# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# 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. 
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#######################################################################

data_1b_GeCl2
_database_code_depnum_ccdc_archive 'CCDC 2357710'
loop_
_audit_author_name
_audit_author_address
'Terrance Hadlington'
;TU Munich
Germany
;
_audit_update_record             
;
2024-05-23 deposited with the CCDC.	2024-07-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C50 H78 Cl2 Ge N6 O1.50 P2'
_chemical_formula_sum            'C50 H78 Cl2 Ge N6 O1.50 P2'
_chemical_formula_weight         992.61

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_H-M_alt        'P c c n'
_space_group_name_Hall           '-P 2ab 2ac'

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

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

_cell_length_a                   17.370(4)
_cell_length_b                   18.920(4)
_cell_length_c                   33.750(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     11092(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    2000
_cell_measurement_theta_min      1.92
_cell_measurement_theta_max      32.50

_exptl_crystal_description       rod
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.189
_exptl_crystal_F_000             4224
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_exptl_absorpt_coefficient_mu    0.746
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.776
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'STOE X-AREA 1.76'

_diffrn_ambient_temperature      150(2)
_diffrn_source                   'Genix 3D HF Mo'
_diffrn_source_voltage           50
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_collimation    '0.6 mm diameter'
_diffrn_measurement_device_type  'STOE StadiVari'
_diffrn_measurement_method       'ω scans'
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_reflns_number            36330
_diffrn_reflns_av_unetI/netI     0.0886
_diffrn_reflns_av_R_equivalents  0.0661
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_theta_min         2.525
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             10849
_reflns_number_gt                5428
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1470P)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         10849
_refine_ls_number_parameters     556
_refine_ls_number_restraints     17
_refine_ls_R_factor_all          0.1609
_refine_ls_R_factor_gt           0.0792
_refine_ls_wR_factor_ref         0.2622
_refine_ls_wR_factor_gt          0.2137
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_restrained_S_all      1.002
_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
Ge1 Ge 0.46073(4) 0.53029(4) 0.60429(2) 0.0525(2) Uani 1 1 d . . . . .
Cl2 Cl 0.37313(8) 0.13325(8) 0.50135(4) 0.0479(4) Uani 1 1 d . . . . .
P03 P 0.56803(8) 0.58206(9) 0.64199(4) 0.0449(4) Uani 1 1 d . . . . .
P004 P 0.44719(8) 0.41985(9) 0.64232(5) 0.0486(4) Uani 1 1 d . . . . .
Cl1 Cl 0.54104(11) 0.47773(11) 0.55867(5) 0.0774(6) Uani 1 1 d . . . . .
O1 O 0.45326(19) 0.5388(2) 0.69027(11) 0.0459(10) Uani 1 1 d . . . . .
N3 N 0.3262(3) 0.3876(3) 0.58478(15) 0.0509(13) Uani 1 1 d . . . . .
N4 N 0.4151(3) 0.3078(3) 0.59078(15) 0.0529(13) Uani 1 1 d . . . . .
N1 N 0.5759(3) 0.6858(3) 0.57776(14) 0.0495(12) Uani 1 1 d . . . . .
N2 N 0.6822(3) 0.6281(3) 0.58947(15) 0.0526(13) Uani 1 1 d . . . . .
C1 C 0.4579(3) 0.6110(3) 0.69641(17) 0.0436(13) Uani 1 1 d . . . . .
C2 C 0.5137(3) 0.6448(3) 0.67310(17) 0.0459(15) Uani 1 1 d . . . . .
C3 C 0.5259(3) 0.7164(3) 0.67991(17) 0.0490(15) Uani 1 1 d . . . . .
H3 H 0.563845 0.740779 0.664962 0.059 Uiso 1 1 calc R U . . .
C24 C 0.6069(3) 0.6376(3) 0.60234(17) 0.0474(15) Uani 1 1 d . . . . .
C4 C 0.4821(3) 0.7541(4) 0.70916(19) 0.0519(16) Uani 1 1 d . . . . .
C33 C 0.3925(3) 0.3707(4) 0.60468(18) 0.0517(15) Uani 1 1 d . . . . .
C13 C 0.3844(3) 0.5059(3) 0.69893(17) 0.0461(14) Uani 1 1 d . . . . .
C6 C 0.4117(3) 0.6451(4) 0.72396(17) 0.0478(15) Uani 1 1 d . . . . .
C12 C 0.3707(3) 0.4454(3) 0.67714(17) 0.0481(15) Uani 1 1 d . . . . .
C8 C 0.3339(3) 0.5347(4) 0.72683(17) 0.0510(16) Uani 1 1 d . . . . .
C11 C 0.3035(3) 0.4063(4) 0.68708(18) 0.0555(17) Uani 1 1 d . . . . .
H11 H 0.293537 0.362983 0.673790 0.067 Uiso 1 1 calc R U . . .
C7 C 0.3538(3) 0.6028(4) 0.74854(17) 0.0528(16) Uani 1 1 d . . . . .
C5 C 0.4272(3) 0.7164(4) 0.72981(19) 0.0551(16) Uani 1 1 d . . . . .
H5 H 0.398074 0.740767 0.749315 0.066 Uiso 1 1 calc R U . . .
C9 C 0.2680(3) 0.4939(4) 0.7340(2) 0.0609(18) Uani 1 1 d . . . . .
H9 H 0.231607 0.511239 0.752648 0.073 Uiso 1 1 calc R U . . .
C36 C 0.2816(3) 0.4541(3) 0.58672(19) 0.0552(16) Uani 1 1 d . . . . .
H36 H 0.305330 0.485087 0.607387 0.066 Uiso 1 1 calc R U . . .
C10 C 0.2523(3) 0.4297(4) 0.71563(19) 0.0582(17) Uani 1 1 d . . . . .
C27 C 0.7399(3) 0.5799(4) 0.60631(19) 0.0582(17) Uani 1 1 d . . . . .
H27 H 0.717759 0.557856 0.630728 0.070 Uiso 1 1 calc R U . . .
C39 C 0.4864(4) 0.2681(4) 0.60256(19) 0.0584(17) Uani 1 1 d . . . . .
H39 H 0.510118 0.292793 0.625742 0.070 Uiso 1 1 calc R U . . .
C34 C 0.3096(4) 0.3342(4) 0.55850(19) 0.0600(17) Uani 1 1 d . . . . .
H34 H 0.266930 0.332715 0.540927 0.072 Uiso 1 1 calc R U . . .
C37 C 0.2863(4) 0.4921(4) 0.5471(2) 0.070(2) Uani 1 1 d . . . . .
H37A H 0.340373 0.498634 0.539715 0.105 Uiso 1 1 calc R U . . .
H37B H 0.261192 0.538391 0.549251 0.105 Uiso 1 1 calc R U . . .
H37C H 0.260211 0.463935 0.526758 0.105 Uiso 1 1 calc R U . . .
C16 C 0.4996(3) 0.8328(3) 0.71730(17) 0.0599(17) Uani 1 1 d D . . . .
C21 C 0.2033(9) 0.3540(10) 0.7693(3) 0.069(5) Uani 0.843(14) 1 d D . P A 1
H21A H 0.158473 0.329240 0.780172 0.104 Uiso 0.843(14) 1 calc R U P A 1
H21B H 0.219152 0.391498 0.787590 0.104 Uiso 0.843(14) 1 calc R U P A 1
H21C H 0.245793 0.320382 0.765887 0.104 Uiso 0.843(14) 1 calc R U P A 1
C35 C 0.3648(4) 0.2843(4) 0.5620(2) 0.0666(19) Uani 1 1 d . . . . .
H35 H 0.368207 0.241396 0.547553 0.080 Uiso 1 1 calc R U . . .
C32 C 0.4884(4) 0.7881(4) 0.5792(2) 0.078(2) Uani 1 1 d . . . . .
H32A H 0.515976 0.804483 0.602780 0.117 Uiso 1 1 calc R U . . .
H32B H 0.434259 0.802402 0.580911 0.117 Uiso 1 1 calc R U . . .
H32C H 0.511690 0.808996 0.555482 0.117 Uiso 1 1 calc R U . . .
C30 C 0.4933(4) 0.7084(4) 0.5767(2) 0.0617(18) Uani 1 1 d . . . . .
H30 H 0.465942 0.687486 0.599955 0.074 Uiso 1 1 calc R U . . .
C38 C 0.1985(4) 0.4391(4) 0.5987(2) 0.0688(19) Uani 1 1 d . . . . .
H38A H 0.172382 0.413728 0.577220 0.103 Uiso 1 1 calc R U . . .
H38B H 0.171779 0.483869 0.603719 0.103 Uiso 1 1 calc R U . . .
H38C H 0.197849 0.410182 0.622746 0.103 Uiso 1 1 calc R U . . .
C14 C 0.2809(3) 0.6465(4) 0.7566(2) 0.069(2) Uani 1 1 d . . . . .
H14A H 0.257081 0.659927 0.731340 0.103 Uiso 1 1 calc R U . . .
H14B H 0.294559 0.689192 0.771430 0.103 Uiso 1 1 calc R U . . .
H14C H 0.244409 0.618247 0.772082 0.103 Uiso 1 1 calc R U . . .
C25 C 0.6945(4) 0.6701(4) 0.5570(2) 0.0606(17) Uani 1 1 d . . . . .
H25 H 0.740910 0.673233 0.542204 0.073 Uiso 1 1 calc R U . . .
C26 C 0.6284(4) 0.7067(4) 0.5498(2) 0.0641(18) Uani 1 1 d . . . . .
H26 H 0.620211 0.740227 0.529252 0.077 Uiso 1 1 calc R U . . .
C15 C 0.3906(4) 0.5828(4) 0.78875(18) 0.0636(18) Uani 1 1 d . . . . .
H15A H 0.352544 0.558024 0.805115 0.095 Uiso 1 1 calc R U . . .
H15B H 0.407504 0.625738 0.802411 0.095 Uiso 1 1 calc R U . . .
H15C H 0.434939 0.551826 0.784184 0.095 Uiso 1 1 calc R U . . .
C29 C 0.7588(4) 0.5225(4) 0.5777(2) 0.074(2) Uani 1 1 d . . . . .
H29A H 0.711495 0.497677 0.570056 0.110 Uiso 1 1 calc R U . . .
H29B H 0.794509 0.489012 0.590042 0.110 Uiso 1 1 calc R U . . .
H29C H 0.782802 0.542966 0.554024 0.110 Uiso 1 1 calc R U . . .
C20 C 0.1826(4) 0.3861(4) 0.72941(19) 0.075(2) Uani 1 1 d D . . . .
O2 O 0.250000 0.750000 0.6098(4) 0.173(5) Uiso 1 2 d S . P . .
C28 C 0.8106(4) 0.6242(4) 0.6183(2) 0.078(2) Uani 1 1 d . . . . .
H28A H 0.832748 0.646485 0.594707 0.117 Uiso 1 1 calc R U . . .
H28B H 0.849181 0.593376 0.630630 0.117 Uiso 1 1 calc R U . . .
H28C H 0.794962 0.660748 0.637207 0.117 Uiso 1 1 calc R U . . .
C31 C 0.4558(5) 0.6806(5) 0.5384(3) 0.099(3) Uani 1 1 d . . . . .
H31A H 0.477200 0.705919 0.515565 0.148 Uiso 1 1 calc R U . . .
H31B H 0.400086 0.688357 0.539572 0.148 Uiso 1 1 calc R U . . .
H31C H 0.466331 0.629982 0.535687 0.148 Uiso 1 1 calc R U . . .
C19 C 0.4595(6) 0.8616(6) 0.7541(3) 0.094(4) Uani 0.843(14) 1 d D . P A 1
H19A H 0.477613 0.909689 0.759423 0.140 Uiso 0.843(14) 1 calc R U P A 1
H19B H 0.471331 0.831232 0.776843 0.140 Uiso 0.843(14) 1 calc R U P A 1
H19C H 0.403705 0.862236 0.749734 0.140 Uiso 0.843(14) 1 calc R U P A 1
C40 C 0.4664(5) 0.1953(5) 0.6147(3) 0.118(4) Uani 1 1 d . . . . .
H40A H 0.432448 0.197004 0.637896 0.177 Uiso 1 1 calc R U . . .
H40B H 0.513556 0.169527 0.621506 0.177 Uiso 1 1 calc R U . . .
H40C H 0.440103 0.171262 0.592900 0.177 Uiso 1 1 calc R U . . .
C48 C 0.5168(6) 1.0055(6) 0.5900(4) 0.113(3) Uiso 1 1 d . . . . .
C41 C 0.5431(5) 0.2689(6) 0.5692(3) 0.124(4) Uani 1 1 d . . . . .
H41A H 0.589870 0.243643 0.577164 0.186 Uiso 1 1 calc R U . . .
H41B H 0.556072 0.317842 0.562479 0.186 Uiso 1 1 calc R U . . .
H41C H 0.520502 0.245581 0.545977 0.186 Uiso 1 1 calc R U . . .
C47 C 0.4905(6) 0.9896(6) 0.5531(3) 0.117(3) Uiso 1 1 d . . . . .
H47A H 0.447520 0.956222 0.555119 0.176 Uiso 1 1 calc R U . . .
H47B H 0.532053 0.968237 0.537506 0.176 Uiso 1 1 calc R U . . .
H47C H 0.472862 1.032909 0.539949 0.176 Uiso 1 1 calc R U . . .
C18 C 0.5853(3) 0.8434(5) 0.7253(3) 0.079(3) Uani 0.843(14) 1 d D . P A 1
H18A H 0.596813 0.894083 0.726415 0.118 Uiso 0.843(14) 1 calc R U P A 1
H18B H 0.615348 0.821441 0.704075 0.118 Uiso 0.843(14) 1 calc R U P A 1
H18C H 0.598805 0.821481 0.750722 0.118 Uiso 0.843(14) 1 calc R U P A 1
C46 C 0.7163(5) 0.2314(6) 0.5158(3) 0.115(3) Uiso 1 1 d D . . . .
H46A H 0.684463 0.248253 0.493373 0.138 Uiso 1 1 calc R U . . .
H46B H 0.688098 0.242696 0.540510 0.138 Uiso 1 1 calc R U . . .
C17 C 0.4769(10) 0.8787(5) 0.6821(3) 0.122(6) Uani 0.843(14) 1 d D . P A 1
H17A H 0.423341 0.868871 0.674789 0.184 Uiso 0.843(14) 1 calc R U P A 1
H17B H 0.510593 0.868037 0.659568 0.184 Uiso 0.843(14) 1 calc R U P A 1
H17C H 0.482165 0.928666 0.689219 0.184 Uiso 0.843(14) 1 calc R U P A 1
C43 C 0.2360(7) 0.6322(7) 0.6336(4) 0.151(4) Uiso 1 1 d D . . . .
H43A H 0.209918 0.643830 0.658492 0.226 Uiso 1 1 calc R U . . .
H43B H 0.262974 0.586952 0.636445 0.226 Uiso 1 1 calc R U . . .
H43C H 0.197918 0.628514 0.612269 0.226 Uiso 1 1 calc R U . . .
N5 N 0.5357(7) 1.0198(7) 0.6198(5) 0.184(5) Uiso 1 1 d . . . . .
C23 C 0.1722(9) 0.3221(7) 0.7026(4) 0.157(8) Uani 0.843(14) 1 d D . P A 1
H23A H 0.130273 0.292563 0.712756 0.236 Uiso 0.843(14) 1 calc R U P A 1
H23B H 0.219978 0.294619 0.702006 0.236 Uiso 0.843(14) 1 calc R U P A 1
H23C H 0.159586 0.337960 0.675700 0.236 Uiso 0.843(14) 1 calc R U P A 1
C22 C 0.1096(5) 0.4308(7) 0.7301(7) 0.197(12) Uani 0.843(14) 1 d D . P A 1
H22A H 0.097691 0.446914 0.703225 0.296 Uiso 0.843(14) 1 calc R U P A 1
H22B H 0.117387 0.471794 0.747397 0.296 Uiso 0.843(14) 1 calc R U P A 1
H22C H 0.066721 0.402315 0.740229 0.296 Uiso 0.843(14) 1 calc R U P A 1
C42 C 0.2933(12) 0.6894(10) 0.6237(7) 0.294(11) Uiso 1 1 d D . . . .
H42A H 0.323583 0.702136 0.647485 0.353 Uiso 1 1 calc R U . . .
H42B H 0.329164 0.672879 0.602873 0.353 Uiso 1 1 calc R U . . .
C45 C 0.7235(11) 0.1523(6) 0.5127(6) 0.246(9) Uiso 1 1 d D . . . .
H45A H 0.755381 0.133960 0.534786 0.295 Uiso 1 1 calc R U . . .
H45B H 0.748699 0.139309 0.487428 0.295 Uiso 1 1 calc R U . . .
C44 C 0.6430(11) 0.1203(13) 0.5146(6) 0.300(11) Uiso 1 1 d D . . . .
H44A H 0.604573 0.157943 0.512265 0.450 Uiso 1 1 calc R U . . .
H44B H 0.636316 0.095749 0.539939 0.450 Uiso 1 1 calc R U . . .
H44C H 0.636489 0.086597 0.492801 0.450 Uiso 1 1 calc R U . . .
C49 C 0.6815(11) 0.3053(12) 0.6464(6) 0.252(9) Uiso 1 1 d D . . . .
N6 N 0.6460(10) 0.2656(7) 0.6622(5) 0.232(6) Uiso 1 1 d D . . . .
C50 C 0.6830(10) 0.3868(8) 0.6405(5) 0.244(9) Uiso 1 1 d D . . . .
H50A H 0.652967 0.399168 0.616900 0.366 Uiso 1 1 calc R U . . .
H50B H 0.736322 0.402566 0.637010 0.366 Uiso 1 1 calc R U . . .
H50C H 0.660682 0.409966 0.663762 0.366 Uiso 1 1 calc R U . . .
C17A C 0.424(2) 0.862(4) 0.701(2) 0.12(3) Uiso 0.157(14) 1 d D . P A 2
H17D H 0.380949 0.840549 0.715074 0.175 Uiso 0.157(14) 1 calc R U P A 2
H17E H 0.420444 0.849725 0.672544 0.175 Uiso 0.157(14) 1 calc R U P A 2
H17F H 0.423104 0.913085 0.703928 0.175 Uiso 0.157(14) 1 calc R U P A 2
C18A C 0.5706(15) 0.859(2) 0.6956(12) 0.048(11) Uiso 0.157(14) 1 d D . P A 2
H18D H 0.565180 0.909813 0.690071 0.072 Uiso 0.157(14) 1 calc R U P A 2
H18E H 0.576278 0.833397 0.670560 0.072 Uiso 0.157(14) 1 calc R U P A 2
H18F H 0.616275 0.851382 0.712069 0.072 Uiso 0.157(14) 1 calc R U P A 2
C19A C 0.498(5) 0.843(5) 0.7620(4) 0.11(3) Uiso 0.157(14) 1 d D . P A 2
H19D H 0.546344 0.825398 0.773400 0.166 Uiso 0.1565 1 calc . U P A 2
H19E H 0.454599 0.817649 0.773299 0.166 Uiso 0.1565 1 calc . U P A 2
H19F H 0.493247 0.893834 0.767944 0.166 Uiso 0.1565 1 calc . U P A 2
C22A C 0.124(3) 0.436(4) 0.748(2) 0.09(2) Uiso 0.157(14) 1 d D . P A 2
H22D H 0.127677 0.482461 0.735535 0.138 Uiso 0.157(14) 1 calc R U P A 2
H22E H 0.134593 0.440347 0.776503 0.138 Uiso 0.157(14) 1 calc R U P A 2
H22F H 0.072074 0.416840 0.744263 0.138 Uiso 0.157(14) 1 calc R U P A 2
C23A C 0.1362(19) 0.343(2) 0.7000(11) 0.032(10) Uiso 0.157(14) 1 d D . P A 2
H23D H 0.092927 0.320335 0.713685 0.048 Uiso 0.157(14) 1 calc R U P A 2
H23E H 0.169155 0.306545 0.688200 0.048 Uiso 0.157(14) 1 calc R U P A 2
H23F H 0.116448 0.373988 0.679084 0.048 Uiso 0.157(14) 1 calc R U P A 2
C21A C 0.186(5) 0.350(5) 0.7696(15) 0.05(2) Uiso 0.157(14) 1 d D . P A 2
H21D H 0.140120 0.320992 0.773361 0.082 Uiso 0.157(14) 1 calc R U P A 2
H21E H 0.189235 0.385700 0.790495 0.082 Uiso 0.157(14) 1 calc R U P A 2
H21F H 0.232095 0.319673 0.770702 0.082 Uiso 0.157(14) 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
Ge1 Cl1 2.303(2) . ?
Ge1 P03 2.4601(16) . ?
Ge1 P004 2.4633(19) . ?
P03 C24 1.830(6) . ?
P03 C2 1.845(6) . ?
P004 C33 1.839(6) . ?
P004 C12 1.839(6) . ?
O1 C13 1.380(6) . ?
O1 C1 1.384(7) . ?
N3 C33 1.372(7) . ?
N3 C34 1.374(8) . ?
N3 C36 1.479(8) . ?
N4 C33 1.338(8) . ?
N4 C35 1.379(8) . ?
N4 C39 1.501(8) . ?
N1 C24 1.345(7) . ?
N1 C26 1.371(7) . ?
N1 C30 1.498(8) . ?
N2 C25 1.371(8) . ?
N2 C24 1.391(7) . ?
N2 C27 1.469(8) . ?
C1 C6 1.387(8) . ?
C1 C2 1.403(8) . ?
C2 C3 1.389(8) . ?
C3 C4 1.436(8) . ?
C4 C5 1.379(9) . ?
C4 C16 1.546(9) . ?
C13 C12 1.381(8) . ?
C13 C8 1.398(8) . ?
C6 C5 1.389(9) . ?
C6 C7 1.530(8) . ?
C12 C11 1.422(8) . ?
C8 C9 1.402(8) . ?
C8 C7 1.521(9) . ?
C11 C10 1.385(9) . ?
C7 C14 1.537(8) . ?
C7 C15 1.547(8) . ?
C9 C10 1.391(10) . ?
C36 C37 1.521(9) . ?
C36 C38 1.526(8) . ?
C10 C20 1.536(8) . ?
C27 C29 1.491(9) . ?
C27 C28 1.542(9) . ?
C39 C40 1.478(11) . ?
C39 C41 1.497(10) . ?
C34 C35 1.350(9) . ?
C16 C18A 1.520(5) . ?
C16 C19A 1.520(5) . ?
C16 C17A 1.522(5) . ?
C16 C17 1.523(5) . ?
C16 C19 1.524(5) . ?
C16 C18 1.527(5) . ?
C21 C20 1.522(5) . ?
C32 C30 1.513(10) . ?
C30 C31 1.539(10) . ?
C25 C26 1.363(9) . ?
C20 C23A 1.518(5) . ?
C20 C21A 1.520(5) . ?
C20 C22A 1.522(5) . ?
C20 C22 1.523(5) . ?
C20 C23 1.523(5) . ?
O2 C42 1.45(2) 2_565 ?
O2 C42 1.45(2) . ?
C48 N5 1.094(15) . ?
C48 C47 1.361(14) . ?
C46 C46 1.366(17) 2_655 ?
C46 C45 1.507(5) . ?
C43 C42 1.508(5) . ?
C45 C44 1.525(5) . ?
C49 N6 1.108(5) . ?
C49 C50 1.554(19) . ?

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
Cl1 Ge1 P03 93.37(6) . . ?
Cl1 Ge1 P004 92.28(7) . . ?
P03 Ge1 P004 98.08(6) . . ?
C24 P03 C2 103.6(3) . . ?
C24 P03 Ge1 97.45(18) . . ?
C2 P03 Ge1 99.38(18) . . ?
C33 P004 C12 101.6(3) . . ?
C33 P004 Ge1 96.8(2) . . ?
C12 P004 Ge1 100.3(2) . . ?
C13 O1 C1 117.6(4) . . ?
C33 N3 C34 108.7(5) . . ?
C33 N3 C36 128.1(5) . . ?
C34 N3 C36 123.0(5) . . ?
C33 N4 C35 110.3(5) . . ?
C33 N4 C39 126.4(5) . . ?
C35 N4 C39 123.3(6) . . ?
C24 N1 C26 110.8(5) . . ?
C24 N1 C30 126.3(5) . . ?
C26 N1 C30 122.5(5) . . ?
C25 N2 C24 108.8(5) . . ?
C25 N2 C27 124.3(5) . . ?
C24 N2 C27 127.0(5) . . ?
O1 C1 C6 121.8(5) . . ?
O1 C1 C2 114.0(5) . . ?
C6 C1 C2 124.2(6) . . ?
C3 C2 C1 117.2(5) . . ?
C3 C2 P03 130.0(4) . . ?
C1 C2 P03 112.2(5) . . ?
C2 C3 C4 121.1(6) . . ?
N1 C24 N2 105.7(5) . . ?
N1 C24 P03 133.9(4) . . ?
N2 C24 P03 120.0(5) . . ?
C5 C4 C3 117.2(6) . . ?
C5 C4 C16 123.0(6) . . ?
C3 C4 C16 119.8(5) . . ?
N4 C33 N3 106.4(5) . . ?
N4 C33 P004 122.7(4) . . ?
N3 C33 P004 130.8(5) . . ?
O1 C13 C12 114.2(5) . . ?
O1 C13 C8 120.7(5) . . ?
C12 C13 C8 125.1(5) . . ?
C1 C6 C5 115.8(5) . . ?
C1 C6 C7 120.0(6) . . ?
C5 C6 C7 123.9(5) . . ?
C13 C12 C11 116.6(5) . . ?
C13 C12 P004 115.7(4) . . ?
C11 C12 P004 127.4(5) . . ?
C13 C8 C9 114.4(6) . . ?
C13 C8 C7 120.8(5) . . ?
C9 C8 C7 124.7(5) . . ?
C10 C11 C12 121.7(6) . . ?
C8 C7 C6 109.3(5) . . ?
C8 C7 C14 110.7(5) . . ?
C6 C7 C14 110.9(6) . . ?
C8 C7 C15 108.0(5) . . ?
C6 C7 C15 109.4(5) . . ?
C14 C7 C15 108.5(5) . . ?
C4 C5 C6 124.3(6) . . ?
C10 C9 C8 124.4(6) . . ?
N3 C36 C37 109.6(5) . . ?
N3 C36 C38 110.4(5) . . ?
C37 C36 C38 111.7(5) . . ?
C11 C10 C9 117.6(6) . . ?
C11 C10 C20 123.1(7) . . ?
C9 C10 C20 119.2(6) . . ?
N2 C27 C29 110.6(5) . . ?
N2 C27 C28 107.9(6) . . ?
C29 C27 C28 113.0(5) . . ?
C40 C39 C41 111.9(8) . . ?
C40 C39 N4 110.2(6) . . ?
C41 C39 N4 109.8(6) . . ?
C35 C34 N3 108.0(6) . . ?
C18A C16 C19A 117(4) . . ?
C18A C16 C17A 114(3) . . ?
C19A C16 C17A 108(4) . . ?
C17 C16 C19 108.4(9) . . ?
C17 C16 C18 108.5(8) . . ?
C19 C16 C18 104.7(7) . . ?
C18A C16 C4 113.0(17) . . ?
C19A C16 C4 107(3) . . ?
C17A C16 C4 96(3) . . ?
C17 C16 C4 111.1(6) . . ?
C19 C16 C4 113.5(6) . . ?
C18 C16 C4 110.4(5) . . ?
C34 C35 N4 106.7(6) . . ?
N1 C30 C32 109.7(5) . . ?
N1 C30 C31 109.2(6) . . ?
C32 C30 C31 111.3(6) . . ?
C26 C25 N2 107.8(6) . . ?
C25 C26 N1 106.9(6) . . ?
C23A C20 C21A 111(4) . . ?
C23A C20 C22A 104(3) . . ?
C21A C20 C22A 86(5) . . ?
C21 C20 C22 113.9(12) . . ?
C21 C20 C23 103.6(11) . . ?
C22 C20 C23 110.6(10) . . ?
C23A C20 C10 120.6(19) . . ?
C21A C20 C10 119(3) . . ?
C21 C20 C10 107.2(7) . . ?
C22A C20 C10 109(3) . . ?
C22 C20 C10 111.3(7) . . ?
C23 C20 C10 109.9(7) . . ?
C42 O2 C42 142(2) 2_565 . ?
N5 C48 C47 177.4(14) . . ?
C46 C46 C45 116.1(14) 2_655 . ?
O2 C42 C43 107.3(15) . . ?
C46 C45 C44 108.4(15) . . ?
N6 C49 C50 138(2) . . ?

_refine_diff_density_max         1.225
_refine_diff_density_min         -0.643
_refine_diff_density_rms         0.090



####################################################################### 
# 
# 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_2b
_database_code_depnum_ccdc_archive 'CCDC 2357711'
loop_
_audit_author_name
_audit_author_address
'Terrance Hadlington'
;TU Munich
Germany
;
_audit_update_record             
;
2024-05-23 deposited with the CCDC.	2024-07-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C82 H120 N8 Ni2 O2 P4'
_chemical_formula_sum            'C82 H120 N8 Ni2 O2 P4'
_chemical_formula_weight         1491.15

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   10.760(2)
_cell_length_b                   12.310(3)
_cell_length_c                   15.630(3)
_cell_angle_alpha                97.50(3)
_cell_angle_beta                 99.40(3)
_cell_angle_gamma                96.00(3)
_cell_volume                     2008.2(7)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    2000
_cell_measurement_theta_min      1.92
_cell_measurement_theta_max      32.50

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.233
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.22
_exptl_absorpt_coefficient_mu    0.599
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.826
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'STOE X-AREA 1.76'

_diffrn_ambient_temperature      150(2)
_diffrn_source                   'Genix 3D HF Mo'
_diffrn_source_voltage           50
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_collimation    '0.6 mm diameter'
_diffrn_measurement_device_type  'STOE StadiVari'
_diffrn_measurement_method       'ω scans'
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_reflns_number            20319
_diffrn_reflns_av_unetI/netI     0.0883
_diffrn_reflns_av_R_equivalents  0.0411
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.395
_diffrn_reflns_theta_max         25.996
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             7853
_reflns_number_gt                5047
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0347P)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         7853
_refine_ls_number_parameters     474
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0684
_refine_ls_R_factor_gt           0.0375
_refine_ls_wR_factor_ref         0.0792
_refine_ls_wR_factor_gt          0.0739
_refine_ls_goodness_of_fit_ref   0.877
_refine_ls_restrained_S_all      0.877
_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 0.34950(3) 0.68023(2) 0.66942(2) 0.02122(9) Uani 1 1 d . . . . .
P2 P 0.59022(6) 0.40783(5) 0.45060(4) 0.02129(15) Uani 1 1 d . . . . .
P1 P 0.53420(6) 0.73106(5) 0.62565(4) 0.02193(15) Uani 1 1 d . . . . .
O1 O 0.63230(15) 0.49698(12) 0.63815(9) 0.0264(4) Uani 1 1 d . . . . .
N1 N 0.35177(19) 0.74502(15) 0.85838(11) 0.0277(5) Uani 1 1 d . . . . .
N3 N 0.18614(19) 0.46672(15) 0.66278(12) 0.0271(5) Uani 1 1 d . . . . .
N4 N 0.0764(2) 0.60034(16) 0.64208(12) 0.0302(5) Uani 1 1 d . . . . .
N2 N 0.3749(2) 0.89009(15) 0.79787(12) 0.0298(5) Uani 1 1 d . . . . .
C1 C 0.6766(2) 0.39508(17) 0.62958(14) 0.0197(5) Uani 1 1 d . . . . .
C13 C 0.6698(2) 0.56961(17) 0.71597(13) 0.0219(5) Uani 1 1 d . . . . .
C12 C 0.6330(2) 0.67578(18) 0.71459(13) 0.0220(5) Uani 1 1 d . . . . .
C2 C 0.6579(2) 0.33815(17) 0.54293(13) 0.0206(5) Uani 1 1 d . . . . .
C11 C 0.6798(2) 0.75295(18) 0.79090(14) 0.0241(5) Uani 1 1 d . . . . .
H11 H 0.658663 0.826057 0.791597 0.029 Uiso 1 1 calc R U . . .
C6 C 0.7351(2) 0.35260(18) 0.70158(13) 0.0222(5) Uani 1 1 d . . . . .
C7 C 0.7555(2) 0.41714(18) 0.79459(13) 0.0246(6) Uani 1 1 d . . . . .
C8 C 0.7378(2) 0.53828(18) 0.79034(14) 0.0232(5) Uani 1 1 d . . . . .
C5 C 0.7698(2) 0.24714(18) 0.68717(14) 0.0275(6) Uani 1 1 d . . . . .
H5 H 0.807623 0.216198 0.736092 0.033 Uiso 1 1 calc R U . . .
C3 C 0.6985(2) 0.23369(18) 0.53350(14) 0.0253(6) Uani 1 1 d . . . . .
H3 H 0.689604 0.193907 0.476056 0.030 Uiso 1 1 calc R U . . .
C10 C 0.7546(2) 0.72836(19) 0.86485(14) 0.0265(6) Uani 1 1 d . . . . .
C33 C 0.1995(2) 0.57876(18) 0.65848(13) 0.0252(6) Uani 1 1 d . . . . .
C9 C 0.7802(2) 0.61923(19) 0.86377(14) 0.0267(6) Uani 1 1 d . . . . .
H9 H 0.828069 0.599392 0.914731 0.032 Uiso 1 1 calc R U . . .
C24 C 0.3589(2) 0.77661(18) 0.77815(14) 0.0238(5) Uani 1 1 d . . . . .
C39 C 0.0418(3) 0.7136(2) 0.64109(15) 0.0333(6) Uani 1 1 d . . . . .
H39 H 0.115403 0.761398 0.628174 0.040 Uiso 1 1 calc R U . . .
C30 C 0.3793(3) 0.96653(19) 0.73284(16) 0.0365(7) Uani 1 1 d . . . . .
H30 H 0.390275 0.923395 0.676354 0.044 Uiso 1 1 calc R U . . .
C38 C 0.3114(3) 0.32183(19) 0.60729(16) 0.0379(7) Uani 1 1 d . . . . .
H38A H 0.236802 0.265624 0.590088 0.057 Uiso 1 1 calc R U . . .
H38B H 0.387164 0.286133 0.623898 0.057 Uiso 1 1 calc R U . . .
H38C H 0.322009 0.361315 0.557891 0.057 Uiso 1 1 calc R U . . .
C4 C 0.7515(2) 0.18497(18) 0.60436(15) 0.0276(6) Uani 1 1 d . . . . .
C40 C 0.0164(3) 0.7602(2) 0.73097(15) 0.0386(7) Uani 1 1 d . . . . .
H40A H -0.051385 0.711398 0.746784 0.058 Uiso 1 1 calc R U . . .
H40B H -0.009694 0.833948 0.729116 0.058 Uiso 1 1 calc R U . . .
H40C H 0.093944 0.765323 0.774785 0.058 Uiso 1 1 calc R U . . .
C36 C 0.2932(2) 0.40342(19) 0.68507(15) 0.0317(6) Uani 1 1 d . . . . .
H36 H 0.372446 0.457126 0.703578 0.038 Uiso 1 1 calc R U . . .
C20 C 0.8083(2) 0.8144(2) 0.94687(15) 0.0318(6) Uani 1 1 d . . . . .
C27 C 0.3311(2) 0.62919(19) 0.87197(15) 0.0294(6) Uani 1 1 d . . . . .
H27 H 0.318372 0.582572 0.813067 0.035 Uiso 1 1 calc R U . . .
C19 C 0.8882(3) 0.4066(2) 0.84506(15) 0.0401(7) Uani 1 1 d . . . . .
H19A H 0.953398 0.438246 0.815120 0.060 Uiso 1 1 calc R U . . .
H19B H 0.896445 0.328380 0.847236 0.060 Uiso 1 1 calc R U . . .
H19C H 0.899242 0.446312 0.904893 0.060 Uiso 1 1 calc R U . . .
C25 C 0.3626(3) 0.8348(2) 0.92391(15) 0.0381(7) Uani 1 1 d . . . . .
H25 H 0.360108 0.832496 0.984131 0.046 Uiso 1 1 calc R U . . .
C26 C 0.3771(3) 0.9255(2) 0.88578(15) 0.0383(7) Uani 1 1 d . . . . .
H26 H 0.387095 0.999964 0.913804 0.046 Uiso 1 1 calc R U . . .
C35 C 0.0589(3) 0.4238(2) 0.64892(16) 0.0369(7) Uani 1 1 d . . . . .
H35 H 0.026197 0.349057 0.648681 0.044 Uiso 1 1 calc R U . . .
C29 C 0.4473(3) 0.5974(2) 0.92736(16) 0.0402(7) Uani 1 1 d . . . . .
H29A H 0.520885 0.609540 0.898612 0.060 Uiso 1 1 calc R U . . .
H29B H 0.432088 0.519329 0.933921 0.060 Uiso 1 1 calc R U . . .
H29C H 0.463876 0.642968 0.985321 0.060 Uiso 1 1 calc R U . . .
C18 C 0.6526(3) 0.3686(2) 0.84210(15) 0.0389(7) Uani 1 1 d . . . . .
H18A H 0.662739 0.410124 0.901270 0.058 Uiso 1 1 calc R U . . .
H18B H 0.661484 0.290908 0.846009 0.058 Uiso 1 1 calc R U . . .
H18C H 0.568354 0.374004 0.809202 0.058 Uiso 1 1 calc R U . . .
C37 C 0.2737(3) 0.3436(2) 0.76266(16) 0.0461(8) Uani 1 1 d . . . . .
H37A H 0.260546 0.396992 0.811585 0.069 Uiso 1 1 calc R U . . .
H37B H 0.348940 0.308047 0.781034 0.069 Uiso 1 1 calc R U . . .
H37C H 0.199099 0.287394 0.745067 0.069 Uiso 1 1 calc R U . . .
C41 C -0.0711(3) 0.7144(2) 0.57032(17) 0.0534(9) Uani 1 1 d . . . . .
H41A H -0.055978 0.676289 0.514611 0.080 Uiso 1 1 calc R U . . .
H41B H -0.083688 0.790955 0.564255 0.080 Uiso 1 1 calc R U . . .
H41C H -0.147011 0.676609 0.585997 0.080 Uiso 1 1 calc R U . . .
C34 C -0.0093(3) 0.5069(2) 0.63593(17) 0.0404(7) Uani 1 1 d . . . . .
H34 H -0.099335 0.502445 0.624667 0.048 Uiso 1 1 calc R U . . .
C32 C 0.2551(3) 1.0157(2) 0.71668(18) 0.0523(8) Uani 1 1 d . . . . .
H32A H 0.184321 0.955999 0.697587 0.079 Uiso 1 1 calc R U . . .
H32B H 0.257602 1.062982 0.671024 0.079 Uiso 1 1 calc R U . . .
H32C H 0.243363 1.059729 0.771019 0.079 Uiso 1 1 calc R U . . .
C14 C 0.7933(3) 0.0688(2) 0.59075(17) 0.0446(8) Uani 1 1 d . . . . .
C28 C 0.2101(3) 0.6074(2) 0.90879(17) 0.0430(7) Uani 1 1 d . . . . .
H28A H 0.216677 0.656241 0.964570 0.064 Uiso 1 1 calc R U . . .
H28B H 0.198168 0.530255 0.918461 0.064 Uiso 1 1 calc R U . . .
H28C H 0.137429 0.621790 0.867057 0.064 Uiso 1 1 calc R U . . .
C21 C 0.7553(3) 0.7813(2) 1.02625(16) 0.0522(9) Uani 1 1 d . . . . .
H21A H 0.790161 0.836499 1.077951 0.078 Uiso 1 1 calc R U . . .
H21B H 0.779385 0.708985 1.037110 0.078 Uiso 1 1 calc R U . . .
H21C H 0.662529 0.777070 1.014469 0.078 Uiso 1 1 calc R U . . .
C22 C 0.7719(3) 0.9295(2) 0.93475(16) 0.0471(8) Uani 1 1 d . . . . .
H22A H 0.806045 0.953992 0.885050 0.071 Uiso 1 1 calc R U . . .
H22B H 0.807329 0.981779 0.988135 0.071 Uiso 1 1 calc R U . . .
H22C H 0.679205 0.926115 0.923338 0.071 Uiso 1 1 calc R U . . .
C31 C 0.4922(3) 1.0562(2) 0.7624(2) 0.0599(9) Uani 1 1 d . . . . .
H31A H 0.478054 1.105472 0.813519 0.090 Uiso 1 1 calc R U . . .
H31B H 0.501741 1.098830 0.714622 0.090 Uiso 1 1 calc R U . . .
H31C H 0.569433 1.022218 0.778259 0.090 Uiso 1 1 calc R U . . .
C23 C 0.9535(3) 0.8217(2) 0.96595(18) 0.0548(9) Uani 1 1 d . . . . .
H23A H 0.988165 0.847820 0.916976 0.082 Uiso 1 1 calc R U . . .
H23B H 0.978019 0.748525 0.973170 0.082 Uiso 1 1 calc R U . . .
H23C H 0.987244 0.873497 1.019901 0.082 Uiso 1 1 calc R U . . .
C15 C 0.8185(7) 0.0182(4) 0.6730(3) 0.0585(19) Uani 0.620(4) 1 d . . P A 1
H15A H 0.832770 -0.058832 0.658133 0.088 Uiso 0.620(4) 1 calc R U P A 1
H15B H 0.745143 0.020665 0.702685 0.088 Uiso 0.620(4) 1 calc R U P A 1
H15C H 0.893989 0.059507 0.711891 0.088 Uiso 0.620(4) 1 calc R U P A 1
C17 C 0.6668(5) -0.0125(3) 0.5314(3) 0.0579(18) Uani 0.620(4) 1 d . . P A 1
H17A H 0.642363 0.014781 0.475637 0.087 Uiso 0.620(4) 1 calc R U P A 1
H17B H 0.596161 -0.011975 0.563770 0.087 Uiso 0.620(4) 1 calc R U P A 1
H17C H 0.687497 -0.088054 0.519765 0.087 Uiso 0.620(4) 1 calc R U P A 1
C16 C 0.8921(6) 0.0668(4) 0.5385(3) 0.063(2) Uani 0.620(4) 1 d . . P A 1
H16A H 0.967816 0.115905 0.570054 0.094 Uiso 0.620(4) 1 calc R U P A 1
H16B H 0.862445 0.091882 0.482556 0.094 Uiso 0.620(4) 1 calc R U P A 1
H16C H 0.913144 -0.008693 0.527255 0.094 Uiso 0.620(4) 1 calc R U P A 1
C18A C 0.9559(6) 0.0900(5) 0.6277(4) 0.0289(19) Uiso 0.380(4) 1 d . . P A 2
H18D H 0.990049 0.019299 0.620356 0.043 Uiso 0.380(4) 1 calc R U P A 2
H18E H 0.973909 0.122160 0.689825 0.043 Uiso 0.380(4) 1 calc R U P A 2
H18F H 0.995917 0.140649 0.593666 0.043 Uiso 0.380(4) 1 calc R U P A 2
C17A C 0.7797(8) 0.0170(6) 0.5003(4) 0.039(2) Uiso 0.380(4) 1 d . . P A 2
H17D H 0.689320 0.000398 0.474250 0.058 Uiso 0.380(4) 1 calc R U P A 2
H17E H 0.818412 -0.051725 0.498292 0.058 Uiso 0.380(4) 1 calc R U P A 2
H17F H 0.822160 0.067189 0.467167 0.058 Uiso 0.380(4) 1 calc R U P A 2
C15A C 0.7479(9) 0.0005(7) 0.6500(6) 0.041(3) Uiso 0.380(4) 1 d . . P A 2
H15D H 0.654841 -0.012307 0.636957 0.062 Uiso 0.380(4) 1 calc R U P A 2
H15E H 0.776138 0.037755 0.710488 0.062 Uiso 0.380(4) 1 calc R U P A 2
H15F H 0.781657 -0.070359 0.642889 0.062 Uiso 0.380(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
Ni1 C33 1.905(3) . ?
Ni1 C24 1.923(2) . ?
Ni1 P1 2.2594(9) . ?
Ni1 P2 2.2646(9) 2_666 ?
P2 C2 1.860(2) . ?
P2 P1 2.1458(12) 2_666 ?
P1 C12 1.855(2) . ?
O1 C1 1.386(2) . ?
O1 C13 1.386(2) . ?
N1 C24 1.372(3) . ?
N1 C25 1.387(3) . ?
N1 C27 1.468(3) . ?
N3 C33 1.383(3) . ?
N3 C35 1.386(3) . ?
N3 C36 1.477(3) . ?
N4 C33 1.368(3) . ?
N4 C34 1.379(3) . ?
N4 C39 1.482(3) . ?
N2 C24 1.377(3) . ?
N2 C26 1.382(3) . ?
N2 C30 1.475(3) . ?
C1 C6 1.388(3) . ?
C1 C2 1.414(3) . ?
C13 C8 1.391(3) . ?
C13 C12 1.406(3) . ?
C12 C11 1.409(3) . ?
C2 C3 1.398(3) . ?
C11 C10 1.383(3) . ?
C6 C5 1.388(3) . ?
C6 C7 1.533(3) . ?
C7 C8 1.531(3) . ?
C7 C19 1.542(3) . ?
C7 C18 1.542(3) . ?
C8 C9 1.398(3) . ?
C5 C4 1.388(3) . ?
C3 C4 1.396(3) . ?
C10 C9 1.398(3) . ?
C10 C20 1.541(3) . ?
C39 C41 1.505(3) . ?
C39 C40 1.525(3) . ?
C30 C31 1.520(4) . ?
C30 C32 1.522(4) . ?
C38 C36 1.525(3) . ?
C4 C14 1.542(3) . ?
C36 C37 1.530(3) . ?
C20 C21 1.531(3) . ?
C20 C23 1.533(4) . ?
C20 C22 1.536(3) . ?
C27 C29 1.517(3) . ?
C27 C28 1.520(3) . ?
C25 C26 1.339(3) . ?
C35 C34 1.338(4) . ?
C14 C15A 1.438(9) . ?
C14 C16 1.443(5) . ?
C14 C17A 1.451(7) . ?
C14 C15 1.498(5) . ?
C14 C17 1.666(5) . ?
C14 C18A 1.731(7) . ?

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
C33 Ni1 C24 105.31(10) . . ?
C33 Ni1 P1 150.09(7) . . ?
C24 Ni1 P1 103.93(8) . . ?
C33 Ni1 P2 93.68(7) . 2_666 ?
C24 Ni1 P2 160.13(7) . 2_666 ?
P1 Ni1 P2 56.63(3) . 2_666 ?
C2 P2 P1 98.25(7) . 2_666 ?
C2 P2 Ni1 105.13(7) . 2_666 ?
P1 P2 Ni1 61.56(3) 2_666 2_666 ?
C12 P1 P2 106.14(8) . 2_666 ?
C12 P1 Ni1 94.13(8) . . ?
P2 P1 Ni1 61.81(3) 2_666 . ?
C1 O1 C13 119.82(17) . . ?
C24 N1 C25 112.2(2) . . ?
C24 N1 C27 123.43(18) . . ?
C25 N1 C27 124.3(2) . . ?
C33 N3 C35 110.8(2) . . ?
C33 N3 C36 124.3(2) . . ?
C35 N3 C36 124.8(2) . . ?
C33 N4 C34 112.2(2) . . ?
C33 N4 C39 122.8(2) . . ?
C34 N4 C39 124.7(2) . . ?
C24 N2 C26 112.2(2) . . ?
C24 N2 C30 124.79(18) . . ?
C26 N2 C30 122.9(2) . . ?
O1 C1 C6 121.85(18) . . ?
O1 C1 C2 115.40(19) . . ?
C6 C1 C2 122.8(2) . . ?
O1 C13 C8 121.78(19) . . ?
O1 C13 C12 115.52(19) . . ?
C8 C13 C12 122.69(19) . . ?
C13 C12 C11 115.9(2) . . ?
C13 C12 P1 129.48(16) . . ?
C11 C12 P1 114.60(17) . . ?
C3 C2 C1 116.1(2) . . ?
C3 C2 P2 124.84(16) . . ?
C1 C2 P2 119.01(16) . . ?
C10 C11 C12 123.8(2) . . ?
C1 C6 C5 117.70(19) . . ?
C1 C6 C7 121.5(2) . . ?
C5 C6 C7 120.8(2) . . ?
C8 C7 C6 109.91(18) . . ?
C8 C7 C19 111.30(19) . . ?
C6 C7 C19 110.20(19) . . ?
C8 C7 C18 107.4(2) . . ?
C6 C7 C18 108.25(19) . . ?
C19 C7 C18 109.6(2) . . ?
C13 C8 C9 117.9(2) . . ?
C13 C8 C7 121.05(19) . . ?
C9 C8 C7 120.9(2) . . ?
C4 C5 C6 122.8(2) . . ?
C4 C3 C2 123.2(2) . . ?
C11 C10 C9 117.2(2) . . ?
C11 C10 C20 123.3(2) . . ?
C9 C10 C20 119.6(2) . . ?
N4 C33 N3 102.8(2) . . ?
N4 C33 Ni1 127.38(17) . . ?
N3 C33 Ni1 129.76(19) . . ?
C10 C9 C8 122.3(2) . . ?
N1 C24 N2 102.11(18) . . ?
N1 C24 Ni1 126.47(16) . . ?
N2 C24 Ni1 131.42(17) . . ?
N4 C39 C41 110.8(2) . . ?
N4 C39 C40 109.98(19) . . ?
C41 C39 C40 111.3(2) . . ?
N2 C30 C31 110.6(2) . . ?
N2 C30 C32 110.4(2) . . ?
C31 C30 C32 111.4(2) . . ?
C5 C4 C3 117.3(2) . . ?
C5 C4 C14 121.3(2) . . ?
C3 C4 C14 121.3(2) . . ?
N3 C36 C38 112.48(19) . . ?
N3 C36 C37 109.8(2) . . ?
C38 C36 C37 110.6(2) . . ?
C21 C20 C23 109.2(2) . . ?
C21 C20 C22 107.3(2) . . ?
C23 C20 C22 108.7(2) . . ?
C21 C20 C10 110.2(2) . . ?
C23 C20 C10 109.6(2) . . ?
C22 C20 C10 111.8(2) . . ?
N1 C27 C29 111.1(2) . . ?
N1 C27 C28 110.3(2) . . ?
C29 C27 C28 113.4(2) . . ?
C26 C25 N1 106.7(2) . . ?
C25 C26 N2 106.9(2) . . ?
C34 C35 N3 107.5(2) . . ?
C35 C34 N4 106.7(2) . . ?
C15A C14 C17A 116.0(5) . . ?
C16 C14 C15 115.4(4) . . ?
C15A C14 C4 111.6(4) . . ?
C16 C14 C4 110.8(3) . . ?
C17A C14 C4 115.8(4) . . ?
C15 C14 C4 114.2(3) . . ?
C16 C14 C17 106.6(3) . . ?
C15 C14 C17 103.4(4) . . ?
C4 C14 C17 105.3(3) . . ?
C15A C14 C18A 103.0(4) . . ?
C17A C14 C18A 103.9(4) . . ?
C4 C14 C18A 104.6(3) . . ?

_refine_diff_density_max         0.352
_refine_diff_density_min         -0.295
_refine_diff_density_rms         0.056



####################################################################### 
# 
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 2357712'
loop_
_audit_author_name
_audit_author_address
'Terrance Hadlington'
;TU Munich
Germany
;
_audit_update_record             
;
2024-05-23 deposited with the CCDC.	2024-07-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C72 H108 N4 Ni2 O4 P4'
_chemical_formula_sum            'C72 H108 N4 Ni2 O4 P4'
_chemical_formula_weight         1334.92

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 '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                   9.912(2)
_cell_length_b                   14.075(3)
_cell_length_c                   15.094(3)
_cell_angle_alpha                66.91(3)
_cell_angle_beta                 70.89(3)
_cell_angle_gamma                76.79(3)
_cell_volume                     1818.3(8)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    2000
_cell_measurement_theta_min      1.92
_cell_measurement_theta_max      32.50

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.219
_exptl_crystal_F_000             716
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_exptl_absorpt_coefficient_mu    0.654
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.760
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'STOE X-AREA 1.76'

_diffrn_ambient_temperature      150(2)
_diffrn_source                   'Genix 3D HF Mo'
_diffrn_source_voltage           50
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_collimation    '0.6 mm diameter'
_diffrn_measurement_device_type  'STOE StadiVari'
_diffrn_measurement_method       'ω scans'
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_reflns_number            24420
_diffrn_reflns_av_unetI/netI     0.1514
_diffrn_reflns_av_R_equivalents  0.0886
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.189
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             7148
_reflns_number_gt                3550
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0595P)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         7148
_refine_ls_number_parameters     404
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1592
_refine_ls_R_factor_gt           0.0644
_refine_ls_wR_factor_ref         0.1483
_refine_ls_wR_factor_gt          0.1155
_refine_ls_goodness_of_fit_ref   0.964
_refine_ls_restrained_S_all      0.964
_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
Ni1 Ni 0.88528(7) 0.45134(4) 0.57029(5) 0.0331(2) Uani 1 1 d . . . . .
P1 P 0.89485(13) 0.53970(9) 0.40595(10) 0.0324(3) Uani 1 1 d . . . . .
P2 P 0.91430(14) 0.43249(9) 0.71687(10) 0.0350(3) Uani 1 1 d . . . . .
O1 O 0.7772(3) 0.6247(2) 0.5727(2) 0.0347(8) Uani 1 1 d . . . . .
N2 N 0.7331(4) 0.2836(3) 0.5981(3) 0.0377(10) Uani 1 1 d . . . . .
N1 N 0.5822(4) 0.3947(3) 0.6566(3) 0.0371(10) Uani 1 1 d . . . . .
C1 C 0.7771(5) 0.7053(3) 0.4807(4) 0.0337(12) Uani 1 1 d . . . . .
C12 C 0.8626(5) 0.5676(3) 0.7168(4) 0.0331(11) Uani 1 1 d . . . . .
O2 O 0.5949(5) 1.2447(3) -0.0173(3) 0.0726(13) Uani 1 1 d . . . . .
C2 C 0.8276(5) 0.6760(3) 0.3965(4) 0.0335(12) Uani 1 1 d . . . . .
C6 C 0.7281(5) 0.8061(3) 0.4792(4) 0.0347(12) Uani 1 1 d . . . . .
C13 C 0.7999(5) 0.6485(3) 0.6474(4) 0.0334(12) Uani 1 1 d . . . . .
C24 C 0.7249(5) 0.3751(3) 0.6124(4) 0.0323(11) Uani 1 1 d . . . . .
C3 C 0.8228(5) 0.7552(3) 0.3067(4) 0.0349(12) Uani 1 1 d . . . . .
H3 H 0.854674 0.738213 0.247569 0.042 Uiso 1 1 calc R U . . .
C7 C 0.6743(5) 0.8275(3) 0.5779(4) 0.0367(12) Uani 1 1 d . . . . .
C4 C 0.7737(5) 0.8586(3) 0.2983(4) 0.0353(12) Uani 1 1 d . . . . .
C5 C 0.7270(5) 0.8824(3) 0.3859(4) 0.0367(12) Uani 1 1 d . . . . .
H5 H 0.693510 0.952451 0.381910 0.044 Uiso 1 1 calc R U . . .
C11 C 0.8855(5) 0.5924(4) 0.7907(4) 0.0406(13) Uani 1 1 d . . . . .
H11 H 0.926965 0.538736 0.839525 0.049 Uiso 1 1 calc R U . . .
C10 C 0.8510(5) 0.6920(4) 0.7976(4) 0.0372(12) Uani 1 1 d . . . . .
C27 C 0.5142(5) 0.4885(4) 0.6809(4) 0.0432(13) Uani 1 1 d . . . . .
H27 H 0.590510 0.520121 0.686345 0.052 Uiso 1 1 calc R U . . .
C9 C 0.7849(5) 0.7691(4) 0.7266(4) 0.0407(13) Uani 1 1 d . . . . .
H9 H 0.757719 0.837020 0.730091 0.049 Uiso 1 1 calc R U . . .
C8 C 0.7582(5) 0.7481(4) 0.6511(4) 0.0369(12) Uani 1 1 d . . . . .
C20 C 0.8873(6) 0.7153(4) 0.8772(4) 0.0429(13) Uani 1 1 d . . . . .
C14 C 0.7697(5) 0.9460(3) 0.1973(4) 0.0391(13) Uani 1 1 d . . . . .
C30 C 0.8660(6) 0.2276(4) 0.5556(4) 0.0465(14) Uani 1 1 d . . . . .
H30 H 0.946431 0.268764 0.538858 0.056 Uiso 1 1 calc R U . . .
C19 C 0.6917(6) 0.9401(3) 0.5610(4) 0.0445(14) Uani 1 1 d . . . . .
H19A H 0.793224 0.951259 0.531422 0.067 Uiso 1 1 calc R U . . .
H19B H 0.657845 0.951579 0.625128 0.067 Uiso 1 1 calc R U . . .
H19C H 0.634968 0.988854 0.515809 0.067 Uiso 1 1 calc R U . . .
C26 C 0.5981(5) 0.2493(4) 0.6308(4) 0.0430(14) Uani 1 1 d . . . . .
C17 C 0.6144(6) 0.9988(4) 0.2000(4) 0.0518(15) Uani 1 1 d . . . . .
H17A H 0.578965 1.028086 0.253677 0.078 Uiso 1 1 calc R U . . .
H17B H 0.552687 0.947234 0.212053 0.078 Uiso 1 1 calc R U . . .
H17C H 0.613057 1.054508 0.135846 0.078 Uiso 1 1 calc R U . . .
C18 C 0.5146(5) 0.8096(4) 0.6254(4) 0.0475(14) Uani 1 1 d . . . . .
H18A H 0.458616 0.853351 0.577814 0.071 Uiso 1 1 calc R U . . .
H18B H 0.478837 0.827606 0.686126 0.071 Uiso 1 1 calc R U . . .
H18C H 0.504951 0.736288 0.642246 0.071 Uiso 1 1 calc R U . . .
C25 C 0.5049(6) 0.3179(4) 0.6673(4) 0.0427(13) Uani 1 1 d . . . . .
C32 C 0.8605(6) 0.2204(4) 0.4594(4) 0.0578(17) Uani 1 1 d . . . . .
H32A H 0.779386 0.183345 0.472857 0.087 Uiso 1 1 calc R U . . .
H32B H 0.950222 0.182568 0.432060 0.087 Uiso 1 1 calc R U . . .
H32C H 0.848210 0.290516 0.411039 0.087 Uiso 1 1 calc R U . . .
C29 C 0.4532(6) 0.5667(4) 0.5967(5) 0.0627(18) Uani 1 1 d . . . . .
H29A H 0.529609 0.581488 0.534009 0.094 Uiso 1 1 calc R U . . .
H29B H 0.413625 0.631114 0.611187 0.094 Uiso 1 1 calc R U . . .
H29C H 0.376843 0.538124 0.590345 0.094 Uiso 1 1 calc R U . . .
C15 C 0.8235(6) 0.9049(4) 0.1099(4) 0.0557(16) Uani 1 1 d . . . . .
H15A H 0.822870 0.963133 0.047150 0.084 Uiso 1 1 calc R U . . .
H15B H 0.760243 0.855476 0.119371 0.084 Uiso 1 1 calc R U . . .
H15C H 0.921551 0.869999 0.107298 0.084 Uiso 1 1 calc R U . . .
C23 C 0.8280(7) 0.8254(4) 0.8784(5) 0.0628(17) Uani 1 1 d . . . . .
H23A H 0.868201 0.876267 0.813202 0.094 Uiso 1 1 calc R U . . .
H23B H 0.854825 0.836457 0.930336 0.094 Uiso 1 1 calc R U . . .
H23C H 0.723014 0.834044 0.892414 0.094 Uiso 1 1 calc R U . . .
C21 C 1.0506(6) 0.7035(5) 0.8570(5) 0.0654(18) Uani 1 1 d . . . . .
H21A H 1.090111 0.632404 0.859167 0.098 Uiso 1 1 calc R U . . .
H21B H 1.074957 0.717976 0.908098 0.098 Uiso 1 1 calc R U . . .
H21C H 1.091517 0.752703 0.790957 0.098 Uiso 1 1 calc R U . . .
C31 C 0.8960(6) 0.1222(4) 0.6322(5) 0.0624(18) Uani 1 1 d . . . . .
H31A H 0.908035 0.131841 0.689949 0.094 Uiso 1 1 calc R U . . .
H31B H 0.984027 0.084834 0.602319 0.094 Uiso 1 1 calc R U . . .
H31C H 0.815224 0.081882 0.653882 0.094 Uiso 1 1 calc R U . . .
C16 C 0.8649(7) 1.0270(4) 0.1775(4) 0.0671(19) Uani 1 1 d . . . . .
H16A H 0.860470 1.083380 0.114286 0.101 Uiso 1 1 calc R U . . .
H16B H 0.964302 0.994572 0.173623 0.101 Uiso 1 1 calc R U . . .
H16C H 0.831131 1.055218 0.232005 0.101 Uiso 1 1 calc R U . . .
C28 C 0.4013(7) 0.4624(5) 0.7812(5) 0.075(2) Uani 1 1 d . . . . .
H28A H 0.319443 0.439222 0.775586 0.113 Uiso 1 1 calc R U . . .
H28B H 0.368622 0.524398 0.800631 0.113 Uiso 1 1 calc R U . . .
H28C H 0.443218 0.406917 0.831959 0.113 Uiso 1 1 calc R U . . .
C35 C 0.6561(7) 1.3257(5) -0.0165(5) 0.077(2) Uani 1 1 d . . . . .
H35A H 0.651981 1.387272 -0.077333 0.093 Uiso 1 1 calc R U . . .
H35B H 0.758259 1.302911 -0.016352 0.093 Uiso 1 1 calc R U . . .
C22 C 0.8231(7) 0.6391(4) 0.9811(4) 0.072(2) Uani 1 1 d . . . . .
H22A H 0.717968 0.650044 0.995906 0.108 Uiso 1 1 calc R U . . .
H22B H 0.853041 0.651131 1.031256 0.108 Uiso 1 1 calc R U . . .
H22C H 0.857217 0.567625 0.982498 0.108 Uiso 1 1 calc R U . . .
C34 C 0.6737(7) 1.2057(5) -0.0955(5) 0.0735(19) Uani 1 1 d . . . . .
H34A H 0.771380 1.175704 -0.087522 0.088 Uiso 1 1 calc R U . . .
H34B H 0.683101 1.263018 -0.160735 0.088 Uiso 1 1 calc R U . . .
C36 C 0.5764(9) 1.3535(6) 0.0734(6) 0.105(3) Uani 1 1 d . . . . .
H36A H 0.474941 1.374542 0.073715 0.157 Uiso 1 1 calc R U . . .
H36B H 0.617107 1.411097 0.072654 0.157 Uiso 1 1 calc R U . . .
H36C H 0.584225 1.293145 0.133462 0.157 Uiso 1 1 calc R U . . .
C33 C 0.5977(8) 1.1241(5) -0.0928(5) 0.087(2) Uani 1 1 d . . . . .
H33A H 0.596724 1.064643 -0.030838 0.130 Uiso 1 1 calc R U . . .
H33B H 0.647694 1.101473 -0.150194 0.130 Uiso 1 1 calc R U . . .
H33C H 0.498695 1.152749 -0.095738 0.130 Uiso 1 1 calc R U . . .
H25 H 0.391611 0.312415 0.708008 0.064(16) Uiso 1 1 d R . . . .
H26 H 0.580701 0.175315 0.631008 0.046(14) Uiso 1 1 d R . . . .


_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 C24 1.916(5) . ?
Ni1 P2 2.2292(16) . ?
Ni1 P1 2.2781(17) . ?
Ni1 P1 2.3594(15) 2_766 ?
Ni1 Ni1 2.7453(18) 2_766 ?
P1 C2 1.846(4) . ?
P1 P2 2.155(2) 2_766 ?
P2 C12 1.853(5) . ?
O1 C13 1.391(5) . ?
O1 C1 1.407(5) . ?
N2 C24 1.367(6) . ?
N2 C26 1.394(6) . ?
N2 C30 1.462(6) . ?
N1 C24 1.367(6) . ?
N1 C25 1.394(6) . ?
N1 C27 1.464(6) . ?
C1 C6 1.384(6) . ?
C1 C2 1.392(6) . ?
C12 C11 1.387(6) . ?
C12 C13 1.396(6) . ?
O2 C35 1.415(7) . ?
O2 C34 1.418(7) . ?
C2 C3 1.383(6) . ?
C6 C5 1.399(6) . ?
C6 C7 1.534(7) . ?
C13 C8 1.386(6) . ?
C3 C4 1.393(6) . ?
C7 C8 1.539(6) . ?
C7 C18 1.544(7) . ?
C7 C19 1.544(6) . ?
C4 C5 1.396(7) . ?
C4 C14 1.545(6) . ?
C11 C10 1.401(6) . ?
C10 C9 1.406(6) . ?
C10 C20 1.525(7) . ?
C27 C29 1.514(7) . ?
C27 C28 1.525(7) . ?
C9 C8 1.397(7) . ?
C20 C21 1.529(7) . ?
C20 C23 1.533(7) . ?
C20 C22 1.534(7) . ?
C14 C16 1.522(7) . ?
C14 C15 1.536(7) . ?
C14 C17 1.544(6) . ?
C30 C32 1.513(7) . ?
C30 C31 1.518(7) . ?
C26 C25 1.329(7) . ?
C35 C36 1.481(9) . ?
C34 C33 1.492(8) . ?

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
C24 Ni1 P2 101.22(15) . . ?
C24 Ni1 P1 101.52(15) . . ?
P2 Ni1 P1 153.45(5) . . ?
C24 Ni1 P1 147.39(14) . 2_766 ?
P2 Ni1 P1 55.92(6) . 2_766 ?
P1 Ni1 P1 107.43(6) . 2_766 ?
C24 Ni1 Ni1 152.84(15) . 2_766 ?
P2 Ni1 Ni1 105.11(5) . 2_766 ?
P1 Ni1 Ni1 55.09(5) . 2_766 ?
P1 Ni1 Ni1 52.34(4) 2_766 2_766 ?
C2 P1 P2 98.32(17) . 2_766 ?
C2 P1 Ni1 105.59(17) . . ?
P2 P1 Ni1 126.69(7) 2_766 . ?
C2 P1 Ni1 93.20(16) . 2_766 ?
P2 P1 Ni1 58.98(5) 2_766 2_766 ?
Ni1 P1 Ni1 72.57(6) . 2_766 ?
C12 P2 P1 97.49(16) . 2_766 ?
C12 P2 Ni1 100.92(16) . . ?
P1 P2 Ni1 65.10(6) 2_766 . ?
C13 O1 C1 117.7(4) . . ?
C24 N2 C26 111.2(4) . . ?
C24 N2 C30 124.8(4) . . ?
C26 N2 C30 124.0(4) . . ?
C24 N1 C25 111.1(4) . . ?
C24 N1 C27 125.5(4) . . ?
C25 N1 C27 123.1(4) . . ?
C6 C1 C2 124.7(5) . . ?
C6 C1 O1 119.3(4) . . ?
C2 C1 O1 116.0(4) . . ?
C11 C12 C13 116.1(4) . . ?
C11 C12 P2 119.1(4) . . ?
C13 C12 P2 124.8(4) . . ?
C35 O2 C34 113.5(5) . . ?
C3 C2 C1 115.6(4) . . ?
C3 C2 P1 123.0(4) . . ?
C1 C2 P1 121.4(4) . . ?
C1 C6 C5 116.7(5) . . ?
C1 C6 C7 119.3(4) . . ?
C5 C6 C7 124.0(4) . . ?
C8 C13 O1 119.9(4) . . ?
C8 C13 C12 123.5(5) . . ?
O1 C13 C12 116.6(4) . . ?
N2 C24 N1 103.5(4) . . ?
N2 C24 Ni1 123.9(3) . . ?
N1 C24 Ni1 132.5(3) . . ?
C2 C3 C4 123.6(5) . . ?
C6 C7 C8 108.6(4) . . ?
C6 C7 C18 109.6(4) . . ?
C8 C7 C18 106.8(4) . . ?
C6 C7 C19 111.0(4) . . ?
C8 C7 C19 111.2(4) . . ?
C18 C7 C19 109.5(4) . . ?
C3 C4 C5 117.6(5) . . ?
C3 C4 C14 122.8(5) . . ?
C5 C4 C14 119.6(4) . . ?
C4 C5 C6 121.9(4) . . ?
C12 C11 C10 123.9(5) . . ?
C11 C10 C9 116.9(5) . . ?
C11 C10 C20 121.1(5) . . ?
C9 C10 C20 122.0(4) . . ?
N1 C27 C29 109.8(4) . . ?
N1 C27 C28 111.2(4) . . ?
C29 C27 C28 112.4(5) . . ?
C8 C9 C10 121.6(4) . . ?
C13 C8 C9 118.0(5) . . ?
C13 C8 C7 118.8(4) . . ?
C9 C8 C7 123.1(4) . . ?
C10 C20 C21 108.9(4) . . ?
C10 C20 C23 112.8(4) . . ?
C21 C20 C23 108.3(5) . . ?
C10 C20 C22 110.0(4) . . ?
C21 C20 C22 109.5(5) . . ?
C23 C20 C22 107.3(5) . . ?
C16 C14 C15 108.2(5) . . ?
C16 C14 C17 109.0(4) . . ?
C15 C14 C17 107.9(4) . . ?
C16 C14 C4 109.5(4) . . ?
C15 C14 C4 112.1(4) . . ?
C17 C14 C4 110.0(4) . . ?
N2 C30 C32 110.6(4) . . ?
N2 C30 C31 110.3(5) . . ?
C32 C30 C31 113.0(5) . . ?
C25 C26 N2 107.0(4) . . ?
C26 C25 N1 107.2(4) . . ?
O2 C35 C36 109.7(6) . . ?
O2 C34 C33 109.5(6) . . ?

_refine_diff_density_max         0.396
_refine_diff_density_min         -0.453
_refine_diff_density_rms         0.079



####################################################################### 
# 
# 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_2b_prime
_database_code_depnum_ccdc_archive 'CCDC 2357714'
loop_
_audit_author_name
_audit_author_address
'Terrance Hadlington'
;TU Munich
Germany
;
_audit_update_record             
;
2024-05-23 deposited with the CCDC.	2024-07-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C22.50 H34 N2 Ni0.50 O P'
_chemical_formula_sum            'C22.50 H34 N2 Ni0.50 O P'
_chemical_formula_weight         408.84

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 '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                   15.304(3)
_cell_length_b                   34.054(7)
_cell_length_c                   9.7484(19)
_cell_angle_alpha                90
_cell_angle_beta                 97.35(3)
_cell_angle_gamma                90
_cell_volume                     5038.9(18)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    2000
_cell_measurement_theta_min      1.92
_cell_measurement_theta_max      32.50

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.078
_exptl_crystal_F_000             1760
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_exptl_absorpt_coefficient_mu    0.484
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.899
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'STOE X-AREA 1.76'

_diffrn_ambient_temperature      150(2)
_diffrn_source                   'Genix 3D HF Mo'
_diffrn_source_voltage           50
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_collimation    '0.6 mm diameter'
_diffrn_measurement_device_type  'STOE StadiVari'
_diffrn_measurement_method       'ω scans'
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_reflns_number            38479
_diffrn_reflns_av_unetI/netI     0.2289
_diffrn_reflns_av_R_equivalents  0.1622
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.190
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             9847
_reflns_number_gt                3922
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1144P)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         9847
_refine_ls_number_parameters     503
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.2087
_refine_ls_R_factor_gt           0.0772
_refine_ls_wR_factor_ref         0.2419
_refine_ls_wR_factor_gt          0.1869
_refine_ls_goodness_of_fit_ref   0.894
_refine_ls_restrained_S_all      0.894
_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
Ni1 Ni 0.49767(5) 0.39037(2) 0.43668(9) 0.0291(3) Uani 1 1 d . . . . .
P1 P 0.51382(11) 0.45434(5) 0.48667(18) 0.0274(4) Uani 1 1 d . . . . .
P2 P 0.50883(11) 0.58445(5) 0.35007(18) 0.0283(4) Uani 1 1 d . . . . .
O1 O 0.6308(3) 0.50855(12) 0.3475(4) 0.0290(11) Uani 1 1 d . . . . .
N2 N 0.5940(4) 0.38342(16) 0.1967(6) 0.0390(15) Uani 1 1 d . . . . .
N4 N 0.4092(4) 0.31440(16) 0.3737(6) 0.0381(15) Uani 1 1 d . . . . .
N1 N 0.4781(4) 0.41855(16) 0.1460(6) 0.0356(14) Uani 1 1 d . . . . .
N3 N 0.5168(4) 0.30808(16) 0.5377(6) 0.0385(15) Uani 1 1 d . . . . .
C12 C 0.6358(4) 0.45594(18) 0.5118(7) 0.0280(15) Uani 1 1 d . . . . .
C13 C 0.6801(4) 0.48040(18) 0.4285(7) 0.0287(15) Uani 1 1 d . . . . .
C2 C 0.6284(4) 0.57881(19) 0.3402(7) 0.0291(16) Uani 1 1 d . . . . .
C1 C 0.6751(4) 0.54425(19) 0.3353(6) 0.0291(15) Uani 1 1 d . . . . .
C11 C 0.6895(4) 0.43199(19) 0.6041(7) 0.0314(16) Uani 1 1 d . . . . .
H11 H 0.661867 0.415525 0.664374 0.038 Uiso 1 1 calc R U . . .
C6 C 0.7641(4) 0.5439(2) 0.3179(7) 0.0301(16) Uani 1 1 d . . . . .
C9 C 0.8205(4) 0.4541(2) 0.5180(7) 0.0347(17) Uani 1 1 d . . . . .
H9 H 0.882458 0.452857 0.517186 0.042 Uiso 1 1 calc R U . . .
C3 C 0.6752(4) 0.6138(2) 0.3229(6) 0.0324(16) Uani 1 1 d . . . . .
H3 H 0.644381 0.637959 0.324787 0.039 Uiso 1 1 calc R U . . .
C24 C 0.5223(4) 0.39757(19) 0.2527(7) 0.0341(17) Uani 1 1 d . . . . .
C33 C 0.4739(4) 0.33563(19) 0.4511(7) 0.0327(17) Uani 1 1 d . . . . .
C4 C 0.7623(4) 0.6152(2) 0.3033(7) 0.0331(16) Uani 1 1 d . . . . .
C8 C 0.7712(4) 0.47875(19) 0.4255(7) 0.0306(16) Uani 1 1 d . . . . .
C5 C 0.8063(5) 0.5789(2) 0.3027(7) 0.0341(17) Uani 1 1 d . . . . .
H5 H 0.867086 0.578680 0.291459 0.041 Uiso 1 1 calc R U . . .
C14 C 0.8137(4) 0.6532(2) 0.2839(8) 0.0371(18) Uani 1 1 d . . . . .
C7 C 0.8075(4) 0.50358(19) 0.3148(7) 0.0316(16) Uani 1 1 d . . . . .
C10 C 0.7824(4) 0.43087(19) 0.6129(7) 0.0344(17) Uani 1 1 d . . . . .
C30 C 0.6607(5) 0.35843(19) 0.2730(8) 0.0397(18) Uani 1 1 d . . . . .
H30 H 0.651204 0.359136 0.372537 0.048 Uiso 1 1 calc R U . . .
C29 C 0.4138(5) 0.4848(2) 0.1379(8) 0.049(2) Uani 1 1 d . . . . .
H29A H 0.462949 0.493545 0.205400 0.074 Uiso 1 1 calc R U . . .
H29B H 0.360458 0.499398 0.152164 0.074 Uiso 1 1 calc R U . . .
H29C H 0.427889 0.489748 0.044102 0.074 Uiso 1 1 calc R U . . .
C26 C 0.5927(6) 0.3952(2) 0.0600(8) 0.050(2) Uani 1 1 d . . . . .
H26 H 0.634568 0.388597 -0.000265 0.059 Uiso 1 1 calc R U . . .
C25 C 0.5218(6) 0.4172(2) 0.0299(8) 0.047(2) Uani 1 1 d . . . . .
H25 H 0.503895 0.429899 -0.055951 0.056 Uiso 1 1 calc R U . . .
C34 C 0.4114(5) 0.2752(2) 0.4109(9) 0.052(2) Uani 1 1 d . . . . .
H34 H 0.372970 0.255098 0.371804 0.063 Uiso 1 1 calc R U . . .
C36 C 0.3488(5) 0.3309(2) 0.2612(8) 0.045(2) Uani 1 1 d . . . . .
H36 H 0.355437 0.360124 0.264614 0.054 Uiso 1 1 calc R U . . .
C39 C 0.5898(5) 0.3171(2) 0.6444(8) 0.047(2) Uani 1 1 d . . . . .
H39 H 0.605351 0.345453 0.635524 0.056 Uiso 1 1 calc R U . . .
C27 C 0.3985(5) 0.4414(2) 0.1563(8) 0.0407(18) Uani 1 1 d . . . . .
H27 H 0.381288 0.437293 0.250815 0.049 Uiso 1 1 calc R U . . .
C19 C 0.9091(4) 0.5060(2) 0.3370(8) 0.0439(19) Uani 1 1 d . . . . .
H19A H 0.929511 0.520943 0.261352 0.066 Uiso 1 1 calc R U . . .
H19B H 0.933864 0.479400 0.338668 0.066 Uiso 1 1 calc R U . . .
H19C H 0.928539 0.519075 0.425184 0.066 Uiso 1 1 calc R U . . .
C16 C 0.8899(5) 0.6575(2) 0.4019(8) 0.050(2) Uani 1 1 d . . . . .
H16A H 0.866014 0.659895 0.490152 0.075 Uiso 1 1 calc R U . . .
H16B H 0.924244 0.680978 0.386507 0.075 Uiso 1 1 calc R U . . .
H16C H 0.927933 0.634271 0.404400 0.075 Uiso 1 1 calc R U . . .
C15 C 0.8528(5) 0.6515(2) 0.1466(8) 0.048(2) Uani 1 1 d . . . . .
H15A H 0.895356 0.629911 0.149603 0.073 Uiso 1 1 calc R U . . .
H15B H 0.882518 0.676358 0.132051 0.073 Uiso 1 1 calc R U . . .
H15C H 0.805446 0.647134 0.070443 0.073 Uiso 1 1 calc R U . . .
C35 C 0.4789(5) 0.2711(2) 0.5142(9) 0.052(2) Uani 1 1 d . . . . .
H35 H 0.497017 0.247531 0.561568 0.062 Uiso 1 1 calc R U . . .
C18 C 0.7807(5) 0.4839(2) 0.1715(7) 0.0457(19) Uani 1 1 d . . . . .
H18A H 0.716900 0.479435 0.157839 0.068 Uiso 1 1 calc R U . . .
H18B H 0.811444 0.458785 0.168136 0.068 Uiso 1 1 calc R U . . .
H18C H 0.796758 0.501206 0.098353 0.068 Uiso 1 1 calc R U . . .
C20 C 0.8365(5) 0.4051(2) 0.7166(8) 0.045(2) Uani 1 1 d . . . . .
C28 C 0.3227(5) 0.4262(2) 0.0499(9) 0.055(2) Uani 1 1 d . . . . .
H28A H 0.338277 0.429776 -0.043717 0.083 Uiso 1 1 calc R U . . .
H28B H 0.268847 0.440964 0.059530 0.083 Uiso 1 1 calc R U . . .
H28C H 0.312880 0.398269 0.066386 0.083 Uiso 1 1 calc R U . . .
C17 C 0.7545(5) 0.6894(2) 0.2813(9) 0.051(2) Uani 1 1 d . . . . .
H17A H 0.705451 0.686655 0.206772 0.077 Uiso 1 1 calc R U . . .
H17B H 0.788762 0.712866 0.265222 0.077 Uiso 1 1 calc R U . . .
H17C H 0.731409 0.691776 0.370090 0.077 Uiso 1 1 calc R U . . .
C41 C 0.6709(5) 0.2924(2) 0.6229(9) 0.060(2) Uani 1 1 d . . . . .
H41A H 0.657209 0.264518 0.631901 0.091 Uiso 1 1 calc R U . . .
H41B H 0.720216 0.299593 0.692644 0.091 Uiso 1 1 calc R U . . .
H41C H 0.686985 0.297452 0.530349 0.091 Uiso 1 1 calc R U . . .
C38 C 0.3731(6) 0.3168(3) 0.1224(8) 0.067(3) Uani 1 1 d . . . . .
H38A H 0.436635 0.319929 0.120987 0.101 Uiso 1 1 calc R U . . .
H38B H 0.341071 0.332339 0.047652 0.101 Uiso 1 1 calc R U . . .
H38C H 0.357239 0.289035 0.109485 0.101 Uiso 1 1 calc R U . . .
C31 C 0.7534(5) 0.3737(2) 0.2637(9) 0.057(2) Uani 1 1 d . . . . .
H31A H 0.764685 0.373349 0.167022 0.085 Uiso 1 1 calc R U . . .
H31B H 0.796395 0.356853 0.318967 0.085 Uiso 1 1 calc R U . . .
H31C H 0.758684 0.400600 0.299233 0.085 Uiso 1 1 calc R U . . .
C32 C 0.6482(5) 0.3155(2) 0.2229(9) 0.055(2) Uani 1 1 d . . . . .
H32A H 0.590768 0.305888 0.242776 0.083 Uiso 1 1 calc R U . . .
H32B H 0.695001 0.299148 0.271212 0.083 Uiso 1 1 calc R U . . .
H32C H 0.650753 0.314355 0.123104 0.083 Uiso 1 1 calc R U . . .
C37 C 0.2551(5) 0.3214(3) 0.2775(10) 0.074(3) Uani 1 1 d . . . . .
H37A H 0.245755 0.292998 0.267530 0.112 Uiso 1 1 calc R U . . .
H37B H 0.215602 0.335174 0.206353 0.112 Uiso 1 1 calc R U . . .
H37C H 0.242754 0.329714 0.369285 0.112 Uiso 1 1 calc R U . . .
C21 C 0.7878(5) 0.3896(3) 0.8291(9) 0.065(3) Uani 1 1 d . . . . .
H21A H 0.764364 0.411565 0.878020 0.098 Uiso 1 1 calc R U . . .
H21B H 0.828082 0.374137 0.894325 0.098 Uiso 1 1 calc R U . . .
H21C H 0.739097 0.372870 0.788501 0.098 Uiso 1 1 calc R U . . .
C40 C 0.5632(6) 0.3108(3) 0.7873(8) 0.066(3) Uani 1 1 d . . . . .
H40A H 0.512002 0.327268 0.798360 0.100 Uiso 1 1 calc R U . . .
H40B H 0.612317 0.318022 0.857381 0.100 Uiso 1 1 calc R U . . .
H40C H 0.548084 0.283160 0.798477 0.100 Uiso 1 1 calc R U . . .
C22 C 0.8660(7) 0.3683(3) 0.6384(10) 0.088(3) Uani 1 1 d . . . . .
H22A H 0.813818 0.353775 0.597439 0.132 Uiso 1 1 calc R U . . .
H22B H 0.902509 0.351324 0.703614 0.132 Uiso 1 1 calc R U . . .
H22C H 0.900075 0.376764 0.565151 0.132 Uiso 1 1 calc R U . . .
C23 C 0.9190(6) 0.4261(3) 0.7782(11) 0.096(4) Uani 1 1 d . . . . .
H23A H 0.953480 0.433679 0.704343 0.144 Uiso 1 1 calc R U . . .
H23B H 0.954244 0.408630 0.843390 0.144 Uiso 1 1 calc R U . . .
H23C H 0.903041 0.449674 0.827097 0.144 Uiso 1 1 calc R U . . .
C43 C 0.9315(8) 0.5517(4) 0.8801(12) 0.101(4) Uani 1 1 d . . . . .
H43A H 0.901948 0.556776 0.962978 0.121 Uiso 1 1 calc R U . . .
H43B H 0.977398 0.531490 0.903831 0.121 Uiso 1 1 calc R U . . .
C42 C 0.9708(10) 0.5873(4) 0.8373(14) 0.112(4) Uani 1 1 d . . . . .
H42A H 0.969027 0.607983 0.908115 0.135 Uiso 1 1 calc R U . . .
H42B H 1.033074 0.582575 0.824165 0.135 Uiso 1 1 calc R U . . .
C45 C 0.8455(11) 0.5758(4) 0.6882(13) 0.115(4) Uani 1 1 d . . . . .
H45A H 0.830593 0.571649 0.587428 0.138 Uiso 1 1 calc R U . . .
H45B H 0.795594 0.589325 0.723393 0.138 Uiso 1 1 calc R U . . .
C44 C 0.8643(9) 0.5373(4) 0.7613(15) 0.121(5) Uani 1 1 d . . . . .
H44A H 0.890030 0.517816 0.702473 0.145 Uiso 1 1 calc R U . . .
H44B H 0.811165 0.526098 0.794665 0.145 Uiso 1 1 calc R U . . .
O2 O 0.9235(12) 0.5984(5) 0.716(2) 0.326(13) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 C24 1.895(7) . ?
Ni1 C33 1.908(7) . ?
Ni1 P1 2.2390(19) . ?
Ni1 P2 2.263(2) 3_666 ?
P1 C12 1.853(6) . ?
P1 P2 2.131(3) 3_666 ?
P2 C2 1.854(7) . ?
O1 C13 1.400(7) . ?
O1 C1 1.405(7) . ?
N2 C24 1.374(8) . ?
N2 C26 1.390(9) . ?
N2 C30 1.457(8) . ?
N4 C33 1.371(8) . ?
N4 C34 1.382(9) . ?
N4 C36 1.454(9) . ?
N1 C24 1.367(8) . ?
N1 C25 1.388(9) . ?
N1 C27 1.459(9) . ?
N3 C33 1.373(8) . ?
N3 C35 1.392(8) . ?
N3 C39 1.458(9) . ?
C12 C13 1.398(8) . ?
C12 C11 1.400(8) . ?
C13 C8 1.400(9) . ?
C2 C1 1.382(9) . ?
C2 C3 1.412(9) . ?
C1 C6 1.395(8) . ?
C11 C10 1.414(9) . ?
C6 C5 1.375(9) . ?
C6 C7 1.525(9) . ?
C9 C8 1.384(9) . ?
C9 C10 1.399(9) . ?
C3 C4 1.371(9) . ?
C4 C5 1.406(9) . ?
C4 C14 1.540(9) . ?
C8 C7 1.530(9) . ?
C14 C17 1.528(10) . ?
C14 C15 1.535(10) . ?
C14 C16 1.536(10) . ?
C7 C19 1.545(9) . ?
C7 C18 1.556(9) . ?
C10 C20 1.504(9) . ?
C30 C31 1.524(10) . ?
C30 C32 1.544(10) . ?
C29 C27 1.513(10) . ?
C26 C25 1.321(10) . ?
C34 C35 1.355(10) . ?
C36 C37 1.498(10) . ?
C36 C38 1.526(10) . ?
C39 C40 1.515(11) . ?
C39 C41 1.535(10) . ?
C27 C28 1.542(10) . ?
C20 C21 1.500(10) . ?
C20 C23 1.507(11) . ?
C20 C22 1.563(12) . ?
C43 C42 1.438(16) . ?
C43 C44 1.528(15) . ?
C42 O2 1.360(15) . ?
C45 O2 1.416(16) . ?
C45 C44 1.504(16) . ?

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
C24 Ni1 C33 105.0(3) . . ?
C24 Ni1 P1 92.9(2) . . ?
C33 Ni1 P1 162.1(2) . . ?
C24 Ni1 P2 149.1(2) . 3_666 ?
C33 Ni1 P2 105.7(2) . 3_666 ?
P1 Ni1 P2 56.49(7) . 3_666 ?
C12 P1 P2 100.2(2) . 3_666 ?
C12 P1 Ni1 98.0(2) . . ?
P2 P1 Ni1 62.32(7) 3_666 . ?
C2 P2 P1 103.3(2) . 3_666 ?
C2 P2 Ni1 104.3(2) . 3_666 ?
P1 P2 Ni1 61.19(7) 3_666 3_666 ?
C13 O1 C1 114.1(4) . . ?
C24 N2 C26 111.4(6) . . ?
C24 N2 C30 123.0(6) . . ?
C26 N2 C30 125.5(6) . . ?
C33 N4 C34 111.9(6) . . ?
C33 N4 C36 123.7(5) . . ?
C34 N4 C36 124.2(6) . . ?
C24 N1 C25 111.1(6) . . ?
C24 N1 C27 124.2(6) . . ?
C25 N1 C27 124.5(6) . . ?
C33 N3 C35 111.1(6) . . ?
C33 N3 C39 123.9(5) . . ?
C35 N3 C39 125.0(6) . . ?
C13 C12 C11 115.6(6) . . ?
C13 C12 P1 119.8(5) . . ?
C11 C12 P1 124.5(5) . . ?
C12 C13 C8 123.2(6) . . ?
C12 C13 O1 118.0(5) . . ?
C8 C13 O1 118.8(6) . . ?
C1 C2 C3 116.2(6) . . ?
C1 C2 P2 127.5(5) . . ?
C3 C2 P2 116.0(5) . . ?
C2 C1 C6 122.1(6) . . ?
C2 C1 O1 118.4(5) . . ?
C6 C1 O1 119.5(6) . . ?
C12 C11 C10 123.9(6) . . ?
C5 C6 C1 119.0(6) . . ?
C5 C6 C7 124.6(6) . . ?
C1 C6 C7 116.4(6) . . ?
C8 C9 C10 122.4(6) . . ?
C4 C3 C2 124.3(6) . . ?
N1 C24 N2 103.0(6) . . ?
N1 C24 Ni1 130.4(5) . . ?
N2 C24 Ni1 126.6(5) . . ?
N4 C33 N3 103.5(5) . . ?
N4 C33 Ni1 127.3(5) . . ?
N3 C33 Ni1 129.2(5) . . ?
C3 C4 C5 116.5(6) . . ?
C3 C4 C14 124.5(6) . . ?
C5 C4 C14 119.0(6) . . ?
C9 C8 C13 118.1(6) . . ?
C9 C8 C7 125.4(6) . . ?
C13 C8 C7 116.4(6) . . ?
C6 C5 C4 122.0(6) . . ?
C17 C14 C15 108.2(6) . . ?
C17 C14 C16 109.1(6) . . ?
C15 C14 C16 108.3(6) . . ?
C17 C14 C4 111.6(5) . . ?
C15 C14 C4 109.8(6) . . ?
C16 C14 C4 109.8(6) . . ?
C6 C7 C8 106.6(5) . . ?
C6 C7 C19 112.5(6) . . ?
C8 C7 C19 112.3(5) . . ?
C6 C7 C18 109.8(5) . . ?
C8 C7 C18 108.5(5) . . ?
C19 C7 C18 107.1(5) . . ?
C9 C10 C11 116.5(6) . . ?
C9 C10 C20 122.2(6) . . ?
C11 C10 C20 121.3(6) . . ?
N2 C30 C31 111.5(6) . . ?
N2 C30 C32 109.9(6) . . ?
C31 C30 C32 112.5(6) . . ?
C25 C26 N2 106.7(7) . . ?
C26 C25 N1 107.8(7) . . ?
C35 C34 N4 106.5(7) . . ?
N4 C36 C37 111.2(6) . . ?
N4 C36 C38 110.0(6) . . ?
C37 C36 C38 111.8(7) . . ?
N3 C39 C40 110.8(6) . . ?
N3 C39 C41 110.2(6) . . ?
C40 C39 C41 111.4(6) . . ?
N1 C27 C29 111.7(6) . . ?
N1 C27 C28 109.7(6) . . ?
C29 C27 C28 111.3(6) . . ?
C34 C35 N3 106.9(6) . . ?
C21 C20 C10 114.5(6) . . ?
C21 C20 C23 110.2(7) . . ?
C10 C20 C23 110.7(6) . . ?
C21 C20 C22 105.9(7) . . ?
C10 C20 C22 107.9(7) . . ?
C23 C20 C22 107.2(8) . . ?
C42 C43 C44 108.5(12) . . ?
O2 C42 C43 106.9(12) . . ?
O2 C45 C44 106.2(12) . . ?
C45 C44 C43 98.5(11) . . ?
C42 O2 C45 110.9(12) . . ?

_refine_diff_density_max         0.758
_refine_diff_density_min         -0.495
_refine_diff_density_rms         0.107



####################################################################### 
# 
# 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_2a
_database_code_depnum_ccdc_archive 'CCDC 2357713'
loop_
_audit_author_name
_audit_author_address
'Terrance Hadlington'
;TU Munich
Germany
;
_audit_update_record             
;
2024-05-23 deposited with the CCDC.	2024-07-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C66 H88 N8 Ni2 O2 P4'
_chemical_formula_sum            'C66 H88 N8 Ni2 O2 P4'
_chemical_formula_weight         1266.74

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   9.890(2)
_cell_length_b                   21.590(4)
_cell_length_c                   15.520(3)
_cell_angle_alpha                90
_cell_angle_beta                 93.10(3)
_cell_angle_gamma                90
_cell_volume                     3309.1(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    2000
_cell_measurement_theta_min      1.92
_cell_measurement_theta_max      32.50

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.271
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_exptl_absorpt_coefficient_mu    0.714
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.861
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'STOE X-AREA 1.76'

_diffrn_ambient_temperature      150(2)
_diffrn_source                   'Genix 3D HF Mo'
_diffrn_source_voltage           50
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_collimation    '0.6 mm diameter'
_diffrn_measurement_device_type  'STOE StadiVari'
_diffrn_measurement_method       'ω scans'
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_reflns_number            31963
_diffrn_reflns_av_unetI/netI     0.1324
_diffrn_reflns_av_R_equivalents  0.0949
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.299
_diffrn_reflns_theta_max         25.997
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             6499
_reflns_number_gt                3564
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0408P)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         6499
_refine_ls_number_parameters     384
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1306
_refine_ls_R_factor_gt           0.0518
_refine_ls_wR_factor_ref         0.1020
_refine_ls_wR_factor_gt          0.0841
_refine_ls_goodness_of_fit_ref   0.923
_refine_ls_restrained_S_all      0.923
_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 0.19481(4) 0.14285(2) 0.60123(3) 0.01984(13) Uani 1 1 d . . . . .
P2 P -0.02777(8) 0.13768(5) 0.56316(6) 0.0234(2) Uani 1 1 d . . . . .
P1 P 0.10225(9) 0.06663(5) 0.51747(6) 0.0231(2) Uani 1 1 d . . . . .
N2 N 0.4850(3) 0.13974(16) 0.5709(2) 0.0303(8) Uani 1 1 d . . . . .
O1 O -0.0648(2) 0.00289(12) 0.64669(16) 0.0294(6) Uani 1 1 d . . . . .
N3 N 0.1899(3) 0.27490(14) 0.65974(19) 0.0239(7) Uani 1 1 d . . . . .
C25 C 0.2172(3) 0.21383(17) 0.6761(2) 0.0211(8) Uani 1 1 d . . . . .
N4 N 0.2797(3) 0.21518(15) 0.75764(19) 0.0260(8) Uani 1 1 d . . . . .
N1 N 0.4261(3) 0.05724(15) 0.6357(2) 0.0309(8) Uani 1 1 d . . . . .
C28 C 0.1193(3) 0.29793(17) 0.5805(2) 0.0256(9) Uani 1 1 d . . . . .
H28 H 0.100545 0.261810 0.541334 0.031 Uiso 1 1 calc R U . . .
C16 C 0.3741(3) 0.11129(18) 0.6025(2) 0.0245(9) Uani 1 1 d . . . . .
C2 C -0.0751(3) 0.11129(18) 0.6716(2) 0.0228(9) Uani 1 1 d . . . . .
C1 C -0.0876(3) 0.05047(18) 0.7038(2) 0.0233(9) Uani 1 1 d . . . . .
C7 C -0.1101(3) -0.02848(18) 0.8225(2) 0.0259(9) Uani 1 1 d . . . . .
C6 C -0.1207(3) 0.03788(18) 0.7886(2) 0.0239(9) Uani 1 1 d . . . . .
C27 C 0.2356(4) 0.3126(2) 0.7280(3) 0.0357(10) Uani 1 1 d . . . . .
C5 C -0.1503(4) 0.0873(2) 0.8410(3) 0.0321(10) Uani 1 1 d . . . . .
H5 H -0.174351 0.079847 0.898534 0.039 Uiso 1 1 calc R U . . .
C15 C -0.2041(5) -0.0397(2) 0.8966(3) 0.0507(12) Uani 1 1 d . . . . .
H15A H -0.298088 -0.031785 0.876280 0.076 Uiso 1 1 calc R U . . .
H15B H -0.179117 -0.011643 0.944541 0.076 Uiso 1 1 calc R U . . .
H15C H -0.195104 -0.082665 0.916282 0.076 Uiso 1 1 calc R U . . .
C4 C -0.1452(4) 0.1477(2) 0.8107(3) 0.0355(10) Uani 1 1 d . . . . .
H4 H -0.168957 0.181257 0.846564 0.043 Uiso 1 1 calc R U . . .
C3 C -0.1057(3) 0.15884(18) 0.7286(3) 0.0300(10) Uani 1 1 d . . . . .
H3 H -0.098909 0.200527 0.709723 0.036 Uiso 1 1 calc R U . . .
C31 C 0.3253(3) 0.15998(18) 0.8050(2) 0.0299(10) Uani 1 1 d . . . . .
H31 H 0.308408 0.123558 0.766098 0.036 Uiso 1 1 calc R U . . .
C22 C 0.4819(4) 0.20163(19) 0.5317(3) 0.0321(10) Uani 1 1 d . . . . .
H22 H 0.385525 0.215844 0.527529 0.038 Uiso 1 1 calc R U . . .
C19 C 0.3448(4) 0.0096(2) 0.6771(3) 0.0358(10) Uani 1 1 d . . . . .
H19 H 0.253679 0.027812 0.686156 0.043 Uiso 1 1 calc R U . . .
C26 C 0.2914(4) 0.27528(19) 0.7891(3) 0.0317(10) Uani 1 1 d . . . . .
C18 C 0.6007(4) 0.1035(2) 0.5844(3) 0.0403(11) Uani 1 1 d . . . . .
C17 C 0.5640(4) 0.0522(2) 0.6240(3) 0.0404(12) Uani 1 1 d . . . . .
C13 C -0.1114(3) -0.05632(17) 0.6640(2) 0.0223(9) Uani 1 1 d . . . . .
C8 C -0.1388(3) -0.07363(18) 0.7482(2) 0.0231(9) Uani 1 1 d . . . . .
C9 C -0.1822(4) -0.13409(19) 0.7615(2) 0.0323(10) Uani 1 1 d . . . . .
H9 H -0.203604 -0.147019 0.817638 0.039 Uiso 1 1 calc R U . . .
C30 C -0.0154(4) 0.3269(2) 0.6006(3) 0.0425(12) Uani 1 1 d . . . . .
H30A H -0.072565 0.295637 0.626470 0.064 Uiso 1 1 calc R U . . .
H30B H -0.060763 0.342342 0.547159 0.064 Uiso 1 1 calc R U . . .
H30C H 0.000294 0.361273 0.641075 0.064 Uiso 1 1 calc R U . . .
C10 C -0.1944(4) -0.1755(2) 0.6932(3) 0.0378(11) Uani 1 1 d . . . . .
H10 H -0.222950 -0.216860 0.702819 0.045 Uiso 1 1 calc R U . . .
C32 C 0.4770(4) 0.1636(2) 0.8259(3) 0.0452(12) Uani 1 1 d . . . . .
H32A H 0.524407 0.166641 0.772247 0.068 Uiso 1 1 calc R U . . .
H32B H 0.507074 0.126302 0.857451 0.068 Uiso 1 1 calc R U . . .
H32C H 0.497464 0.200224 0.861629 0.068 Uiso 1 1 calc R U . . .
C20 C 0.4086(4) -0.0077(2) 0.7652(3) 0.0471(12) Uani 1 1 d . . . . .
H20A H 0.492083 -0.031124 0.757821 0.071 Uiso 1 1 calc R U . . .
H20B H 0.345140 -0.033239 0.796132 0.071 Uiso 1 1 calc R U . . .
H20C H 0.429617 0.030014 0.798321 0.071 Uiso 1 1 calc R U . . .
C33 C 0.2439(4) 0.1501(2) 0.8847(3) 0.0479(12) Uani 1 1 d . . . . .
H33A H 0.261984 0.184106 0.925575 0.072 Uiso 1 1 calc R U . . .
H33B H 0.270315 0.110735 0.912204 0.072 Uiso 1 1 calc R U . . .
H33C H 0.147068 0.149131 0.867593 0.072 Uiso 1 1 calc R U . . .
C29 C 0.2089(4) 0.34350(19) 0.5342(3) 0.0404(11) Uani 1 1 d . . . . .
H29A H 0.217725 0.381929 0.567627 0.061 Uiso 1 1 calc R U . . .
H29B H 0.167655 0.352575 0.476738 0.061 Uiso 1 1 calc R U . . .
H29C H 0.298639 0.325200 0.528536 0.061 Uiso 1 1 calc R U . . .
C14 C 0.0371(4) -0.0391(2) 0.8570(3) 0.0504(13) Uani 1 1 d . . . . .
H14A H 0.047424 -0.081776 0.877747 0.076 Uiso 1 1 calc R U . . .
H14B H 0.058810 -0.010343 0.904704 0.076 Uiso 1 1 calc R U . . .
H14C H 0.098693 -0.031803 0.810698 0.076 Uiso 1 1 calc R U . . .
C24 C 0.5626(4) 0.2477(2) 0.5881(3) 0.0532(13) Uani 1 1 d . . . . .
H24A H 0.523245 0.250475 0.644629 0.080 Uiso 1 1 calc R U . . .
H24B H 0.559593 0.288530 0.560470 0.080 Uiso 1 1 calc R U . . .
H24C H 0.656788 0.233802 0.595622 0.080 Uiso 1 1 calc R U . . .
C23 C 0.5318(4) 0.1992(2) 0.4403(3) 0.0436(12) Uani 1 1 d . . . . .
H23A H 0.627091 0.186475 0.442659 0.065 Uiso 1 1 calc R U . . .
H23B H 0.522952 0.240266 0.413729 0.065 Uiso 1 1 calc R U . . .
H23C H 0.477503 0.169260 0.405899 0.065 Uiso 1 1 calc R U . . .
C21 C 0.3240(5) -0.0466(2) 0.6193(3) 0.0584(14) Uani 1 1 d . . . . .
H21A H 0.282298 -0.033777 0.563441 0.088 Uiso 1 1 calc R U . . .
H21B H 0.264600 -0.076306 0.646529 0.088 Uiso 1 1 calc R U . . .
H21C H 0.411650 -0.066188 0.610619 0.088 Uiso 1 1 calc R U . . .
C12 C -0.1239(3) -0.09668(17) 0.5933(2) 0.0229(9) Uani 1 1 d . . . . .
C11 C -0.1649(4) -0.15664(18) 0.6114(2) 0.0338(10) Uani 1 1 d . . . . .
H11 H -0.172936 -0.185816 0.565603 0.041 Uiso 1 1 calc R U . . .
H26 H 0.337012 0.285175 0.849290 0.076(16) Uiso 1 1 d R . . . .
H27 H 0.219112 0.356575 0.714980 0.057(14) Uiso 1 1 d R . . . .
H17 H 0.616212 0.011475 0.638180 0.051(13) Uiso 1 1 d R . . . .
H18 H 0.690312 0.115675 0.559290 0.042(11) Uiso 1 1 d R . . . .


_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 C16 1.899(4) . ?
Ni1 C25 1.929(4) . ?
Ni1 P2 2.2510(11) . ?
Ni1 P1 2.2599(11) . ?
P2 C2 1.861(4) . ?
P2 P1 2.1466(14) . ?
P1 C12 1.861(4) 3_556 ?
N2 C16 1.370(4) . ?
N2 C18 1.393(5) . ?
N2 C22 1.468(5) . ?
O1 C1 1.383(4) . ?
O1 C13 1.390(4) . ?
N3 C25 1.367(4) . ?
N3 C27 1.391(5) . ?
N3 C28 1.468(4) . ?
C25 N4 1.377(4) . ?
N4 C26 1.389(5) . ?
N4 C31 1.459(5) . ?
N1 C16 1.365(5) . ?
N1 C17 1.389(4) . ?
N1 C19 1.475(5) . ?
C28 C30 1.519(5) . ?
C28 C29 1.529(5) . ?
C2 C3 1.399(5) . ?
C2 C1 1.413(5) . ?
C1 C6 1.400(5) . ?
C7 C8 1.524(5) . ?
C7 C6 1.528(5) . ?
C7 C15 1.538(5) . ?
C7 C14 1.541(5) . ?
C6 C5 1.382(5) . ?
C27 C26 1.341(5) . ?
C5 C4 1.389(5) . ?
C4 C3 1.374(5) . ?
C31 C32 1.520(5) . ?
C31 C33 1.528(5) . ?
C22 C24 1.522(5) . ?
C22 C23 1.528(5) . ?
C19 C21 1.517(6) . ?
C19 C20 1.521(5) . ?
C18 C17 1.326(6) . ?
C13 C8 1.400(5) . ?
C13 C12 1.401(5) . ?
C8 C9 1.393(5) . ?
C9 C10 1.386(5) . ?
C10 C11 1.380(5) . ?
C12 C11 1.390(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
C16 Ni1 C25 101.64(15) . . ?
C16 Ni1 P2 152.19(12) . . ?
C25 Ni1 P2 106.05(10) . . ?
C16 Ni1 P1 95.39(12) . . ?
C25 Ni1 P1 162.73(10) . . ?
P2 Ni1 P1 56.83(4) . . ?
C2 P2 P1 105.33(13) . . ?
C2 P2 Ni1 93.89(11) . . ?
P1 P2 Ni1 61.79(4) . . ?
C12 P1 P2 99.02(12) 3_556 . ?
C12 P1 Ni1 102.38(12) 3_556 . ?
P2 P1 Ni1 61.37(4) . . ?
C16 N2 C18 111.1(3) . . ?
C16 N2 C22 123.8(3) . . ?
C18 N2 C22 125.0(3) . . ?
C1 O1 C13 119.5(3) . . ?
C25 N3 C27 111.7(3) . . ?
C25 N3 C28 124.3(3) . . ?
C27 N3 C28 124.0(3) . . ?
N3 C25 N4 103.0(3) . . ?
N3 C25 Ni1 129.7(3) . . ?
N4 C25 Ni1 127.0(3) . . ?
C25 N4 C26 111.6(3) . . ?
C25 N4 C31 123.8(3) . . ?
C26 N4 C31 124.6(3) . . ?
C16 N1 C17 111.7(3) . . ?
C16 N1 C19 123.9(3) . . ?
C17 N1 C19 124.4(3) . . ?
N3 C28 C30 110.5(3) . . ?
N3 C28 C29 110.5(3) . . ?
C30 C28 C29 111.6(3) . . ?
N1 C16 N2 103.1(3) . . ?
N1 C16 Ni1 130.0(3) . . ?
N2 C16 Ni1 126.9(3) . . ?
C3 C2 C1 115.6(3) . . ?
C3 C2 P2 114.9(3) . . ?
C1 C2 P2 129.5(3) . . ?
O1 C1 C6 120.9(3) . . ?
O1 C1 C2 116.3(3) . . ?
C6 C1 C2 122.9(3) . . ?
C8 C7 C6 109.5(3) . . ?
C8 C7 C15 111.7(3) . . ?
C6 C7 C15 111.8(3) . . ?
C8 C7 C14 107.6(3) . . ?
C6 C7 C14 107.8(3) . . ?
C15 C7 C14 108.3(3) . . ?
C5 C6 C1 118.1(4) . . ?
C5 C6 C7 122.3(4) . . ?
C1 C6 C7 119.3(3) . . ?
C26 C27 N3 106.9(4) . . ?
C6 C5 C4 120.9(4) . . ?
C3 C4 C5 119.7(4) . . ?
C4 C3 C2 122.7(4) . . ?
N4 C31 C32 109.9(3) . . ?
N4 C31 C33 111.1(3) . . ?
C32 C31 C33 113.1(3) . . ?
N2 C22 C24 111.0(4) . . ?
N2 C22 C23 110.7(3) . . ?
C24 C22 C23 111.8(3) . . ?
N1 C19 C21 111.1(4) . . ?
N1 C19 C20 110.7(3) . . ?
C21 C19 C20 111.8(4) . . ?
C27 C26 N4 106.8(4) . . ?
C17 C18 N2 107.2(3) . . ?
C18 C17 N1 106.9(4) . . ?
O1 C13 C8 120.6(3) . . ?
O1 C13 C12 115.9(3) . . ?
C8 C13 C12 123.5(3) . . ?
C9 C8 C13 117.7(3) . . ?
C9 C8 C7 122.3(3) . . ?
C13 C8 C7 119.8(3) . . ?
C10 C9 C8 120.4(4) . . ?
C11 C10 C9 119.9(4) . . ?
C11 C12 C13 115.8(3) . . ?
C11 C12 P1 124.1(3) . 3_556 ?
C13 C12 P1 119.8(3) . 3_556 ?
C10 C11 C12 122.7(4) . . ?

_refine_diff_density_max         0.386
_refine_diff_density_min         -0.298
_refine_diff_density_rms         0.077



####################################################################### 
# 
# 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_4
_database_code_depnum_ccdc_archive 'CCDC 2357715'
loop_
_audit_author_name
_audit_author_address
'Terrance Hadlington'
;TU Munich
Germany
;
_audit_update_record             
;
2024-05-23 deposited with the CCDC.	2024-07-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C82 H120 Cl2 Cu2 N8 Ni2 O2 P4'
_chemical_formula_sum            'C82 H120 Cl2 Cu2 N8 Ni2 O2 P4'
_chemical_formula_weight         1689.13

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_H-M_alt        'I 41/a'
_space_group_name_Hall           '-I 4ad'

_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'
'-y+3/4, x+1/4, z+1/4'
'-x, -y+1/2, z'
'y+1/4, -x+1/4, z+1/4'
'x+1/2, y+1/2, z+1/2'
'-y+5/4, x+3/4, z+3/4'
'-x+1/2, -y+1, z+1/2'
'y+3/4, -x+3/4, z+3/4'
'-x, -y, -z'
'y-3/4, -x-1/4, -z-1/4'
'x, y-1/2, -z'
'-y-1/4, x-1/4, -z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'y-1/4, -x+1/4, -z+1/4'
'x+1/2, y, -z+1/2'
'-y+1/4, x+1/4, -z+1/4'

_cell_length_a                   35.655(5)
_cell_length_b                   35.655(5)
_cell_length_c                   15.130(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     19234(7)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    2000
_cell_measurement_theta_min      1.92
_cell_measurement_theta_max      32.50

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.167
_exptl_crystal_F_000             7136
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.19
_exptl_absorpt_coefficient_mu    0.987
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.729
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'STOE X-AREA 1.76'

_diffrn_ambient_temperature      150(2)
_diffrn_source                   'Genix 3D HF Mo'
_diffrn_source_voltage           50
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_collimation    '0.6 mm diameter'
_diffrn_measurement_device_type  'STOE StadiVari'
_diffrn_measurement_method       'ω scans'
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_reflns_number            36349
_diffrn_reflns_av_unetI/netI     0.1493
_diffrn_reflns_av_R_equivalents  0.1066
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.460
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             9424
_reflns_number_gt                4012
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          SQUEEZE
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.250 0.965 708 118 ' '
2 0.000 0.750 0.034 708 118 ' '
3 0.218 0.479 0.225 16 1 ' '
4 0.218 0.979 0.775 16 1 ' '
5 0.229 0.032 0.025 16 1 ' '
6 0.229 0.532 0.975 16 1 ' '
7 0.282 0.021 0.275 16 1 ' '
8 0.271 0.468 0.475 16 1 ' '
9 0.282 0.521 0.725 16 1 ' '
10 0.271 0.968 0.525 16 1 ' '
11 0.500 0.250 0.217 708 118 ' '
12 0.500 0.750 0.781 708 118 ' '
13 0.718 0.479 0.275 16 1 ' '
14 0.718 0.979 0.725 16 1 ' '
15 0.729 0.032 0.475 16 1 ' '
16 0.729 0.532 0.525 16 1 ' '
17 0.782 0.021 0.225 16 1 ' '
18 0.771 0.468 0.025 16 1 ' '
19 0.782 0.521 0.775 16 1 ' '
20 0.771 0.968 0.975 16 1 ' '
_platon_squeeze_details          
;
The unit cell contains 32 THF molecules which have been treated
as a diffuse contribution to the overall scattering without specific atom
positions by SQUEEZE/PLATON.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0777P)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         9424
_refine_ls_number_parameters     492
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.1511
_refine_ls_R_factor_gt           0.0635
_refine_ls_wR_factor_ref         0.1618
_refine_ls_wR_factor_gt          0.1364
_refine_ls_goodness_of_fit_ref   0.821
_refine_ls_restrained_S_all      0.821
_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
Cu1 Cu 1.02012(2) 0.51646(2) 0.44210(5) 0.0468(2) Uani 1 1 d . . . . .
Ni1 Ni 0.92523(2) 0.57158(2) 0.51158(5) 0.0503(2) Uani 1 1 d . . . . .
P1 P 0.96128(4) 0.52786(4) 0.46480(10) 0.0426(4) Uani 1 1 d . . . . .
P2 P 1.07448(4) 0.48137(4) 0.40640(10) 0.0463(4) Uani 1 1 d . . . . .
Cl1 Cl 0.92858(6) 0.61275(5) 0.40000(13) 0.0938(7) Uani 1 1 d . . . . .
O1 O 0.99069(9) 0.46419(10) 0.3505(2) 0.0440(9) Uani 1 1 d . . . . .
N3 N 1.02917(12) 0.56597(12) 0.2830(3) 0.0475(12) Uani 1 1 d . . . . .
N1 N 0.90417(13) 0.62979(13) 0.6406(3) 0.0551(13) Uani 1 1 d . . . . .
N4 N 1.05456(13) 0.58698(13) 0.4010(3) 0.0540(13) Uani 1 1 d . . . . .
N2 N 0.85543(13) 0.59974(14) 0.5989(4) 0.0606(14) Uani 1 1 d . . . . .
C6 C 0.93902(14) 0.46054(14) 0.2476(4) 0.0419(13) Uani 1 1 d . . . . .
C8 C 1.00383(15) 0.44150(15) 0.2033(4) 0.0451(14) Uani 1 1 d . . . . .
C9 C 1.03090(16) 0.43505(15) 0.1377(4) 0.0487(15) Uani 1 1 d . . . . .
H9 H 1.022998 0.426517 0.081168 0.058 Uiso 1 1 calc R U . . .
C13 C 1.01621(16) 0.45501(15) 0.2843(4) 0.0457(14) Uani 1 1 d . . . . .
C12 C 1.05395(15) 0.46133(15) 0.3035(4) 0.0461(14) Uani 1 1 d . . . . .
C5 C 0.90221(15) 0.47161(15) 0.2277(4) 0.0481(15) Uani 1 1 d . . . . .
H5 H 0.890635 0.462048 0.175806 0.058 Uiso 1 1 calc R U . . .
C11 C 1.07882(16) 0.45378(15) 0.2366(4) 0.0519(15) Uani 1 1 d . . . . .
H11 H 1.104708 0.457694 0.248308 0.062 Uiso 1 1 calc R U . . .
C3 C 0.90036(14) 0.51102(14) 0.3545(4) 0.0449(14) Uani 1 1 d . . . . .
H3 H 0.886854 0.528396 0.389909 0.054 Uiso 1 1 calc R U . . .
C1 C 0.95448(14) 0.47485(15) 0.3246(4) 0.0420(13) Uani 1 1 d . . . . .
C7 C 0.96147(15) 0.43333(15) 0.1902(4) 0.0485(14) Uani 1 1 d . . . . .
C4 C 0.88252(15) 0.49557(15) 0.2802(4) 0.0464(14) Uani 1 1 d . . . . .
C33 C 1.03370(14) 0.55806(16) 0.3683(4) 0.0453(14) Uani 1 1 d . . . . .
C10 C 1.06899(16) 0.44081(16) 0.1529(4) 0.0506(15) Uani 1 1 d . . . . .
C2 C 0.93689(14) 0.50202(14) 0.3785(4) 0.0415(13) Uani 1 1 d . . . . .
C24 C 0.89338(16) 0.60129(16) 0.5880(4) 0.0523(15) Uani 1 1 d . . . . .
C14 C 0.84163(15) 0.50805(16) 0.2588(4) 0.0534(16) Uani 1 1 d . . . . .
C36 C 1.00481(17) 0.54575(17) 0.2213(4) 0.0552(16) Uani 1 1 d . . . . .
H36 H 0.997871 0.521503 0.250216 0.066 Uiso 1 1 calc R U . . .
C27 C 0.94299(17) 0.64408(17) 0.6470(5) 0.0614(17) Uani 1 1 d . . . . .
H27 H 0.960125 0.623520 0.627214 0.074 Uiso 1 1 calc R U . . .
C25 C 0.87423(17) 0.64611(17) 0.6839(4) 0.0594(17) Uani 1 1 d . . . . .
H25 H 0.875095 0.666393 0.724565 0.071 Uiso 1 1 calc R U . . .
C34 C 1.04746(18) 0.59939(17) 0.2605(5) 0.0637(17) Uani 1 1 d . . . . .
H34 H 1.048118 0.611006 0.204055 0.076 Uiso 1 1 calc R U . . .
C35 C 1.06363(19) 0.61155(18) 0.3338(5) 0.0668(19) Uani 1 1 d . . . . .
H35 H 1.078808 0.633329 0.339188 0.080 Uiso 1 1 calc R U . . .
C19 C 0.95017(16) 0.43653(19) 0.0918(4) 0.0653(18) Uani 1 1 d . . . . .
H19A H 0.923705 0.429692 0.084971 0.098 Uiso 1 1 calc R U . . .
H19B H 0.965707 0.419548 0.056359 0.098 Uiso 1 1 calc R U . . .
H19C H 0.953940 0.462376 0.071603 0.098 Uiso 1 1 calc R U . . .
C26 C 0.84383(19) 0.62754(18) 0.6568(5) 0.0677(19) Uani 1 1 d . . . . .
H26 H 0.818710 0.632489 0.674174 0.081 Uiso 1 1 calc R U . . .
C20 C 1.09701(17) 0.43521(19) 0.0786(4) 0.0638(18) Uani 1 1 d . . . . .
C18 C 0.95374(17) 0.39271(16) 0.2211(5) 0.0650(18) Uani 1 1 d . . . . .
H18A H 0.961697 0.389872 0.282786 0.098 Uiso 1 1 calc R U . . .
H18B H 0.967776 0.375139 0.183906 0.098 Uiso 1 1 calc R U . . .
H18C H 0.926852 0.387383 0.216375 0.098 Uiso 1 1 calc R U . . .
C39 C 1.06355(18) 0.59210(19) 0.4942(4) 0.0690(19) Uani 1 1 d . . . . .
H39 H 1.050081 0.572326 0.528697 0.083 Uiso 1 1 calc R U . . .
C30 C 0.83157(17) 0.5740(2) 0.5491(5) 0.072(2) Uani 1 1 d . . . . .
H30 H 0.847887 0.557905 0.511151 0.087 Uiso 1 1 calc R U . . .
C17 C 0.82703(18) 0.49154(19) 0.1718(5) 0.083(2) Uani 1 1 d . . . . .
H17A H 0.827594 0.464098 0.175045 0.125 Uiso 1 1 calc R U . . .
H17B H 0.842950 0.500004 0.122908 0.125 Uiso 1 1 calc R U . . .
H17C H 0.801215 0.499976 0.161828 0.125 Uiso 1 1 calc R U . . .
C38 C 1.0252(2) 0.53609(18) 0.1362(4) 0.0710(19) Uani 1 1 d . . . . .
H38A H 1.032759 0.559240 0.106242 0.107 Uiso 1 1 calc R U . . .
H38B H 1.008451 0.521687 0.097610 0.107 Uiso 1 1 calc R U . . .
H38C H 1.047471 0.521089 0.149862 0.107 Uiso 1 1 calc R U . . .
C29 C 0.95300(19) 0.65343(19) 0.7409(5) 0.080(2) Uani 1 1 d . . . . .
H29A H 0.937457 0.674369 0.761309 0.120 Uiso 1 1 calc R U . . .
H29B H 0.979519 0.660517 0.744071 0.120 Uiso 1 1 calc R U . . .
H29C H 0.948547 0.631489 0.778440 0.120 Uiso 1 1 calc R U . . .
C37 C 0.96851(18) 0.5670(2) 0.2046(5) 0.076(2) Uani 1 1 d . . . . .
H37A H 0.956970 0.573724 0.261199 0.114 Uiso 1 1 calc R U . . .
H37B H 0.951251 0.551181 0.170733 0.114 Uiso 1 1 calc R U . . .
H37C H 0.973940 0.589908 0.171011 0.114 Uiso 1 1 calc R U . . .
C15 C 0.84047(18) 0.55021(18) 0.2480(5) 0.086(2) Uani 1 1 d . . . . .
H15A H 0.814356 0.558466 0.242612 0.130 Uiso 1 1 calc R U . . .
H15B H 0.854352 0.557350 0.194685 0.130 Uiso 1 1 calc R U . . .
H15C H 0.851961 0.562135 0.299704 0.130 Uiso 1 1 calc R U . . .
C32 C 0.8052(2) 0.5958(2) 0.4901(6) 0.098(3) Uani 1 1 d . . . . .
H32A H 0.789316 0.612135 0.526438 0.147 Uiso 1 1 calc R U . . .
H32B H 0.789363 0.578291 0.456962 0.147 Uiso 1 1 calc R U . . .
H32C H 0.819764 0.611128 0.448763 0.147 Uiso 1 1 calc R U . . .
C16 C 0.81635(18) 0.4964(2) 0.3339(5) 0.101(3) Uani 1 1 d . . . . .
H16A H 0.824462 0.508767 0.388460 0.152 Uiso 1 1 calc R U . . .
H16B H 0.817708 0.469107 0.341562 0.152 Uiso 1 1 calc R U . . .
H16C H 0.790466 0.503636 0.320466 0.152 Uiso 1 1 calc R U . . .
C28 C 0.9483(2) 0.6766(2) 0.5846(5) 0.085(2) Uani 1 1 d . . . . .
H28A H 0.943121 0.668376 0.523980 0.127 Uiso 1 1 calc R U . . .
H28B H 0.974203 0.685620 0.588567 0.127 Uiso 1 1 calc R U . . .
H28C H 0.931049 0.696850 0.600636 0.127 Uiso 1 1 calc R U . . .
C31 C 0.8105(2) 0.5492(2) 0.6125(6) 0.100(3) Uani 1 1 d . . . . .
H31A H 0.828269 0.536639 0.651929 0.150 Uiso 1 1 calc R U . . .
H31B H 0.796307 0.530372 0.579152 0.150 Uiso 1 1 calc R U . . .
H31C H 0.793111 0.564477 0.647499 0.150 Uiso 1 1 calc R U . . .
C40 C 1.1044(2) 0.5874(3) 0.5095(5) 0.124(4) Uani 1 1 d . . . . .
H40A H 1.112655 0.563357 0.485071 0.185 Uiso 1 1 calc R U . . .
H40B H 1.109515 0.587991 0.573178 0.185 Uiso 1 1 calc R U . . .
H40C H 1.118047 0.607873 0.480505 0.185 Uiso 1 1 calc R U . . .
C41 C 1.0495(3) 0.6299(2) 0.5246(5) 0.136(4) Uani 1 1 d . . . . .
H41A H 1.062018 0.649745 0.490879 0.204 Uiso 1 1 calc R U . . .
H41B H 1.054929 0.633090 0.587668 0.204 Uiso 1 1 calc R U . . .
H41C H 1.022330 0.631467 0.515064 0.204 Uiso 1 1 calc R U . . .
C21A C 1.0907(6) 0.3986(5) 0.0307(15) 0.071(6) Uiso 0.421(13) 1 d . . P A 2
H21A H 1.113351 0.391910 -0.002441 0.106 Uiso 0.421(13) 1 calc R U P A 2
H21B H 1.069589 0.401308 -0.010300 0.106 Uiso 0.421(13) 1 calc R U P A 2
H21C H 1.085064 0.378832 0.073679 0.106 Uiso 0.421(13) 1 calc R U P A 2
C23 C 1.1213(6) 0.4702(5) 0.0644(14) 0.157(11) Uani 0.579(13) 1 d . U P A 1
H23A H 1.140343 0.464911 0.019237 0.236 Uiso 0.579(13) 1 calc R U P A 1
H23B H 1.133734 0.476913 0.119960 0.236 Uiso 0.579(13) 1 calc R U P A 1
H23C H 1.105495 0.491039 0.044786 0.236 Uiso 0.579(13) 1 calc R U P A 1
C22 C 1.1274(4) 0.4070(5) 0.1126(10) 0.115(7) Uani 0.579(13) 1 d . . P A 1
H22A H 1.115374 0.383190 0.128582 0.172 Uiso 0.579(13) 1 calc R U P A 1
H22B H 1.139965 0.417473 0.164670 0.172 Uiso 0.579(13) 1 calc R U P A 1
H22C H 1.145944 0.402516 0.065944 0.172 Uiso 0.579(13) 1 calc R U P A 1
C23A C 1.0876(4) 0.4674(4) 0.0054(10) 0.051(5) Uiso 0.421(13) 1 d . . P A 2
H23D H 1.092264 0.492223 0.030957 0.077 Uiso 0.421(13) 1 calc R U P A 2
H23E H 1.061269 0.465457 -0.012330 0.077 Uiso 0.421(13) 1 calc R U P A 2
H23F H 1.103726 0.463855 -0.046433 0.077 Uiso 0.421(13) 1 calc R U P A 2
C22A C 1.1360(5) 0.4414(6) 0.1054(13) 0.073(6) Uiso 0.421(13) 1 d . . P A 2
H22D H 1.137912 0.465069 0.137908 0.109 Uiso 0.421(13) 1 calc R U P A 2
H22E H 1.151996 0.442481 0.052745 0.109 Uiso 0.421(13) 1 calc R U P A 2
H22F H 1.144245 0.420695 0.143400 0.109 Uiso 0.421(13) 1 calc R U P A 2
C21 C 1.0822(4) 0.4184(11) 0.0000(12) 0.23(2) Uani 0.579(13) 1 d . U P A 1
H21D H 1.069187 0.395114 0.015249 0.345 Uiso 0.579(13) 1 calc R U P A 1
H21E H 1.102744 0.412964 -0.041007 0.345 Uiso 0.579(13) 1 calc R U P A 1
H21F H 1.064500 0.435803 -0.028012 0.345 Uiso 0.579(13) 1 calc R U P A 1


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 C33 1.919(6) . ?
Cu1 P1 2.1644(16) . ?
Cu1 P1 2.2185(16) 9_766 ?
Cu1 P2 2.3692(16) . ?
Cu1 Cu1 2.5508(14) 9_766 ?
Ni1 C24 1.936(6) . ?
Ni1 P1 2.1407(16) . ?
Ni1 Cl1 2.240(2) . ?
Ni1 P2 2.2592(17) 9_766 ?
P1 C2 1.819(6) . ?
P1 P2 2.352(2) 9_766 ?
P2 C12 1.863(6) . ?
O1 C13 1.393(6) . ?
O1 C1 1.402(6) . ?
N3 C33 1.331(7) . ?
N3 C34 1.400(7) . ?
N3 C36 1.465(7) . ?
N1 C24 1.347(7) . ?
N1 C25 1.381(7) . ?
N1 C27 1.478(7) . ?
N4 C33 1.364(7) . ?
N4 C35 1.381(7) . ?
N4 C39 1.458(8) . ?
N2 C24 1.364(7) . ?
N2 C26 1.386(7) . ?
N2 C30 1.460(8) . ?
C6 C1 1.386(7) . ?
C6 C5 1.403(7) . ?
C6 C7 1.529(7) . ?
C8 C13 1.388(7) . ?
C8 C9 1.404(7) . ?
C8 C7 1.551(7) . ?
C9 C10 1.393(7) . ?
C9 H9 0.9500 . ?
C13 C12 1.395(7) . ?
C12 C11 1.372(8) . ?
C5 C4 1.361(7) . ?
C5 H5 0.9500 . ?
C11 C10 1.393(8) . ?
C11 H11 0.9500 . ?
C3 C2 1.390(7) . ?
C3 C4 1.405(7) . ?
C3 H3 0.9500 . ?
C1 C2 1.413(7) . ?
C7 C19 1.547(8) . ?
C7 C18 1.547(8) . ?
C4 C14 1.558(7) . ?
C10 C20 1.517(8) . ?
C14 C15 1.513(8) . ?
C14 C16 1.509(9) . ?
C14 C17 1.533(9) . ?
C36 C38 1.517(8) . ?
C36 C37 1.522(8) . ?
C36 H36 1.0000 . ?
C27 C28 1.506(9) . ?
C27 C29 1.502(9) . ?
C27 H27 1.0000 . ?
C25 C26 1.334(8) . ?
C25 H25 0.9500 . ?
C34 C35 1.322(8) . ?
C34 H34 0.9500 . ?
C35 H35 0.9500 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C26 H26 0.9500 . ?
C20 C21 1.432(18) . ?
C20 C22A 1.465(17) . ?
C20 C21A 1.51(2) . ?
C20 C23 1.534(17) . ?
C20 C22 1.567(15) . ?
C20 C23A 1.630(15) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C39 C40 1.485(9) . ?
C39 C41 1.511(10) . ?
C39 H39 1.0000 . ?
C30 C31 1.506(10) . ?
C30 C32 1.511(9) . ?
C30 H30 1.0000 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C21A H21A 0.9800 . ?
C21A H21B 0.9800 . ?
C21A H21C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23A H23D 0.9800 . ?
C23A H23E 0.9800 . ?
C23A H23F 0.9800 . ?
C22A H22D 0.9800 . ?
C22A H22E 0.9800 . ?
C22A H22F 0.9800 . ?
C21 H21D 0.9800 . ?
C21 H21E 0.9800 . ?
C21 H21F 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
C33 Cu1 P1 101.06(16) . . ?
C33 Cu1 P1 147.66(16) . 9_766 ?
P1 Cu1 P1 108.83(5) . 9_766 ?
C33 Cu1 P2 93.96(16) . . ?
P1 Cu1 P2 158.16(6) . . ?
P1 Cu1 P2 61.58(6) 9_766 . ?
C33 Cu1 Cu1 153.84(16) . 9_766 ?
P1 Cu1 Cu1 55.40(5) . 9_766 ?
P1 Cu1 Cu1 53.43(4) 9_766 9_766 ?
P2 Cu1 Cu1 111.94(5) . 9_766 ?
C24 Ni1 P1 161.44(18) . . ?
C24 Ni1 Cl1 97.05(18) . . ?
P1 Ni1 Cl1 101.30(7) . . ?
C24 Ni1 P2 97.58(18) . 9_766 ?
P1 Ni1 P2 64.56(6) . 9_766 ?
Cl1 Ni1 P2 163.99(7) . 9_766 ?
C2 P1 Ni1 108.60(18) . . ?
C2 P1 Cu1 104.74(18) . . ?
Ni1 P1 Cu1 140.47(7) . . ?
C2 P1 Cu1 103.74(17) . 9_766 ?
Ni1 P1 Cu1 119.22(7) . 9_766 ?
Cu1 P1 Cu1 71.17(5) . 9_766 ?
C2 P1 P2 105.34(18) . 9_766 ?
Ni1 P1 P2 60.16(6) . 9_766 ?
Cu1 P1 P2 129.09(8) . 9_766 ?
Cu1 P1 P2 62.37(6) 9_766 9_766 ?
C12 P2 Ni1 98.07(18) . 9_766 ?
C12 P2 P1 115.20(18) . 9_766 ?
Ni1 P2 P1 55.28(5) 9_766 9_766 ?
C12 P2 Cu1 94.12(18) . . ?
Ni1 P2 Cu1 108.66(7) 9_766 . ?
P1 P2 Cu1 56.06(5) 9_766 . ?
C13 O1 C1 117.6(4) . . ?
C33 N3 C34 111.0(5) . . ?
C33 N3 C36 125.8(5) . . ?
C34 N3 C36 122.7(5) . . ?
C24 N1 C25 112.2(5) . . ?
C24 N1 C27 124.5(5) . . ?
C25 N1 C27 123.2(5) . . ?
C33 N4 C35 109.9(5) . . ?
C33 N4 C39 124.5(5) . . ?
C35 N4 C39 125.6(5) . . ?
C24 N2 C26 110.1(5) . . ?
C24 N2 C30 122.8(5) . . ?
C26 N2 C30 126.9(5) . . ?
C1 C6 C5 116.7(5) . . ?
C1 C6 C7 120.2(5) . . ?
C5 C6 C7 123.1(5) . . ?
C13 C8 C9 117.6(5) . . ?
C13 C8 C7 119.2(5) . . ?
C9 C8 C7 123.2(5) . . ?
C10 C9 C8 121.9(5) . . ?
C10 C9 H9 119.0 . . ?
C8 C9 H9 119.0 . . ?
C8 C13 O1 120.6(5) . . ?
C8 C13 C12 123.2(5) . . ?
O1 C13 C12 116.2(5) . . ?
C11 C12 C13 116.0(5) . . ?
C11 C12 P2 116.0(4) . . ?
C13 C12 P2 128.0(4) . . ?
C4 C5 C6 122.2(5) . . ?
C4 C5 H5 118.9 . . ?
C6 C5 H5 118.9 . . ?
C12 C11 C10 125.0(5) . . ?
C12 C11 H11 117.5 . . ?
C10 C11 H11 117.5 . . ?
C2 C3 C4 122.9(5) . . ?
C2 C3 H3 118.6 . . ?
C4 C3 H3 118.6 . . ?
C6 C1 O1 120.1(5) . . ?
C6 C1 C2 124.1(5) . . ?
O1 C1 C2 115.6(5) . . ?
C6 C7 C8 108.5(4) . . ?
C6 C7 C19 111.3(5) . . ?
C8 C7 C19 111.3(5) . . ?
C6 C7 C18 109.2(5) . . ?
C8 C7 C18 108.1(4) . . ?
C19 C7 C18 108.3(5) . . ?
C5 C4 C3 118.7(5) . . ?
C5 C4 C14 122.7(5) . . ?
C3 C4 C14 118.5(5) . . ?
N3 C33 N4 104.9(5) . . ?
N3 C33 Cu1 134.2(4) . . ?
N4 C33 Cu1 120.7(4) . . ?
C9 C10 C11 116.4(5) . . ?
C9 C10 C20 120.0(5) . . ?
C11 C10 C20 123.5(5) . . ?
C3 C2 C1 115.0(5) . . ?
C3 C2 P1 121.2(4) . . ?
C1 C2 P1 123.3(4) . . ?
N1 C24 N2 104.1(5) . . ?
N1 C24 Ni1 126.7(4) . . ?
N2 C24 Ni1 129.2(5) . . ?
C15 C14 C16 109.8(6) . . ?
C15 C14 C17 106.2(5) . . ?
C16 C14 C17 109.7(5) . . ?
C15 C14 C4 109.4(5) . . ?
C16 C14 C4 108.9(5) . . ?
C17 C14 C4 112.7(5) . . ?
N3 C36 C38 111.6(5) . . ?
N3 C36 C37 111.4(5) . . ?
C38 C36 C37 112.3(5) . . ?
N3 C36 H36 107.1 . . ?
C38 C36 H36 107.1 . . ?
C37 C36 H36 107.1 . . ?
N1 C27 C28 110.0(5) . . ?
N1 C27 C29 111.1(5) . . ?
C28 C27 C29 113.1(6) . . ?
N1 C27 H27 107.5 . . ?
C28 C27 H27 107.5 . . ?
C29 C27 H27 107.5 . . ?
C26 C25 N1 105.9(6) . . ?
C26 C25 H25 127.1 . . ?
N1 C25 H25 127.1 . . ?
C35 C34 N3 106.2(6) . . ?
C35 C34 H34 126.9 . . ?
N3 C34 H34 126.9 . . ?
C34 C35 N4 107.9(6) . . ?
C34 C35 H35 126.1 . . ?
N4 C35 H35 126.1 . . ?
C7 C19 H19A 109.5 . . ?
C7 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C7 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C25 C26 N2 107.9(6) . . ?
C25 C26 H26 126.1 . . ?
N2 C26 H26 126.1 . . ?
C22A C20 C21A 113.8(11) . . ?
C21 C20 C10 115.3(8) . . ?
C22A C20 C10 113.6(9) . . ?
C21A C20 C10 111.8(10) . . ?
C21 C20 C23 115.5(16) . . ?
C10 C20 C23 111.7(8) . . ?
C21 C20 C22 105.1(14) . . ?
C10 C20 C22 107.3(7) . . ?
C23 C20 C22 100.2(11) . . ?
C22A C20 C23A 106.1(10) . . ?
C21A C20 C23A 104.6(10) . . ?
C10 C20 C23A 106.0(7) . . ?
C7 C18 H18A 109.5 . . ?
C7 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C7 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N4 C39 C40 110.7(6) . . ?
N4 C39 C41 109.5(6) . . ?
C40 C39 C41 112.2(7) . . ?
N4 C39 H39 108.1 . . ?
C40 C39 H39 108.1 . . ?
C41 C39 H39 108.1 . . ?
N2 C30 C31 109.4(6) . . ?
N2 C30 C32 110.2(6) . . ?
C31 C30 C32 111.5(6) . . ?
N2 C30 H30 108.6 . . ?
C31 C30 H30 108.6 . . ?
C32 C30 H30 108.6 . . ?
C14 C17 H17A 109.5 . . ?
C14 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C14 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
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 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
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 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
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 . . ?
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 . . ?
C20 C21A H21A 109.5 . . ?
C20 C21A H21B 109.5 . . ?
H21A C21A H21B 109.5 . . ?
C20 C21A H21C 109.5 . . ?
H21A C21A H21C 109.5 . . ?
H21B C21A H21C 109.5 . . ?
C20 C23 H23A 109.5 . . ?
C20 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C20 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C20 C23A H23D 109.5 . . ?
C20 C23A H23E 109.5 . . ?
H23D C23A H23E 109.5 . . ?
C20 C23A H23F 109.5 . . ?
H23D C23A H23F 109.5 . . ?
H23E C23A H23F 109.5 . . ?
C20 C22A H22D 109.5 . . ?
C20 C22A H22E 109.5 . . ?
H22D C22A H22E 109.5 . . ?
C20 C22A H22F 109.5 . . ?
H22D C22A H22F 109.5 . . ?
H22E C22A H22F 109.5 . . ?
C20 C21 H21D 109.5 . . ?
C20 C21 H21E 109.5 . . ?
H21D C21 H21E 109.5 . . ?
C20 C21 H21F 109.5 . . ?
H21D C21 H21F 109.5 . . ?
H21E C21 H21F 109.5 . . ?

_refine_diff_density_max         0.402
_refine_diff_density_min         -0.359
_refine_diff_density_rms         0.073



####################################################################### 
# 
# 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_1c
_database_code_depnum_ccdc_archive 'CCDC 2357716'
loop_
_audit_author_name
_audit_author_address
'Terrance Hadlington'
;TU Munich
Germany
;
_audit_update_record             
;
2024-05-23 deposited with the CCDC.	2024-07-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H38 N4 O P2'
_chemical_formula_sum            'C30 H38 N4 O P2'
_chemical_formula_weight         532.58

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   10.840(2)
_cell_length_b                   23.820(5)
_cell_length_c                   26.540(5)
_cell_angle_alpha                90
_cell_angle_beta                 100.20(3)
_cell_angle_gamma                90
_cell_volume                     6745(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    2000
_cell_measurement_theta_min      1.92
_cell_measurement_theta_max      32.50

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.049
_exptl_crystal_F_000             2272
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.13
_exptl_absorpt_coefficient_mu    0.154
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.974
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'STOE X-AREA 1.76'

_diffrn_ambient_temperature      150(2)
_diffrn_source                   'Genix 3D HF Mo'
_diffrn_source_voltage           50
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_collimation    '0.6 mm diameter'
_diffrn_measurement_device_type  'STOE StadiVari'
_diffrn_measurement_method       'ω scans'
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_reflns_number            50683
_diffrn_reflns_av_unetI/netI     0.2084
_diffrn_reflns_av_R_equivalents  0.1505
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         2.563
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             13267
_reflns_number_gt                5464
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          SQUEEZE
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 -0.010 0.500 0.000 586 83 'C7 H8'
2 0.438 1.000 0.500 586 83 'C7 H8'
_platon_squeeze_details          
;
The unit cell contains 16 toluene molecules which have been treated
as a diffuse contribution to the overall scattering without specific atom
positions by SQUEEZE/PLATON.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0848P)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         13267
_refine_ls_number_parameters     691
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1688
_refine_ls_R_factor_gt           0.0764
_refine_ls_wR_factor_ref         0.1929
_refine_ls_wR_factor_gt          0.1693
_refine_ls_goodness_of_fit_ref   0.862
_refine_ls_restrained_S_all      0.862
_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
P2 P 0.02927(10) 0.39858(5) 0.74221(4) 0.0336(3) Uani 1 1 d . . . . .
P3 P 0.50645(10) 0.19583(5) 0.87425(5) 0.0354(3) Uani 1 1 d . . . . .
P1 P -0.43730(10) 0.44530(5) 0.61476(5) 0.0400(3) Uani 1 1 d . . . . .
P4 P 0.39179(12) 0.36901(5) 1.00211(5) 0.0461(4) Uani 1 1 d . . . . .
O1 O -0.1366(2) 0.41839(11) 0.63828(10) 0.0266(6) Uani 1 1 d . . . . .
O2 O 0.5574(2) 0.30813(11) 0.92581(10) 0.0325(7) Uani 1 1 d . . . . .
N6 N 0.6800(3) 0.10618(14) 0.86627(13) 0.0318(8) Uani 1 1 d . . . . .
N3 N 0.2484(3) 0.33277(15) 0.78055(12) 0.0342(9) Uani 1 1 d . . . . .
C1 C -0.1944(3) 0.42966(16) 0.58828(15) 0.0266(10) Uani 1 1 d . . . . .
C12 C -0.0088(3) 0.41506(16) 0.63760(15) 0.0243(9) Uani 1 1 d . . . . .
N1 N -0.3458(3) 0.34390(15) 0.66710(13) 0.0354(9) Uani 1 1 d . . . . .
N4 N 0.2226(3) 0.40370(14) 0.82876(13) 0.0333(9) Uani 1 1 d . . . . .
N5 N 0.4906(3) 0.09161(14) 0.82553(13) 0.0300(8) Uani 1 1 d . . . . .
N2 N -0.3765(3) 0.41144(16) 0.71780(14) 0.0417(10) Uani 1 1 d . . . . .
N7 N 0.2994(3) 0.25929(16) 0.98262(13) 0.0390(9) Uani 1 1 d . . . . .
C11 C 0.0797(3) 0.40454(16) 0.68087(15) 0.0267(9) Uani 1 1 d . . . . .
C7 C 0.0148(4) 0.42474(17) 0.58830(15) 0.0294(10) Uani 1 1 d . . . . .
C43 C 0.5655(4) 0.13099(17) 0.85379(15) 0.0278(10) Uani 1 1 d . . . . .
C42 C 0.5989(4) 0.35980(18) 0.94665(16) 0.0361(11) Uani 1 1 d . . . . .
C22 C 0.1733(3) 0.37832(17) 0.78286(15) 0.0290(10) Uani 1 1 d . . . . .
C2 C -0.3220(3) 0.43745(17) 0.57341(16) 0.0284(10) Uani 1 1 d . . . . .
C55 C 0.1822(4) 0.2782(2) 0.94949(18) 0.0498(13) Uani 1 1 d . . . . .
H55 H 0.192746 0.318392 0.940121 0.060 Uiso 1 1 calc R U . . .
C31 C 0.6406(4) 0.29356(18) 0.89377(15) 0.0313(10) Uani 1 1 d . . . . .
C45 C 0.6767(4) 0.05223(18) 0.84660(16) 0.0346(11) Uani 1 1 d . . . . .
C3 C -0.3597(4) 0.44744(17) 0.51999(16) 0.0357(11) Uani 1 1 d . . . . .
H3 H -0.446557 0.451311 0.506634 0.043 Uiso 1 1 calc R U . . .
C13 C -0.3794(4) 0.39904(19) 0.66693(17) 0.0341(11) Uani 1 1 d . . . . .
C6 C -0.1056(4) 0.43408(17) 0.55601(15) 0.0287(10) Uani 1 1 d . . . . .
C19 C -0.3488(4) 0.30869(19) 0.62060(17) 0.0428(12) Uani 1 1 d . . . . .
H19 H -0.353467 0.334069 0.590310 0.051 Uiso 1 1 calc R U . . .
C8 C 0.1398(4) 0.42319(18) 0.57980(17) 0.0356(11) Uani 1 1 d . . . . .
H8 H 0.159971 0.429575 0.546878 0.043 Uiso 1 1 calc R U . . .
C44 C 0.5591(4) 0.04335(18) 0.82117(16) 0.0340(11) Uani 1 1 d . . . . .
N8 N 0.4903(3) 0.25750(17) 1.02329(13) 0.0425(10) Uani 1 1 d . . . . .
C10 C 0.2034(4) 0.40334(17) 0.67026(16) 0.0344(11) Uani 1 1 d . . . . .
H10 H 0.270875 0.396331 0.697642 0.041 Uiso 1 1 calc R U . . .
C9 C 0.2302(4) 0.41200(19) 0.62149(18) 0.0395(12) Uani 1 1 d . . . . .
H9 H 0.315043 0.410049 0.616923 0.047 Uiso 1 1 calc R U . . .
C33 C 0.7268(4) 0.23798(18) 0.83649(16) 0.0367(11) Uani 1 1 d . . . . .
H33 H 0.727484 0.205089 0.816290 0.044 Uiso 1 1 calc R U . . .
C49 C 0.7822(4) 0.12649(19) 0.90689(16) 0.0385(11) Uani 1 1 d . . . . .
H49 H 0.773529 0.168102 0.909840 0.046 Uiso 1 1 calc R U . . .
C5 C -0.1478(4) 0.44553(17) 0.50324(16) 0.0355(11) Uani 1 1 d . . . . .
H5 H -0.090171 0.448775 0.480258 0.043 Uiso 1 1 calc R U . . .
C46 C 0.3558(4) 0.09919(19) 0.80750(16) 0.0380(11) Uani 1 1 d . . . . .
H46 H 0.339580 0.140009 0.800425 0.046 Uiso 1 1 calc R U . . .
C23 C 0.3391(4) 0.32950(19) 0.82466(16) 0.0383(11) Uani 1 1 d . . . . .
C32 C 0.6320(4) 0.24362(18) 0.86720(15) 0.0332(10) Uani 1 1 d . . . . .
C25 C 0.2252(4) 0.28768(18) 0.74152(16) 0.0367(11) Uani 1 1 d . . . . .
H25 H 0.174262 0.303778 0.709696 0.044 Uiso 1 1 calc R U . . .
C4 C -0.2746(4) 0.45177(19) 0.48644(17) 0.0405(12) Uani 1 1 d . . . . .
H4 H -0.304784 0.459184 0.451244 0.049 Uiso 1 1 calc R U . . .
C36 C 0.7307(4) 0.33632(19) 0.89299(17) 0.0392(11) Uani 1 1 d . . . . .
C16 C -0.3892(4) 0.4687(2) 0.73849(19) 0.0507(13) Uani 1 1 d . . . . .
H16 H -0.381468 0.496307 0.710800 0.061 Uiso 1 1 calc R U . . .
C26 C 0.1506(4) 0.2407(2) 0.76013(18) 0.0539(14) Uani 1 1 d . . . . .
H26A H 0.198097 0.225021 0.791858 0.081 Uiso 1 1 calc R U . . .
H26B H 0.134986 0.211288 0.733998 0.081 Uiso 1 1 calc R U . . .
H26C H 0.070507 0.255506 0.766605 0.081 Uiso 1 1 calc R U . . .
C24 C 0.3222(4) 0.37329(19) 0.85432(16) 0.0397(11) Uani 1 1 d . . . . .
C28 C 0.1780(4) 0.45690(18) 0.84737(16) 0.0358(11) Uani 1 1 d . . . . .
H28 H 0.127155 0.476740 0.817510 0.043 Uiso 1 1 calc R U . . .
C37 C 0.7039(4) 0.3793(2) 0.92802(18) 0.0429(12) Uani 1 1 d . . . . .
C52 C 0.3984(4) 0.29313(19) 1.00086(15) 0.0377(11) Uani 1 1 d . . . . .
C34 C 0.8176(4) 0.2782(2) 0.83484(18) 0.0433(12) Uani 1 1 d . . . . .
H34 H 0.878472 0.271914 0.813722 0.052 Uiso 1 1 calc R U . . .
C15 C -0.3456(4) 0.3649(2) 0.74756(17) 0.0480(13) Uani 1 1 d . . . . .
C48 C 0.3110(4) 0.0666(2) 0.75790(18) 0.0569(14) Uani 1 1 d . . . . .
H48A H 0.368632 0.073263 0.733943 0.085 Uiso 1 1 calc R U . . .
H48B H 0.226723 0.079205 0.742477 0.085 Uiso 1 1 calc R U . . .
H48C H 0.308992 0.026357 0.765531 0.085 Uiso 1 1 calc R U . . .
C54 C 0.3314(5) 0.2043(2) 0.99336(18) 0.0474(13) Uani 1 1 d . . . . .
C40 C 0.5948(5) 0.4402(2) 0.9967(2) 0.0590(14) Uani 1 1 d . . . . .
H40 H 0.560990 0.462212 1.020839 0.071 Uiso 1 1 calc R U . . .
C29 C 0.2865(5) 0.4942(2) 0.86913(19) 0.0570(14) Uani 1 1 d . . . . .
H29A H 0.334021 0.476925 0.900112 0.085 Uiso 1 1 calc R U . . .
H29B H 0.254893 0.530878 0.877676 0.085 Uiso 1 1 calc R U . . .
H29C H 0.341285 0.499023 0.843769 0.085 Uiso 1 1 calc R U . . .
C35 C 0.8232(4) 0.3274(2) 0.86287(19) 0.0523(14) Uani 1 1 d . . . . .
H35 H 0.887449 0.354216 0.861797 0.063 Uiso 1 1 calc R U . . .
C41 C 0.5378(4) 0.38850(19) 0.98188(17) 0.0411(12) Uani 1 1 d . . . . .
C51 C 0.9106(4) 0.1142(2) 0.8930(2) 0.0536(14) Uani 1 1 d . . . . .
H51A H 0.923369 0.073457 0.892238 0.080 Uiso 1 1 calc R U . . .
H51B H 0.976220 0.131039 0.918724 0.080 Uiso 1 1 calc R U . . .
H51C H 0.914496 0.130059 0.859310 0.080 Uiso 1 1 calc R U . . .
C14 C -0.3253(4) 0.3231(2) 0.71613(19) 0.0481(13) Uani 1 1 d . . . . .
C53 C 0.4485(5) 0.2026(2) 1.01856(19) 0.0494(13) Uani 1 1 d . . . . .
C38 C 0.7540(5) 0.4310(2) 0.9439(2) 0.0635(15) Uani 1 1 d . . . . .
H38 H 0.825032 0.445485 0.931857 0.076 Uiso 1 1 calc R U . . .
C47 C 0.2843(4) 0.0813(2) 0.84985(19) 0.0559(14) Uani 1 1 d . . . . .
H47A H 0.297721 0.041112 0.856866 0.084 Uiso 1 1 calc R U . . .
H47B H 0.194575 0.088410 0.838694 0.084 Uiso 1 1 calc R U . . .
H47C H 0.314871 0.102776 0.881029 0.084 Uiso 1 1 calc R U . . .
C58 C 0.6129(5) 0.2741(2) 1.05238(19) 0.0623(15) Uani 1 1 d . . . . .
H58 H 0.622809 0.315488 1.048307 0.075 Uiso 1 1 calc R U . . .
C50 C 0.7663(5) 0.1000(2) 0.95807(17) 0.0553(14) Uani 1 1 d . . . . .
H50A H 0.684171 0.110179 0.965869 0.083 Uiso 1 1 calc R U . . .
H50B H 0.832377 0.113754 0.985324 0.083 Uiso 1 1 calc R U . . .
H50C H 0.772273 0.059030 0.955680 0.083 Uiso 1 1 calc R U . . .
C21 C -0.2281(4) 0.2744(2) 0.6258(2) 0.0600(15) Uani 1 1 d . . . . .
H21A H -0.156036 0.299861 0.629613 0.090 Uiso 1 1 calc R U . . .
H21B H -0.230096 0.251208 0.595224 0.090 Uiso 1 1 calc R U . . .
H21C H -0.220800 0.250180 0.656072 0.090 Uiso 1 1 calc R U . . .
C39 C 0.6966(6) 0.4611(2) 0.9783(2) 0.0719(17) Uani 1 1 d . . . . .
H39 H 0.728537 0.497002 0.989395 0.086 Uiso 1 1 calc R U . . .
C20 C -0.4661(5) 0.2729(2) 0.6133(2) 0.0649(16) Uani 1 1 d . . . . .
H20A H -0.464398 0.248685 0.643323 0.097 Uiso 1 1 calc R U . . .
H20B H -0.469541 0.249537 0.582693 0.097 Uiso 1 1 calc R U . . .
H20C H -0.540096 0.297169 0.609275 0.097 Uiso 1 1 calc R U . . .
C57 C 0.1566(4) 0.2437(3) 0.90036(19) 0.0708(17) Uani 1 1 d . . . . .
H57A H 0.232173 0.242595 0.884875 0.106 Uiso 1 1 calc R U . . .
H57B H 0.087903 0.260870 0.876333 0.106 Uiso 1 1 calc R U . . .
H57C H 0.133172 0.205374 0.908312 0.106 Uiso 1 1 calc R U . . .
C60 C 0.6178(6) 0.2617(3) 1.1087(2) 0.100(2) Uani 1 1 d . . . . .
H60A H 0.554902 0.284512 1.121649 0.150 Uiso 1 1 calc R U . . .
H60B H 0.701326 0.270809 1.127749 0.150 Uiso 1 1 calc R U . . .
H60C H 0.600259 0.221834 1.113139 0.150 Uiso 1 1 calc R U . . .
C17 C -0.2819(5) 0.4793(3) 0.7827(2) 0.089(2) Uani 1 1 d . . . . .
H17A H -0.300021 0.461011 0.813611 0.133 Uiso 1 1 calc R U . . .
H17B H -0.272111 0.519767 0.788627 0.133 Uiso 1 1 calc R U . . .
H17C H -0.204194 0.463864 0.774222 0.133 Uiso 1 1 calc R U . . .
C27 C 0.3488(4) 0.2678(2) 0.72896(18) 0.0544(14) Uani 1 1 d . . . . .
H27A H 0.390861 0.299129 0.715110 0.082 Uiso 1 1 calc R U . . .
H27B H 0.333475 0.237612 0.703516 0.082 Uiso 1 1 calc R U . . .
H27C H 0.402000 0.253717 0.760127 0.082 Uiso 1 1 calc R U . . .
C56 C 0.0736(5) 0.2745(3) 0.9794(2) 0.081(2) Uani 1 1 d . . . . .
H56A H 0.061880 0.235359 0.988892 0.122 Uiso 1 1 calc R U . . .
H56B H -0.003447 0.288353 0.958011 0.122 Uiso 1 1 calc R U . . .
H56C H 0.092904 0.297463 1.010466 0.122 Uiso 1 1 calc R U . . .
C18 C -0.5151(5) 0.4766(2) 0.7530(3) 0.083(2) Uani 1 1 d . . . . .
H18A H -0.579839 0.475564 0.722159 0.124 Uiso 1 1 calc R U . . .
H18B H -0.517734 0.512964 0.770078 0.124 Uiso 1 1 calc R U . . .
H18C H -0.530188 0.446485 0.776311 0.124 Uiso 1 1 calc R U . . .
C59 C 0.7179(5) 0.2449(3) 1.0319(2) 0.091(2) Uani 1 1 d . . . . .
H59A H 0.714234 0.204416 1.038246 0.136 Uiso 1 1 calc R U . . .
H59B H 0.798782 0.259659 1.049107 0.136 Uiso 1 1 calc R U . . .
H59C H 0.708604 0.251572 0.994949 0.136 Uiso 1 1 calc R U . . .
C30 C 0.0937(5) 0.4447(2) 0.8854(2) 0.0750(19) Uani 1 1 d . . . . .
H30A H 0.024035 0.420887 0.869405 0.113 Uiso 1 1 calc R U . . .
H30B H 0.060731 0.480059 0.896513 0.113 Uiso 1 1 calc R U . . .
H30C H 0.141626 0.425301 0.915137 0.113 Uiso 1 1 calc R U . . .
H1 H 0.758176 0.028555 0.847323 0.024(10) Uiso 1 1 d R . . . .
H11 H -0.328524 0.366055 0.790823 0.042(11) Uiso 1 1 d R . . . .
H12 H 0.517476 0.170155 1.027423 0.060(14) Uiso 1 1 d R . . . .
H14 H 0.520576 0.009055 0.802923 0.034(11) Uiso 1 1 d R . . . .
H15 H 0.397276 0.298555 0.830223 0.027(10) Uiso 1 1 d R . . . .
H17 H 0.263376 0.171055 0.985223 0.062(14) Uiso 1 1 d R . . . .
H2 H -0.307824 0.281855 0.728023 0.058(14) Uiso 1 1 d R . . . .
H6 H 0.362716 0.382205 0.894273 0.090(17) Uiso 1 1 d R . . . .


_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
P2 C22 1.800(4) . ?
P2 C11 1.812(4) . ?
P3 C43 1.793(4) . ?
P3 C32 1.809(4) . ?
P1 C13 1.794(5) . ?
P1 C2 1.813(4) . ?
P4 C52 1.809(5) . ?
P4 C41 1.819(5) . ?
O1 C1 1.390(4) . ?
O1 C12 1.391(4) . ?
O2 C31 1.388(5) . ?
O2 C42 1.391(5) . ?
N6 C43 1.362(5) . ?
N6 C45 1.385(5) . ?
N6 C49 1.483(5) . ?
N3 C22 1.364(5) . ?
N3 C23 1.391(5) . ?
N3 C25 1.482(5) . ?
C1 C2 1.382(5) . ?
C1 C6 1.401(5) . ?
C12 C11 1.383(5) . ?
C12 C7 1.396(5) . ?
N1 C13 1.363(5) . ?
N1 C14 1.373(5) . ?
N1 C19 1.488(5) . ?
N4 C24 1.375(5) . ?
N4 C22 1.380(5) . ?
N4 C28 1.473(5) . ?
N5 C43 1.373(5) . ?
N5 C44 1.385(5) . ?
N5 C46 1.466(5) . ?
N2 C15 1.368(6) . ?
N2 C13 1.377(5) . ?
N2 C16 1.487(6) . ?
N7 C52 1.361(5) . ?
N7 C54 1.373(6) . ?
N7 C55 1.481(5) . ?
C11 C10 1.418(5) . ?
C7 C8 1.413(5) . ?
C7 C6 1.446(5) . ?
C42 C37 1.399(6) . ?
C42 C41 1.414(6) . ?
C2 C3 1.424(6) . ?
C55 C57 1.525(7) . ?
C55 C56 1.536(6) . ?
C31 C32 1.377(6) . ?
C31 C36 1.414(6) . ?
C45 C44 1.349(6) . ?
C3 C4 1.395(6) . ?
C6 C5 1.421(5) . ?
C19 C20 1.515(6) . ?
C19 C21 1.528(6) . ?
C8 C9 1.368(6) . ?
N8 C52 1.363(5) . ?
N8 C53 1.383(6) . ?
N8 C58 1.468(6) . ?
C10 C9 1.391(6) . ?
C33 C34 1.380(6) . ?
C33 C32 1.427(6) . ?
C49 C51 1.529(6) . ?
C49 C50 1.535(6) . ?
C5 C4 1.376(6) . ?
C46 C48 1.532(6) . ?
C46 C47 1.535(6) . ?
C23 C24 1.339(6) . ?
C25 C27 1.512(5) . ?
C25 C26 1.513(6) . ?
C36 C35 1.405(6) . ?
C36 C37 1.447(6) . ?
C16 C18 1.494(6) . ?
C16 C17 1.519(7) . ?
C28 C30 1.505(6) . ?
C28 C29 1.505(6) . ?
C37 C38 1.381(6) . ?
C34 C35 1.383(6) . ?
C15 C14 1.342(6) . ?
C54 C53 1.326(6) . ?
C40 C39 1.376(7) . ?
C40 C41 1.403(6) . ?
C38 C39 1.390(7) . ?
C58 C60 1.515(7) . ?
C58 C59 1.515(7) . ?

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
C22 P2 C11 101.05(18) . . ?
C43 P3 C32 101.25(19) . . ?
C13 P1 C2 102.68(19) . . ?
C52 P4 C41 102.1(2) . . ?
C1 O1 C12 106.3(3) . . ?
C31 O2 C42 105.4(3) . . ?
C43 N6 C45 110.4(3) . . ?
C43 N6 C49 124.5(3) . . ?
C45 N6 C49 122.9(3) . . ?
C22 N3 C23 110.2(3) . . ?
C22 N3 C25 125.4(3) . . ?
C23 N3 C25 123.7(4) . . ?
C2 C1 O1 123.9(3) . . ?
C2 C1 C6 125.2(4) . . ?
O1 C1 C6 110.9(3) . . ?
C11 C12 O1 123.1(3) . . ?
C11 C12 C7 126.4(3) . . ?
O1 C12 C7 110.6(3) . . ?
C13 N1 C14 110.4(4) . . ?
C13 N1 C19 125.0(4) . . ?
C14 N1 C19 123.9(4) . . ?
C24 N4 C22 110.6(3) . . ?
C24 N4 C28 124.3(3) . . ?
C22 N4 C28 125.0(3) . . ?
C43 N5 C44 109.8(3) . . ?
C43 N5 C46 123.6(3) . . ?
C44 N5 C46 126.4(4) . . ?
C15 N2 C13 110.7(4) . . ?
C15 N2 C16 124.1(4) . . ?
C13 N2 C16 124.9(4) . . ?
C52 N7 C54 109.7(4) . . ?
C52 N7 C55 124.8(4) . . ?
C54 N7 C55 124.9(4) . . ?
C12 C11 C10 112.4(3) . . ?
C12 C11 P2 119.0(3) . . ?
C10 C11 P2 128.5(3) . . ?
C12 C7 C8 119.0(4) . . ?
C12 C7 C6 106.5(3) . . ?
C8 C7 C6 134.4(4) . . ?
N6 C43 N5 105.2(3) . . ?
N6 C43 P3 131.3(3) . . ?
N5 C43 P3 123.0(3) . . ?
O2 C42 C37 112.3(4) . . ?
O2 C42 C41 122.3(4) . . ?
C37 C42 C41 125.4(4) . . ?
N3 C22 N4 104.3(3) . . ?
N3 C22 P2 130.3(3) . . ?
N4 C22 P2 124.8(3) . . ?
C1 C2 C3 113.8(4) . . ?
C1 C2 P1 127.1(3) . . ?
C3 C2 P1 118.6(3) . . ?
N7 C55 C57 110.5(4) . . ?
N7 C55 C56 109.3(4) . . ?
C57 C55 C56 111.8(4) . . ?
C32 C31 O2 122.5(4) . . ?
C32 C31 C36 126.8(4) . . ?
O2 C31 C36 110.7(4) . . ?
C44 C45 N6 107.1(4) . . ?
C4 C3 C2 122.8(4) . . ?
N1 C13 N2 104.1(4) . . ?
N1 C13 P1 130.6(3) . . ?
N2 C13 P1 124.7(3) . . ?
C1 C6 C5 118.8(4) . . ?
C1 C6 C7 105.8(3) . . ?
C5 C6 C7 135.4(4) . . ?
N1 C19 C20 108.6(3) . . ?
N1 C19 C21 109.4(4) . . ?
C20 C19 C21 113.3(4) . . ?
C9 C8 C7 116.5(4) . . ?
C45 C44 N5 107.5(4) . . ?
C52 N8 C53 110.3(4) . . ?
C52 N8 C58 125.9(4) . . ?
C53 N8 C58 123.6(4) . . ?
C9 C10 C11 122.8(4) . . ?
C8 C9 C10 122.9(4) . . ?
C34 C33 C32 122.9(4) . . ?
N6 C49 C51 110.9(4) . . ?
N6 C49 C50 108.8(4) . . ?
C51 C49 C50 112.5(4) . . ?
C4 C5 C6 117.9(4) . . ?
N5 C46 C48 111.4(3) . . ?
N5 C46 C47 109.3(4) . . ?
C48 C46 C47 111.3(4) . . ?
C24 C23 N3 107.5(4) . . ?
C31 C32 C33 112.6(4) . . ?
C31 C32 P3 118.3(3) . . ?
C33 C32 P3 129.1(3) . . ?
N3 C25 C27 109.5(3) . . ?
N3 C25 C26 110.0(3) . . ?
C27 C25 C26 112.7(4) . . ?
C5 C4 C3 121.4(4) . . ?
C35 C36 C31 117.6(4) . . ?
C35 C36 C37 135.8(4) . . ?
C31 C36 C37 106.5(4) . . ?
N2 C16 C18 111.1(4) . . ?
N2 C16 C17 109.2(4) . . ?
C18 C16 C17 112.9(4) . . ?
C23 C24 N4 107.3(4) . . ?
N4 C28 C30 109.5(4) . . ?
N4 C28 C29 110.8(4) . . ?
C30 C28 C29 112.5(4) . . ?
C38 C37 C42 119.3(5) . . ?
C38 C37 C36 135.7(5) . . ?
C42 C37 C36 105.1(4) . . ?
N7 C52 N8 104.8(4) . . ?
N7 C52 P4 124.5(3) . . ?
N8 C52 P4 130.0(4) . . ?
C33 C34 C35 122.3(4) . . ?
C14 C15 N2 107.0(4) . . ?
C53 C54 N7 108.6(4) . . ?
C39 C40 C41 124.0(5) . . ?
C34 C35 C36 117.9(4) . . ?
C40 C41 C42 112.0(4) . . ?
C40 C41 P4 120.3(4) . . ?
C42 C41 P4 127.3(3) . . ?
C15 C14 N1 107.7(4) . . ?
C54 C53 N8 106.6(4) . . ?
C37 C38 C39 117.6(5) . . ?
N8 C58 C60 109.7(4) . . ?
N8 C58 C59 110.8(5) . . ?
C60 C58 C59 111.6(5) . . ?
C40 C39 C38 121.8(5) . . ?

_refine_diff_density_max         0.324
_refine_diff_density_min         -0.433
_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_1b
_database_code_depnum_ccdc_archive 'CCDC 2357717'
loop_
_audit_author_name
_audit_author_address
'Terrance Hadlington'
;TU Munich
Germany
;
_audit_update_record             
;
2024-05-23 deposited with the CCDC.	2024-07-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C41 H60 N4 O P2'
_chemical_formula_sum            'C41 H60 N4 O P2'
_chemical_formula_weight         686.87

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   18.707(4)
_cell_length_b                   15.187(3)
_cell_length_c                   31.540(6)
_cell_angle_alpha                90
_cell_angle_beta                 99.45(3)
_cell_angle_gamma                90
_cell_volume                     8839(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    2000
_cell_measurement_theta_min      1.92
_cell_measurement_theta_max      32.50

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.032
_exptl_crystal_F_000             2976
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.21
_exptl_absorpt_coefficient_mu    0.130
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.959
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'STOE X-AREA 1.76'

_diffrn_ambient_temperature      150(2)
_diffrn_source                   'Genix 3D HF Mo'
_diffrn_source_voltage           50
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_collimation    '0.6 mm diameter'
_diffrn_measurement_device_type  'STOE StadiVari'
_diffrn_measurement_method       'ω scans'
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_reflns_number            66457
_diffrn_reflns_av_unetI/netI     0.0893
_diffrn_reflns_av_R_equivalents  0.0636
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_theta_min         2.063
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             17265
_reflns_number_gt                9744
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          SQUEEZE
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 0.750 -0.009 0.250 745 60 'C7 H16'
2 0.250 -0.014 0.750 745 60 'C7 H16'
3 0.004 0.115 0.649 16 1 ' '
4 0.868 0.156 0.498 40 1 ' '
5 0.385 0.236 0.497 19 1 ' '
6 0.885 0.264 -0.003 19 1 ' '
7 0.368 0.344 -0.002 40 1 ' '
8 0.504 0.385 0.149 16 1 ' '
9 0.496 0.615 0.851 16 1 ' '
10 0.632 0.656 0.002 40 1 ' '
11 0.115 0.736 0.003 19 1 ' '
12 0.615 0.764 0.503 19 1 ' '
13 0.132 0.844 0.502 40 1 ' '
14 -0.004 0.885 0.351 16 1 ' '
_platon_squeeze_details          
;
The unit cell contains 16 heptane molecules which have been treated
as a diffuse contribution to the overall scattering without specific atom
positions by SQUEEZE/PLATON.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0801P)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         17265
_refine_ls_number_parameters     898
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1088
_refine_ls_R_factor_gt           0.0561
_refine_ls_wR_factor_ref         0.1496
_refine_ls_wR_factor_gt          0.1337
_refine_ls_goodness_of_fit_ref   0.911
_refine_ls_restrained_S_all      0.911
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.28397(4) 0.59424(5) 0.25241(2) 0.02889(17) Uani 1 1 d . . . . .
P4 P 0.26333(4) 0.04164(5) 0.49087(2) 0.03314(18) Uani 1 1 d . . . . .
P2 P 0.46450(3) 0.68453(5) 0.35210(2) 0.03288(18) Uani 1 1 d . . . . .
P3 P 0.23749(4) 0.31989(5) 0.44841(2) 0.03583(19) Uani 1 1 d . . . . .
O1 O 0.31242(8) 0.70669(12) 0.33475(5) 0.0265(4) Uani 1 1 d . . . . .
O2 O 0.18754(9) 0.21584(12) 0.51147(5) 0.0282(4) Uani 1 1 d . . . . .
N5 N 0.29020(11) 0.44802(15) 0.39648(7) 0.0299(5) Uani 1 1 d . . . . .
N7 N 0.24899(11) 0.10095(15) 0.40767(6) 0.0306(5) Uani 1 1 d . . . . .
N6 N 0.17416(11) 0.45882(15) 0.39234(7) 0.0320(5) Uani 1 1 d . . . . .
N2 N 0.37285(11) 0.74878(15) 0.24568(6) 0.0294(5) Uani 1 1 d . . . . .
N1 N 0.42606(11) 0.62118(16) 0.24453(7) 0.0316(5) Uani 1 1 d . . . . .
N8 N 0.14284(11) 0.09977(16) 0.42697(7) 0.0333(5) Uani 1 1 d . . . . .
C2 C 0.22250(12) 0.66108(18) 0.27859(8) 0.0262(6) Uani 1 1 d . . . . .
C13 C 0.33512(12) 0.73539(17) 0.37697(8) 0.0243(6) Uani 1 1 d . . . . .
C12 C 0.41062(12) 0.72805(18) 0.39056(8) 0.0263(6) Uani 1 1 d . . . . .
C1 C 0.23973(12) 0.70309(17) 0.31871(8) 0.0236(6) Uani 1 1 d . . . . .
C11 C 0.43529(13) 0.75064(18) 0.43347(8) 0.0288(6) Uani 1 1 d . . . . .
H11 H 0.485647 0.745916 0.444191 0.035 Uiso 1 1 calc R U . . .
C8 C 0.28746(12) 0.76582(17) 0.40241(8) 0.0244(6) Uani 1 1 d . . . . .
C6 C 0.18746(13) 0.73676(17) 0.34067(8) 0.0254(6) Uani 1 1 d . . . . .
C53 C 0.19281(12) 0.36410(18) 0.49062(8) 0.0274(6) Uani 1 1 d . . . . .
C65 C 0.23264(14) 0.41464(18) 0.41324(8) 0.0299(6) Uani 1 1 d . . . . .
C7 C 0.20723(13) 0.77845(18) 0.38511(8) 0.0275(6) Uani 1 1 d . . . . .
N4 N 0.57994(11) 0.79726(18) 0.38995(8) 0.0402(6) Uani 1 1 d . . . . .
C54 C 0.17261(12) 0.30282(18) 0.52042(8) 0.0264(6) Uani 1 1 d . . . . .
C42 C 0.18443(12) 0.15256(18) 0.54228(8) 0.0257(6) Uani 1 1 d . . . . .
C3 C 0.14937(13) 0.65738(18) 0.26032(8) 0.0301(6) Uani 1 1 d . . . . .
H3 H 0.136450 0.629727 0.233120 0.036 Uiso 1 1 calc R U . . .
C43 C 0.21263(13) 0.06968(18) 0.53385(8) 0.0280(6) Uani 1 1 d . . . . .
C10 C 0.38961(13) 0.77968(17) 0.46116(8) 0.0266(6) Uani 1 1 d . . . . .
C74 C 0.21485(13) 0.08630(18) 0.44237(8) 0.0289(6) Uani 1 1 d . . . . .
C47 C 0.15605(13) 0.16967(19) 0.57948(8) 0.0287(6) Uani 1 1 d . . . . .
C9 C 0.31646(13) 0.78804(18) 0.44521(8) 0.0283(6) Uani 1 1 d . . . . .
H9 H 0.284899 0.809352 0.463606 0.034 Uiso 1 1 calc R U . . .
C49 C 0.14332(13) 0.32722(19) 0.55610(8) 0.0286(6) Uani 1 1 d . . . . .
C24 C 0.36178(13) 0.66052(19) 0.24975(8) 0.0281(6) Uani 1 1 d . . . . .
C44 C 0.21306(13) 0.0052(2) 0.56557(8) 0.0328(6) Uani 1 1 d . . . . .
H44 H 0.232463 -0.051051 0.560765 0.039 Uiso 1 1 calc R U . . .
C45 C 0.18658(13) 0.01897(19) 0.60383(8) 0.0306(6) Uani 1 1 d . . . . .
C46 C 0.15746(13) 0.1008(2) 0.60969(8) 0.0329(7) Uani 1 1 d . . . . .
H46 H 0.137565 0.111143 0.635082 0.040 Uiso 1 1 calc R U . . .
C5 C 0.11499(12) 0.73123(19) 0.32042(8) 0.0290(6) Uani 1 1 d . . . . .
H5 H 0.078501 0.754952 0.334783 0.035 Uiso 1 1 calc R U . . .
C75 C 0.19909(15) 0.1212(2) 0.37197(9) 0.0390(7) Uani 1 1 d . . . . .
H75 H 0.209185 0.133249 0.343991 0.047 Uiso 1 1 calc R U . . .
C4 C 0.09406(13) 0.69268(19) 0.28032(8) 0.0312(6) Uani 1 1 d . . . . .
C52 C 0.18135(13) 0.45256(19) 0.49955(8) 0.0306(6) Uani 1 1 d . . . . .
H52 H 0.194851 0.495730 0.480548 0.037 Uiso 1 1 calc R U . . .
N3 N 0.60630(12) 0.65924(19) 0.39798(9) 0.0528(7) Uani 1 1 d . . . . .
C33 C 0.55200(13) 0.7149(2) 0.38196(8) 0.0331(7) Uani 1 1 d . . . . .
C76 C 0.13414(16) 0.1208(2) 0.38380(9) 0.0414(7) Uani 1 1 d . . . . .
H76 H 0.089421 0.132953 0.365712 0.050 Uiso 1 1 calc R U . . .
C68 C 0.36710(14) 0.4296(2) 0.41301(9) 0.0367(7) Uani 1 1 d . . . . .
H68 H 0.369802 0.375525 0.431272 0.044 Uiso 1 1 calc R U . . .
C51 C 0.15113(13) 0.48127(18) 0.53488(8) 0.0301(6) Uani 1 1 d . . . . .
C67 C 0.19485(15) 0.51758(19) 0.36335(9) 0.0356(7) Uani 1 1 d . . . . .
H67 H 0.163790 0.555561 0.344746 0.043 Uiso 1 1 calc R U . . .
C66 C 0.26659(14) 0.51119(19) 0.36626(8) 0.0338(6) Uani 1 1 d . . . . .
H66 H 0.296060 0.544369 0.350297 0.041 Uiso 1 1 calc R U . . .
C18 C 0.16239(14) 0.7350(2) 0.41670(9) 0.0397(7) Uani 1 1 d . . . . .
H18A H 0.175661 0.672753 0.420384 0.060 Uiso 1 1 calc R U . . .
H18B H 0.110633 0.739947 0.405097 0.060 Uiso 1 1 calc R U . . .
H18C H 0.172527 0.764968 0.444563 0.060 Uiso 1 1 calc R U . . .
C26 C 0.47465(15) 0.6854(2) 0.23656(9) 0.0386(7) Uani 1 1 d . . . . .
H26 H 0.522530 0.675575 0.231210 0.046 Uiso 1 1 calc R U . . .
C25 C 0.44241(14) 0.7632(2) 0.23771(8) 0.0373(7) Uani 1 1 d . . . . .
H25 H 0.463475 0.818922 0.233759 0.045 Uiso 1 1 calc R U . . .
C30 C 0.31824(14) 0.81850(19) 0.24743(9) 0.0343(7) Uani 1 1 d . . . . .
H30 H 0.286701 0.799732 0.268506 0.041 Uiso 1 1 calc R U . . .
C20 C 0.42175(14) 0.7999(2) 0.50838(8) 0.0327(7) Uani 1 1 d . . . . .
C27 C 0.44197(14) 0.5274(2) 0.25205(9) 0.0361(7) Uani 1 1 d . . . . .
H27 H 0.412226 0.506184 0.273603 0.043 Uiso 1 1 calc R U . . .
C71 C 0.09774(13) 0.4384(2) 0.39649(9) 0.0347(7) Uani 1 1 d . . . . .
H71 H 0.097267 0.412636 0.425608 0.042 Uiso 1 1 calc R U . . .
C50 C 0.13272(13) 0.41737(19) 0.56244(9) 0.0323(6) Uani 1 1 d . . . . .
H50 H 0.112065 0.435290 0.586640 0.039 Uiso 1 1 calc R U . . .
C48 C 0.12416(14) 0.2584(2) 0.58797(9) 0.0353(7) Uani 1 1 d . . . . .
C55 C 0.19020(14) -0.0549(2) 0.63729(9) 0.0376(7) Uani 1 1 d . . . . .
C19 C 0.18955(14) 0.87750(19) 0.38228(9) 0.0382(7) Uani 1 1 d . . . . .
H19A H 0.203139 0.904402 0.410707 0.057 Uiso 1 1 calc R U . . .
H19B H 0.137502 0.885563 0.372415 0.057 Uiso 1 1 calc R U . . .
H19C H 0.216755 0.905572 0.361925 0.057 Uiso 1 1 calc R U . . .
C14 C 0.01555(14) 0.6876(2) 0.25716(9) 0.0406(8) Uani 1 1 d . . . . .
C77 C 0.32812(14) 0.1000(2) 0.40962(9) 0.0360(7) Uani 1 1 d . . . . .
H77 H 0.350817 0.113050 0.439925 0.043 Uiso 1 1 calc R U . . .
C70 C 0.40826(16) 0.4123(2) 0.37631(10) 0.0488(8) Uani 1 1 d . . . . .
H70A H 0.383723 0.365944 0.357785 0.073 Uiso 1 1 calc R U . . .
H70B H 0.457718 0.393495 0.387890 0.073 Uiso 1 1 calc R U . . .
H70C H 0.409955 0.466367 0.359523 0.073 Uiso 1 1 calc R U . . .
C61 C 0.13926(16) 0.5796(2) 0.54279(10) 0.0431(7) Uani 1 1 d . . . . .
C23 C 0.47057(17) 0.8812(2) 0.50976(10) 0.0514(9) Uani 1 1 d . . . . .
H23A H 0.509812 0.869543 0.493421 0.077 Uiso 1 1 calc R U . . .
H23B H 0.491182 0.894645 0.539666 0.077 Uiso 1 1 calc R U . . .
H23C H 0.441920 0.931541 0.497075 0.077 Uiso 1 1 calc R U . . .
C21 C 0.36382(15) 0.8191(2) 0.53565(9) 0.0456(8) Uani 1 1 d . . . . .
H21A H 0.335282 0.870203 0.523924 0.068 Uiso 1 1 calc R U . . .
H21B H 0.386861 0.831525 0.565239 0.068 Uiso 1 1 calc R U . . .
H21C H 0.331930 0.767798 0.535393 0.068 Uiso 1 1 calc R U . . .
C80 C 0.08228(14) 0.0843(2) 0.45030(9) 0.0409(7) Uani 1 1 d . . . . .
H80 H 0.102970 0.074759 0.481255 0.049 Uiso 1 1 calc R U . . .
C64 C 0.1403(2) 0.5990(2) 0.59054(11) 0.0635(10) Uani 1 1 d . . . . .
H64A H 0.134104 0.662375 0.594554 0.095 Uiso 1 1 calc R U . . .
H64B H 0.186813 0.580104 0.607045 0.095 Uiso 1 1 calc R U . . .
H64C H 0.100827 0.566991 0.600582 0.095 Uiso 1 1 calc R U . . .
C81 C 0.04195(17) 0.0012(3) 0.43377(11) 0.0587(10) Uani 1 1 d . . . . .
H81A H 0.022719 0.007935 0.403117 0.088 Uiso 1 1 calc R U . . .
H81B H 0.001878 -0.008901 0.449669 0.088 Uiso 1 1 calc R U . . .
H81C H 0.075222 -0.049056 0.437860 0.088 Uiso 1 1 calc R U . . .
C79 C 0.35146(17) 0.1717(2) 0.38119(10) 0.0503(8) Uani 1 1 d . . . . .
H79A H 0.334935 0.156712 0.350942 0.075 Uiso 1 1 calc R U . . .
H79B H 0.404414 0.176557 0.386532 0.075 Uiso 1 1 calc R U . . .
H79C H 0.330094 0.227934 0.387758 0.075 Uiso 1 1 calc R U . . .
C59 C 0.1542(2) 0.2893(2) 0.63420(10) 0.0600(10) Uani 1 1 d . . . . .
H59A H 0.141395 0.246314 0.654862 0.090 Uiso 1 1 calc R U . . .
H59B H 0.133258 0.346681 0.639368 0.090 Uiso 1 1 calc R U . . .
H59C H 0.207080 0.294573 0.637647 0.090 Uiso 1 1 calc R U . . .
C29 C 0.52103(15) 0.5135(3) 0.27102(10) 0.0539(9) Uani 1 1 d . . . . .
H29A H 0.551465 0.530000 0.249791 0.081 Uiso 1 1 calc R U . . .
H29B H 0.529121 0.451393 0.278774 0.081 Uiso 1 1 calc R U . . .
H29C H 0.533591 0.550124 0.296746 0.081 Uiso 1 1 calc R U . . .
C17 C -0.03687(15) 0.7348(3) 0.28187(11) 0.0607(10) Uani 1 1 d . . . . .
H17A H -0.086459 0.728480 0.266342 0.091 Uiso 1 1 calc R U . . .
H17B H -0.024233 0.797413 0.284539 0.091 Uiso 1 1 calc R U . . .
H17C H -0.033540 0.708829 0.310566 0.091 Uiso 1 1 calc R U . . .
C39 C 0.54365(16) 0.8787(2) 0.37374(10) 0.0467(8) Uani 1 1 d . . . . .
H39 H 0.490204 0.870025 0.371664 0.056 Uiso 1 1 calc R U . . .
C31 C 0.27120(17) 0.8288(3) 0.20450(10) 0.0582(10) Uani 1 1 d . . . . .
H31A H 0.301172 0.845367 0.183044 0.087 Uiso 1 1 calc R U . . .
H31B H 0.235015 0.874733 0.206203 0.087 Uiso 1 1 calc R U . . .
H31C H 0.246617 0.772927 0.196141 0.087 Uiso 1 1 calc R U . . .
C78 C 0.35405(16) 0.0098(2) 0.39818(12) 0.0535(9) Uani 1 1 d . . . . .
H78A H 0.337317 -0.034667 0.416840 0.080 Uiso 1 1 calc R U . . .
H78B H 0.407122 0.009250 0.402208 0.080 Uiso 1 1 calc R U . . .
H78C H 0.334474 -0.003547 0.368115 0.080 Uiso 1 1 calc R U . . .
C82 C 0.03365(17) 0.1655(3) 0.44747(12) 0.0630(10) Uani 1 1 d . . . . .
H82A H 0.063141 0.217540 0.456553 0.095 Uiso 1 1 calc R U . . .
H82B H -0.002683 0.157677 0.466279 0.095 Uiso 1 1 calc R U . . .
H82C H 0.009254 0.173265 0.417748 0.095 Uiso 1 1 calc R U . . .
C69 C 0.39875(17) 0.5066(2) 0.44131(11) 0.0560(9) Uani 1 1 d . . . . .
H69A H 0.400168 0.559212 0.423508 0.084 Uiso 1 1 calc R U . . .
H69B H 0.447992 0.491773 0.455316 0.084 Uiso 1 1 calc R U . . .
H69C H 0.368382 0.517973 0.463242 0.084 Uiso 1 1 calc R U . . .
C28 C 0.42005(17) 0.4744(2) 0.21125(10) 0.0537(9) Uani 1 1 d . . . . .
H28A H 0.370551 0.490144 0.198124 0.081 Uiso 1 1 calc R U . . .
H28B H 0.422143 0.411415 0.218190 0.081 Uiso 1 1 calc R U . . .
H28C H 0.453296 0.487219 0.191058 0.081 Uiso 1 1 calc R U . . .
C36 C 0.60105(17) 0.5636(2) 0.40042(12) 0.0588(10) Uani 1 1 d . . . . .
H36 H 0.551970 0.545769 0.385293 0.071 Uiso 1 1 calc R U . . .
C60 C 0.04156(16) 0.2502(2) 0.58300(13) 0.0628(10) Uani 1 1 d . . . . .
H60A H 0.021908 0.232968 0.553434 0.094 Uiso 1 1 calc R U . . .
H60B H 0.020874 0.306929 0.589469 0.094 Uiso 1 1 calc R U . . .
H60C H 0.029077 0.205373 0.602922 0.094 Uiso 1 1 calc R U . . .
C22 C 0.46659(19) 0.7212(2) 0.52782(10) 0.0578(10) Uani 1 1 d . . . . .
H22A H 0.436003 0.668484 0.525472 0.087 Uiso 1 1 calc R U . . .
H22B H 0.485302 0.732996 0.558159 0.087 Uiso 1 1 calc R U . . .
H22C H 0.507197 0.711752 0.512272 0.087 Uiso 1 1 calc R U . . .
C72 C 0.06712(17) 0.3714(3) 0.36318(12) 0.0624(10) Uani 1 1 d . . . . .
H72A H 0.062963 0.397517 0.334475 0.094 Uiso 1 1 calc R U . . .
H72B H 0.019108 0.352780 0.368309 0.094 Uiso 1 1 calc R U . . .
H72C H 0.099392 0.320176 0.365103 0.094 Uiso 1 1 calc R U . . .
C73 C 0.05338(17) 0.5229(2) 0.39270(15) 0.0763(13) Uani 1 1 d . . . . .
H73A H 0.077629 0.566748 0.412920 0.114 Uiso 1 1 calc R U . . .
H73B H 0.005042 0.510652 0.399421 0.114 Uiso 1 1 calc R U . . .
H73C H 0.048913 0.545764 0.363323 0.114 Uiso 1 1 calc R U . . .
C57 C 0.26846(19) -0.0640(3) 0.66013(13) 0.0778(13) Uani 1 1 d . . . . .
H57A H 0.272058 -0.113512 0.680266 0.117 Uiso 1 1 calc R U . . .
H57B H 0.283317 -0.009643 0.675922 0.117 Uiso 1 1 calc R U . . .
H57C H 0.300205 -0.074546 0.638834 0.117 Uiso 1 1 calc R U . . .
C40 C 0.56628(18) 0.9545(3) 0.40456(12) 0.0617(10) Uani 1 1 d . . . . .
H40A H 0.556747 0.938898 0.433256 0.093 Uiso 1 1 calc R U . . .
H40B H 0.538553 1.007326 0.394395 0.093 Uiso 1 1 calc R U . . .
H40C H 0.618127 0.966157 0.405879 0.093 Uiso 1 1 calc R U . . .
C32 C 0.35479(19) 0.9036(2) 0.26335(14) 0.0757(12) Uani 1 1 d . . . . .
H32A H 0.389864 0.892297 0.289454 0.114 Uiso 1 1 calc R U . . .
H32B H 0.318268 0.945613 0.269804 0.114 Uiso 1 1 calc R U . . .
H32C H 0.379954 0.928231 0.241144 0.114 Uiso 1 1 calc R U . . .
C38 C 0.6570(2) 0.5206(3) 0.37756(15) 0.0846(14) Uani 1 1 d . . . . .
H38A H 0.650151 0.540699 0.347639 0.127 Uiso 1 1 calc R U . . .
H38B H 0.651422 0.456501 0.378262 0.127 Uiso 1 1 calc R U . . .
H38C H 0.705672 0.536822 0.391981 0.127 Uiso 1 1 calc R U . . .
C62 C 0.2019(2) 0.6355(2) 0.53055(13) 0.0757(12) Uani 1 1 d . . . . .
H62A H 0.203163 0.628782 0.499773 0.114 Uiso 1 1 calc R U . . .
H62B H 0.247973 0.615459 0.547104 0.114 Uiso 1 1 calc R U . . .
H62C H 0.194230 0.697538 0.536997 0.114 Uiso 1 1 calc R U . . .
C15 C 0.01004(18) 0.7349(4) 0.21368(11) 0.0874(16) Uani 1 1 d . . . . .
H15A H 0.038424 0.702748 0.195232 0.131 Uiso 1 1 calc R U . . .
H15B H 0.028974 0.794920 0.218272 0.131 Uiso 1 1 calc R U . . .
H15C H -0.040793 0.737219 0.199799 0.131 Uiso 1 1 calc R U . . .
C41 C 0.5598(2) 0.8966(3) 0.32886(12) 0.0772(12) Uani 1 1 d . . . . .
H41A H 0.612228 0.902878 0.330022 0.116 Uiso 1 1 calc R U . . .
H41B H 0.535521 0.950997 0.317704 0.116 Uiso 1 1 calc R U . . .
H41C H 0.542085 0.847400 0.309898 0.116 Uiso 1 1 calc R U . . .
C56 C 0.1667(2) -0.1422(3) 0.61693(12) 0.0787(13) Uani 1 1 d . . . . .
H56A H 0.116832 -0.137517 0.601594 0.118 Uiso 1 1 calc R U . . .
H56B H 0.169026 -0.187382 0.639320 0.118 Uiso 1 1 calc R U . . .
H56C H 0.198874 -0.158597 0.596648 0.118 Uiso 1 1 calc R U . . .
C37 C 0.6077(2) 0.5353(3) 0.44779(13) 0.0816(13) Uani 1 1 d . . . . .
H37A H 0.656022 0.550516 0.463104 0.122 Uiso 1 1 calc R U . . .
H37B H 0.600477 0.471496 0.449293 0.122 Uiso 1 1 calc R U . . .
H37C H 0.570884 0.565725 0.461106 0.122 Uiso 1 1 calc R U . . .
C58 C 0.1418(2) -0.0360(3) 0.67088(13) 0.0907(15) Uani 1 1 d . . . . .
H58A H 0.091006 -0.034401 0.656894 0.136 Uiso 1 1 calc R U . . .
H58B H 0.155094 0.020957 0.684536 0.136 Uiso 1 1 calc R U . . .
H58C H 0.148280 -0.082464 0.692738 0.136 Uiso 1 1 calc R U . . .
C35 C 0.65022(18) 0.7922(3) 0.41066(15) 0.0831(14) Uani 1 1 d . . . . .
H35 H 0.681469 0.840251 0.419887 0.100 Uiso 1 1 calc R U . . .
C16 C -0.00661(19) 0.5930(3) 0.25037(17) 0.0971(17) Uani 1 1 d . . . . .
H16A H 0.027461 0.562696 0.234834 0.146 Uiso 1 1 calc R U . . .
H16B H -0.055501 0.589940 0.233562 0.146 Uiso 1 1 calc R U . . .
H16C H -0.006260 0.564490 0.278289 0.146 Uiso 1 1 calc R U . . .
C34 C 0.6662(2) 0.7070(3) 0.41532(17) 0.0984(17) Uani 1 1 d . . . . .
H34 H 0.711435 0.683333 0.428453 0.118 Uiso 1 1 calc R U . . .
C63 C 0.0674(3) 0.6080(3) 0.51649(19) 0.136(3) Uani 1 1 d . . . . .
H63A H 0.069625 0.601596 0.485811 0.204 Uiso 1 1 calc R U . . .
H63B H 0.057883 0.669636 0.522798 0.204 Uiso 1 1 calc R U . . .
H63C H 0.028379 0.570894 0.523908 0.204 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1 C24 1.783(3) . ?
P1 C2 1.829(3) . ?
P4 C74 1.779(3) . ?
P4 C43 1.828(3) . ?
P2 C33 1.809(3) . ?
P2 C12 1.824(3) . ?
P3 C65 1.810(3) . ?
P3 C53 1.813(3) . ?
O1 C1 1.372(3) . ?
O1 C13 1.399(3) . ?
O2 C42 1.375(3) . ?
O2 C54 1.389(3) . ?
N5 C65 1.372(3) . ?
N5 C66 1.373(3) . ?
N5 C68 1.474(3) . ?
N7 C74 1.373(3) . ?
N7 C75 1.374(3) . ?
N7 C77 1.472(3) . ?
N6 C65 1.358(3) . ?
N6 C67 1.378(3) . ?
N6 C71 1.489(3) . ?
N2 C24 1.366(3) . ?
N2 C25 1.383(3) . ?
N2 C30 1.479(3) . ?
N1 C24 1.377(3) . ?
N1 C26 1.384(4) . ?
N1 C27 1.466(4) . ?
N8 C74 1.370(3) . ?
N8 C76 1.382(3) . ?
N8 C80 1.468(3) . ?
C2 C3 1.396(3) . ?
C2 C1 1.406(3) . ?
C13 C8 1.374(3) . ?
C13 C12 1.411(3) . ?
C12 C11 1.399(3) . ?
C1 C6 1.386(3) . ?
C11 C10 1.390(3) . ?
C11 H11 0.9500 . ?
C8 C9 1.411(3) . ?
C8 C7 1.523(3) . ?
C6 C5 1.403(3) . ?
C6 C7 1.527(3) . ?
C53 C52 1.396(4) . ?
C53 C54 1.417(4) . ?
C7 C19 1.540(4) . ?
C7 C18 1.551(4) . ?
N4 C33 1.362(4) . ?
N4 C35 1.371(4) . ?
N4 C39 1.463(4) . ?
C54 C49 1.381(3) . ?
C42 C47 1.389(3) . ?
C42 C43 1.407(4) . ?
C3 C4 1.404(4) . ?
C3 H3 0.9500 . ?
C43 C44 1.399(4) . ?
C10 C9 1.384(3) . ?
C10 C20 1.543(3) . ?
C47 C46 1.412(4) . ?
C47 C48 1.515(4) . ?
C9 H9 0.9500 . ?
C49 C50 1.403(4) . ?
C49 C48 1.533(4) . ?
C44 C45 1.393(4) . ?
C44 H44 0.9500 . ?
C45 C46 1.381(4) . ?
C45 C55 1.534(4) . ?
C46 H46 0.9500 . ?
C5 C4 1.390(4) . ?
C5 H5 0.9500 . ?
C75 C76 1.328(4) . ?
C75 H75 0.9500 . ?
C4 C14 1.531(3) . ?
C52 C51 1.400(3) . ?
C52 H52 0.9500 . ?
N3 C33 1.354(4) . ?
N3 C34 1.371(4) . ?
N3 C36 1.459(4) . ?
C76 H76 0.9500 . ?
C68 C70 1.515(4) . ?
C68 C69 1.529(4) . ?
C68 H68 1.0000 . ?
C51 C50 1.384(4) . ?
C51 C61 1.536(4) . ?
C67 C66 1.334(4) . ?
C67 H67 0.9500 . ?
C66 H66 0.9500 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C26 C25 1.331(4) . ?
C26 H26 0.9500 . ?
C25 H25 0.9500 . ?
C30 C31 1.497(4) . ?
C30 C32 1.509(4) . ?
C30 H30 1.0000 . ?
C20 C21 1.518(4) . ?
C20 C22 1.529(4) . ?
C20 C23 1.533(4) . ?
C27 C29 1.516(4) . ?
C27 C28 1.517(4) . ?
C27 H27 1.0000 . ?
C71 C72 1.507(4) . ?
C71 C73 1.522(4) . ?
C71 H71 1.0000 . ?
C50 H50 0.9500 . ?
C48 C60 1.532(4) . ?
C48 C59 1.547(4) . ?
C55 C56 1.508(5) . ?
C55 C57 1.528(4) . ?
C55 C58 1.530(4) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C14 C16 1.501(5) . ?
C14 C17 1.528(4) . ?
C14 C15 1.537(5) . ?
C77 C78 1.517(4) . ?
C77 C79 1.519(4) . ?
C77 H77 1.0000 . ?
C70 H70A 0.9800 . ?
C70 H70B 0.9800 . ?
C70 H70C 0.9800 . ?
C61 C63 1.521(5) . ?
C61 C64 1.531(4) . ?
C61 C62 1.546(5) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C80 C81 1.518(4) . ?
C80 C82 1.526(4) . ?
C80 H80 1.0000 . ?
C64 H64A 0.9800 . ?
C64 H64B 0.9800 . ?
C64 H64C 0.9800 . ?
C81 H81A 0.9800 . ?
C81 H81B 0.9800 . ?
C81 H81C 0.9800 . ?
C79 H79A 0.9800 . ?
C79 H79B 0.9800 . ?
C79 H79C 0.9800 . ?
C59 H59A 0.9800 . ?
C59 H59B 0.9800 . ?
C59 H59C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C39 C41 1.520(5) . ?
C39 C40 1.521(4) . ?
C39 H39 1.0000 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C78 H78A 0.9800 . ?
C78 H78B 0.9800 . ?
C78 H78C 0.9800 . ?
C82 H82A 0.9800 . ?
C82 H82B 0.9800 . ?
C82 H82C 0.9800 . ?
C69 H69A 0.9800 . ?
C69 H69B 0.9800 . ?
C69 H69C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C36 C38 1.513(5) . ?
C36 C37 1.540(5) . ?
C36 H36 1.0000 . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C72 H72A 0.9800 . ?
C72 H72B 0.9800 . ?
C72 H72C 0.9800 . ?
C73 H73A 0.9800 . ?
C73 H73B 0.9800 . ?
C73 H73C 0.9800 . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C62 H62A 0.9800 . ?
C62 H62B 0.9800 . ?
C62 H62C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 0.9800 . ?
C35 C34 1.331(6) . ?
C35 H35 0.9500 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C34 H34 0.9500 . ?
C63 H63A 0.9800 . ?
C63 H63B 0.9800 . ?
C63 H63C 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
C24 P1 C2 106.65(12) . . ?
C74 P4 C43 107.19(12) . . ?
C33 P2 C12 96.48(12) . . ?
C65 P3 C53 99.95(12) . . ?
C1 O1 C13 119.40(18) . . ?
C42 O2 C54 119.21(19) . . ?
C65 N5 C66 110.0(2) . . ?
C65 N5 C68 125.2(2) . . ?
C66 N5 C68 124.2(2) . . ?
C74 N7 C75 110.3(2) . . ?
C74 N7 C77 124.2(2) . . ?
C75 N7 C77 125.4(2) . . ?
C65 N6 C67 110.5(2) . . ?
C65 N6 C71 124.3(2) . . ?
C67 N6 C71 124.8(2) . . ?
C24 N2 C25 109.5(2) . . ?
C24 N2 C30 125.7(2) . . ?
C25 N2 C30 124.7(2) . . ?
C24 N1 C26 109.2(2) . . ?
C24 N1 C27 124.1(2) . . ?
C26 N1 C27 126.3(2) . . ?
C74 N8 C76 109.5(2) . . ?
C74 N8 C80 126.4(2) . . ?
C76 N8 C80 123.7(2) . . ?
C3 C2 C1 117.0(2) . . ?
C3 C2 P1 115.94(19) . . ?
C1 C2 P1 126.13(18) . . ?
C8 C13 O1 122.4(2) . . ?
C8 C13 C12 124.2(2) . . ?
O1 C13 C12 113.4(2) . . ?
C11 C12 C13 115.4(2) . . ?
C11 C12 P2 127.00(18) . . ?
C13 C12 P2 117.48(18) . . ?
O1 C1 C6 122.6(2) . . ?
O1 C1 C2 114.6(2) . . ?
C6 C1 C2 122.7(2) . . ?
C10 C11 C12 123.1(2) . . ?
C10 C11 H11 118.4 . . ?
C12 C11 H11 118.4 . . ?
C13 C8 C9 117.1(2) . . ?
C13 C8 C7 121.9(2) . . ?
C9 C8 C7 121.0(2) . . ?
C1 C6 C5 117.3(2) . . ?
C1 C6 C7 121.8(2) . . ?
C5 C6 C7 120.8(2) . . ?
C52 C53 C54 115.6(2) . . ?
C52 C53 P3 127.5(2) . . ?
C54 C53 P3 116.7(2) . . ?
N6 C65 N5 104.5(2) . . ?
N6 C65 P3 130.2(2) . . ?
N5 C65 P3 124.49(19) . . ?
C8 C7 C6 110.6(2) . . ?
C8 C7 C19 109.5(2) . . ?
C6 C7 C19 109.5(2) . . ?
C8 C7 C18 108.8(2) . . ?
C6 C7 C18 109.8(2) . . ?
C19 C7 C18 108.6(2) . . ?
C33 N4 C35 110.2(3) . . ?
C33 N4 C39 124.7(2) . . ?
C35 N4 C39 124.6(3) . . ?
C49 C54 O2 122.7(2) . . ?
C49 C54 C53 123.3(3) . . ?
O2 C54 C53 113.9(2) . . ?
O2 C42 C47 122.2(2) . . ?
O2 C42 C43 115.5(2) . . ?
C47 C42 C43 122.3(2) . . ?
C2 C3 C4 122.9(2) . . ?
C2 C3 H3 118.5 . . ?
C4 C3 H3 118.5 . . ?
C44 C43 C42 116.7(2) . . ?
C44 C43 P4 115.1(2) . . ?
C42 C43 P4 127.2(2) . . ?
C9 C10 C11 118.3(2) . . ?
C9 C10 C20 122.5(2) . . ?
C11 C10 C20 119.2(2) . . ?
N8 C74 N7 104.6(2) . . ?
N8 C74 P4 134.0(2) . . ?
N7 C74 P4 120.59(18) . . ?
C42 C47 C46 117.6(2) . . ?
C42 C47 C48 122.1(2) . . ?
C46 C47 C48 120.2(2) . . ?
C10 C9 C8 121.9(2) . . ?
C10 C9 H9 119.1 . . ?
C8 C9 H9 119.1 . . ?
C54 C49 C50 117.5(2) . . ?
C54 C49 C48 121.2(3) . . ?
C50 C49 C48 121.2(2) . . ?
N2 C24 N1 105.4(2) . . ?
N2 C24 P1 134.12(19) . . ?
N1 C24 P1 119.8(2) . . ?
C45 C44 C43 123.6(3) . . ?
C45 C44 H44 118.2 . . ?
C43 C44 H44 118.2 . . ?
C46 C45 C44 117.1(2) . . ?
C46 C45 C55 122.7(2) . . ?
C44 C45 C55 120.3(3) . . ?
C45 C46 C47 122.7(2) . . ?
C45 C46 H46 118.7 . . ?
C47 C46 H46 118.7 . . ?
C4 C5 C6 123.1(2) . . ?
C4 C5 H5 118.5 . . ?
C6 C5 H5 118.5 . . ?
C76 C75 N7 107.4(2) . . ?
C76 C75 H75 126.3 . . ?
N7 C75 H75 126.3 . . ?
C5 C4 C3 116.8(2) . . ?
C5 C4 C14 124.1(2) . . ?
C3 C4 C14 119.1(2) . . ?
C53 C52 C51 123.8(3) . . ?
C53 C52 H52 118.1 . . ?
C51 C52 H52 118.1 . . ?
C33 N3 C34 109.4(3) . . ?
C33 N3 C36 126.1(2) . . ?
C34 N3 C36 124.3(3) . . ?
N3 C33 N4 105.2(2) . . ?
N3 C33 P2 126.4(2) . . ?
N4 C33 P2 128.1(2) . . ?
C75 C76 N8 108.2(2) . . ?
C75 C76 H76 125.9 . . ?
N8 C76 H76 125.9 . . ?
N5 C68 C70 110.6(2) . . ?
N5 C68 C69 108.9(2) . . ?
C70 C68 C69 112.4(3) . . ?
N5 C68 H68 108.3 . . ?
C70 C68 H68 108.3 . . ?
C69 C68 H68 108.3 . . ?
C50 C51 C52 117.2(3) . . ?
C50 C51 C61 121.5(2) . . ?
C52 C51 C61 121.3(3) . . ?
C66 C67 N6 107.2(2) . . ?
C66 C67 H67 126.4 . . ?
N6 C67 H67 126.4 . . ?
C67 C66 N5 107.7(2) . . ?
C67 C66 H66 126.2 . . ?
N5 C66 H66 126.2 . . ?
C7 C18 H18A 109.5 . . ?
C7 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C7 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C25 C26 N1 107.9(2) . . ?
C25 C26 H26 126.1 . . ?
N1 C26 H26 126.1 . . ?
C26 C25 N2 108.0(3) . . ?
C26 C25 H25 126.0 . . ?
N2 C25 H25 126.0 . . ?
N2 C30 C31 110.4(2) . . ?
N2 C30 C32 110.4(2) . . ?
C31 C30 C32 112.2(3) . . ?
N2 C30 H30 107.9 . . ?
C31 C30 H30 107.9 . . ?
C32 C30 H30 107.9 . . ?
C21 C20 C22 108.5(3) . . ?
C21 C20 C23 107.9(3) . . ?
C22 C20 C23 109.5(2) . . ?
C21 C20 C10 112.6(2) . . ?
C22 C20 C10 109.4(2) . . ?
C23 C20 C10 108.9(2) . . ?
N1 C27 C29 111.0(3) . . ?
N1 C27 C28 111.1(2) . . ?
C29 C27 C28 111.8(2) . . ?
N1 C27 H27 107.6 . . ?
C29 C27 H27 107.6 . . ?
C28 C27 H27 107.6 . . ?
N6 C71 C72 109.9(2) . . ?
N6 C71 C73 109.7(2) . . ?
C72 C71 C73 112.0(3) . . ?
N6 C71 H71 108.4 . . ?
C72 C71 H71 108.4 . . ?
C73 C71 H71 108.4 . . ?
C51 C50 C49 122.7(2) . . ?
C51 C50 H50 118.7 . . ?
C49 C50 H50 118.7 . . ?
C47 C48 C60 109.2(2) . . ?
C47 C48 C49 110.5(2) . . ?
C60 C48 C49 109.2(2) . . ?
C47 C48 C59 110.1(2) . . ?
C60 C48 C59 109.0(3) . . ?
C49 C48 C59 108.8(2) . . ?
C56 C55 C57 108.1(3) . . ?
C56 C55 C58 107.2(3) . . ?
C57 C55 C58 108.7(3) . . ?
C56 C55 C45 111.9(2) . . ?
C57 C55 C45 108.7(2) . . ?
C58 C55 C45 112.0(3) . . ?
C7 C19 H19A 109.5 . . ?
C7 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C7 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C16 C14 C17 109.7(3) . . ?
C16 C14 C4 109.7(3) . . ?
C17 C14 C4 112.3(2) . . ?
C16 C14 C15 110.1(3) . . ?
C17 C14 C15 106.3(3) . . ?
C4 C14 C15 108.7(2) . . ?
N7 C77 C78 111.0(2) . . ?
N7 C77 C79 110.7(2) . . ?
C78 C77 C79 111.9(2) . . ?
N7 C77 H77 107.7 . . ?
C78 C77 H77 107.7 . . ?
C79 C77 H77 107.7 . . ?
C68 C70 H70A 109.5 . . ?
C68 C70 H70B 109.5 . . ?
H70A C70 H70B 109.5 . . ?
C68 C70 H70C 109.5 . . ?
H70A C70 H70C 109.5 . . ?
H70B C70 H70C 109.5 . . ?
C63 C61 C64 110.5(3) . . ?
C63 C61 C51 109.0(3) . . ?
C64 C61 C51 111.6(3) . . ?
C63 C61 C62 110.3(4) . . ?
C64 C61 C62 104.6(3) . . ?
C51 C61 C62 110.9(3) . . ?
C20 C23 H23A 109.5 . . ?
C20 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C20 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N8 C80 C81 110.0(2) . . ?
N8 C80 C82 110.1(3) . . ?
C81 C80 C82 113.2(2) . . ?
N8 C80 H80 107.8 . . ?
C81 C80 H80 107.8 . . ?
C82 C80 H80 107.8 . . ?
C61 C64 H64A 109.5 . . ?
C61 C64 H64B 109.5 . . ?
H64A C64 H64B 109.5 . . ?
C61 C64 H64C 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
C80 C81 H81A 109.5 . . ?
C80 C81 H81B 109.5 . . ?
H81A C81 H81B 109.5 . . ?
C80 C81 H81C 109.5 . . ?
H81A C81 H81C 109.5 . . ?
H81B C81 H81C 109.5 . . ?
C77 C79 H79A 109.5 . . ?
C77 C79 H79B 109.5 . . ?
H79A C79 H79B 109.5 . . ?
C77 C79 H79C 109.5 . . ?
H79A C79 H79C 109.5 . . ?
H79B C79 H79C 109.5 . . ?
C48 C59 H59A 109.5 . . ?
C48 C59 H59B 109.5 . . ?
H59A C59 H59B 109.5 . . ?
C48 C59 H59C 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C14 C17 H17A 109.5 . . ?
C14 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C14 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N4 C39 C41 108.9(3) . . ?
N4 C39 C40 110.6(3) . . ?
C41 C39 C40 112.5(3) . . ?
N4 C39 H39 108.2 . . ?
C41 C39 H39 108.2 . . ?
C40 C39 H39 108.2 . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C77 C78 H78A 109.5 . . ?
C77 C78 H78B 109.5 . . ?
H78A C78 H78B 109.5 . . ?
C77 C78 H78C 109.5 . . ?
H78A C78 H78C 109.5 . . ?
H78B C78 H78C 109.5 . . ?
C80 C82 H82A 109.5 . . ?
C80 C82 H82B 109.5 . . ?
H82A C82 H82B 109.5 . . ?
C80 C82 H82C 109.5 . . ?
H82A C82 H82C 109.5 . . ?
H82B C82 H82C 109.5 . . ?
C68 C69 H69A 109.5 . . ?
C68 C69 H69B 109.5 . . ?
H69A C69 H69B 109.5 . . ?
C68 C69 H69C 109.5 . . ?
H69A C69 H69C 109.5 . . ?
H69B C69 H69C 109.5 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
N3 C36 C38 110.3(3) . . ?
N3 C36 C37 109.5(3) . . ?
C38 C36 C37 112.9(3) . . ?
N3 C36 H36 108.0 . . ?
C38 C36 H36 108.0 . . ?
C37 C36 H36 108.0 . . ?
C48 C60 H60A 109.5 . . ?
C48 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
C48 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C71 C72 H72A 109.5 . . ?
C71 C72 H72B 109.5 . . ?
H72A C72 H72B 109.5 . . ?
C71 C72 H72C 109.5 . . ?
H72A C72 H72C 109.5 . . ?
H72B C72 H72C 109.5 . . ?
C71 C73 H73A 109.5 . . ?
C71 C73 H73B 109.5 . . ?
H73A C73 H73B 109.5 . . ?
C71 C73 H73C 109.5 . . ?
H73A C73 H73C 109.5 . . ?
H73B C73 H73C 109.5 . . ?
C55 C57 H57A 109.5 . . ?
C55 C57 H57B 109.5 . . ?
H57A C57 H57B 109.5 . . ?
C55 C57 H57C 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 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 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
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 . . ?
C61 C62 H62A 109.5 . . ?
C61 C62 H62B 109.5 . . ?
H62A C62 H62B 109.5 . . ?
C61 C62 H62C 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
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 . . ?
C55 C56 H56A 109.5 . . ?
C55 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C55 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 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 . . ?
C55 C58 H58A 109.5 . . ?
C55 C58 H58B 109.5 . . ?
H58A C58 H58B 109.5 . . ?
C55 C58 H58C 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C34 C35 N4 106.7(3) . . ?
C34 C35 H35 126.7 . . ?
N4 C35 H35 126.7 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C35 C34 N3 108.5(3) . . ?
C35 C34 H34 125.8 . . ?
N3 C34 H34 125.8 . . ?
C61 C63 H63A 109.5 . . ?
C61 C63 H63B 109.5 . . ?
H63A C63 H63B 109.5 . . ?
C61 C63 H63C 109.5 . . ?
H63A C63 H63C 109.5 . . ?
H63B C63 H63C 109.5 . . ?

_refine_diff_density_max         0.369
_refine_diff_density_min         -0.262
_refine_diff_density_rms         0.056


