound_3
_database_code_depnum_ccdc_archive 'CCDC 1579157'
_audit_update_record             
;
2017-10-10 deposited with the CCDC.
2018-02-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C44 H71 B Cl N5 Ni O3 Si2'
_chemical_formula_sum            'C44 H71 B Cl N5 Ni O3 Si2'
_chemical_formula_weight         879.20

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 '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                   10.87820(10)
_cell_length_b                   25.2119(2)
_cell_length_c                   17.86600(10)
_cell_angle_alpha                90
_cell_angle_beta                 91.9480(10)
_cell_angle_gamma                90
_cell_volume                     4897.10(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    10458
_cell_measurement_theta_min      3.0130
_cell_measurement_theta_max      73.5070

_exptl_crystal_description       rod
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.193
_exptl_crystal_F_000             1888
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    1.859
_shelx_estimated_absorpt_T_min   0.664
_shelx_estimated_absorpt_T_max   0.768
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.71312
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43c (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.5435
_diffrn_reflns_number            19886
_diffrn_reflns_av_unetI/netI     0.0231
_diffrn_reflns_av_R_equivalents  0.0200
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         6.522
_diffrn_reflns_theta_max         70.000
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             9232
_reflns_number_gt                8391
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'CrysAlisPro 1.171.38.43c (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43c (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43c (Rigaku OD, 2015)'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0453P)²+1.8496P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9232
_refine_ls_number_parameters     551
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0328
_refine_ls_wR_factor_ref         0.0889
_refine_ls_wR_factor_gt          0.0858
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.030
_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
Ni1 Ni -0.00296(2) 0.30923(2) 0.71476(2) 0.02351(8) Uani 1 1 d . . . . .
Si1 Si -0.27041(3) 0.40143(2) 0.71749(2) 0.02046(9) Uani 1 1 d . . . . .
Cl1 Cl 0.14242(3) 0.30340(2) 0.81215(2) 0.03146(9) Uani 1 1 d . . . . .
Si2 Si -0.40131(4) 0.50315(2) 0.76370(2) 0.02841(10) Uani 1 1 d . . . . .
O3 O -0.18805(10) 0.30330(5) 0.60018(6) 0.0309(2) Uani 1 1 d . . . . .
O2 O -0.17535(9) 0.43130(4) 0.65638(6) 0.0276(2) Uani 1 1 d . . . . .
N2 N -0.37838(11) 0.26259(5) 0.75597(7) 0.0231(2) Uani 1 1 d . . . . .
N3 N -0.24346(11) 0.25903(5) 0.84775(6) 0.0222(2) Uani 1 1 d . . . . .
O1 O -0.39130(9) 0.39962(4) 0.65476(5) 0.0266(2) Uani 1 1 d . . . . .
C44 C -0.14395(13) 0.31180(5) 0.66133(8) 0.0222(3) Uani 1 1 d . . . . .
N4 N 0.10233(11) 0.22770(5) 0.62009(8) 0.0298(3) Uani 1 1 d . . . . .
N5 N 0.15994(11) 0.30535(5) 0.58677(7) 0.0245(3) Uani 1 1 d . . . . .
C33 C 0.09156(13) 0.27997(6) 0.63804(8) 0.0263(3) Uani 1 1 d . . . . .
N1 N -0.31616(11) 0.44475(5) 0.78558(6) 0.0228(2) Uani 1 1 d . . . . .
C1 C -0.28148(14) 0.43729(6) 0.86414(8) 0.0241(3) Uani 1 1 d . . . . .
C22 C -0.27163(12) 0.28466(5) 0.78257(7) 0.0202(3) Uani 1 1 d . . . . .
C6 C -0.16175(14) 0.45032(6) 0.89024(9) 0.0281(3) Uani 1 1 d . . . . .
C35 C 0.21274(13) 0.26921(7) 0.53757(8) 0.0289(3) Uani 1 1 d . . . . .
B1 B -0.19519(14) 0.33072(6) 0.74313(8) 0.0198(3) Uani 1 1 d . . . . .
C16 C -0.35786(15) 0.42102(6) 0.58773(8) 0.0292(3) Uani 1 1 d . . . . .
C24 C -0.33424(14) 0.22195(6) 0.86290(8) 0.0265(3) Uani 1 1 d . . . . .
C25 C -0.43821(13) 0.27730(6) 0.68302(8) 0.0262(3) Uani 1 1 d . . . . .
H25 H -0.385094 0.304984 0.660409 0.031 Uiso 1 1 calc R U . . .
C3 C -0.33990(16) 0.41995(7) 0.99092(9) 0.0331(3) Uani 1 1 d . . . . .
H3 H -0.399791 0.409348 1.025394 0.040 Uiso 1 1 calc R U . . .
C34 C 0.17693(14) 0.22057(7) 0.55871(9) 0.0314(3) Uani 1 1 d . . . . .
C28 C -0.13084(13) 0.26938(6) 0.89482(8) 0.0269(3) Uani 1 1 d . . . . .
H28 H -0.075960 0.292046 0.864427 0.032 Uiso 1 1 calc R U . . .
C21 C -0.23655(16) 0.43855(6) 0.58871(8) 0.0304(3) Uani 1 1 d . . . . .
C2 C -0.37031(14) 0.42003(6) 0.91423(8) 0.0263(3) Uani 1 1 d . . . . .
C30 C -0.16046(17) 0.30106(7) 0.96402(9) 0.0379(4) Uani 1 1 d . . . . .
H30A H -0.203826 0.333649 0.949072 0.057 Uiso 1 1 calc R U . . .
H30B H -0.083959 0.310162 0.991610 0.057 Uiso 1 1 calc R U . . .
H30C H -0.212749 0.279848 0.996108 0.057 Uiso 1 1 calc R U . . .
C13 C -0.56358(16) 0.48915(8) 0.73206(10) 0.0403(4) Uani 1 1 d . . . . .
H13A H -0.563957 0.465455 0.688579 0.061 Uiso 1 1 calc R U . . .
H13B H -0.604750 0.522488 0.718230 0.061 Uiso 1 1 calc R U . . .
H13C H -0.607126 0.472185 0.772793 0.061 Uiso 1 1 calc R U . . .
C23 C -0.41853(14) 0.22422(6) 0.80553(8) 0.0274(3) Uani 1 1 d . . . . .
C7 C -0.49660(14) 0.39992(7) 0.88836(9) 0.0296(3) Uani 1 1 d . . . . .
H7 H -0.504485 0.404973 0.832891 0.036 Uiso 1 1 calc R U . . .
C39 C 0.17471(14) 0.36329(6) 0.57992(9) 0.0300(3) Uani 1 1 d . . . . .
H39 H 0.258824 0.369945 0.561049 0.036 Uiso 1 1 calc R U . . .
C41 C 0.08251(18) 0.38526(7) 0.52175(11) 0.0443(4) Uani 1 1 d . . . . .
H41A H 0.093466 0.367392 0.473716 0.066 Uiso 1 1 calc R U . . .
H41B H 0.096016 0.423435 0.515797 0.066 Uiso 1 1 calc R U . . .
H41C H -0.001247 0.379074 0.538313 0.066 Uiso 1 1 calc R U . . .
C15 C -0.32777(17) 0.54134(6) 0.68744(9) 0.0374(4) Uani 1 1 d . . . . .
H15A H -0.238655 0.542778 0.697287 0.056 Uiso 1 1 calc R U . . .
H15B H -0.361065 0.577457 0.685810 0.056 Uiso 1 1 calc R U . . .
H15C H -0.345054 0.523804 0.639277 0.056 Uiso 1 1 calc R U . . .
C29 C -0.06003(16) 0.21881(7) 0.91319(10) 0.0379(4) Uani 1 1 d . . . . .
H29A H -0.098790 0.200340 0.954498 0.057 Uiso 1 1 calc R U . . .
H29B H 0.025091 0.227709 0.927924 0.057 Uiso 1 1 calc R U . . .
H29C H -0.060713 0.195770 0.869001 0.057 Uiso 1 1 calc R U . . .
C8 C -0.50804(15) 0.34056(7) 0.90433(10) 0.0349(4) Uani 1 1 d . . . . .
H8A H -0.440026 0.321582 0.881675 0.052 Uiso 1 1 calc R U . . .
H8B H -0.586428 0.327422 0.882968 0.052 Uiso 1 1 calc R U . . .
H8C H -0.504988 0.334635 0.958571 0.052 Uiso 1 1 calc R U . . .
C32 C -0.33655(16) 0.18796(7) 0.93138(10) 0.0371(4) Uani 1 1 d . . . . .
H32A H -0.420474 0.175169 0.938283 0.056 Uiso 1 1 calc R U . . .
H32B H -0.309326 0.208793 0.975187 0.056 Uiso 1 1 calc R U . . .
H32C H -0.281349 0.157625 0.925568 0.056 Uiso 1 1 calc R U . . .
C43 C 0.29223(16) 0.28506(8) 0.47515(10) 0.0405(4) Uani 1 1 d . . . . .
H43A H 0.317197 0.253387 0.447746 0.061 Uiso 1 1 calc R U . . .
H43B H 0.365477 0.303344 0.495549 0.061 Uiso 1 1 calc R U . . .
H43C H 0.246321 0.308898 0.441078 0.061 Uiso 1 1 calc R U . . .
C4 C -0.22441(17) 0.43499(7) 1.01742(9) 0.0378(4) Uani 1 1 d . . . . .
H4 H -0.206022 0.435945 1.069763 0.045 Uiso 1 1 calc R U . . .
C9 C -0.60275(16) 0.42975(8) 0.92365(11) 0.0426(4) Uani 1 1 d . . . . .
H9A H -0.599362 0.424161 0.977960 0.064 Uiso 1 1 calc R U . . .
H9B H -0.681225 0.416460 0.902619 0.064 Uiso 1 1 calc R U . . .
H9C H -0.595583 0.467730 0.912936 0.064 Uiso 1 1 calc R U . . .
C31 C -0.53663(17) 0.19427(8) 0.79704(11) 0.0434(4) Uani 1 1 d . . . . .
H31A H -0.544049 0.169790 0.839256 0.065 Uiso 1 1 calc R U . . .
H31B H -0.537632 0.174131 0.750109 0.065 Uiso 1 1 calc R U . . .
H31C H -0.605704 0.219240 0.796192 0.065 Uiso 1 1 calc R U . . .
C20 C -0.1896(2) 0.46286(7) 0.52676(10) 0.0425(4) Uani 1 1 d . . . . .
H20 H -0.107155 0.475272 0.526915 0.051 Uiso 1 1 calc R U . . .
C11 C 0.06416(17) 0.44404(8) 0.85879(11) 0.0443(4) Uani 1 1 d . . . . .
H11A H 0.093530 0.458239 0.907225 0.066 Uiso 1 1 calc R U . . .
H11B H 0.122496 0.453312 0.820277 0.066 Uiso 1 1 calc R U . . .
H11C H 0.057184 0.405365 0.862122 0.066 Uiso 1 1 calc R U . . .
C40 C 0.16625(17) 0.39209(7) 0.65408(10) 0.0383(4) Uani 1 1 d . . . . .
H40A H 0.080829 0.391773 0.669831 0.058 Uiso 1 1 calc R U . . .
H40B H 0.193737 0.428833 0.648340 0.058 Uiso 1 1 calc R U . . .
H40C H 0.218706 0.374260 0.692006 0.058 Uiso 1 1 calc R U . . .
C18 C -0.3884(2) 0.45161(8) 0.46309(10) 0.0509(5) Uani 1 1 d . . . . .
H18 H -0.439615 0.456338 0.419468 0.061 Uiso 1 1 calc R U . . .
C5 C -0.13574(16) 0.44865(7) 0.96731(9) 0.0350(4) Uani 1 1 d . . . . .
H5 H -0.055153 0.457115 0.985717 0.042 Uiso 1 1 calc R U . . .
C14 C -0.40344(18) 0.54635(7) 0.84872(10) 0.0406(4) Uani 1 1 d . . . . .
H14A H -0.445605 0.527827 0.888680 0.061 Uiso 1 1 calc R U . . .
H14B H -0.447003 0.579413 0.836464 0.061 Uiso 1 1 calc R U . . .
H14C H -0.318842 0.554442 0.865564 0.061 Uiso 1 1 calc R U . . .
C10 C -0.06162(15) 0.46773(7) 0.83812(9) 0.0347(4) Uani 1 1 d . . . . .
H10 H -0.085606 0.455169 0.786574 0.042 Uiso 1 1 calc R U . . .
C42 C 0.20481(18) 0.16780(8) 0.52473(12) 0.0466(5) Uani 1 1 d . . . . .
H42A H 0.248917 0.173093 0.478391 0.070 Uiso 1 1 calc R U . . .
H42B H 0.127760 0.148820 0.513495 0.070 Uiso 1 1 calc R U . . .
H42C H 0.255983 0.146974 0.560064 0.070 Uiso 1 1 calc R U . . .
C12 C -0.05237(18) 0.52826(8) 0.83545(12) 0.0491(5) Uani 1 1 d . . . . .
H12A H -0.131156 0.543100 0.817349 0.074 Uiso 1 1 calc R U . . .
H12B H 0.012378 0.538574 0.801514 0.074 Uiso 1 1 calc R U . . .
H12C H -0.032395 0.541865 0.885791 0.074 Uiso 1 1 calc R U . . .
C17 C -0.43590(19) 0.42761(7) 0.52577(9) 0.0397(4) Uani 1 1 d . . . . .
H17 H -0.519052 0.416123 0.526059 0.048 Uiso 1 1 calc R U . . .
C27 C -0.56383(15) 0.30266(8) 0.69302(10) 0.0390(4) Uani 1 1 d . . . . .
H27A H -0.622498 0.275480 0.708018 0.059 Uiso 1 1 calc R U . . .
H27B H -0.592604 0.318732 0.645650 0.059 Uiso 1 1 calc R U . . .
H27C H -0.557129 0.330081 0.731831 0.059 Uiso 1 1 calc R U . . .
C19 C -0.2687(2) 0.46860(8) 0.46322(10) 0.0540(6) Uani 1 1 d . . . . .
H19 H -0.238361 0.484617 0.419399 0.065 Uiso 1 1 calc R U . . .
C26 C -0.44220(17) 0.23053(7) 0.62875(9) 0.0392(4) Uani 1 1 d . . . . .
H26A H -0.360742 0.213987 0.627813 0.059 Uiso 1 1 calc R U . . .
H26B H -0.466030 0.243121 0.578429 0.059 Uiso 1 1 calc R U . . .
H26C H -0.502399 0.204440 0.645160 0.059 Uiso 1 1 calc R U . . .
C38 C 0.1468(6) 0.1681(3) 0.7244(4) 0.0427(18) Uani 0.774(6) 1 d . . P A 1
H38A H 0.227886 0.160108 0.704916 0.064 Uiso 0.774(6) 1 calc R U P A 1
H38B H 0.117251 0.137467 0.752328 0.064 Uiso 0.774(6) 1 calc R U P A 1
H38C H 0.153209 0.198930 0.757750 0.064 Uiso 0.774(6) 1 calc R U P A 1
C36 C 0.05706(19) 0.18029(11) 0.65959(16) 0.0292(6) Uani 0.774(6) 1 d . . P A 1
H36 H 0.059511 0.149788 0.623893 0.035 Uiso 0.774(6) 1 calc R U P A 1
C37 C -0.0744(2) 0.18600(9) 0.68365(15) 0.0372(7) Uani 0.774(6) 1 d . . P A 1
H37A H -0.078416 0.213333 0.722489 0.056 Uiso 0.774(6) 1 calc R U P A 1
H37B H -0.102847 0.152111 0.703586 0.056 Uiso 0.774(6) 1 calc R U P A 1
H37C H -0.126989 0.196263 0.640431 0.056 Uiso 0.774(6) 1 calc R U P A 1
C37A C -0.0543(7) 0.1626(3) 0.6473(5) 0.037(2) Uiso 0.226(6) 1 d D . P A 2
H37D H -0.022212 0.141524 0.606164 0.056 Uiso 0.226(6) 1 calc R U P A 2
H37E H -0.118545 0.186554 0.627604 0.056 Uiso 0.226(6) 1 calc R U P A 2
H37F H -0.089068 0.138836 0.684492 0.056 Uiso 0.226(6) 1 calc R U P A 2
C36A C 0.0493(8) 0.1948(4) 0.6838(5) 0.031(2) Uiso 0.226(6) 1 d D . P A 2
H36A H 0.012452 0.219887 0.720132 0.037 Uiso 0.226(6) 1 calc R U P A 2
C38A C 0.1444(19) 0.1613(10) 0.7262(13) 0.032(5) Uiso 0.226(6) 1 d D . P A 2
H38D H 0.104035 0.140582 0.764736 0.049 Uiso 0.226(6) 1 calc R U P A 2
H38E H 0.206729 0.184435 0.749869 0.049 Uiso 0.226(6) 1 calc R U P A 2
H38F H 0.183812 0.137164 0.691263 0.049 Uiso 0.226(6) 1 calc R U P A 2
H1 H -0.1053(16) 0.3399(7) 0.7771(9) 0.028 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
Ni1 C44 1.7799(14) . ?
Ni1 C33 1.8909(15) . ?
Ni1 B1 2.2351(15) . ?
Ni1 Cl1 2.3158(4) . ?
Si1 O1 1.6992(10) . ?
Si1 O2 1.7045(10) . ?
Si1 N1 1.7208(12) . ?
Si1 B1 2.0080(16) . ?
Si2 N1 1.7758(12) . ?
Si2 C13 1.8687(18) . ?
Si2 C14 1.8699(17) . ?
Si2 C15 1.8701(18) . ?
O3 C44 1.1977(18) . ?
O2 C21 1.3724(18) . ?
N2 C22 1.3588(18) . ?
N2 C23 1.3918(19) . ?
N2 C25 1.4839(18) . ?
N3 C22 1.3577(18) . ?
N3 C24 1.3930(19) . ?
N3 C28 1.4852(18) . ?
O1 C16 1.3737(18) . ?
C44 B1 1.652(2) . ?
N4 C33 1.362(2) . ?
N4 C34 1.398(2) . ?
N4 C36 1.481(2) . ?
N4 C36A 1.536(9) . ?
N5 C33 1.3595(19) . ?
N5 C35 1.4026(19) . ?
N5 C39 1.475(2) . ?
N1 C1 1.4532(18) . ?
C1 C6 1.407(2) . ?
C1 C2 1.408(2) . ?
C22 B1 1.605(2) . ?
C6 C5 1.397(2) . ?
C6 C10 1.522(2) . ?
C35 C34 1.345(2) . ?
C35 C43 1.489(2) . ?
C16 C17 1.382(2) . ?
C16 C21 1.391(2) . ?
C24 C23 1.353(2) . ?
C24 C32 1.495(2) . ?
C25 C27 1.525(2) . ?
C25 C26 1.526(2) . ?
C3 C4 1.381(2) . ?
C3 C2 1.398(2) . ?
C34 C42 1.498(2) . ?
C28 C30 1.516(2) . ?
C28 C29 1.520(2) . ?
C21 C20 1.378(2) . ?
C2 C7 1.521(2) . ?
C23 C31 1.493(2) . ?
C7 C8 1.529(2) . ?
C7 C9 1.532(2) . ?
C39 C40 1.516(2) . ?
C39 C41 1.524(2) . ?
C4 C5 1.382(3) . ?
C20 C19 1.408(3) . ?
C11 C10 1.527(2) . ?
C18 C19 1.371(3) . ?
C18 C17 1.388(3) . ?
C10 C12 1.530(3) . ?
C38 C36 1.520(5) . ?
C36 C37 1.514(3) . ?
C37A C36A 1.519(5) . ?
C36A C38A 1.519(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C44 Ni1 C33 96.05(6) . . ?
C44 Ni1 B1 46.92(6) . . ?
C33 Ni1 B1 142.65(6) . . ?
C44 Ni1 Cl1 163.58(5) . . ?
C33 Ni1 Cl1 98.37(5) . . ?
B1 Ni1 Cl1 117.73(4) . . ?
O1 Si1 O2 93.56(5) . . ?
O1 Si1 N1 104.33(6) . . ?
O2 Si1 N1 111.64(6) . . ?
O1 Si1 B1 115.26(6) . . ?
O2 Si1 B1 106.67(6) . . ?
N1 Si1 B1 121.85(6) . . ?
N1 Si2 C13 112.98(7) . . ?
N1 Si2 C14 108.96(7) . . ?
C13 Si2 C14 108.54(9) . . ?
N1 Si2 C15 110.76(7) . . ?
C13 Si2 C15 107.45(8) . . ?
C14 Si2 C15 108.01(8) . . ?
C21 O2 Si1 109.66(10) . . ?
C22 N2 C23 110.18(12) . . ?
C22 N2 C25 123.29(12) . . ?
C23 N2 C25 126.49(12) . . ?
C22 N3 C24 110.19(12) . . ?
C22 N3 C28 124.05(12) . . ?
C24 N3 C28 125.76(12) . . ?
C16 O1 Si1 110.03(10) . . ?
O3 C44 B1 136.22(13) . . ?
O3 C44 Ni1 142.55(12) . . ?
B1 C44 Ni1 81.18(8) . . ?
C33 N4 C34 111.46(13) . . ?
C33 N4 C36 129.49(17) . . ?
C34 N4 C36 118.79(17) . . ?
C33 N4 C36A 108.1(4) . . ?
C34 N4 C36A 139.0(4) . . ?
C33 N5 C35 111.19(13) . . ?
C33 N5 C39 125.85(13) . . ?
C35 N5 C39 122.91(13) . . ?
N5 C33 N4 104.08(13) . . ?
N5 C33 Ni1 128.92(12) . . ?
N4 C33 Ni1 126.95(11) . . ?
C1 N1 Si1 121.92(9) . . ?
C1 N1 Si2 115.87(9) . . ?
Si1 N1 Si2 122.13(7) . . ?
C6 C1 C2 120.59(13) . . ?
C6 C1 N1 119.79(13) . . ?
C2 C1 N1 119.52(13) . . ?
N3 C22 N2 105.69(12) . . ?
N3 C22 B1 128.00(12) . . ?
N2 C22 B1 126.30(12) . . ?
C5 C6 C1 118.28(15) . . ?
C5 C6 C10 119.12(14) . . ?
C1 C6 C10 122.56(13) . . ?
C34 C35 N5 106.72(13) . . ?
C34 C35 C43 129.53(15) . . ?
N5 C35 C43 123.75(15) . . ?
C22 B1 C44 112.01(11) . . ?
C22 B1 Si1 121.96(10) . . ?
C44 B1 Si1 101.64(9) . . ?
C22 B1 Ni1 115.26(9) . . ?
C44 B1 Ni1 51.90(6) . . ?
Si1 B1 Ni1 122.73(7) . . ?
O1 C16 C17 124.89(16) . . ?
O1 C16 C21 113.14(13) . . ?
C17 C16 C21 121.90(16) . . ?
C23 C24 N3 106.93(13) . . ?
C23 C24 C32 127.91(14) . . ?
N3 C24 C32 125.14(14) . . ?
N2 C25 C27 111.71(12) . . ?
N2 C25 C26 111.53(13) . . ?
C27 C25 C26 113.09(14) . . ?
C4 C3 C2 121.18(16) . . ?
C35 C34 N4 106.54(14) . . ?
C35 C34 C42 129.17(15) . . ?
N4 C34 C42 124.27(16) . . ?
N3 C28 C30 111.12(13) . . ?
N3 C28 C29 112.17(13) . . ?
C30 C28 C29 112.72(13) . . ?
O2 C21 C20 125.79(17) . . ?
O2 C21 C16 113.60(13) . . ?
C20 C21 C16 120.54(16) . . ?
C3 C2 C1 118.59(14) . . ?
C3 C2 C7 118.57(14) . . ?
C1 C2 C7 122.81(13) . . ?
C24 C23 N2 106.98(13) . . ?
C24 C23 C31 127.89(14) . . ?
N2 C23 C31 125.05(14) . . ?
C2 C7 C8 110.35(13) . . ?
C2 C7 C9 113.38(14) . . ?
C8 C7 C9 109.67(14) . . ?
N5 C39 C40 113.05(13) . . ?
N5 C39 C41 110.21(13) . . ?
C40 C39 C41 111.34(15) . . ?
C3 C4 C5 119.57(15) . . ?
C21 C20 C19 117.4(2) . . ?
C19 C18 C17 120.97(18) . . ?
C4 C5 C6 121.58(15) . . ?
C6 C10 C11 113.17(14) . . ?
C6 C10 C12 110.85(15) . . ?
C11 C10 C12 109.77(14) . . ?
C16 C17 C18 117.61(19) . . ?
C18 C19 C20 121.57(18) . . ?
N4 C36 C37 113.02(18) . . ?
N4 C36 C38 108.1(4) . . ?
C37 C36 C38 113.0(4) . . ?
C38A C36A C37A 113.5(13) . . ?
C38A C36A N4 113.8(11) . . ?
C37A C36A N4 105.2(6) . . ?

_refine_diff_density_max         0.424
_refine_diff_density_min         -0.379
_refine_diff_density_rms         0.043

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

data_compound_5-Bz
_database_code_depnum_ccdc_archive 'CCDC 1579160'
_audit_update_record             
;
2017-10-10 deposited with the CCDC.
2018-02-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C38 H63 B Cl N5 O2'
_chemical_formula_sum            'C38 H63 B Cl N5 O2'
_chemical_formula_weight         668.19

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   9.8905(12)
_cell_length_b                   12.6054(14)
_cell_length_c                   16.945(2)
_cell_angle_alpha                69.660(11)
_cell_angle_beta                 89.159(10)
_cell_angle_gamma                78.594(10)
_cell_volume                     1938.4(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    1728
_cell_measurement_theta_min      3.8030
_cell_measurement_theta_max      73.0110

_exptl_crystal_description       rod
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.145
_exptl_crystal_F_000             728
_exptl_crystal_size_max          0.364
_exptl_crystal_size_mid          0.064
_exptl_crystal_size_min          0.054
_exptl_absorpt_coefficient_mu    1.157
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.63664
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43c (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.5435
_diffrn_reflns_number            13387
_diffrn_reflns_av_unetI/netI     0.1065
_diffrn_reflns_av_R_equivalents  0.0807
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         6.444
_diffrn_reflns_theta_max         69.995
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             7283
_reflns_number_gt                3933
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'CrysAlisPro 1.171.38.43c (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43c (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43c (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1572P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7283
_refine_ls_number_parameters     436
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1551
_refine_ls_R_factor_gt           0.0939
_refine_ls_wR_factor_ref         0.2981
_refine_ls_wR_factor_gt          0.2404
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_restrained_S_all      1.017
_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
Cl1 Cl 0.11689(13) 0.25809(10) 0.61533(8) 0.0510(4) Uani 1 1 d . . . . .
N1 N 0.3877(4) 0.4242(3) 0.3414(2) 0.0372(8) Uani 1 1 d . . . . .
N3 N 0.7656(4) 0.2341(3) 0.3372(2) 0.0373(8) Uani 1 1 d . . . . .
N2 N 0.3347(4) 0.5471(3) 0.2137(2) 0.0359(8) Uani 1 1 d . . . . .
N4 N 0.7376(4) 0.4209(3) 0.2990(2) 0.0358(8) Uani 1 1 d . . . . .
C12 C 0.6842(4) 0.3345(4) 0.2882(2) 0.0331(9) Uani 1 1 d . . . . .
N5 N 0.6387(5) 0.4423(4) 0.0727(3) 0.0589(12) Uani 1 1 d . . . . .
C1 C 0.4195(4) 0.4465(4) 0.2597(2) 0.0344(9) Uani 1 1 d . . . . .
C13 C 0.8679(5) 0.2568(4) 0.3825(3) 0.0399(10) Uani 1 1 d . . . . .
C3 C 0.2504(5) 0.5907(4) 0.2681(3) 0.0406(10) Uani 1 1 d . . . . .
C14 C 0.8498(4) 0.3735(4) 0.3577(3) 0.0364(9) Uani 1 1 d . . . . .
C2 C 0.2832(5) 0.5138(4) 0.3472(3) 0.0407(10) Uani 1 1 d . . . . .
C18 C 0.6892(5) 0.5450(4) 0.2483(3) 0.0386(10) Uani 1 1 d . . . . .
H18 H 0.615816 0.549905 0.206505 0.046 Uiso 1 1 calc R U . . .
C4 C 0.4517(5) 0.3179(4) 0.4121(3) 0.0418(10) Uani 1 1 d . . . . .
H4 H 0.522627 0.272168 0.387332 0.050 Uiso 1 1 calc R U . . .
C24 C 0.3286(5) 0.2877(4) 0.1837(3) 0.0432(11) Uani 1 1 d . . . . .
C23 C 0.4696(5) 0.2513(4) 0.2291(3) 0.0422(10) Uani 1 1 d . . . . .
H23A H 0.532158 0.203915 0.202280 0.051 Uiso 1 1 calc R U . . .
H23B H 0.461875 0.201817 0.288169 0.051 Uiso 1 1 calc R U . . .
C15 C 0.7576(5) 0.1168(4) 0.3366(3) 0.0423(10) Uani 1 1 d . . . . .
H15 H 0.681715 0.129703 0.293914 0.051 Uiso 1 1 calc R U . . .
C30 C 0.5890(5) 0.4154(4) 0.1360(3) 0.0427(10) Uani 1 1 d . . . . .
C22 C 0.9382(5) 0.4389(4) 0.3855(3) 0.0440(11) Uani 1 1 d . . . . .
H22A H 0.976490 0.393779 0.443135 0.066 Uiso 1 1 calc R U . . .
H22B H 0.882243 0.513092 0.383949 0.066 Uiso 1 1 calc R U . . .
H22C H 1.013755 0.452668 0.347638 0.066 Uiso 1 1 calc R U . . .
C11 C 0.1465(5) 0.7019(4) 0.2401(3) 0.0520(12) Uani 1 1 d . . . . .
H11A H 0.069407 0.694938 0.207853 0.078 Uiso 1 1 calc R U . . .
H11B H 0.189911 0.764167 0.204601 0.078 Uiso 1 1 calc R U . . .
H11C H 0.111963 0.719591 0.289609 0.078 Uiso 1 1 calc R U . . .
C21 C 0.9745(5) 0.1689(4) 0.4450(3) 0.0511(12) Uani 1 1 d . . . . .
H21A H 1.050299 0.139625 0.415285 0.077 Uiso 1 1 calc R U . . .
H21B H 0.933048 0.104783 0.479730 0.077 Uiso 1 1 calc R U . . .
H21C H 1.010297 0.204366 0.481159 0.077 Uiso 1 1 calc R U . . .
C7 C 0.3252(5) 0.5984(4) 0.1202(3) 0.0430(11) Uani 1 1 d . . . . .
H7 H 0.381511 0.539464 0.099364 0.052 Uiso 1 1 calc R U . . .
C5 C 0.3521(6) 0.2404(5) 0.4533(3) 0.0510(12) Uani 1 1 d . . . . .
H5A H 0.287002 0.277797 0.484556 0.077 Uiso 1 1 calc R U . . .
H5B H 0.403831 0.166354 0.492216 0.077 Uiso 1 1 calc R U . . .
H5C H 0.300948 0.226834 0.409816 0.077 Uiso 1 1 calc R U . . .
C36 C 0.4059(6) 0.9517(5) 0.3700(3) 0.0551(13) Uani 1 1 d . . . . .
H36A H 0.430547 0.890063 0.425891 0.066 Uiso 1 1 calc R U . . .
H36B H 0.429388 1.023101 0.372798 0.066 Uiso 1 1 calc R U . . .
C29 C 0.2081(5) 0.2956(4) 0.2271(3) 0.0490(12) Uani 1 1 d . . . . .
H29 H 0.215361 0.279768 0.286123 0.059 Uiso 1 1 calc R U . . .
C19 C 0.6238(5) 0.6164(4) 0.3004(3) 0.0477(12) Uani 1 1 d . . . . .
H19A H 0.551145 0.581048 0.332684 0.072 Uiso 1 1 calc R U . . .
H19B H 0.583647 0.695121 0.262805 0.072 Uiso 1 1 calc R U . . .
H19C H 0.694507 0.618990 0.339208 0.072 Uiso 1 1 calc R U . . .
C10 C 0.2263(5) 0.5228(4) 0.4274(3) 0.0469(11) Uani 1 1 d . . . . .
H10A H 0.294116 0.544299 0.457482 0.070 Uiso 1 1 calc R U . . .
H10B H 0.206633 0.448183 0.462809 0.070 Uiso 1 1 calc R U . . .
H10C H 0.140909 0.582010 0.414413 0.070 Uiso 1 1 calc R U . . .
C28 C 0.0795(6) 0.3256(5) 0.1869(4) 0.0567(13) Uani 1 1 d . . . . .
H28 H -0.000663 0.330926 0.218042 0.068 Uiso 1 1 calc R U . . .
C6 C 0.5303(6) 0.3466(5) 0.4776(3) 0.0529(13) Uani 1 1 d . . . . .
H6A H 0.594122 0.396113 0.448941 0.079 Uiso 1 1 calc R U . . .
H6B H 0.582510 0.274808 0.518860 0.079 Uiso 1 1 calc R U . . .
H6C H 0.464127 0.386997 0.506494 0.079 Uiso 1 1 calc R U . . .
C20 C 0.8065(6) 0.5937(4) 0.1979(3) 0.0535(13) Uani 1 1 d . . . . .
H20A H 0.870024 0.607857 0.235158 0.080 Uiso 1 1 calc R U . . .
H20B H 0.768041 0.666406 0.152276 0.080 Uiso 1 1 calc R U . . .
H20C H 0.856625 0.537917 0.173848 0.080 Uiso 1 1 calc R U . . .
C9 C 0.3868(6) 0.7056(5) 0.0874(3) 0.0575(13) Uani 1 1 d . . . . .
H9A H 0.332604 0.766630 0.105009 0.086 Uiso 1 1 calc R U . . .
H9B H 0.385308 0.732111 0.025744 0.086 Uiso 1 1 calc R U . . .
H9C H 0.482436 0.687171 0.110383 0.086 Uiso 1 1 calc R U . . .
C16 C 0.7166(6) 0.0389(4) 0.4191(3) 0.0559(13) Uani 1 1 d . . . . .
H16A H 0.781834 0.031182 0.464676 0.084 Uiso 1 1 calc R U . . .
H16B H 0.717818 -0.037487 0.415943 0.084 Uiso 1 1 calc R U . . .
H16C H 0.623316 0.072193 0.430331 0.084 Uiso 1 1 calc R U . . .
C25 C 0.3131(6) 0.3133(5) 0.0981(3) 0.0564(13) Uani 1 1 d . . . . .
H25 H 0.392726 0.309725 0.066277 0.068 Uiso 1 1 calc R U . . .
C8 C 0.1775(6) 0.6213(5) 0.0841(3) 0.0567(13) Uani 1 1 d . . . . .
H8A H 0.132517 0.558621 0.117195 0.085 Uiso 1 1 calc R U . . .
H8B H 0.179068 0.625173 0.025371 0.085 Uiso 1 1 calc R U . . .
H8C H 0.126118 0.694854 0.086671 0.085 Uiso 1 1 calc R U . . .
B1 B 0.5400(5) 0.3600(4) 0.2292(3) 0.0371(11) Uani 1 1 d . . . . .
C27 C 0.0664(6) 0.3481(5) 0.1013(4) 0.0624(15) Uani 1 1 d . . . . .
H27 H -0.022396 0.365895 0.073692 0.075 Uiso 1 1 calc R U . . .
C26 C 0.1814(6) 0.3445(6) 0.0570(4) 0.0650(15) Uani 1 1 d . . . . .
H26 H 0.172725 0.363374 -0.002283 0.078 Uiso 1 1 calc R U . . .
C17 C 0.8886(6) 0.0634(5) 0.3049(4) 0.0643(15) Uani 1 1 d . . . . .
H17A H 0.907997 0.117982 0.250786 0.096 Uiso 1 1 calc R U . . .
H17B H 0.876274 -0.007924 0.297607 0.096 Uiso 1 1 calc R U . . .
H17C H 0.966032 0.045688 0.345998 0.096 Uiso 1 1 calc R U . . .
C35 C 0.4833(8) 0.9188(6) 0.3086(4) 0.0753(18) Uani 1 1 d . . . . .
H35A H 0.552644 0.846729 0.335883 0.090 Uiso 1 1 calc R U . . .
H35B H 0.532154 0.980220 0.276181 0.090 Uiso 1 1 calc R U . . .
O1 O 0.6500(9) 0.8921(8) 0.0990(5) 0.157(3) Uani 1 1 d . . . . .
C37 C 0.2664(8) 0.9706(8) 0.3516(5) 0.101(3) Uani 1 1 d . . . . .
H37A H 0.217938 1.043506 0.357982 0.122 Uiso 1 1 calc R U . . .
H37B H 0.226675 0.906091 0.389227 0.122 Uiso 1 1 calc R U . . .
C38 C 0.2531(8) 0.9782(7) 0.2574(5) 0.090(2) Uani 1 1 d . . . . .
H38A H 0.172381 0.948554 0.246589 0.108 Uiso 1 1 calc R U . . .
H38B H 0.247024 1.058122 0.217543 0.108 Uiso 1 1 calc R U . . .
O2 O 0.3863(9) 0.9007(11) 0.2531(7) 0.217(5) Uani 1 1 d . . . . .
C31 C 0.6884(12) 0.9335(9) 0.0133(6) 0.124(3) Uani 1 1 d . . . . .
H31A H 0.632845 1.011841 -0.016648 0.149 Uiso 1 1 calc R U . . .
H31B H 0.669393 0.881715 -0.015863 0.149 Uiso 1 1 calc R U . . .
C32 C 0.8332(10) 0.9370(11) 0.0115(8) 0.140(4) Uani 1 1 d . . . . .
H32A H 0.849579 1.007054 -0.034045 0.168 Uiso 1 1 calc R U . . .
H32B H 0.888421 0.867824 0.002768 0.168 Uiso 1 1 calc R U . . .
C34 C 0.7334(15) 0.9425(10) 0.1376(8) 0.155(5) Uani 1 1 d . . . . .
H34A H 0.747771 0.898337 0.198915 0.186 Uiso 1 1 calc R U . . .
H34B H 0.687831 1.023257 0.129312 0.186 Uiso 1 1 calc R U . . .
C33 C 0.8694(14) 0.9395(16) 0.0969(9) 0.242(11) Uani 1 1 d . . . . .
H33A H 0.938266 0.869574 0.129505 0.290 Uiso 1 1 calc R U . . .
H33B H 0.906415 1.008957 0.091568 0.290 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C1 1.359(5) . ?
N1 C2 1.402(6) . ?
N1 C4 1.485(6) . ?
N3 C12 1.351(5) . ?
N3 C13 1.409(6) . ?
N3 C15 1.499(5) . ?
N2 C1 1.352(5) . ?
N2 C3 1.413(6) . ?
N2 C7 1.485(5) . ?
N4 C12 1.366(5) . ?
N4 C14 1.391(5) . ?
N4 C18 1.483(5) . ?
C12 B1 1.666(6) . ?
N5 C30 1.143(6) . ?
C1 B1 1.654(6) . ?
C13 C14 1.357(6) . ?
C13 C21 1.489(6) . ?
C3 C2 1.351(6) . ?
C3 C11 1.493(6) . ?
C14 C22 1.494(6) . ?
C2 C10 1.495(6) . ?
C18 C19 1.520(6) . ?
C18 C20 1.530(7) . ?
C18 H18 1.0000 . ?
C4 C5 1.517(6) . ?
C4 C6 1.543(6) . ?
C4 H4 1.0000 . ?
C24 C25 1.377(7) . ?
C24 C29 1.397(7) . ?
C24 C23 1.509(6) . ?
C23 B1 1.656(7) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C15 C16 1.507(7) . ?
C15 C17 1.518(7) . ?
C15 H15 1.0000 . ?
C30 B1 1.601(7) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C7 C9 1.516(7) . ?
C7 C8 1.525(7) . ?
C7 H7 1.0000 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C36 C37 1.375(9) . ?
C36 C35 1.410(8) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C29 C28 1.371(7) . ?
C29 H29 0.9500 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C28 C27 1.381(8) . ?
C28 H28 0.9500 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C25 C26 1.403(8) . ?
C25 H25 0.9500 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C27 C26 1.355(8) . ?
C27 H27 0.9500 . ?
C26 H26 0.9500 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C35 O2 1.455(10) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
O1 C34 1.422(12) . ?
O1 C31 1.436(11) . ?
C37 C38 1.570(10) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C38 O2 1.494(10) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C31 C32 1.441(13) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 C33 1.508(18) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C34 C33 1.503(18) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 N1 C2 109.8(4) . . ?
C1 N1 C4 124.1(4) . . ?
C2 N1 C4 126.1(4) . . ?
C12 N3 C13 109.9(3) . . ?
C12 N3 C15 125.0(3) . . ?
C13 N3 C15 124.8(4) . . ?
C1 N2 C3 109.4(3) . . ?
C1 N2 C7 124.9(3) . . ?
C3 N2 C7 125.6(4) . . ?
C12 N4 C14 109.8(3) . . ?
C12 N4 C18 123.6(3) . . ?
C14 N4 C18 126.3(3) . . ?
N3 C12 N4 106.3(3) . . ?
N3 C12 B1 130.9(4) . . ?
N4 C12 B1 122.7(4) . . ?
N2 C1 N1 106.8(4) . . ?
N2 C1 B1 130.1(4) . . ?
N1 C1 B1 123.1(4) . . ?
C14 C13 N3 106.5(4) . . ?
C14 C13 C21 127.3(4) . . ?
N3 C13 C21 126.2(4) . . ?
C2 C3 N2 107.0(4) . . ?
C2 C3 C11 128.3(4) . . ?
N2 C3 C11 124.6(4) . . ?
C13 C14 N4 107.4(4) . . ?
C13 C14 C22 126.2(4) . . ?
N4 C14 C22 126.4(4) . . ?
C3 C2 N1 107.0(4) . . ?
C3 C2 C10 127.6(4) . . ?
N1 C2 C10 125.3(4) . . ?
N4 C18 C19 113.2(4) . . ?
N4 C18 C20 110.2(4) . . ?
C19 C18 C20 112.3(4) . . ?
N4 C18 H18 106.9 . . ?
C19 C18 H18 106.9 . . ?
C20 C18 H18 106.9 . . ?
N1 C4 C5 114.1(4) . . ?
N1 C4 C6 111.4(4) . . ?
C5 C4 C6 111.6(4) . . ?
N1 C4 H4 106.4 . . ?
C5 C4 H4 106.4 . . ?
C6 C4 H4 106.4 . . ?
C25 C24 C29 117.1(5) . . ?
C25 C24 C23 121.6(5) . . ?
C29 C24 C23 121.3(4) . . ?
C24 C23 B1 114.4(4) . . ?
C24 C23 H23A 108.7 . . ?
B1 C23 H23A 108.7 . . ?
C24 C23 H23B 108.7 . . ?
B1 C23 H23B 108.7 . . ?
H23A C23 H23B 107.6 . . ?
N3 C15 C16 113.2(4) . . ?
N3 C15 C17 110.8(4) . . ?
C16 C15 C17 113.9(4) . . ?
N3 C15 H15 106.1 . . ?
C16 C15 H15 106.1 . . ?
C17 C15 H15 106.1 . . ?
N5 C30 B1 170.6(5) . . ?
C14 C22 H22A 109.5 . . ?
C14 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C14 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C3 C11 H11A 109.5 . . ?
C3 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C3 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C13 C21 H21A 109.5 . . ?
C13 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C13 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N2 C7 C9 112.6(4) . . ?
N2 C7 C8 111.8(4) . . ?
C9 C7 C8 111.6(4) . . ?
N2 C7 H7 106.8 . . ?
C9 C7 H7 106.8 . . ?
C8 C7 H7 106.8 . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C37 C36 C35 111.3(5) . . ?
C37 C36 H36A 109.4 . . ?
C35 C36 H36A 109.4 . . ?
C37 C36 H36B 109.4 . . ?
C35 C36 H36B 109.4 . . ?
H36A C36 H36B 108.0 . . ?
C28 C29 C24 121.8(5) . . ?
C28 C29 H29 119.1 . . ?
C24 C29 H29 119.1 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C2 C10 H10A 109.5 . . ?
C2 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C2 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C29 C28 C27 120.1(6) . . ?
C29 C28 H28 120.0 . . ?
C27 C28 H28 120.0 . . ?
C4 C6 H6A 109.5 . . ?
C4 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C4 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C24 C25 C26 121.0(5) . . ?
C24 C25 H25 119.5 . . ?
C26 C25 H25 119.5 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C30 B1 C1 115.3(4) . . ?
C30 B1 C23 106.4(4) . . ?
C1 B1 C23 105.8(4) . . ?
C30 B1 C12 101.9(4) . . ?
C1 B1 C12 107.7(3) . . ?
C23 B1 C12 120.1(4) . . ?
C26 C27 C28 119.4(5) . . ?
C26 C27 H27 120.3 . . ?
C28 C27 H27 120.3 . . ?
C27 C26 C25 120.5(5) . . ?
C27 C26 H26 119.7 . . ?
C25 C26 H26 119.7 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C36 C35 O2 107.1(7) . . ?
C36 C35 H35A 110.3 . . ?
O2 C35 H35A 110.3 . . ?
C36 C35 H35B 110.3 . . ?
O2 C35 H35B 110.3 . . ?
H35A C35 H35B 108.5 . . ?
C34 O1 C31 101.0(9) . . ?
C36 C37 C38 105.0(6) . . ?
C36 C37 H37A 110.7 . . ?
C38 C37 H37A 110.7 . . ?
C36 C37 H37B 110.7 . . ?
C38 C37 H37B 110.7 . . ?
H37A C37 H37B 108.8 . . ?
O2 C38 C37 100.0(7) . . ?
O2 C38 H38A 111.8 . . ?
C37 C38 H38A 111.8 . . ?
O2 C38 H38B 111.8 . . ?
C37 C38 H38B 111.8 . . ?
H38A C38 H38B 109.5 . . ?
C35 O2 C38 104.4(8) . . ?
O1 C31 C32 109.9(9) . . ?
O1 C31 H31A 109.7 . . ?
C32 C31 H31A 109.7 . . ?
O1 C31 H31B 109.7 . . ?
C32 C31 H31B 109.7 . . ?
H31A C31 H31B 108.2 . . ?
C31 C32 C33 104.3(10) . . ?
C31 C32 H32A 110.9 . . ?
C33 C32 H32A 110.9 . . ?
C31 C32 H32B 110.9 . . ?
C33 C32 H32B 110.9 . . ?
H32A C32 H32B 108.9 . . ?
O1 C34 C33 107.4(11) . . ?
O1 C34 H34A 110.2 . . ?
C33 C34 H34A 110.2 . . ?
O1 C34 H34B 110.2 . . ?
C33 C34 H34B 110.2 . . ?
H34A C34 H34B 108.5 . . ?
C34 C33 C32 103.1(9) . . ?
C34 C33 H33A 111.1 . . ?
C32 C33 H33A 111.1 . . ?
C34 C33 H33B 111.1 . . ?
C32 C33 H33B 111.1 . . ?
H33A C33 H33B 109.1 . . ?

_refine_diff_density_max         0.691
_refine_diff_density_min         -0.458
_refine_diff_density_rms         0.075

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

data_compound_2-Xyl
_database_code_depnum_ccdc_archive 'CCDC 1579156'
_audit_update_record             
;
2017-10-10 deposited with the CCDC.
2018-02-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C66 H105 B Cl N6 Ni O6 Si2'
_chemical_formula_sum            'C66 H105 B Cl N6 Ni O6 Si2'
_chemical_formula_weight         1239.70

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 '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                   11.0148(4)
_cell_length_b                   14.6131(5)
_cell_length_c                   22.7930(8)
_cell_angle_alpha                84.552(3)
_cell_angle_beta                 83.601(3)
_cell_angle_gamma                70.398(4)
_cell_volume                     3428.1(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    8739
_cell_measurement_theta_min      3.1980
_cell_measurement_theta_max      73.0800

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.201
_exptl_crystal_F_000             1338
_exptl_crystal_size_max          0.186
_exptl_crystal_size_mid          0.146
_exptl_crystal_size_min          0.136
_exptl_absorpt_coefficient_mu    1.508
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.25515
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43c (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.5435
_diffrn_reflns_number            24731
_diffrn_reflns_av_unetI/netI     0.0455
_diffrn_reflns_av_R_equivalents  0.0350
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         6.399
_diffrn_reflns_theta_max         69.999
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             12907
_reflns_number_gt                10375
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'CrysAlisPro 1.171.38.43c (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43c (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43c (Rigaku OD, 2015)'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0883P)²+2.1411P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         12907
_refine_ls_number_parameters     783
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0701
_refine_ls_R_factor_gt           0.0565
_refine_ls_wR_factor_ref         0.1660
_refine_ls_wR_factor_gt          0.1518
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.046
_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
Ni1 Ni 0.61047(4) 0.71904(3) 0.23263(2) 0.02552(12) Uani 1 1 d . . . . .
Si1 Si 0.58467(6) 0.86547(5) 0.25832(3) 0.02456(15) Uani 1 1 d . . . . .
Cl1 Cl 0.75697(6) 0.69464(5) 0.15477(3) 0.03683(16) Uani 1 1 d . . . . .
Si2 Si 0.61007(7) 1.03196(5) 0.16805(3) 0.03440(17) Uani 1 1 d . . . . .
O1 O 0.72585(16) 0.88405(13) 0.27021(8) 0.0313(4) Uani 1 1 d . . . . .
O2 O 0.51287(16) 0.89949(12) 0.32753(7) 0.0297(4) Uani 1 1 d . . . . .
N1 N 0.51777(18) 0.96757(14) 0.20950(9) 0.0261(4) Uani 1 1 d . . . . .
N6 N 0.56546(19) 0.65472(15) 0.35633(9) 0.0291(4) Uani 1 1 d . . . . .
N3 N 0.53357(19) 0.43948(15) 0.32419(9) 0.0291(4) Uani 1 1 d . . . . .
N4 N 0.33454(19) 0.58297(15) 0.19915(9) 0.0293(4) Uani 1 1 d . . . . .
N2 N 0.69502(19) 0.42228(15) 0.25741(10) 0.0297(4) Uani 1 1 d . . . . .
N5 N 0.25584(19) 0.69186(15) 0.26424(9) 0.0282(4) Uani 1 1 d . . . . .
C22 C 0.5832(2) 0.48799(17) 0.27938(10) 0.0260(5) Uani 1 1 d . . . . .
C21 C 0.5892(3) 0.93755(18) 0.35394(11) 0.0319(5) Uani 1 1 d . . . . .
C33 C 0.3678(2) 0.62514(17) 0.24273(11) 0.0258(5) Uani 1 1 d . . . . .
C1 C 0.3811(2) 0.99803(18) 0.20115(11) 0.0294(5) Uani 1 1 d . . . . .
C44 C 0.5520(2) 0.67028(17) 0.30143(11) 0.0267(5) Uani 1 1 d . . . . .
C35 C 0.1536(2) 0.69194(19) 0.23305(12) 0.0331(6) Uani 1 1 d . . . . .
C28 C 0.4181(2) 0.48848(18) 0.36371(12) 0.0315(5) Uani 1 1 d . . . . .
H28 H 0.393062 0.559612 0.351902 0.038 Uiso 1 1 calc R U . . .
C45 C 0.6258(2) 0.69522(18) 0.39293(11) 0.0281(5) Uani 1 1 d . . . . .
C36 C 0.4298(2) 0.50751(19) 0.16294(12) 0.0333(6) Uani 1 1 d . . . . .
H36 H 0.517283 0.505733 0.172081 0.040 Uiso 1 1 calc R U . . .
C46 C 0.7597(2) 0.67852(19) 0.38408(12) 0.0330(6) Uani 1 1 d . . . . .
C16 C 0.7081(3) 0.92827(18) 0.32231(12) 0.0337(6) Uani 1 1 d . . . . .
C39 C 0.2460(2) 0.75200(19) 0.31436(12) 0.0314(5) Uani 1 1 d . . . . .
H39 H 0.333863 0.730874 0.329232 0.038 Uiso 1 1 calc R U . . .
C49 C 0.6165(3) 0.7727(2) 0.48304(12) 0.0367(6) Uani 1 1 d . . . . .
H49 H 0.568125 0.804519 0.516798 0.044 Uiso 1 1 calc R U . . .
C24 C 0.6124(2) 0.34223(18) 0.32912(12) 0.0331(6) Uani 1 1 d . . . . .
C6 C 0.3369(3) 0.9614(2) 0.15573(12) 0.0351(6) Uani 1 1 d . . . . .
C34 C 0.2023(2) 0.6226(2) 0.19334(12) 0.0342(6) Uani 1 1 d . . . . .
C25 C 0.7828(3) 0.4448(2) 0.20791(13) 0.0390(6) Uani 1 1 d . . . . .
H25 H 0.746480 0.516053 0.197031 0.047 Uiso 1 1 calc R U . . .
C7 C 0.3323(3) 1.11577(19) 0.28472(12) 0.0350(6) Uani 1 1 d . . . . .
H7 H 0.427481 1.083942 0.287412 0.042 Uiso 1 1 calc R U . . .
C40 C 0.2132(3) 0.8590(2) 0.29539(14) 0.0428(7) Uani 1 1 d . . . . .
H40A H 0.268006 0.866867 0.259662 0.064 Uiso 1 1 calc R U . . .
H40B H 0.228136 0.893681 0.327151 0.064 Uiso 1 1 calc R U . . .
H40C H 0.122082 0.885773 0.287069 0.064 Uiso 1 1 calc R U . . .
C50 C 0.5535(3) 0.74277(19) 0.44274(11) 0.0317(5) Uani 1 1 d . . . . .
C23 C 0.7133(2) 0.33188(18) 0.28789(12) 0.0339(6) Uani 1 1 d . . . . .
C20 C 0.5577(3) 0.98156(19) 0.40739(12) 0.0399(6) Uani 1 1 d . . . . .
H20 H 0.476629 0.988411 0.429071 0.048 Uiso 1 1 calc R U . . .
C52 C 0.4099(3) 0.7632(2) 0.44996(13) 0.0404(6) Uani 1 1 d . . . . .
H52A H 0.374407 0.793452 0.487456 0.061 Uiso 1 1 calc R U . . .
H52B H 0.391532 0.702007 0.450015 0.061 Uiso 1 1 calc R U . . .
H52C H 0.370022 0.807298 0.417140 0.061 Uiso 1 1 calc R U . . .
C41 C 0.1541(3) 0.7340(2) 0.36590(13) 0.0399(6) Uani 1 1 d . . . . .
H41A H 0.064654 0.763692 0.355591 0.060 Uiso 1 1 calc R U . . .
H41B H 0.165803 0.762944 0.401032 0.060 Uiso 1 1 calc R U . . .
H41C H 0.172981 0.663788 0.374182 0.060 Uiso 1 1 calc R U . . .
C2 C 0.2922(2) 1.06765(18) 0.23730(12) 0.0329(6) Uani 1 1 d . . . . .
C47 C 0.8186(3) 0.7102(2) 0.42520(13) 0.0398(6) Uani 1 1 d . . . . .
H47 H 0.908863 0.699650 0.419371 0.048 Uiso 1 1 calc R U . . .
C19 C 0.6473(4) 1.0154(2) 0.42853(13) 0.0480(8) Uani 1 1 d . . . . .
H19 H 0.626980 1.045574 0.465132 0.058 Uiso 1 1 calc R U . . .
C51 C 0.8389(3) 0.6232(2) 0.33249(13) 0.0413(7) Uani 1 1 d . . . . .
H51A H 0.930933 0.611049 0.336136 0.062 Uiso 1 1 calc R U . . .
H51B H 0.813995 0.661663 0.295491 0.062 Uiso 1 1 calc R U . . .
H51C H 0.823370 0.561040 0.332337 0.062 Uiso 1 1 calc R U . . .
C48 C 0.7479(3) 0.7571(2) 0.47494(13) 0.0417(7) Uani 1 1 d . . . . .
H48 H 0.789674 0.777895 0.502779 0.050 Uiso 1 1 calc R U . . .
C43 C 0.0183(3) 0.7625(2) 0.23970(15) 0.0436(7) Uani 1 1 d . . . . .
H43A H 0.018384 0.827678 0.224995 0.065 Uiso 1 1 calc R U . . .
H43B H -0.014120 0.763516 0.281535 0.065 Uiso 1 1 calc R U . . .
H43C H -0.037640 0.742210 0.216895 0.065 Uiso 1 1 calc R U . . .
C10 C 0.4262(3) 0.8875(2) 0.11442(12) 0.0392(6) Uani 1 1 d . . . . .
H10 H 0.517449 0.878179 0.121928 0.047 Uiso 1 1 calc R U . . .
C3 C 0.1605(3) 1.0967(2) 0.22875(16) 0.0495(8) Uani 1 1 d . . . . .
H3 H 0.100092 1.142882 0.253436 0.059 Uiso 1 1 calc R U . . .
B1 B 0.5170(2) 0.60109(19) 0.25865(12) 0.0257(5) Uani 1 1 d . . . . .
C5 C 0.2040(3) 0.9929(2) 0.14929(15) 0.0488(7) Uani 1 1 d . . . . .
H5 H 0.173176 0.967721 0.119297 0.059 Uiso 1 1 calc R U . . .
C17 C 0.7976(3) 0.9619(2) 0.34344(14) 0.0421(7) Uani 1 1 d . . . . .
H17 H 0.878679 0.955197 0.321850 0.051 Uiso 1 1 calc R U . . .
C30 C 0.3039(3) 0.4571(2) 0.35440(15) 0.0447(7) Uani 1 1 d . . . . .
H30A H 0.285320 0.470212 0.312787 0.067 Uiso 1 1 calc R U . . .
H30B H 0.227924 0.493484 0.379410 0.067 Uiso 1 1 calc R U . . .
H30C H 0.324594 0.387265 0.364988 0.067 Uiso 1 1 calc R U . . .
C12 C 0.4044(3) 0.7896(2) 0.12610(14) 0.0452(7) Uani 1 1 d . . . . .
H12A H 0.417053 0.766768 0.167526 0.068 Uiso 1 1 calc R U . . .
H12B H 0.466130 0.742244 0.100258 0.068 Uiso 1 1 calc R U . . .
H12C H 0.316019 0.796765 0.118047 0.068 Uiso 1 1 calc R U . . .
C38 C 0.4213(3) 0.4071(2) 0.18109(15) 0.0478(7) Uani 1 1 d . . . . .
H38A H 0.434696 0.392016 0.223179 0.072 Uiso 1 1 calc R U . . .
H38B H 0.487921 0.358693 0.157680 0.072 Uiso 1 1 calc R U . . .
H38C H 0.335675 0.405793 0.174142 0.072 Uiso 1 1 calc R U . . .
C29 C 0.4490(3) 0.4769(2) 0.42826(13) 0.0438(7) Uani 1 1 d . . . . .
H29A H 0.462578 0.409500 0.443419 0.066 Uiso 1 1 calc R U . . .
H29B H 0.376756 0.520760 0.451806 0.066 Uiso 1 1 calc R U . . .
H29C H 0.527636 0.493057 0.430937 0.066 Uiso 1 1 calc R U . . .
C13 C 0.7524(3) 0.9485(3) 0.12534(17) 0.0561(9) Uani 1 1 d . . . . .
H13A H 0.804173 0.898181 0.152505 0.084 Uiso 1 1 calc R U . . .
H13B H 0.805465 0.985820 0.104935 0.084 Uiso 1 1 calc R U . . .
H13C H 0.722146 0.917786 0.096189 0.084 Uiso 1 1 calc R U . . .
C14 C 0.6696(3) 1.1067(2) 0.21254(15) 0.0502(8) Uani 1 1 d . . . . .
H14A H 0.597572 1.146009 0.238369 0.075 Uiso 1 1 calc R U . . .
H14B H 0.705585 1.149603 0.185905 0.075 Uiso 1 1 calc R U . . .
H14C H 0.736837 1.063596 0.236706 0.075 Uiso 1 1 calc R U . . .
C15 C 0.5053(3) 1.1214(2) 0.11511(14) 0.0493(8) Uani 1 1 d . . . . .
H15A H 0.470577 1.086798 0.090047 0.074 Uiso 1 1 calc R U . . .
H15B H 0.556614 1.155877 0.090274 0.074 Uiso 1 1 calc R U . . .
H15C H 0.433715 1.168262 0.137250 0.074 Uiso 1 1 calc R U . . .
C18 C 0.7651(4) 1.0061(2) 0.39745(15) 0.0504(8) Uani 1 1 d . . . . .
H18 H 0.824802 1.029846 0.412816 0.061 Uiso 1 1 calc R U . . .
C42 C 0.1318(3) 0.5916(3) 0.15075(15) 0.0488(8) Uani 1 1 d . . . . .
H42A H 0.038347 0.619951 0.160507 0.073 Uiso 1 1 calc R U . . .
H42B H 0.156512 0.520498 0.153383 0.073 Uiso 1 1 calc R U . . .
H42C H 0.154278 0.614184 0.110444 0.073 Uiso 1 1 calc R U . . .
C26 C 0.9186(3) 0.4257(3) 0.22612(17) 0.0537(8) Uani 1 1 d . . . . .
H26A H 0.912893 0.451428 0.264880 0.081 Uiso 1 1 calc R U . . .
H26B H 0.965318 0.458003 0.196781 0.081 Uiso 1 1 calc R U . . .
H26C H 0.964926 0.355509 0.228388 0.081 Uiso 1 1 calc R U . . .
C8 C 0.2641(3) 1.1032(2) 0.34571(14) 0.0463(7) Uani 1 1 d . . . . .
H8A H 0.170746 1.135801 0.344618 0.069 Uiso 1 1 calc R U . . .
H8B H 0.296564 1.131979 0.375082 0.069 Uiso 1 1 calc R U . . .
H8C H 0.281412 1.033723 0.356491 0.069 Uiso 1 1 calc R U . . .
C32 C 0.5861(3) 0.2654(2) 0.37205(15) 0.0461(7) Uani 1 1 d . . . . .
H32A H 0.628535 0.201353 0.356110 0.069 Uiso 1 1 calc R U . . .
H32B H 0.492639 0.277800 0.378306 0.069 Uiso 1 1 calc R U . . .
H32C H 0.619983 0.266949 0.409788 0.069 Uiso 1 1 calc R U . . .
C31 C 0.8290(3) 0.2427(2) 0.27911(15) 0.0422(7) Uani 1 1 d . . . . .
H31A H 0.901462 0.249089 0.297759 0.063 Uiso 1 1 calc R U . . .
H31B H 0.852808 0.235056 0.236689 0.063 Uiso 1 1 calc R U . . .
H31C H 0.808407 0.185446 0.297137 0.063 Uiso 1 1 calc R U . . .
C37 C 0.4231(3) 0.5324(2) 0.09674(13) 0.0454(7) Uani 1 1 d . . . . .
H37A H 0.350588 0.517394 0.083574 0.068 Uiso 1 1 calc R U . . .
H37B H 0.503996 0.494028 0.075623 0.068 Uiso 1 1 calc R U . . .
H37C H 0.410503 0.601889 0.088413 0.068 Uiso 1 1 calc R U . . .
C27 C 0.7846(3) 0.3915(3) 0.15280(15) 0.0582(9) Uani 1 1 d . . . . .
H27A H 0.834426 0.322331 0.159085 0.087 Uiso 1 1 calc R U . . .
H27B H 0.824786 0.419690 0.118518 0.087 Uiso 1 1 calc R U . . .
H27C H 0.695827 0.398355 0.145599 0.087 Uiso 1 1 calc R U . . .
C4 C 0.1169(3) 1.0597(3) 0.18543(18) 0.0593(9) Uani 1 1 d . . . . .
H4 H 0.027067 1.079974 0.180344 0.071 Uiso 1 1 calc R U . . .
C9 C 0.3074(4) 1.2241(2) 0.26763(16) 0.0510(8) Uani 1 1 d . . . . .
H9A H 0.352718 1.231417 0.228874 0.077 Uiso 1 1 calc R U . . .
H9B H 0.339210 1.252725 0.297302 0.077 Uiso 1 1 calc R U . . .
H9C H 0.214346 1.257375 0.265770 0.077 Uiso 1 1 calc R U . . .
C11 C 0.4093(5) 0.9209(3) 0.04888(15) 0.0705(12) Uani 1 1 d . . . . .
H11A H 0.323562 0.923282 0.039497 0.106 Uiso 1 1 calc R U . . .
H11B H 0.475946 0.874841 0.024019 0.106 Uiso 1 1 calc R U . . .
H11C H 0.417684 0.985715 0.041383 0.106 Uiso 1 1 calc R U . . .
C54 C 0.0019(3) 0.4267(2) 0.44090(14) 0.0456(7) Uani 1 1 d . . . . .
H54A H 0.072377 0.409758 0.467533 0.055 Uiso 1 1 calc R U . . .
H54B H -0.017007 0.495498 0.425894 0.055 Uiso 1 1 calc R U . . .
C53 C 0.0383(4) 0.3606(3) 0.39077(17) 0.0607(9) Uani 1 1 d . . . . .
H53A H 0.066151 0.393864 0.354534 0.073 Uiso 1 1 calc R U . A 1
H53B H 0.110817 0.301140 0.400629 0.073 Uiso 1 1 calc R U . A 1
O3 O -0.0696(6) 0.3361(6) 0.3815(3) 0.083(2) Uani 0.77(2) 1 d . . P B 1
C55 C -0.1155(5) 0.4106(5) 0.4722(2) 0.102(2) Uani 1 1 d . . . . .
H55A H -0.093171 0.363726 0.506790 0.122 Uiso 1 1 calc R U . . .
H55B H -0.178855 0.472450 0.485627 0.122 Uiso 1 1 calc R U . . .
C56 C -0.1674(5) 0.3707(5) 0.4271(3) 0.1012(18) Uani 1 1 d . . . . .
H56A H -0.197387 0.317016 0.445402 0.121 Uiso 1 1 calc R U . B 1
H56B H -0.242078 0.422141 0.410749 0.121 Uiso 1 1 calc R U . B 1
C60 C 1.0507(7) 0.8053(6) 0.0463(3) 0.133(3) Uani 1 1 d . . . . .
H60A H 0.976445 0.786425 0.065257 0.160 Uiso 1 1 calc R U . B 1
H60B H 1.078911 0.839097 0.075073 0.160 Uiso 1 1 calc R U . B 1
C61 C 0.7089(10) 0.6309(11) 0.0011(4) 0.225(8) Uani 1 1 d D . . . .
H61A H 0.669428 0.628798 0.042178 0.270 Uiso 1 1 calc R U . . .
H61B H 0.647031 0.627561 -0.026338 0.270 Uiso 1 1 calc R U . . .
O4 O 1.1561(12) 0.7200(11) 0.0273(7) 0.204(7) Uani 0.77(2) 1 d . . P B 1
C59 C 1.0157(11) 0.8663(7) -0.0054(5) 0.203(5) Uani 1 1 d . . . . .
H59A H 1.003950 0.934625 0.001754 0.243 Uiso 1 1 calc R U . . .
H59B H 0.933857 0.863315 -0.017888 0.243 Uiso 1 1 calc R U . . .
C58 C 1.1232(10) 0.8294(6) -0.0514(3) 0.160(4) Uani 1 1 d . . . . .
H58A H 1.161687 0.880315 -0.066383 0.192 Uiso 1 1 calc R U . . .
H58B H 1.093089 0.807084 -0.085055 0.192 Uiso 1 1 calc R U . . .
C57 C 1.2181(7) 0.7466(6) -0.0202(3) 0.126(2) Uani 1 1 d . . . . .
H57A H 1.255666 0.691701 -0.046186 0.151 Uiso 1 1 calc R U . B 1
H57B H 1.289131 0.766955 -0.009014 0.151 Uiso 1 1 calc R U . B 1
C62 C 0.7452(12) 0.7227(6) -0.0129(4) 0.231(7) Uani 1 1 d D . . . .
H62A H 0.669547 0.780189 -0.022090 0.277 Uiso 1 1 calc R U . . .
H62B H 0.788165 0.736339 0.019623 0.277 Uiso 1 1 calc R U . . .
C63 C 0.8385(12) 0.6909(9) -0.0672(5) 0.277(8) Uani 1 1 d D . . . .
H63A H 0.803892 0.728389 -0.103664 0.332 Uiso 1 1 calc R U . . .
H63B H 0.924354 0.696212 -0.062912 0.332 Uiso 1 1 calc R U . . .
O5 O 0.8284(18) 0.5528(6) -0.0066(6) 0.519(16) Uani 1 1 d D . . . .
C64 C 0.8435(15) 0.5875(8) -0.0661(5) 0.288(9) Uani 1 1 d D . . . .
H64A H 0.773543 0.582823 -0.088204 0.345 Uiso 1 1 calc R U . . .
H64B H 0.927426 0.547485 -0.085125 0.345 Uiso 1 1 calc R U . . .
C66 C 1.0889(4) 0.9872(3) 0.46159(18) 0.0696(11) Uani 1 1 d . . . . .
O6 O 1.1040(6) 0.8971(4) 0.5002(3) 0.159(2) Uani 1 1 d . . . . .
C65 C 1.0146(5) 1.0814(5) 0.4824(4) 0.126(3) Uani 1 1 d . . . . .
O4A O 1.1780(19) 0.7617(14) 0.0378(9) 0.071(6) Uiso 0.23(2) 1 d . . P B 2
O3A O -0.045(2) 0.3019(17) 0.4087(15) 0.098(7) Uiso 0.23(2) 1 d . . P B 2
H1 H 0.570(3) 0.613(2) 0.2136(12) 0.028(7) 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
Ni1 C44 1.803(2) . ?
Ni1 Si1 2.1898(8) . ?
Ni1 Cl1 2.2309(7) . ?
Ni1 B1 2.290(3) . ?
Si1 O1 1.7194(18) . ?
Si1 O2 1.7229(17) . ?
Si1 N1 1.771(2) . ?
Si2 N1 1.752(2) . ?
Si2 C14 1.868(3) . ?
Si2 C15 1.869(3) . ?
Si2 C13 1.869(3) . ?
O1 C16 1.369(3) . ?
O2 C21 1.367(3) . ?
N1 C1 1.449(3) . ?
N6 C44 1.267(3) . ?
N6 C45 1.404(3) . ?
N3 C22 1.358(3) . ?
N3 C24 1.396(3) . ?
N3 C28 1.482(3) . ?
N4 C33 1.360(3) . ?
N4 C34 1.392(3) . ?
N4 C36 1.484(3) . ?
N2 C22 1.360(3) . ?
N2 C23 1.395(3) . ?
N2 C25 1.489(3) . ?
N5 C33 1.364(3) . ?
N5 C35 1.397(3) . ?
N5 C39 1.479(3) . ?
C22 B1 1.614(3) . ?
C21 C20 1.387(4) . ?
C21 C16 1.394(4) . ?
C33 B1 1.636(3) . ?
C1 C2 1.408(4) . ?
C1 C6 1.410(4) . ?
C44 B1 1.629(4) . ?
C35 C34 1.354(4) . ?
C35 C43 1.502(3) . ?
C28 C30 1.518(4) . ?
C28 C29 1.528(4) . ?
C45 C46 1.405(4) . ?
C45 C50 1.408(4) . ?
C36 C38 1.517(4) . ?
C36 C37 1.522(4) . ?
C46 C47 1.390(4) . ?
C46 C51 1.509(4) . ?
C16 C17 1.386(4) . ?
C39 C40 1.513(4) . ?
C39 C41 1.526(4) . ?
C49 C48 1.381(4) . ?
C49 C50 1.392(4) . ?
C24 C23 1.350(4) . ?
C24 C32 1.499(4) . ?
C6 C5 1.400(4) . ?
C6 C10 1.515(4) . ?
C34 C42 1.496(4) . ?
C25 C26 1.524(4) . ?
C25 C27 1.535(5) . ?
C7 C2 1.522(4) . ?
C7 C8 1.531(4) . ?
C7 C9 1.532(4) . ?
C50 C52 1.501(4) . ?
C23 C31 1.497(3) . ?
C20 C19 1.389(5) . ?
C2 C3 1.399(4) . ?
C47 C48 1.398(4) . ?
C19 C18 1.378(5) . ?
C10 C12 1.522(4) . ?
C10 C11 1.538(4) . ?
C3 C4 1.370(5) . ?
C5 C4 1.378(5) . ?
C17 C18 1.399(4) . ?
C54 C55 1.484(5) . ?
C54 C53 1.499(5) . ?
C53 O3 1.394(6) . ?
C53 O3A 1.46(2) . ?
O3 C56 1.408(7) . ?
C55 C56 1.480(7) . ?
C56 O3A 1.43(2) . ?
C60 O4A 1.33(2) . ?
C60 C59 1.417(10) . ?
C60 O4 1.452(13) . ?
C61 O5 1.429(5) . ?
C61 C62 1.521(5) . ?
C61 C64 1.998(11) . ?
O4 C57 1.312(10) . ?
C59 C58 1.482(10) . ?
C58 C57 1.489(10) . ?
C57 O4A 1.36(2) . ?
C62 C63 1.520(5) . ?
C63 C64 1.493(5) . ?
O5 C64 1.414(5) . ?
C66 C65 1.439(7) . ?
C66 O6 1.483(7) . ?
C66 C65 2.034(10) 2_776 ?
O6 C65 1.263(7) 2_776 ?

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
C44 Ni1 Si1 99.19(8) . . ?
C44 Ni1 Cl1 147.71(8) . . ?
Si1 Ni1 Cl1 105.27(3) . . ?
C44 Ni1 B1 44.99(10) . . ?
Si1 Ni1 B1 137.30(7) . . ?
Cl1 Ni1 B1 117.12(7) . . ?
O1 Si1 O2 93.42(9) . . ?
O1 Si1 N1 100.15(9) . . ?
O2 Si1 N1 105.39(9) . . ?
O1 Si1 Ni1 114.33(6) . . ?
O2 Si1 Ni1 119.25(7) . . ?
N1 Si1 Ni1 119.73(7) . . ?
N1 Si2 C14 114.42(13) . . ?
N1 Si2 C15 108.45(13) . . ?
C14 Si2 C15 105.06(16) . . ?
N1 Si2 C13 111.34(13) . . ?
C14 Si2 C13 108.31(17) . . ?
C15 Si2 C13 108.96(17) . . ?
C16 O1 Si1 108.84(16) . . ?
C21 O2 Si1 108.84(16) . . ?
C1 N1 Si2 117.57(16) . . ?
C1 N1 Si1 119.16(16) . . ?
Si2 N1 Si1 123.22(12) . . ?
C44 N6 C45 130.1(2) . . ?
C22 N3 C24 110.0(2) . . ?
C22 N3 C28 122.7(2) . . ?
C24 N3 C28 127.1(2) . . ?
C33 N4 C34 110.3(2) . . ?
C33 N4 C36 123.1(2) . . ?
C34 N4 C36 126.5(2) . . ?
C22 N2 C23 109.8(2) . . ?
C22 N2 C25 124.4(2) . . ?
C23 N2 C25 125.9(2) . . ?
C33 N5 C35 109.7(2) . . ?
C33 N5 C39 124.2(2) . . ?
C35 N5 C39 126.0(2) . . ?
N3 C22 N2 106.0(2) . . ?
N3 C22 B1 124.7(2) . . ?
N2 C22 B1 129.3(2) . . ?
O2 C21 C20 125.8(3) . . ?
O2 C21 C16 113.9(2) . . ?
C20 C21 C16 120.3(3) . . ?
N4 C33 N5 105.8(2) . . ?
N4 C33 B1 123.5(2) . . ?
N5 C33 B1 130.6(2) . . ?
C2 C1 C6 119.7(2) . . ?
C2 C1 N1 119.6(2) . . ?
C6 C1 N1 120.6(2) . . ?
N6 C44 B1 126.9(2) . . ?
N6 C44 Ni1 144.5(2) . . ?
B1 C44 Ni1 83.52(15) . . ?
C34 C35 N5 107.3(2) . . ?
C34 C35 C43 127.3(3) . . ?
N5 C35 C43 125.3(3) . . ?
N3 C28 C30 111.5(2) . . ?
N3 C28 C29 111.7(2) . . ?
C30 C28 C29 113.4(2) . . ?
N6 C45 C46 120.4(2) . . ?
N6 C45 C50 118.9(2) . . ?
C46 C45 C50 120.3(2) . . ?
N4 C36 C38 111.5(2) . . ?
N4 C36 C37 113.0(2) . . ?
C38 C36 C37 112.7(2) . . ?
C47 C46 C45 118.7(3) . . ?
C47 C46 C51 120.6(2) . . ?
C45 C46 C51 120.6(2) . . ?
O1 C16 C17 124.8(3) . . ?
O1 C16 C21 114.0(2) . . ?
C17 C16 C21 121.1(3) . . ?
N5 C39 C40 112.3(2) . . ?
N5 C39 C41 112.4(2) . . ?
C40 C39 C41 112.0(2) . . ?
C48 C49 C50 121.3(3) . . ?
C23 C24 N3 106.9(2) . . ?
C23 C24 C32 127.7(2) . . ?
N3 C24 C32 125.4(2) . . ?
C5 C6 C1 118.6(3) . . ?
C5 C6 C10 118.3(3) . . ?
C1 C6 C10 123.1(2) . . ?
C35 C34 N4 106.8(2) . . ?
C35 C34 C42 128.3(2) . . ?
N4 C34 C42 124.8(2) . . ?
N2 C25 C26 112.3(2) . . ?
N2 C25 C27 111.5(3) . . ?
C26 C25 C27 111.9(2) . . ?
C2 C7 C8 112.4(2) . . ?
C2 C7 C9 110.7(2) . . ?
C8 C7 C9 110.0(2) . . ?
C49 C50 C45 119.1(2) . . ?
C49 C50 C52 121.6(2) . . ?
C45 C50 C52 119.3(2) . . ?
C24 C23 N2 107.3(2) . . ?
C24 C23 C31 126.8(3) . . ?
N2 C23 C31 125.7(2) . . ?
C21 C20 C19 118.5(3) . . ?
C3 C2 C1 119.1(3) . . ?
C3 C2 C7 117.6(2) . . ?
C1 C2 C7 123.2(2) . . ?
C46 C47 C48 121.5(3) . . ?
C18 C19 C20 121.3(3) . . ?
C49 C48 C47 119.0(3) . . ?
C6 C10 C12 111.1(2) . . ?
C6 C10 C11 112.4(3) . . ?
C12 C10 C11 108.7(3) . . ?
C4 C3 C2 121.3(3) . . ?
C22 B1 C44 110.1(2) . . ?
C22 B1 C33 112.2(2) . . ?
C44 B1 C33 120.17(19) . . ?
C22 B1 Ni1 129.47(17) . . ?
C44 B1 Ni1 51.50(11) . . ?
C33 B1 Ni1 117.19(16) . . ?
C4 C5 C6 121.6(3) . . ?
C16 C17 C18 118.2(3) . . ?
C19 C18 C17 120.5(3) . . ?
C3 C4 C5 119.7(3) . . ?
C55 C54 C53 104.6(3) . . ?
O3 C53 C54 108.1(3) . . ?
O3A C53 C54 99.7(10) . . ?
C53 O3 C56 109.3(4) . . ?
C56 C55 C54 103.9(4) . . ?
O3 C56 C55 109.2(4) . . ?
O3A C56 C55 94.7(12) . . ?
O4A C60 C59 105.3(11) . . ?
C59 C60 O4 106.1(7) . . ?
O5 C61 C62 104.7(4) . . ?
O5 C61 C64 45.1(4) . . ?
C62 C61 C64 80.3(3) . . ?
C57 O4 C60 107.8(9) . . ?
C60 C59 C58 106.2(7) . . ?
C59 C58 C57 103.9(6) . . ?
O4 C57 C58 107.6(7) . . ?
O4A C57 C58 103.0(10) . . ?
C63 C62 C61 98.6(4) . . ?
C64 C63 C62 99.4(4) . . ?
C64 O5 C61 89.3(7) . . ?
O5 C64 C63 108.7(4) . . ?
O5 C64 C61 45.7(4) . . ?
C63 C64 C61 81.3(3) . . ?
C65 C66 O6 121.3(5) . . ?
C65 C66 C65 92.9(5) . 2_776 ?
O6 C66 C65 38.2(3) . 2_776 ?
C65 O6 C66 95.2(6) 2_776 . ?
O6 C65 C66 121.9(7) 2_776 . ?
O6 C65 C66 46.6(5) 2_776 2_776 ?
C66 C65 C66 87.1(5) . 2_776 ?
C60 O4A C57 112.2(14) . . ?
C56 O3A C53 104.5(14) . . ?

_refine_diff_density_max         0.674
_refine_diff_density_min         -0.738
_refine_diff_density_rms         0.065

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

data_compound_4-tBu
_database_code_depnum_ccdc_archive 'CCDC 1579159'
_audit_update_record             
;
2017-10-10 deposited with the CCDC.
2018-02-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C27 H49 B Cl N5'
_chemical_formula_sum            'C27 H49 B Cl N5'
_chemical_formula_weight         489.97

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   13.7173(2)
_cell_length_b                   15.3059(2)
_cell_length_c                   15.7157(2)
_cell_angle_alpha                90
_cell_angle_beta                 110.275(2)
_cell_angle_gamma                90
_cell_volume                     3095.16(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    6817
_cell_measurement_theta_min      2.8540
_cell_measurement_theta_max      73.3560

_exptl_crystal_description       rod
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.051
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.132
_exptl_absorpt_coefficient_mu    1.241
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.75453
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43c (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.5435
_diffrn_reflns_number            12159
_diffrn_reflns_av_unetI/netI     0.0206
_diffrn_reflns_av_R_equivalents  0.0177
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         6.476
_diffrn_reflns_theta_max         69.995
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             5837
_reflns_number_gt                5160
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'CrysAlisPro 1.171.38.43c (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43c (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43c (Rigaku OD, 2015)'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0584P)²+0.9889P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5837
_refine_ls_number_parameters     322
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0468
_refine_ls_R_factor_gt           0.0409
_refine_ls_wR_factor_ref         0.1198
_refine_ls_wR_factor_gt          0.1096
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_restrained_S_all      1.065
_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
Cl1 Cl 0.45276(4) 0.78341(3) 0.17166(3) 0.04885(14) Uani 1 1 d . . . . .
N3 N 0.62121(8) 0.20689(7) 0.16144(7) 0.0259(2) Uani 1 1 d . . . . .
N5 N 0.44374(10) 0.41401(8) 0.22108(8) 0.0342(3) Uani 1 1 d . . . . .
N2 N 0.65158(9) 0.22169(8) 0.44458(8) 0.0330(3) Uani 1 1 d . . . . .
N1 N 0.48907(9) 0.24307(7) 0.42504(8) 0.0270(2) Uani 1 1 d . . . . .
C1 C 0.55844(10) 0.24191(8) 0.38132(9) 0.0251(3) Uani 1 1 d . . . . .
N4 N 0.54040(9) 0.10794(8) 0.21000(8) 0.0292(3) Uani 1 1 d . . . . .
C12 C 0.56539(10) 0.19410(9) 0.21664(9) 0.0249(3) Uani 1 1 d . . . . .
C23 C 0.49276(10) 0.34663(9) 0.24616(9) 0.0271(3) Uani 1 1 d . . . . .
C3 C 0.53915(12) 0.22432(10) 0.51654(10) 0.0347(3) Uani 1 1 d . . . . .
C2 C 0.64056(13) 0.21053(11) 0.52859(10) 0.0402(4) Uani 1 1 d . . . . .
B1 B 0.53696(11) 0.26287(10) 0.27826(10) 0.0254(3) Uani 1 1 d . . . . .
C7 C 0.37643(11) 0.25959(10) 0.37765(10) 0.0335(3) Uani 1 1 d . . . . .
H7 H 0.365500 0.262271 0.311401 0.040 Uiso 1 1 calc R U . . .
C15 C 0.66537(11) 0.29302(10) 0.15260(10) 0.0336(3) Uani 1 1 d . . . . .
H15 H 0.655154 0.331437 0.200290 0.040 Uiso 1 1 calc R U . . .
C13 C 0.63113(11) 0.12886(10) 0.11970(9) 0.0300(3) Uani 1 1 d . . . . .
C21 C 0.68466(13) 0.11830(11) 0.05233(10) 0.0397(4) Uani 1 1 d . . . . .
H21A H 0.678370 0.057556 0.031398 0.060 Uiso 1 1 calc R U . . .
H21B H 0.758302 0.133351 0.080816 0.060 Uiso 1 1 calc R U . . .
H21C H 0.652491 0.157050 0.000530 0.060 Uiso 1 1 calc R U . . .
C14 C 0.58167(12) 0.06644(10) 0.15091(10) 0.0328(3) Uani 1 1 d . . . . .
C18 C 0.46705(12) 0.07030(10) 0.25077(10) 0.0343(3) Uani 1 1 d . . . . .
H18 H 0.444024 0.119580 0.281076 0.041 Uiso 1 1 calc R U . . .
C4 C 0.74894(11) 0.22084(12) 0.42326(12) 0.0418(4) Uani 1 1 d . . . . .
H4 H 0.729144 0.238412 0.358168 0.050 Uiso 1 1 calc R U . . .
C9 C 0.34409(14) 0.34795(11) 0.40289(14) 0.0490(4) Uani 1 1 d . . . . .
H9A H 0.357448 0.349730 0.468294 0.073 Uiso 1 1 calc R U . . .
H9B H 0.269813 0.357101 0.369888 0.073 Uiso 1 1 calc R U . . .
H9C H 0.384127 0.394063 0.386764 0.073 Uiso 1 1 calc R U . . .
C11 C 0.48741(16) 0.22136(13) 0.58571(12) 0.0501(4) Uani 1 1 d . . . . .
H11A H 0.440398 0.171041 0.573848 0.075 Uiso 1 1 calc R U . . .
H11B H 0.447631 0.275212 0.582446 0.075 Uiso 1 1 calc R U . . .
H11C H 0.540183 0.215872 0.646316 0.075 Uiso 1 1 calc R U . . .
C24 C 0.48693(13) 0.50439(10) 0.22496(11) 0.0397(4) Uani 1 1 d . . . . .
C26 C 0.44330(16) 0.54063(11) 0.12922(12) 0.0511(4) Uani 1 1 d . . . . .
H26A H 0.471917 0.507814 0.089734 0.077 Uiso 1 1 calc R U . . .
H26B H 0.462391 0.602369 0.129608 0.077 Uiso 1 1 calc R U . . .
H26C H 0.367418 0.535110 0.106523 0.077 Uiso 1 1 calc R U . . .
C5 C 0.82696(14) 0.28790(13) 0.47748(15) 0.0537(5) Uani 1 1 d . . . . .
H5A H 0.792380 0.344506 0.473911 0.081 Uiso 1 1 calc R U . . .
H5B H 0.883093 0.293361 0.452646 0.081 Uiso 1 1 calc R U . . .
H5C H 0.855910 0.269234 0.540974 0.081 Uiso 1 1 calc R U . . .
C22 C 0.57540(16) -0.02896(11) 0.13076(13) 0.0484(4) Uani 1 1 d . . . . .
H22A H 0.542590 -0.038011 0.065258 0.073 Uiso 1 1 calc R U . . .
H22B H 0.533927 -0.057725 0.162389 0.073 Uiso 1 1 calc R U . . .
H22C H 0.645547 -0.053889 0.151392 0.073 Uiso 1 1 calc R U . . .
C8 C 0.30951(13) 0.18471(12) 0.38992(13) 0.0469(4) Uani 1 1 d . . . . .
H8A H 0.336336 0.129281 0.375862 0.070 Uiso 1 1 calc R U . . .
H8B H 0.237718 0.192917 0.348971 0.070 Uiso 1 1 calc R U . . .
H8C H 0.311373 0.183724 0.452811 0.070 Uiso 1 1 calc R U . . .
C20 C 0.37004(14) 0.03412(13) 0.17949(13) 0.0527(5) Uani 1 1 d . . . . .
H20A H 0.343408 0.076579 0.130171 0.079 Uiso 1 1 calc R U . . .
H20B H 0.317056 0.022986 0.206932 0.079 Uiso 1 1 calc R U . . .
H20C H 0.386953 -0.020584 0.155316 0.079 Uiso 1 1 calc R U . . .
C27 C 0.4454(2) 0.55654(12) 0.28708(14) 0.0628(6) Uani 1 1 d . . . . .
H27A H 0.369836 0.549245 0.267755 0.094 Uiso 1 1 calc R U . . .
H27B H 0.461955 0.618492 0.284110 0.094 Uiso 1 1 calc R U . . .
H27C H 0.477504 0.535573 0.349523 0.094 Uiso 1 1 calc R U . . .
C19 C 0.51805(16) 0.00375(14) 0.32377(13) 0.0547(5) Uani 1 1 d . . . . .
H19A H 0.535497 -0.048568 0.296065 0.082 Uiso 1 1 calc R U . . .
H19B H 0.470095 -0.011975 0.355226 0.082 Uiso 1 1 calc R U . . .
H19C H 0.581592 0.028681 0.367320 0.082 Uiso 1 1 calc R U . . .
C16 C 0.78129(16) 0.28867(17) 0.1720(2) 0.0783(8) Uani 1 1 d . . . . .
H16A H 0.814744 0.256619 0.228589 0.117 Uiso 1 1 calc R U . . .
H16B H 0.809646 0.348022 0.177778 0.117 Uiso 1 1 calc R U . . .
H16C H 0.794541 0.258534 0.122018 0.117 Uiso 1 1 calc R U . . .
C17 C 0.60490(19) 0.33420(12) 0.06215(12) 0.0581(5) Uani 1 1 d . . . . .
H17A H 0.610118 0.297187 0.013025 0.087 Uiso 1 1 calc R U . . .
H17B H 0.633635 0.392086 0.058301 0.087 Uiso 1 1 calc R U . . .
H17C H 0.531778 0.340017 0.056526 0.087 Uiso 1 1 calc R U . . .
C25 C 0.60509(15) 0.50586(13) 0.25767(15) 0.0608(5) Uani 1 1 d . . . . .
H25A H 0.632943 0.477159 0.316962 0.091 Uiso 1 1 calc R U . . .
H25B H 0.629354 0.566523 0.263094 0.091 Uiso 1 1 calc R U . . .
H25C H 0.629098 0.474853 0.214042 0.091 Uiso 1 1 calc R U . . .
C6 C 0.79494(15) 0.13056(14) 0.4305(2) 0.0723(7) Uani 1 1 d . . . . .
H6A H 0.816795 0.110735 0.493605 0.108 Uiso 1 1 calc R U . . .
H6B H 0.855217 0.131979 0.410613 0.108 Uiso 1 1 calc R U . . .
H6C H 0.742710 0.090268 0.391871 0.108 Uiso 1 1 calc R U . . .
C10 C 0.72600(17) 0.18722(19) 0.61493(13) 0.0722(7) Uani 1 1 d . . . . .
H10A H 0.697121 0.179398 0.663392 0.108 Uiso 1 1 calc R U . . .
H10B H 0.777709 0.234220 0.631508 0.108 Uiso 1 1 calc R U . . .
H10C H 0.759106 0.132789 0.606422 0.108 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N3 C12 1.3556(17) . ?
N3 C13 1.3918(18) . ?
N3 C15 1.4773(17) . ?
N5 C23 1.2196(18) . ?
N5 C24 1.4978(18) . ?
N2 C1 1.3551(17) . ?
N2 C2 1.390(2) . ?
N2 C4 1.4853(19) . ?
N1 C1 1.3532(17) . ?
N1 C3 1.3918(18) . ?
N1 C7 1.4861(18) . ?
C1 B1 1.5754(19) . ?
N4 C12 1.3574(18) . ?
N4 C14 1.3968(18) . ?
N4 C18 1.4837(17) . ?
C12 B1 1.568(2) . ?
C23 B1 1.433(2) . ?
C3 C2 1.354(2) . ?
C3 C11 1.491(2) . ?
C2 C10 1.497(2) . ?
C7 C9 1.518(2) . ?
C7 C8 1.522(2) . ?
C15 C17 1.513(2) . ?
C15 C16 1.513(2) . ?
C13 C14 1.358(2) . ?
C13 C21 1.4917(19) . ?
C14 C22 1.490(2) . ?
C18 C19 1.512(2) . ?
C18 C20 1.516(2) . ?
C4 C6 1.507(3) . ?
C4 C5 1.514(2) . ?
C24 C27 1.517(3) . ?
C24 C26 1.518(2) . ?
C24 C25 1.521(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C12 N3 C13 110.29(11) . . ?
C12 N3 C15 122.01(11) . . ?
C13 N3 C15 127.68(11) . . ?
C23 N5 C24 127.00(13) . . ?
C1 N2 C2 109.86(12) . . ?
C1 N2 C4 121.96(12) . . ?
C2 N2 C4 127.97(13) . . ?
C1 N1 C3 109.86(12) . . ?
C1 N1 C7 122.66(11) . . ?
C3 N1 C7 127.45(12) . . ?
N1 C1 N2 106.29(11) . . ?
N1 C1 B1 127.26(12) . . ?
N2 C1 B1 126.42(12) . . ?
C12 N4 C14 110.07(11) . . ?
C12 N4 C18 122.35(11) . . ?
C14 N4 C18 127.03(12) . . ?
N3 C12 N4 105.95(11) . . ?
N3 C12 B1 127.93(12) . . ?
N4 C12 B1 126.10(11) . . ?
N5 C23 B1 171.44(14) . . ?
C2 C3 N1 106.98(13) . . ?
C2 C3 C11 128.24(15) . . ?
N1 C3 C11 124.78(15) . . ?
C3 C2 N2 107.01(13) . . ?
C3 C2 C10 127.44(16) . . ?
N2 C2 C10 125.56(16) . . ?
C23 B1 C12 123.26(12) . . ?
C23 B1 C1 116.72(12) . . ?
C12 B1 C1 120.01(12) . . ?
N1 C7 C9 111.58(13) . . ?
N1 C7 C8 112.11(12) . . ?
C9 C7 C8 113.21(13) . . ?
N3 C15 C17 110.55(13) . . ?
N3 C15 C16 112.23(15) . . ?
C17 C15 C16 113.77(17) . . ?
C14 C13 N3 106.91(11) . . ?
C14 C13 C21 127.63(14) . . ?
N3 C13 C21 125.45(13) . . ?
C13 C14 N4 106.77(12) . . ?
C13 C14 C22 127.73(13) . . ?
N4 C14 C22 125.45(13) . . ?
N4 C18 C19 112.61(13) . . ?
N4 C18 C20 112.07(13) . . ?
C19 C18 C20 111.80(14) . . ?
N2 C4 C6 112.14(15) . . ?
N2 C4 C5 112.49(14) . . ?
C6 C4 C5 112.54(15) . . ?
N5 C24 C27 106.30(14) . . ?
N5 C24 C26 106.42(13) . . ?
C27 C24 C26 109.79(15) . . ?
N5 C24 C25 112.80(13) . . ?
C27 C24 C25 111.63(17) . . ?
C26 C24 C25 109.72(15) . . ?

_refine_diff_density_max         0.296
_refine_diff_density_min         -0.354
_refine_diff_density_rms         0.039

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

data_compound_4-Cy
_database_code_depnum_ccdc_archive 'CCDC 1579158'
_audit_update_record             
;
2017-10-10 deposited with the CCDC.
2018-02-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C33 H59 B Cl N5 O'
_chemical_formula_sum            'C33 H59 B Cl N5 O'
_chemical_formula_weight         588.11

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'

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

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

_cell_length_a                   15.6878(2)
_cell_length_b                   12.34570(10)
_cell_length_c                   36.8495(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     7136.90(14)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    8513
_cell_measurement_theta_min      2.3760
_cell_measurement_theta_max      73.4970

_exptl_crystal_description       rod
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.095
_exptl_crystal_F_000             2576
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    1.172
_shelx_estimated_absorpt_T_min   0.727
_shelx_estimated_absorpt_T_max   0.872
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.52737
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43c (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.5435
_diffrn_reflns_number            27357
_diffrn_reflns_av_unetI/netI     0.0267
_diffrn_reflns_av_R_equivalents  0.0372
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_theta_min         6.627
_diffrn_reflns_theta_max         69.998
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             6743
_reflns_number_gt                5544
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'CrysAlisPro 1.171.38.43c (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43c (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43c (Rigaku OD, 2015)'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1134P)²+3.7558P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6743
_refine_ls_number_parameters     415
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0765
_refine_ls_R_factor_gt           0.0650
_refine_ls_wR_factor_ref         0.1974
_refine_ls_wR_factor_gt          0.1842
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.028
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl1 Cl 0.42445(4) 0.17963(5) 0.06359(2) 0.0576(2) Uani 1 1 d . . . . .
N1 N -0.21079(11) 0.19030(13) 0.07971(5) 0.0318(4) Uani 1 1 d . . . . .
N2 N -0.24297(11) 0.14184(14) 0.13459(5) 0.0324(4) Uani 1 1 d . . . . .
N3 N 0.05490(11) 0.22925(14) 0.08774(5) 0.0356(4) Uani 1 1 d . . . . .
N4 N 0.01869(11) 0.06403(14) 0.10093(5) 0.0355(4) Uani 1 1 d . . . . .
C12 C -0.00498(13) 0.16901(17) 0.10486(6) 0.0338(4) Uani 1 1 d . . . . .
C1 C -0.17856(13) 0.18143(15) 0.11381(5) 0.0308(4) Uani 1 1 d . . . . .
C2 C -0.29537(14) 0.15752(16) 0.07912(6) 0.0345(4) Uani 1 1 d . . . . .
C14 C 0.09477(14) 0.05804(19) 0.08155(6) 0.0390(5) Uani 1 1 d . . . . .
C7 C -0.23116(14) 0.11191(19) 0.17322(6) 0.0397(5) Uani 1 1 d . . . . .
H7 H -0.169210 0.122060 0.178640 0.048 Uiso 1 1 calc R U . . .
C13 C 0.11793(14) 0.16137(19) 0.07354(6) 0.0391(5) Uani 1 1 d . . . . .
C3 C -0.31615(14) 0.12741(17) 0.11355(6) 0.0361(5) Uani 1 1 d . . . . .
C4 C -0.16173(15) 0.23982(18) 0.04947(6) 0.0387(5) Uani 1 1 d . . . . .
H4 H -0.102186 0.249574 0.058588 0.046 Uiso 1 1 calc R U . . .
C15 C 0.04918(16) 0.34901(18) 0.08432(6) 0.0413(5) Uani 1 1 d . . . . .
H15 H -0.009079 0.369661 0.092881 0.050 Uiso 1 1 calc R U . . .
B1 B -0.08561(15) 0.2117(2) 0.12626(7) 0.0340(5) Uani 1 1 d . . . . .
C21 C 0.19659(16) 0.1983(2) 0.05427(8) 0.0540(6) Uani 1 1 d . . . . .
H21A H 0.240141 0.141506 0.055630 0.081 Uiso 1 1 calc R U . . .
H21B H 0.218133 0.264413 0.065763 0.081 Uiso 1 1 calc R U . . .
H21C H 0.183066 0.213078 0.028785 0.081 Uiso 1 1 calc R U . . .
C18 C -0.03203(16) -0.02577(19) 0.11671(7) 0.0460(6) Uani 1 1 d . . . . .
H18 H -0.073800 0.008699 0.133648 0.055 Uiso 1 1 calc R U . . .
C6 C -0.19481(18) 0.35249(19) 0.04056(7) 0.0468(6) Uani 1 1 d . . . . .
H6A H -0.254239 0.347589 0.032529 0.070 Uiso 1 1 calc R U . . .
H6B H -0.160094 0.384217 0.021168 0.070 Uiso 1 1 calc R U . . .
H6C H -0.191414 0.398296 0.062229 0.070 Uiso 1 1 calc R U . . .
C17 C 0.0553(2) 0.3861(2) 0.04479(7) 0.0562(7) Uani 1 1 d . . . . .
H17A H 0.114006 0.376951 0.036177 0.084 Uiso 1 1 calc R U . . .
H17B H 0.039148 0.462572 0.043076 0.084 Uiso 1 1 calc R U . . .
H17C H 0.016820 0.342453 0.029802 0.084 Uiso 1 1 calc R U . . .
C10 C -0.35156(16) 0.15495(19) 0.04636(7) 0.0438(5) Uani 1 1 d . . . . .
H10A H -0.334973 0.094204 0.030762 0.066 Uiso 1 1 calc R U . . .
H10B H -0.345506 0.222980 0.032901 0.066 Uiso 1 1 calc R U . . .
H10C H -0.411014 0.145972 0.053941 0.066 Uiso 1 1 calc R U . . .
C8 C -0.25010(18) -0.0074(2) 0.17927(8) 0.0563(7) Uani 1 1 d . . . . .
H8A H -0.311822 -0.019343 0.178340 0.084 Uiso 1 1 calc R U . . .
H8B H -0.228376 -0.029538 0.203085 0.084 Uiso 1 1 calc R U . . .
H8C H -0.222309 -0.050435 0.160302 0.084 Uiso 1 1 calc R U . . .
C16 C 0.11164(19) 0.4054(2) 0.10935(8) 0.0553(7) Uani 1 1 d . . . . .
H16A H 0.100079 0.384205 0.134501 0.083 Uiso 1 1 calc R U . . .
H16B H 0.105313 0.484035 0.106888 0.083 Uiso 1 1 calc R U . . .
H16C H 0.169928 0.384455 0.102850 0.083 Uiso 1 1 calc R U . . .
C11 C -0.39985(15) 0.0873(2) 0.12713(8) 0.0513(6) Uani 1 1 d . . . . .
H11A H -0.444143 0.102558 0.109082 0.077 Uiso 1 1 calc R U . . .
H11B H -0.413936 0.123964 0.149939 0.077 Uiso 1 1 calc R U . . .
H11C H -0.396523 0.009016 0.131284 0.077 Uiso 1 1 calc R U . . .
C9 C -0.27887(19) 0.1863(3) 0.19857(7) 0.0584(7) Uani 1 1 d . . . . .
H9A H -0.265135 0.261721 0.192728 0.088 Uiso 1 1 calc R U . . .
H9B H -0.262167 0.170830 0.223666 0.088 Uiso 1 1 calc R U . . .
H9C H -0.340309 0.174570 0.195777 0.088 Uiso 1 1 calc R U . . .
C22 C 0.14125(18) -0.0438(2) 0.07300(8) 0.0529(6) Uani 1 1 d . . . . .
H22A H 0.184524 -0.029385 0.054445 0.079 Uiso 1 1 calc R U . . .
H22B H 0.100917 -0.098058 0.063921 0.079 Uiso 1 1 calc R U . . .
H22C H 0.168929 -0.071194 0.095013 0.079 Uiso 1 1 calc R U . . .
C19 C -0.08385(19) -0.0819(2) 0.08826(9) 0.0599(7) Uani 1 1 d . . . . .
H19A H -0.118273 -0.028449 0.075144 0.090 Uiso 1 1 calc R U . . .
H19B H -0.121457 -0.135082 0.099800 0.090 Uiso 1 1 calc R U . . .
H19C H -0.045741 -0.118838 0.071210 0.090 Uiso 1 1 calc R U . . .
C5 C -0.1556(2) 0.1661(2) 0.01676(7) 0.0544(7) Uani 1 1 d . . . . .
H5A H -0.129557 0.097227 0.023927 0.082 Uiso 1 1 calc R U . . .
H5B H -0.120568 0.200707 -0.001948 0.082 Uiso 1 1 calc R U . . .
H5C H -0.212887 0.152631 0.007105 0.082 Uiso 1 1 calc R U . . .
C20 C 0.0206(2) -0.1026(2) 0.13950(9) 0.0621(7) Uani 1 1 d . . . . .
H20A H 0.054058 -0.149860 0.123573 0.093 Uiso 1 1 calc R U . . .
H20B H -0.017214 -0.146696 0.154626 0.093 Uiso 1 1 calc R U . . .
H20C H 0.059219 -0.060858 0.155071 0.093 Uiso 1 1 calc R U . . .
C23 C -0.07297(16) 0.2809(3) 0.15806(7) 0.0350(6) Uani 0.845(4) 1 d . . P A 1
N5 N -0.06179(15) 0.3432(2) 0.18346(6) 0.0424(6) Uani 0.845(4) 1 d . . P A 1
C24 C -0.0505(2) 0.3017(3) 0.22148(8) 0.0536(8) Uani 0.845(4) 1 d . . P A 1
H24 H -0.084246 0.233562 0.224563 0.064 Uiso 0.845(4) 1 calc R U P A 1
C25 C -0.0840(3) 0.3876(5) 0.24769(12) 0.0653(13) Uani 0.845(4) 1 d . . P A 1
H25A H -0.142779 0.407400 0.240538 0.078 Uiso 0.845(4) 1 calc R U P A 1
H25B H -0.086467 0.356285 0.272395 0.078 Uiso 0.845(4) 1 calc R U P A 1
C29 C 0.0431(3) 0.2779(3) 0.22843(10) 0.0683(11) Uani 0.845(4) 1 d . . P A 1
H29A H 0.064813 0.229455 0.209133 0.082 Uiso 0.845(4) 1 calc R U P A 1
H29B H 0.048875 0.239592 0.251904 0.082 Uiso 0.845(4) 1 calc R U P A 1
C28 C 0.0967(3) 0.3806(4) 0.22932(13) 0.0758(12) Uani 0.845(4) 1 d . . P A 1
H28A H 0.097651 0.413516 0.204829 0.091 Uiso 0.845(4) 1 calc R U P A 1
H28B H 0.155982 0.361945 0.236036 0.091 Uiso 0.845(4) 1 calc R U P A 1
C26 C -0.0314(3) 0.4865(4) 0.24865(13) 0.0759(12) Uani 0.845(4) 1 d . . P A 1
H26A H -0.054608 0.536347 0.267237 0.091 Uiso 0.845(4) 1 calc R U P A 1
H26B H -0.035213 0.523378 0.224844 0.091 Uiso 0.845(4) 1 calc R U P A 1
C27 C 0.0606(3) 0.4642(4) 0.25705(15) 0.0833(14) Uani 0.845(4) 1 d . . P A 1
H27A H 0.065909 0.435186 0.281985 0.100 Uiso 0.845(4) 1 calc R U P A 1
H27B H 0.093757 0.532363 0.255633 0.100 Uiso 0.845(4) 1 calc R U P A 1
O1 O -0.1904(3) 0.1350(4) 0.29081(11) 0.1524(17) Uani 1 1 d . . . . .
C30 C -0.2764(4) 0.1230(6) 0.34094(15) 0.137(2) Uani 1 1 d . . . . .
H30A H -0.269971 0.061913 0.358126 0.164 Uiso 1 1 calc R U . . .
H30B H -0.333030 0.156652 0.344530 0.164 Uiso 1 1 calc R U . . .
C31 C -0.2063(4) 0.2048(6) 0.34602(17) 0.145(2) Uani 1 1 d . . . . .
H31A H -0.225966 0.278809 0.339903 0.174 Uiso 1 1 calc R U . . .
H31B H -0.184571 0.204220 0.371249 0.174 Uiso 1 1 calc R U . . .
C32 C -0.1430(4) 0.1683(6) 0.32111(17) 0.132(2) Uani 1 1 d . . . . .
H32A H -0.103289 0.227544 0.314647 0.158 Uiso 1 1 calc R U . . .
H32B H -0.109983 0.107211 0.331394 0.158 Uiso 1 1 calc R U . . .
C33 C -0.2659(4) 0.0872(5) 0.30414(17) 0.1240(18) Uani 1 1 d . . . . .
H33A H -0.261489 0.007265 0.303240 0.149 Uiso 1 1 calc R U . . .
H33B H -0.315327 0.109867 0.289261 0.149 Uiso 1 1 calc R U . . .
N5A N -0.0379(7) 0.2444(9) 0.1916(3) 0.034(3) Uiso 0.155(4) 1 d . . P A 2
C23A C -0.0624(8) 0.2314(14) 0.1601(3) 0.023(3) Uiso 0.155(4) 1 d . . P A 2
C24A C -0.0188(7) 0.3501(10) 0.2077(3) 0.026(3) Uiso 0.155(4) 1 d D . P A 2
H24A H -0.032497 0.410743 0.190658 0.031 Uiso 0.155(4) 1 calc R U P A 2
C29A C 0.0746(9) 0.3451(14) 0.2159(4) 0.042(4) Uiso 0.155(4) 1 d D . P A 2
H29C H 0.107482 0.337429 0.193104 0.051 Uiso 0.155(4) 1 calc R U P A 2
H29D H 0.086988 0.281761 0.231511 0.051 Uiso 0.155(4) 1 calc R U P A 2
C27A C 0.0514(14) 0.451(3) 0.2732(6) 0.092(11) Uiso 0.155(4) 1 d D . P A 2
H27C H 0.065214 0.382950 0.286419 0.110 Uiso 0.155(4) 1 calc R U P A 2
H27D H 0.067997 0.512807 0.288647 0.110 Uiso 0.155(4) 1 calc R U P A 2
C28A C 0.1011(10) 0.455(2) 0.2363(7) 0.090(8) Uiso 0.155(4) 1 d D . P A 2
H28C H 0.163398 0.456994 0.240450 0.108 Uiso 0.155(4) 1 calc R U P A 2
H28D H 0.084160 0.518760 0.221885 0.108 Uiso 0.155(4) 1 calc R U P A 2
C25A C -0.0719(8) 0.3573(15) 0.2430(5) 0.032(5) Uiso 0.155(4) 1 d D . P A 2
H25C H -0.133150 0.363746 0.236969 0.038 Uiso 0.155(4) 1 calc R U P A 2
H25D H -0.063846 0.290530 0.257513 0.038 Uiso 0.155(4) 1 calc R U P A 2
C26A C -0.0439(13) 0.455(2) 0.2650(5) 0.075(7) Uiso 0.155(4) 1 d D . P A 2
H26C H -0.076179 0.457388 0.288111 0.091 Uiso 0.155(4) 1 calc R U P A 2
H26D H -0.056806 0.522129 0.251344 0.091 Uiso 0.155(4) 1 calc R U P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C1 1.359(3) . ?
N1 C2 1.387(3) . ?
N1 C4 1.486(3) . ?
N2 C1 1.359(3) . ?
N2 C3 1.397(3) . ?
N2 C7 1.482(3) . ?
N3 C12 1.354(3) . ?
N3 C13 1.398(3) . ?
N3 C15 1.487(3) . ?
N4 C12 1.356(3) . ?
N4 C14 1.393(3) . ?
N4 C18 1.483(3) . ?
C12 B1 1.581(3) . ?
C1 B1 1.574(3) . ?
C2 C3 1.362(3) . ?
C2 C10 1.495(3) . ?
C14 C13 1.359(3) . ?
C14 C22 1.488(3) . ?
C7 C9 1.509(4) . ?
C7 C8 1.520(3) . ?
C13 C21 1.495(3) . ?
C3 C11 1.490(3) . ?
C4 C5 1.513(3) . ?
C4 C6 1.521(3) . ?
C15 C16 1.515(4) . ?
C15 C17 1.530(3) . ?
B1 C23A 1.322(13) . ?
B1 C23 1.464(4) . ?
C18 C19 1.497(4) . ?
C18 C20 1.512(4) . ?
C23 N5 1.224(4) . ?
N5 C24 1.502(4) . ?
C24 C29 1.519(5) . ?
C24 C25 1.528(6) . ?
C25 C26 1.474(7) . ?
C29 C28 1.521(7) . ?
C28 C27 1.559(8) . ?
C26 C27 1.502(7) . ?
O1 C32 1.404(7) . ?
O1 C33 1.411(7) . ?
C30 C33 1.436(7) . ?
C30 C31 1.505(8) . ?
C31 C32 1.426(8) . ?
N5A C23A 1.234(17) . ?
N5A C24A 1.464(15) . ?
C24A C29A 1.497(18) . ?
C24A C25A 1.549(18) . ?
C29A C28A 1.60(2) . ?
C27A C26A 1.53(3) . ?
C27A C28A 1.57(3) . ?
C25A C26A 1.52(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 N1 C2 110.28(17) . . ?
C1 N1 C4 122.27(18) . . ?
C2 N1 C4 127.14(18) . . ?
C1 N2 C3 110.16(17) . . ?
C1 N2 C7 122.53(17) . . ?
C3 N2 C7 127.15(17) . . ?
C12 N3 C13 109.62(18) . . ?
C12 N3 C15 122.96(18) . . ?
C13 N3 C15 127.38(18) . . ?
C12 N4 C14 109.89(18) . . ?
C12 N4 C18 121.70(18) . . ?
C14 N4 C18 128.39(19) . . ?
N3 C12 N4 106.57(18) . . ?
N3 C12 B1 127.19(19) . . ?
N4 C12 B1 126.21(18) . . ?
N2 C1 N1 105.86(17) . . ?
N2 C1 B1 127.62(18) . . ?
N1 C1 B1 126.52(18) . . ?
C3 C2 N1 107.10(18) . . ?
C3 C2 C10 127.3(2) . . ?
N1 C2 C10 125.6(2) . . ?
C13 C14 N4 106.89(19) . . ?
C13 C14 C22 128.1(2) . . ?
N4 C14 C22 125.0(2) . . ?
N2 C7 C9 112.4(2) . . ?
N2 C7 C8 111.0(2) . . ?
C9 C7 C8 113.7(2) . . ?
C14 C13 N3 107.00(19) . . ?
C14 C13 C21 127.6(2) . . ?
N3 C13 C21 125.4(2) . . ?
C2 C3 N2 106.59(18) . . ?
C2 C3 C11 127.9(2) . . ?
N2 C3 C11 125.5(2) . . ?
N1 C4 C5 112.49(19) . . ?
N1 C4 C6 111.20(18) . . ?
C5 C4 C6 113.56(19) . . ?
N3 C15 C16 111.5(2) . . ?
N3 C15 C17 112.0(2) . . ?
C16 C15 C17 113.7(2) . . ?
C23A B1 C1 125.1(6) . . ?
C23 B1 C1 119.8(2) . . ?
C23A B1 C12 108.1(6) . . ?
C23 B1 C12 119.0(2) . . ?
C1 B1 C12 121.15(19) . . ?
N4 C18 C19 111.3(2) . . ?
N4 C18 C20 113.1(2) . . ?
C19 C18 C20 113.3(2) . . ?
N5 C23 B1 176.7(3) . . ?
C23 N5 C24 121.0(3) . . ?
N5 C24 C29 109.7(3) . . ?
N5 C24 C25 108.2(3) . . ?
C29 C24 C25 111.1(3) . . ?
C26 C25 C24 113.5(4) . . ?
C24 C29 C28 112.1(3) . . ?
C29 C28 C27 111.4(4) . . ?
C25 C26 C27 113.0(4) . . ?
C26 C27 C28 109.6(3) . . ?
C32 O1 C33 106.9(4) . . ?
C33 C30 C31 103.9(4) . . ?
C32 C31 C30 102.5(5) . . ?
O1 C32 C31 103.6(5) . . ?
O1 C33 C30 107.2(4) . . ?
C23A N5A C24A 124.1(12) . . ?
N5A C23A B1 176.3(16) . . ?
N5A C24A C29A 104.2(10) . . ?
N5A C24A C25A 106.3(11) . . ?
C29A C24A C25A 111.0(10) . . ?
C24A C29A C28A 108.3(12) . . ?
C26A C27A C28A 108.3(16) . . ?
C27A C28A C29A 104.6(15) . . ?
C26A C25A C24A 109.8(12) . . ?
C25A C26A C27A 111.1(15) . . ?

_refine_diff_density_max         0.736
_refine_diff_density_min         -0.551
_refine_diff_density_rms         0.054

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

data_compound_2-Bz
_database_code_depnum_ccdc_archive 'CCDC 1579155'
_audit_update_record             
;
2017-10-10 deposited with the CCDC.
2018-02-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C51 H78 B Cl N6 Ni O2 Si2'
_chemical_formula_sum            'C51 H78 B Cl N6 Ni O2 Si2'
_chemical_formula_weight         968.34

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 '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                   14.0633(7)
_cell_length_b                   26.4632(11)
_cell_length_c                   18.1718(10)
_cell_angle_alpha                90
_cell_angle_beta                 100.801(5)
_cell_angle_gamma                90
_cell_volume                     6643.0(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    2007
_cell_measurement_theta_min      3.1790
_cell_measurement_theta_max      50.0470

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    0.968
_exptl_crystal_F_000             2080
_exptl_crystal_size_max          0.162
_exptl_crystal_size_mid          0.092
_exptl_crystal_size_min          0.063
_exptl_absorpt_coefficient_mu    1.401
_shelx_estimated_absorpt_T_min   0.805
_shelx_estimated_absorpt_T_max   0.917
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.08011
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43c (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.5435
_diffrn_reflns_number            46775
_diffrn_reflns_av_unetI/netI     0.2691
_diffrn_reflns_av_R_equivalents  0.2168
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         6.332
_diffrn_reflns_theta_max         67.497
_diffrn_reflns_theta_full        67.497
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             11947
_reflns_number_gt                3978
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'CrysAlisPro 1.171.38.43c (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43c (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43c (Rigaku OD, 2015)'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0336P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         11947
_refine_ls_number_parameters     598
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1852
_refine_ls_R_factor_gt           0.0929
_refine_ls_wR_factor_ref         0.2240
_refine_ls_wR_factor_gt          0.1819
_refine_ls_goodness_of_fit_ref   0.819
_refine_ls_restrained_S_all      0.819
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.177 0.250 0.594 905 350 ' '
2 0.177 0.750 0.904 905 337 ' '

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
Ni1 Ni 0.54874(8) 0.59078(4) 0.22429(6) 0.0443(3) Uani 1 1 d . . . . .
Cl1 Cl 0.52245(13) 0.64353(6) 0.12640(11) 0.0574(5) Uani 1 1 d . . . . .
Si03 Si 0.70209(13) 0.60767(6) 0.26294(11) 0.0446(5) Uani 1 1 d . . . . .
Si1 Si 0.64984(14) 0.69816(7) 0.35537(12) 0.0509(5) Uani 1 1 d . . . . .
O1 O 0.7644(3) 0.61465(14) 0.1890(2) 0.0440(11) Uani 1 1 d . . . . .
O2 O 0.7783(3) 0.55959(15) 0.3027(3) 0.0464(11) Uani 1 1 d . . . . .
N4 N 0.2990(4) 0.50024(18) 0.2968(3) 0.0459(14) Uani 1 1 d . . . . .
N2 N 0.4850(4) 0.44641(18) 0.1677(3) 0.0489(15) Uani 1 1 d . . . . .
N5 N 0.2724(4) 0.57850(18) 0.2599(3) 0.0387(12) Uani 1 1 d . . . . .
N3 N 0.3692(4) 0.4873(2) 0.0968(3) 0.0518(15) Uani 1 1 d . . . . .
N6 N 0.5374(4) 0.52164(19) 0.3546(3) 0.0494(14) Uani 1 1 d . . . . .
N1 N 0.7328(4) 0.66163(17) 0.3190(3) 0.0443(14) Uani 1 1 d . . . . .
C22 C 0.4283(4) 0.4883(2) 0.1629(4) 0.0430(16) Uani 1 1 d . . . . .
C34 C 0.2146(5) 0.5177(3) 0.3237(4) 0.0525(19) Uani 1 1 d . . . . .
C33 C 0.3315(5) 0.5376(3) 0.2583(4) 0.0513(18) Uani 1 1 d . . . . .
C20 C 0.9078(5) 0.5086(2) 0.2683(4) 0.0470(17) Uani 1 1 d . . . . .
H20 H 0.911229 0.486898 0.310369 0.056 Uiso 1 1 calc R U . . .
C21 C 0.8422(4) 0.5473(2) 0.2576(4) 0.0444(16) Uani 1 1 d . . . . .
C28 C 0.5661(5) 0.4368(2) 0.2298(4) 0.0453(17) Uani 1 1 d . . . . .
H28 H 0.559140 0.460785 0.271025 0.054 Uiso 1 1 calc R U . . .
C45 C 0.6203(5) 0.5314(2) 0.4130(4) 0.058(2) Uani 1 1 d . . . . .
H45A H 0.600258 0.550713 0.454142 0.070 Uiso 1 1 calc R U . . .
H45B H 0.668755 0.551669 0.392724 0.070 Uiso 1 1 calc R U . . .
C1 C 0.8320(5) 0.6778(2) 0.3313(5) 0.054(2) Uani 1 1 d . . . . .
C35 C 0.1996(5) 0.5658(3) 0.3015(5) 0.060(2) Uani 1 1 d . . . . .
C23 C 0.4587(5) 0.4196(2) 0.1002(4) 0.0554(19) Uani 1 1 d . . . . .
C44 C 0.5242(5) 0.5424(2) 0.2899(4) 0.0497(18) Uani 1 1 d . . . . .
C46 C 0.6638(5) 0.4817(2) 0.4419(4) 0.0479(17) Uani 1 1 d . . . . .
C6 C 0.8979(5) 0.6614(2) 0.3989(4) 0.0464(17) Uani 1 1 d . . . . .
C16 C 0.8369(4) 0.5790(2) 0.1925(4) 0.0462(17) Uani 1 1 d . . . . .
C18 C 0.9662(6) 0.5325(3) 0.1547(5) 0.068(2) Uani 1 1 d . . . . .
H18 H 1.007698 0.527424 0.119707 0.081 Uiso 1 1 calc R U . . .
C17 C 0.8970(5) 0.5730(2) 0.1447(4) 0.0568(19) Uani 1 1 d . . . . .
H17 H 0.894210 0.595611 0.103775 0.068 Uiso 1 1 calc R U . . .
C10 C 0.8688(5) 0.6231(3) 0.4541(4) 0.0574(19) Uani 1 1 d . . . . .
H10 H 0.800220 0.613032 0.434397 0.069 Uiso 1 1 calc R U . . .
C36 C 0.3427(5) 0.4487(2) 0.3050(4) 0.057(2) Uani 1 1 d . . . . .
H36 H 0.406587 0.451253 0.288671 0.068 Uiso 1 1 calc R U . . .
C42 C 0.1591(5) 0.4869(3) 0.3727(4) 0.065(2) Uani 1 1 d . . . . .
H42A H 0.188639 0.491655 0.425513 0.098 Uiso 1 1 calc R U . . .
H42B H 0.161591 0.450994 0.359730 0.098 Uiso 1 1 calc R U . . .
H42C H 0.091579 0.498105 0.364285 0.098 Uiso 1 1 calc R U . . .
C39 C 0.2875(5) 0.6279(2) 0.2265(5) 0.063(2) Uani 1 1 d . . . . .
H39 H 0.340591 0.623701 0.197268 0.076 Uiso 1 1 calc R U . . .
C2 C 0.8635(5) 0.7107(2) 0.2814(5) 0.060(2) Uani 1 1 d . . . . .
C4 C 1.0262(5) 0.7144(2) 0.3655(5) 0.059(2) Uani 1 1 d . . . . .
H4 H 1.090259 0.727394 0.376946 0.071 Uiso 1 1 calc R U . . .
C5 C 0.9919(5) 0.6810(2) 0.4132(5) 0.056(2) Uani 1 1 d . . . . .
H5 H 1.034370 0.670899 0.457806 0.068 Uiso 1 1 calc R U . . .
C15 C 0.7163(5) 0.7514(2) 0.4139(4) 0.060(2) Uani 1 1 d . . . . .
H15A H 0.763191 0.737106 0.455373 0.090 Uiso 1 1 calc R U . . .
H15B H 0.669664 0.772373 0.433867 0.090 Uiso 1 1 calc R U . . .
H15C H 0.750433 0.772189 0.382448 0.090 Uiso 1 1 calc R U . . .
C19 C 0.9714(5) 0.5008(3) 0.2163(5) 0.063(2) Uani 1 1 d . . . . .
H19 H 1.017074 0.473947 0.223863 0.075 Uiso 1 1 calc R U . . .
C25 C 0.2936(5) 0.5277(2) 0.0706(4) 0.0529(18) Uani 1 1 d . . . . .
H25 H 0.300163 0.553085 0.112079 0.063 Uiso 1 1 calc R U . . .
C47 C 0.7471(5) 0.4622(2) 0.4177(4) 0.0551(19) Uani 1 1 d . . . . .
H47 H 0.778011 0.481782 0.385175 0.066 Uiso 1 1 calc R U . . .
C29 C 0.5619(5) 0.3832(2) 0.2610(4) 0.059(2) Uani 1 1 d . . . . .
H29A H 0.590949 0.359463 0.230177 0.089 Uiso 1 1 calc R U . . .
H29B H 0.494274 0.373759 0.259988 0.089 Uiso 1 1 calc R U . . .
H29C H 0.597761 0.382083 0.312675 0.089 Uiso 1 1 calc R U . . .
C3 C 0.9631(6) 0.7282(2) 0.3004(5) 0.068(2) Uani 1 1 d . . . . .
H3 H 0.986250 0.750232 0.266365 0.082 Uiso 1 1 calc R U . . .
C24 C 0.3871(6) 0.4435(3) 0.0570(4) 0.063(2) Uani 1 1 d . . . . .
C38 C 0.3631(5) 0.4288(2) 0.3844(4) 0.058(2) Uani 1 1 d . . . . .
H38A H 0.390124 0.455927 0.418757 0.086 Uiso 1 1 calc R U . . .
H38B H 0.409699 0.400920 0.388167 0.086 Uiso 1 1 calc R U . . .
H38C H 0.302818 0.416584 0.397839 0.086 Uiso 1 1 calc R U . . .
C11 C 0.9300(5) 0.5757(3) 0.4582(5) 0.068(2) Uani 1 1 d . . . . .
H11A H 0.996972 0.583763 0.481367 0.102 Uiso 1 1 calc R U . . .
H11B H 0.928211 0.562553 0.407603 0.102 Uiso 1 1 calc R U . . .
H11C H 0.904439 0.550214 0.488455 0.102 Uiso 1 1 calc R U . . .
C43 C 0.1209(5) 0.5990(3) 0.3158(5) 0.062(2) Uani 1 1 d . . . . .
H43A H 0.065741 0.596314 0.274097 0.093 Uiso 1 1 calc R U . . .
H43B H 0.143741 0.634005 0.320439 0.093 Uiso 1 1 calc R U . . .
H43C H 0.100800 0.588604 0.362364 0.093 Uiso 1 1 calc R U . . .
C51 C 0.6161(6) 0.4528(3) 0.4872(4) 0.070(2) Uani 1 1 d . . . . .
H51 H 0.558382 0.464468 0.501596 0.084 Uiso 1 1 calc R U . . .
C30 C 0.6596(5) 0.4490(2) 0.2058(4) 0.057(2) Uani 1 1 d . . . . .
H30A H 0.664234 0.429869 0.160461 0.086 Uiso 1 1 calc R U . . .
H30B H 0.713790 0.439955 0.245884 0.086 Uiso 1 1 calc R U . . .
H30C H 0.662106 0.485293 0.195345 0.086 Uiso 1 1 calc R U . . .
C50 C 0.6580(6) 0.4032(3) 0.5125(5) 0.067(2) Uani 1 1 d . . . . .
H50 H 0.629141 0.383478 0.546100 0.081 Uiso 1 1 calc R U . . .
C41 C 0.3228(5) 0.6669(2) 0.2896(4) 0.059(2) Uani 1 1 d . . . . .
H41A H 0.344734 0.697642 0.267687 0.088 Uiso 1 1 calc . U . . .
H41B H 0.376452 0.652461 0.325628 0.088 Uiso 1 1 calc . U . . .
H41C H 0.269371 0.675273 0.315173 0.088 Uiso 1 1 calc . U . . .
C31 C 0.5024(6) 0.3722(2) 0.0836(4) 0.067(2) Uani 1 1 d . . . . .
H31A H 0.493099 0.367754 0.029162 0.101 Uiso 1 1 calc R U . . .
H31B H 0.471756 0.344179 0.105526 0.101 Uiso 1 1 calc R U . . .
H31C H 0.571795 0.372820 0.104781 0.101 Uiso 1 1 calc R U . . .
C37 C 0.2785(5) 0.4143(2) 0.2479(4) 0.062(2) Uani 1 1 d . . . . .
H37A H 0.314225 0.383441 0.240559 0.094 Uiso 1 1 calc R U . . .
H37B H 0.260663 0.432105 0.199994 0.094 Uiso 1 1 calc R U . . .
H37C H 0.219778 0.405338 0.266661 0.094 Uiso 1 1 calc R U . . .
C49 C 0.7381(6) 0.3853(3) 0.4879(5) 0.077(3) Uani 1 1 d . . . . .
H49 H 0.762212 0.352640 0.502984 0.093 Uiso 1 1 calc R U . . .
C7 C 0.8026(6) 0.7291(2) 0.2103(4) 0.059(2) Uani 1 1 d . . . . .
H7 H 0.739085 0.711105 0.204270 0.071 Uiso 1 1 calc R U . . .
C13 C 0.5860(6) 0.6596(3) 0.4159(5) 0.073(2) Uani 1 1 d . . . . .
H13A H 0.554190 0.631003 0.387197 0.109 Uiso 1 1 calc R U . . .
H13B H 0.537378 0.680477 0.433763 0.109 Uiso 1 1 calc R U . . .
H13C H 0.632798 0.647074 0.458905 0.109 Uiso 1 1 calc R U . . .
C40 C 0.1996(5) 0.6456(2) 0.1731(4) 0.068(2) Uani 1 1 d . . . . .
H40A H 0.163074 0.616279 0.150037 0.102 Uiso 1 1 calc R U . . .
H40B H 0.219342 0.666484 0.134100 0.102 Uiso 1 1 calc R U . . .
H40C H 0.158721 0.665559 0.200342 0.102 Uiso 1 1 calc R U . . .
C14 C 0.5557(5) 0.7288(2) 0.2824(5) 0.073(3) Uani 1 1 d . . . . .
H14A H 0.587064 0.745087 0.244796 0.109 Uiso 1 1 calc R U . . .
H14B H 0.520675 0.754238 0.306098 0.109 Uiso 1 1 calc R U . . .
H14C H 0.510159 0.703122 0.258199 0.109 Uiso 1 1 calc R U . . .
C32 C 0.3322(6) 0.4291(3) -0.0197(5) 0.087(3) Uani 1 1 d . . . . .
H32A H 0.320468 0.459311 -0.051161 0.130 Uiso 1 1 calc R U . . .
H32B H 0.270172 0.413769 -0.014922 0.130 Uiso 1 1 calc R U . . .
H32C H 0.370347 0.404737 -0.042626 0.130 Uiso 1 1 calc R U . . .
C48 C 0.7845(6) 0.4139(3) 0.4415(5) 0.070(2) Uani 1 1 d . . . . .
H48 H 0.840777 0.401389 0.425762 0.084 Uiso 1 1 calc R U . . .
B1 B 0.4284(5) 0.5350(3) 0.2230(4) 0.0434(19) Uani 1 1 d . . . . .
C8 C 0.8453(6) 0.7175(3) 0.1413(4) 0.072(2) Uani 1 1 d . . . . .
H8A H 0.887393 0.745371 0.132053 0.108 Uiso 1 1 calc R U . . .
H8B H 0.792932 0.713320 0.097842 0.108 Uiso 1 1 calc R U . . .
H8C H 0.883251 0.686214 0.149454 0.108 Uiso 1 1 calc R U . . .
C26 C 0.1912(5) 0.5090(3) 0.0591(5) 0.074(2) Uani 1 1 d . . . . .
H26A H 0.173389 0.494165 0.009032 0.112 Uiso 1 1 calc R U . . .
H26B H 0.147786 0.537303 0.063890 0.112 Uiso 1 1 calc R U . . .
H26C H 0.185538 0.483359 0.096950 0.112 Uiso 1 1 calc R U . . .
C9 C 0.7818(6) 0.7877(3) 0.2190(5) 0.096(3) Uani 1 1 d . . . . .
H9A H 0.748561 0.792657 0.261290 0.144 Uiso 1 1 calc R U . . .
H9B H 0.740869 0.800156 0.172983 0.144 Uiso 1 1 calc R U . . .
H9C H 0.843163 0.806247 0.228190 0.144 Uiso 1 1 calc R U . . .
C12 C 0.8721(6) 0.6467(3) 0.5313(4) 0.081(3) Uani 1 1 d . . . . .
H12A H 0.846275 0.622752 0.563576 0.121 Uiso 1 1 calc R U . . .
H12B H 0.832974 0.677630 0.526055 0.121 Uiso 1 1 calc R U . . .
H12C H 0.939243 0.655039 0.553604 0.121 Uiso 1 1 calc R U . . .
C27 C 0.3166(6) 0.5563(3) 0.0021(5) 0.081(3) Uani 1 1 d . . . . .
H27A H 0.265578 0.549638 -0.041474 0.122 Uiso 1 1 calc R U . . .
H27B H 0.378916 0.544720 -0.008269 0.122 Uiso 1 1 calc R U . . .
H27C H 0.319791 0.592626 0.012628 0.122 Uiso 1 1 calc R U . . .
H1 H 0.418(4) 0.5763(18) 0.163(3) 0.050 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
Ni1 C44 1.825(7) . ?
Ni1 Si03 2.185(2) . ?
Ni1 Cl1 2.237(2) . ?
Ni1 B1 2.243(7) . ?
Ni1 H1 2.00(6) . ?
Si03 O2 1.732(4) . ?
Si03 O1 1.746(5) . ?
Si03 N1 1.760(5) . ?
Si1 N1 1.738(5) . ?
Si1 C13 1.851(7) . ?
Si1 C14 1.873(7) . ?
Si1 C15 1.902(6) . ?
O1 C16 1.383(7) . ?
O2 C21 1.364(8) . ?
N4 C33 1.341(8) . ?
N4 C34 1.441(8) . ?
N4 C36 1.492(8) . ?
N2 C22 1.359(7) . ?
N2 C23 1.404(9) . ?
N2 C28 1.469(8) . ?
N5 C33 1.368(8) . ?
N5 C35 1.423(9) . ?
N5 C39 1.474(8) . ?
N3 C22 1.327(8) . ?
N3 C24 1.413(9) . ?
N3 C25 1.521(8) . ?
N6 C44 1.280(9) . ?
N6 C45 1.445(8) . ?
N1 C1 1.436(8) . ?
C22 B1 1.649(9) . ?
C34 C35 1.340(9) . ?
C34 C42 1.527(9) . ?
C33 B1 1.612(10) . ?
C20 C21 1.367(8) . ?
C20 C19 1.434(9) . ?
C20 H20 0.9500 . ?
C21 C16 1.440(9) . ?
C28 C30 1.497(9) . ?
C28 C29 1.533(8) . ?
C28 H28 1.0000 . ?
C45 C46 1.503(8) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C1 C2 1.390(10) . ?
C1 C6 1.458(10) . ?
C35 C43 1.473(8) . ?
C23 C24 1.318(9) . ?
C23 C31 1.451(9) . ?
C44 B1 1.649(10) . ?
C46 C51 1.386(9) . ?
C46 C47 1.424(9) . ?
C6 C5 1.399(9) . ?
C6 C10 1.535(9) . ?
C16 C17 1.330(9) . ?
C18 C19 1.389(10) . ?
C18 C17 1.435(9) . ?
C18 H18 0.9500 . ?
C17 H17 0.9500 . ?
C10 C11 1.514(8) . ?
C10 C12 1.528(10) . ?
C10 H10 1.0000 . ?
C36 C38 1.513(9) . ?
C36 C37 1.540(8) . ?
C36 H36 1.0000 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C39 C40 1.496(9) . ?
C39 C41 1.553(9) . ?
C39 H39 1.0000 . ?
C2 C3 1.453(10) . ?
C2 C7 1.491(10) . ?
C4 C5 1.387(9) . ?
C4 C3 1.389(10) . ?
C4 H4 0.9500 . ?
C5 H5 0.9500 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C19 H19 0.9500 . ?
C25 C26 1.501(9) . ?
C25 C27 1.540(10) . ?
C25 H25 1.0000 . ?
C47 C48 1.418(9) . ?
C47 H47 0.9500 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C3 H3 0.9500 . ?
C24 C32 1.510(10) . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C51 C50 1.475(10) . ?
C51 H51 0.9500 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C50 C49 1.372(11) . ?
C50 H50 0.9500 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C49 C48 1.385(11) . ?
C49 H49 0.9500 . ?
C7 C8 1.520(10) . ?
C7 C9 1.591(8) . ?
C7 H7 1.0000 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C48 H48 0.9500 . ?
B1 H1 1.53(5) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C44 Ni1 Si03 103.2(2) . . ?
C44 Ni1 Cl1 159.0(2) . . ?
Si03 Ni1 Cl1 97.71(8) . . ?
C44 Ni1 B1 46.4(3) . . ?
Si03 Ni1 B1 146.6(2) . . ?
Cl1 Ni1 B1 113.0(2) . . ?
C44 Ni1 H1 87.7(16) . . ?
Si03 Ni1 H1 165.4(17) . . ?
Cl1 Ni1 H1 71.4(15) . . ?
B1 Ni1 H1 41.7(15) . . ?
O2 Si03 O1 92.2(2) . . ?
O2 Si03 N1 106.8(2) . . ?
O1 Si03 N1 104.8(2) . . ?
O2 Si03 Ni1 118.71(17) . . ?
O1 Si03 Ni1 112.46(17) . . ?
N1 Si03 Ni1 118.17(19) . . ?
N1 Si1 C13 110.8(3) . . ?
N1 Si1 C14 114.0(3) . . ?
C13 Si1 C14 107.6(4) . . ?
N1 Si1 C15 109.3(3) . . ?
C13 Si1 C15 108.5(4) . . ?
C14 Si1 C15 106.4(3) . . ?
C16 O1 Si03 111.4(4) . . ?
C21 O2 Si03 110.5(4) . . ?
C33 N4 C34 108.8(5) . . ?
C33 N4 C36 123.5(6) . . ?
C34 N4 C36 127.6(6) . . ?
C22 N2 C23 107.6(6) . . ?
C22 N2 C28 123.5(5) . . ?
C23 N2 C28 128.5(5) . . ?
C33 N5 C35 109.0(5) . . ?
C33 N5 C39 123.9(6) . . ?
C35 N5 C39 127.0(6) . . ?
C22 N3 C24 109.8(5) . . ?
C22 N3 C25 123.4(6) . . ?
C24 N3 C25 126.8(6) . . ?
C44 N6 C45 123.7(6) . . ?
C1 N1 Si1 118.5(4) . . ?
C1 N1 Si03 117.2(4) . . ?
Si1 N1 Si03 124.2(3) . . ?
N3 C22 N2 107.5(6) . . ?
N3 C22 B1 122.6(6) . . ?
N2 C22 B1 129.9(6) . . ?
C35 C34 N4 107.3(6) . . ?
C35 C34 C42 127.9(7) . . ?
N4 C34 C42 124.7(6) . . ?
N4 C33 N5 107.7(6) . . ?
N4 C33 B1 124.9(6) . . ?
N5 C33 B1 127.2(6) . . ?
C21 C20 C19 120.1(7) . . ?
C21 C20 H20 119.9 . . ?
C19 C20 H20 119.9 . . ?
O2 C21 C20 126.5(7) . . ?
O2 C21 C16 114.6(5) . . ?
C20 C21 C16 118.8(6) . . ?
N2 C28 C30 109.7(6) . . ?
N2 C28 C29 111.5(5) . . ?
C30 C28 C29 113.9(5) . . ?
N2 C28 H28 107.2 . . ?
C30 C28 H28 107.2 . . ?
C29 C28 H28 107.2 . . ?
N6 C45 C46 108.6(5) . . ?
N6 C45 H45A 110.0 . . ?
C46 C45 H45A 110.0 . . ?
N6 C45 H45B 110.0 . . ?
C46 C45 H45B 110.0 . . ?
H45A C45 H45B 108.3 . . ?
C2 C1 N1 120.3(7) . . ?
C2 C1 C6 120.4(6) . . ?
N1 C1 C6 119.3(6) . . ?
C34 C35 N5 107.2(6) . . ?
C34 C35 C43 126.5(8) . . ?
N5 C35 C43 126.4(6) . . ?
C24 C23 N2 108.8(6) . . ?
C24 C23 C31 126.6(7) . . ?
N2 C23 C31 124.5(6) . . ?
N6 C44 B1 125.7(6) . . ?
N6 C44 Ni1 152.8(6) . . ?
B1 C44 Ni1 80.2(4) . . ?
C51 C46 C47 120.1(7) . . ?
C51 C46 C45 118.8(7) . . ?
C47 C46 C45 120.8(7) . . ?
C5 C6 C1 118.5(6) . . ?
C5 C6 C10 118.8(7) . . ?
C1 C6 C10 122.8(6) . . ?
C17 C16 O1 127.2(7) . . ?
C17 C16 C21 121.7(6) . . ?
O1 C16 C21 111.0(6) . . ?
C19 C18 C17 119.0(8) . . ?
C19 C18 H18 120.5 . . ?
C17 C18 H18 120.5 . . ?
C16 C17 C18 120.3(7) . . ?
C16 C17 H17 119.9 . . ?
C18 C17 H17 119.9 . . ?
C11 C10 C12 112.0(6) . . ?
C11 C10 C6 111.2(6) . . ?
C12 C10 C6 111.3(6) . . ?
C11 C10 H10 107.4 . . ?
C12 C10 H10 107.4 . . ?
C6 C10 H10 107.4 . . ?
N4 C36 C38 114.5(6) . . ?
N4 C36 C37 107.2(6) . . ?
C38 C36 C37 114.8(6) . . ?
N4 C36 H36 106.6 . . ?
C38 C36 H36 106.6 . . ?
C37 C36 H36 106.6 . . ?
C34 C42 H42A 109.5 . . ?
C34 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C34 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
N5 C39 C40 112.3(6) . . ?
N5 C39 C41 109.7(7) . . ?
C40 C39 C41 112.4(6) . . ?
N5 C39 H39 107.4 . . ?
C40 C39 H39 107.4 . . ?
C41 C39 H39 107.4 . . ?
C1 C2 C3 117.1(7) . . ?
C1 C2 C7 124.6(7) . . ?
C3 C2 C7 118.3(7) . . ?
C5 C4 C3 117.3(7) . . ?
C5 C4 H4 121.3 . . ?
C3 C4 H4 121.3 . . ?
C4 C5 C6 123.2(7) . . ?
C4 C5 H5 118.4 . . ?
C6 C5 H5 118.4 . . ?
Si1 C15 H15A 109.5 . . ?
Si1 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
Si1 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C18 C19 C20 119.9(7) . . ?
C18 C19 H19 120.0 . . ?
C20 C19 H19 120.0 . . ?
C26 C25 N3 114.0(6) . . ?
C26 C25 C27 113.0(7) . . ?
N3 C25 C27 111.0(6) . . ?
C26 C25 H25 106.0 . . ?
N3 C25 H25 106.0 . . ?
C27 C25 H25 106.0 . . ?
C48 C47 C46 120.8(7) . . ?
C48 C47 H47 119.6 . . ?
C46 C47 H47 119.6 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C4 C3 C2 123.5(7) . . ?
C4 C3 H3 118.3 . . ?
C2 C3 H3 118.3 . . ?
C23 C24 N3 106.2(7) . . ?
C23 C24 C32 129.0(8) . . ?
N3 C24 C32 124.8(7) . . ?
C36 C38 H38A 109.5 . . ?
C36 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C36 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
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 . . ?
C35 C43 H43A 109.5 . . ?
C35 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C35 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C46 C51 C50 117.8(8) . . ?
C46 C51 H51 121.1 . . ?
C50 C51 H51 121.1 . . ?
C28 C30 H30A 109.5 . . ?
C28 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C28 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C49 C50 C51 120.6(8) . . ?
C49 C50 H50 119.7 . . ?
C51 C50 H50 119.7 . . ?
C39 C41 H41A 109.5 . . ?
C39 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C39 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C23 C31 H31A 109.5 . . ?
C23 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C23 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
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 . . ?
C50 C49 C48 121.3(7) . . ?
C50 C49 H49 119.4 . . ?
C48 C49 H49 119.4 . . ?
C2 C7 C8 113.4(7) . . ?
C2 C7 C9 108.5(6) . . ?
C8 C7 C9 112.8(6) . . ?
C2 C7 H7 107.3 . . ?
C8 C7 H7 107.3 . . ?
C9 C7 H7 107.3 . . ?
Si1 C13 H13A 109.5 . . ?
Si1 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
Si1 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
Si1 C14 H14A 109.5 . . ?
Si1 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
Si1 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C24 C32 H32A 109.5 . . ?
C24 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C24 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C49 C48 C47 119.2(8) . . ?
C49 C48 H48 120.4 . . ?
C47 C48 H48 120.4 . . ?
C33 B1 C22 113.6(5) . . ?
C33 B1 C44 109.7(6) . . ?
C22 B1 C44 118.5(6) . . ?
C33 B1 Ni1 131.3(5) . . ?
C22 B1 Ni1 114.0(5) . . ?
C44 B1 Ni1 53.3(3) . . ?
C33 B1 H1 106(2) . . ?
C22 B1 H1 94(2) . . ?
C44 B1 H1 113(2) . . ?
Ni1 B1 H1 61(2) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 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 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?

_refine_diff_density_max         0.677
_refine_diff_density_min         -0.588
_refine_diff_density_rms         0.071

