# Supplementary Information (SI) for Dalton Transactions.
# 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. 
# 
#######################################################################

data_shelx
_database_code_depnum_ccdc_archive 'CCDC 2386108'
loop_
_audit_author_name
_audit_author_address
'Lukasz Ponikiewski'
;Gdansk University of Technology
Poland
;
_audit_update_record             
;
2024-09-23 deposited with the CCDC.	2024-11-13 downloaded from the CCDC.
;

_audit_creation_date             2024-03-14T11:24:23-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_moiety         'C66 H76 N4 P4, C5 H12'
_chemical_formula_sum            'C71 H88 N4 P4'
_chemical_formula_weight         1121.33

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_Int_Tables_number      14
loop_
_symmetry_equiv_pos_as_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                   14.2680(10)
_cell_length_b                   23.3514(16)
_cell_length_c                   18.7576(13)
_cell_angle_alpha                90
_cell_angle_beta                 96.391(5)
_cell_angle_gamma                90
_cell_volume                     6210.8(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    20990
_cell_measurement_theta_min      2.09
_cell_measurement_theta_max      29.57
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_exptl_crystal_density_diffrn    1.199
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2408

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.167
_exptl_absorpt_correction_type   none
_shelx_estimated_absorpt_T_min   0.975
_shelx_estimated_absorpt_T_max   0.977

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_type            'STOE Imaging Plate'
_diffrn_detector_area_resol_mean 6.67
_diffrn_source                   'GeniX Mo, 0.05 x 0.05 mm2 microfocus'
_diffrn_source_target            ?
_diffrn_source_voltage           50
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_radiation_monochromator  'parabolic x-ray mirror'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_collimation    '0.6 mm diameter'
_diffrn_measurement_method       'rotation method, ω scans'
_diffrn_measurement_details      
; 203 frames, detector distance = 100 mm
;
_diffrn_reflns_av_R_equivalents  0.0639
_diffrn_reflns_av_unetI/netI     0.0911
_diffrn_reflns_number            35140
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.058
_diffrn_reflns_theta_max         29.334
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.977
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.977
_reflns_Friedel_coverage         0
_reflns_number_total             16647
_reflns_number_gt                10035
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       
;
X-Area WinXpose 2.0.22.0 (STOE, 2016)
;
_computing_cell_refinement       
;
X-Area Recipe 1.34.0.0 (STOE, 2019)
;
_computing_data_reduction        
;
X-Area Integrate 1.77.0.0 (STOE, 2019)
X-Area LANA 1.77.1.0 (STOE, 2019)
;
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0126P)²+17.8271P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         16647
_refine_ls_number_parameters     722
_refine_ls_number_restraints     0
_refine_ls_number_constraints    0
_refine_ls_R_factor_all          0.1605
_refine_ls_R_factor_gt           0.0839
_refine_ls_wR_factor_ref         0.1775
_refine_ls_wR_factor_gt          0.1429
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_restrained_S_all      1.111
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.428
_refine_diff_density_min         -0.445
_refine_diff_density_rms         0.086

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.5677(2) 0.33524(15) 0.57331(17) 0.0212(7) Uani 1 1 d . . . . .
C2 C 0.4607(2) 0.34221(15) 0.55544(17) 0.0208(7) Uani 1 1 d . . . . .
C3 C 0.4033(2) 0.29419(15) 0.56075(18) 0.0230(7) Uani 1 1 d . . . . .
H3 H 0.430831 0.259338 0.578866 0.028 Uiso 1 1 calc R U . . .
C4 C 0.3070(2) 0.29649(15) 0.54008(18) 0.0227(7) Uani 1 1 d . . . . .
H4 H 0.269642 0.263311 0.544861 0.027 Uiso 1 1 calc R U . . .
C5 C 0.2638(2) 0.34658(15) 0.51241(17) 0.0217(7) Uani 1 1 d . . . . .
C6 C 0.3213(2) 0.39454(15) 0.50721(18) 0.0222(7) Uani 1 1 d . . . . .
H6 H 0.293842 0.429367 0.488982 0.027 Uiso 1 1 calc R U . . .
C7 C 0.4176(2) 0.39238(15) 0.52809(17) 0.0219(7) Uani 1 1 d . . . . .
H7 H 0.454826 0.425658 0.523671 0.026 Uiso 1 1 calc R U . . .
C8 C 0.1610(2) 0.34964(15) 0.48977(18) 0.0225(7) Uani 1 1 d . . . . .
C9 C 0.0966(3) 0.32212(16) 0.5291(2) 0.0288(8) Uani 1 1 d . . . . .
H9 H 0.118878 0.300338 0.570268 0.035 Uiso 1 1 calc R U . . .
C10 C 0.0002(3) 0.32629(17) 0.5085(2) 0.0322(9) Uani 1 1 d . . . . .
H10 H -0.042822 0.307603 0.535979 0.039 Uiso 1 1 calc R U . . .
C11 C -0.0335(3) 0.35733(17) 0.4486(2) 0.0330(9) Uani 1 1 d . . . . .
H11 H -0.09938 0.359967 0.434605 0.04 Uiso 1 1 calc R U . . .
C12 C 0.0295(3) 0.38465(18) 0.4089(2) 0.0316(8) Uani 1 1 d . . . . .
H12 H 0.006601 0.405801 0.367327 0.038 Uiso 1 1 calc R U . . .
C13 C 0.1259(2) 0.38137(16) 0.42942(19) 0.0268(8) Uani 1 1 d . . . . .
H13 H 0.168333 0.400849 0.402229 0.032 Uiso 1 1 calc R U . . .
C14 C 0.6089(2) 0.30833(14) 0.50839(18) 0.0206(7) Uani 1 1 d . . . . .
C15 C 0.5527(2) 0.29166(15) 0.44695(18) 0.0233(7) Uani 1 1 d . . . . .
H15 H 0.486792 0.298623 0.44343 0.028 Uiso 1 1 calc R U . . .
C16 C 0.5904(2) 0.26493(16) 0.39012(19) 0.0257(7) Uani 1 1 d . . . . .
H16 H 0.549686 0.254739 0.348503 0.031 Uiso 1 1 calc R U . . .
C17 C 0.6865(2) 0.25279(15) 0.39294(18) 0.0220(7) Uani 1 1 d . . . . .
C18 C 0.7435(2) 0.26994(15) 0.45459(18) 0.0233(7) Uani 1 1 d . . . . .
H18 H 0.809375 0.262792 0.458403 0.028 Uiso 1 1 calc R U . . .
C19 C 0.7053(2) 0.29729(15) 0.51047(18) 0.0236(7) Uani 1 1 d . . . . .
H19 H 0.746132 0.308859 0.551409 0.028 Uiso 1 1 calc R U . . .
C20 C 0.7264(3) 0.22211(15) 0.33332(18) 0.0248(7) Uani 1 1 d . . . . .
C21 C 0.6712(3) 0.18513(16) 0.28830(19) 0.0290(8) Uani 1 1 d . . . . .
H21 H 0.607404 0.178866 0.296129 0.035 Uiso 1 1 calc R U . . .
C22 C 0.7074(3) 0.15723(18) 0.2323(2) 0.0331(9) Uani 1 1 d . . . . .
H22 H 0.668104 0.132641 0.201651 0.04 Uiso 1 1 calc R U . . .
C23 C 0.8003(3) 0.16505(17) 0.2208(2) 0.0320(9) Uani 1 1 d . . . . .
H23 H 0.82554 0.145819 0.182602 0.038 Uiso 1 1 calc R U . . .
C24 C 0.8561(3) 0.20127(18) 0.2657(2) 0.0330(9) Uani 1 1 d . . . . .
H24 H 0.920259 0.206857 0.258247 0.04 Uiso 1 1 calc R U . . .
C25 C 0.8198(3) 0.22946(17) 0.3213(2) 0.0301(8) Uani 1 1 d . . . . .
H25 H 0.859268 0.254171 0.351617 0.036 Uiso 1 1 calc R U . . .
C26 C 0.6265(2) 0.39089(14) 0.60435(18) 0.0212(7) Uani 1 1 d . . . . .
C27 C 0.6823(2) 0.41977(14) 0.54957(17) 0.0192(7) Uani 1 1 d . . . . .
C28 C 0.6408(2) 0.43210(15) 0.48048(18) 0.0225(7) Uani 1 1 d . . . . .
H28 H 0.5762 0.422997 0.467824 0.027 Uiso 1 1 calc R U . . .
C29 C 0.6911(2) 0.45725(14) 0.42978(18) 0.0226(7) Uani 1 1 d . . . . .
H29 H 0.660271 0.465106 0.383289 0.027 Uiso 1 1 calc R U . . .
C30 C 0.7861(2) 0.47129(14) 0.44557(17) 0.0200(7) Uani 1 1 d . . . . .
C31 C 0.8275(2) 0.46201(14) 0.51562(17) 0.0209(7) Uani 1 1 d . . . . .
H31 H 0.890934 0.473332 0.528992 0.025 Uiso 1 1 calc R U . . .
C32 C 0.7765(2) 0.43634(15) 0.56599(18) 0.0225(7) Uani 1 1 d . . . . .
H32 H 0.806534 0.429842 0.61306 0.027 Uiso 1 1 calc R U . . .
C33 C 0.8408(2) 0.49464(15) 0.38914(18) 0.0225(7) Uani 1 1 d . . . . .
C34 C 0.8199(3) 0.47619(17) 0.31784(19) 0.0284(8) Uani 1 1 d . . . . .
H34 H 0.770377 0.449482 0.305942 0.034 Uiso 1 1 calc R U . . .
C35 C 0.8713(3) 0.49687(18) 0.2648(2) 0.0322(9) Uani 1 1 d . . . . .
H35 H 0.856615 0.484334 0.216661 0.039 Uiso 1 1 calc R U . . .
C36 C 0.9433(3) 0.53531(18) 0.2812(2) 0.0331(9) Uani 1 1 d . . . . .
H36 H 0.977798 0.549499 0.24449 0.04 Uiso 1 1 calc R U . . .
C37 C 0.9658(3) 0.55350(17) 0.3518(2) 0.0298(8) Uani 1 1 d . . . . .
H37 H 1.016232 0.579651 0.363303 0.036 Uiso 1 1 calc R U . . .
C38 C 0.9144(2) 0.53332(15) 0.40526(18) 0.0238(7) Uani 1 1 d . . . . .
H38 H 0.929506 0.546051 0.453267 0.029 Uiso 1 1 calc R U . . .
C39 C 0.5693(2) 0.43555(15) 0.64103(17) 0.0207(7) Uani 1 1 d . . . . .
C40 C 0.5845(2) 0.49404(15) 0.63293(18) 0.0236(7) Uani 1 1 d . . . . .
H40 H 0.627123 0.506508 0.600654 0.028 Uiso 1 1 calc R U . . .
C41 C 0.5386(2) 0.53479(15) 0.67112(19) 0.0243(7) Uani 1 1 d . . . . .
H41 H 0.550441 0.574311 0.664114 0.029 Uiso 1 1 calc R U . . .
C42 C 0.4759(2) 0.51860(15) 0.71924(18) 0.0232(7) Uani 1 1 d . . . . .
C43 C 0.4577(2) 0.46015(15) 0.72539(18) 0.0239(7) Uani 1 1 d . . . . .
H43 H 0.413113 0.447789 0.756152 0.029 Uiso 1 1 calc R U . . .
C44 C 0.5036(2) 0.41970(15) 0.68734(17) 0.0222(7) Uani 1 1 d . . . . .
H44 H 0.489818 0.380259 0.692958 0.027 Uiso 1 1 calc R U . . .
C45 C 0.4315(2) 0.56166(15) 0.76299(19) 0.0249(7) Uani 1 1 d . . . . .
C46 C 0.4092(3) 0.61685(16) 0.7381(2) 0.0294(8) Uani 1 1 d . . . . .
H46 H 0.4226 0.627258 0.691341 0.035 Uiso 1 1 calc R U . . .
C47 C 0.3682(3) 0.65683(18) 0.7792(2) 0.0360(9) Uani 1 1 d . . . . .
H47 H 0.354199 0.694183 0.760922 0.043 Uiso 1 1 calc R U . . .
C48 C 0.3477(3) 0.64195(19) 0.8473(2) 0.0422(10) Uani 1 1 d . . . . .
H48 H 0.319512 0.669049 0.876039 0.051 Uiso 1 1 calc R U . . .
C49 C 0.3685(4) 0.5877(2) 0.8730(2) 0.0457(11) Uani 1 1 d . . . . .
H49 H 0.353934 0.577346 0.919452 0.055 Uiso 1 1 calc R U . . .
C50 C 0.4103(3) 0.54804(18) 0.8318(2) 0.0374(9) Uani 1 1 d . . . . .
H50 H 0.424867 0.51095 0.850703 0.045 Uiso 1 1 calc R U . . .
C51 C 0.5089(3) 0.12383(17) 0.5806(2) 0.0342(9) Uani 1 1 d . . . . .
H51A H 0.533039 0.133828 0.53469 0.041 Uiso 1 1 calc R U . . .
H51B H 0.439175 0.124257 0.572289 0.041 Uiso 1 1 calc R U . . .
C52 C 0.5408(4) 0.06382(18) 0.6013(2) 0.0458(11) Uani 1 1 d . . . . .
H52A H 0.609827 0.062687 0.609324 0.069 Uiso 1 1 calc R U . . .
H52B H 0.518596 0.037268 0.562592 0.069 Uiso 1 1 calc R U . . .
H52C H 0.514654 0.052579 0.645365 0.069 Uiso 1 1 calc R U . . .
C53 C 0.5044(3) 0.16155(17) 0.7039(2) 0.0329(9) Uani 1 1 d . . . . .
H53A H 0.524939 0.194925 0.734263 0.039 Uiso 1 1 calc R U . . .
H53B H 0.533005 0.126882 0.727687 0.039 Uiso 1 1 calc R U . . .
C54 C 0.3981(3) 0.1566(2) 0.6995(3) 0.0466(11) Uani 1 1 d . . . . .
H54A H 0.36899 0.190039 0.674371 0.07 Uiso 1 1 calc R U . . .
H54B H 0.378884 0.154795 0.747996 0.07 Uiso 1 1 calc R U . . .
H54C H 0.377488 0.121719 0.673163 0.07 Uiso 1 1 calc R U . . .
C55 C 0.8207(3) 0.1710(2) 0.6473(3) 0.0444(11) Uani 1 1 d . . . . .
H55A H 0.806527 0.161343 0.595859 0.053 Uiso 1 1 calc R U . . .
H55B H 0.852296 0.137428 0.671619 0.053 Uiso 1 1 calc R U . . .
C56 C 0.8885(3) 0.2212(2) 0.6543(3) 0.0519(13) Uani 1 1 d . . . . .
H56A H 0.85707 0.255208 0.632348 0.078 Uiso 1 1 calc R U . . .
H56B H 0.943852 0.212117 0.629813 0.078 Uiso 1 1 calc R U . . .
H56C H 0.908301 0.228624 0.705125 0.078 Uiso 1 1 calc R U . . .
C57 C 0.7390(3) 0.1945(2) 0.7541(2) 0.0400(10) Uani 1 1 d . . . . .
H57A H 0.675924 0.19026 0.770823 0.048 Uiso 1 1 calc R U . . .
H57B H 0.757557 0.235189 0.760303 0.048 Uiso 1 1 calc R U . . .
C58 C 0.8082(3) 0.1585(2) 0.8016(3) 0.0472(11) Uani 1 1 d . . . . .
H58A H 0.792948 0.117908 0.794144 0.071 Uiso 1 1 calc R U . . .
H58B H 0.804371 0.168536 0.85196 0.071 Uiso 1 1 calc R U . . .
H58C H 0.872256 0.165827 0.789634 0.071 Uiso 1 1 calc R U . . .
C59 C 0.7046(3) 0.29780(19) 0.8909(2) 0.0398(10) Uani 1 1 d . . . . .
H59A H 0.710331 0.323938 0.93271 0.048 Uiso 1 1 calc R U . . .
H59B H 0.743236 0.263461 0.90449 0.048 Uiso 1 1 calc R U . . .
C60 C 0.6030(3) 0.2797(2) 0.8755(2) 0.0483(12) Uani 1 1 d . . . . .
H60A H 0.563052 0.313658 0.866913 0.072 Uiso 1 1 calc R U . . .
H60B H 0.584153 0.25844 0.91665 0.072 Uiso 1 1 calc R U . . .
H60C H 0.59571 0.255101 0.832863 0.072 Uiso 1 1 calc R U . . .
C61 C 0.8470(3) 0.32216(18) 0.8335(2) 0.0347(9) Uani 1 1 d . . . . .
H61A H 0.867201 0.341263 0.790656 0.042 Uiso 1 1 calc R U . . .
H61B H 0.863968 0.281162 0.830975 0.042 Uiso 1 1 calc R U . . .
C62 C 0.9015(3) 0.3481(2) 0.9001(2) 0.0459(11) Uani 1 1 d . . . . .
H62A H 0.883539 0.388364 0.904324 0.069 Uiso 1 1 calc R U . . .
H62B H 0.969303 0.345552 0.896248 0.069 Uiso 1 1 calc R U . . .
H62C H 0.886763 0.327082 0.942711 0.069 Uiso 1 1 calc R U . . .
C63 C 0.6850(3) 0.48125(18) 0.8434(2) 0.0347(9) Uani 1 1 d . . . . .
H63A H 0.615973 0.474872 0.838449 0.042 Uiso 1 1 calc R U . . .
H63B H 0.695951 0.521553 0.830207 0.042 Uiso 1 1 calc R U . . .
C64 C 0.7236(3) 0.4723(2) 0.9212(2) 0.0462(11) Uani 1 1 d . . . . .
H64A H 0.713424 0.432498 0.934804 0.069 Uiso 1 1 calc R U . . .
H64B H 0.690955 0.497944 0.951672 0.069 Uiso 1 1 calc R U . . .
H64C H 0.79124 0.480834 0.927325 0.069 Uiso 1 1 calc R U . . .
C65 C 0.8202(3) 0.46000(17) 0.7743(2) 0.0300(8) Uani 1 1 d . . . . .
H65A H 0.843679 0.429789 0.743808 0.036 Uiso 1 1 calc R U . . .
H65B H 0.864222 0.462434 0.818874 0.036 Uiso 1 1 calc R U . . .
C66 C 0.8203(3) 0.51747(18) 0.7346(2) 0.0365(9) Uani 1 1 d . . . . .
H66A H 0.772698 0.516616 0.692732 0.055 Uiso 1 1 calc R U . . .
H66B H 0.882627 0.524098 0.718976 0.055 Uiso 1 1 calc R U . . .
H66C H 0.805519 0.548396 0.766912 0.055 Uiso 1 1 calc R U . . .
C67 C 0.4884(4) 0.4061(3) 0.9440(3) 0.0737(17) Uani 1 1 d . . . . .
H67A H 0.484474 0.402633 0.89164 0.111 Uiso 1 1 calc R U . . .
H67B H 0.539414 0.38162 0.966075 0.111 Uiso 1 1 calc R U . . .
H67C H 0.501301 0.446003 0.957887 0.111 Uiso 1 1 calc R U . . .
C68 C 0.3985(4) 0.3880(2) 0.9684(3) 0.0587(14) Uani 1 1 d . . . . .
H68A H 0.40062 0.396092 1.020359 0.07 Uiso 1 1 calc R U . . .
H68B H 0.391752 0.346125 0.961797 0.07 Uiso 1 1 calc R U . . .
C69 C 0.3125(4) 0.4170(2) 0.9298(3) 0.0528(13) Uani 1 1 d . . . . .
H69A H 0.322682 0.458951 0.932191 0.063 Uiso 1 1 calc R U . . .
H69B H 0.307412 0.405839 0.878628 0.063 Uiso 1 1 calc R U . . .
C70 C 0.2198(4) 0.4040(2) 0.9580(3) 0.0520(12) Uani 1 1 d . . . . .
H70A H 0.206119 0.362578 0.951992 0.062 Uiso 1 1 calc R U . . .
H70B H 0.225303 0.412689 1.009956 0.062 Uiso 1 1 calc R U . . .
C71 C 0.1390(4) 0.4377(2) 0.9204(3) 0.0556(13) Uani 1 1 d . . . . .
H71A H 0.152179 0.478727 0.926099 0.083 Uiso 1 1 calc R U . . .
H71B H 0.080973 0.428375 0.941342 0.083 Uiso 1 1 calc R U . . .
H71C H 0.131367 0.427928 0.869271 0.083 Uiso 1 1 calc R U . . .
N1 N 0.5397(2) 0.16812(13) 0.63383(17) 0.0286(7) Uani 1 1 d . . . . .
N2 N 0.7309(2) 0.18088(14) 0.67747(18) 0.0330(7) Uani 1 1 d . . . . .
N3 N 0.7442(2) 0.32677(14) 0.83071(16) 0.0308(7) Uani 1 1 d . . . . .
N4 N 0.7269(2) 0.44353(13) 0.79271(16) 0.0278(7) Uani 1 1 d . . . . .
P1 P 0.63991(7) 0.20283(4) 0.61773(5) 0.0254(2) Uani 1 1 d . . . . .
P2 P 0.59268(6) 0.28794(4) 0.65915(5) 0.02171(18) Uani 1 1 d . . . . .
P3 P 0.71065(6) 0.34945(4) 0.67616(5) 0.02139(18) Uani 1 1 d . . . . .
P4 P 0.67685(7) 0.37784(4) 0.78488(5) 0.0242(2) Uani 1 1 d . . . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.535(4) . ?
C1 C14 1.543(5) . ?
C1 C26 1.619(5) . ?
C1 P2 1.952(3) . ?
C2 C7 1.394(5) . ?
C2 C3 1.399(5) . ?
C3 C4 1.387(5) . ?
C3 H3 0.95 . ?
C4 C5 1.395(5) . ?
C4 H4 0.95 . ?
C5 C6 1.398(5) . ?
C5 C8 1.483(4) . ?
C6 C7 1.387(5) . ?
C6 H6 0.95 . ?
C7 H7 0.95 . ?
C8 C9 1.397(5) . ?
C8 C13 1.398(5) . ?
C9 C10 1.390(5) . ?
C9 H9 0.95 . ?
C10 C11 1.378(6) . ?
C10 H10 0.95 . ?
C11 C12 1.385(6) . ?
C11 H11 0.95 . ?
C12 C13 1.388(5) . ?
C12 H12 0.95 . ?
C13 H13 0.95 . ?
C14 C15 1.384(5) . ?
C14 C19 1.396(5) . ?
C15 C16 1.394(5) . ?
C15 H15 0.95 . ?
C16 C17 1.396(5) . ?
C16 H16 0.95 . ?
C17 C18 1.396(5) . ?
C17 C20 1.493(5) . ?
C18 C19 1.389(5) . ?
C18 H18 0.95 . ?
C19 H19 0.95 . ?
C20 C25 1.386(5) . ?
C20 C21 1.390(5) . ?
C21 C22 1.384(5) . ?
C21 H21 0.95 . ?
C22 C23 1.378(5) . ?
C22 H22 0.95 . ?
C23 C24 1.382(5) . ?
C23 H23 0.95 . ?
C24 C25 1.382(5) . ?
C24 H24 0.95 . ?
C25 H25 0.95 . ?
C26 C27 1.525(5) . ?
C26 C39 1.533(5) . ?
C26 P3 1.958(3) . ?
C27 C28 1.394(4) . ?
C27 C32 1.399(5) . ?
C28 C29 1.384(5) . ?
C28 H28 0.95 . ?
C29 C30 1.394(5) . ?
C29 H29 0.95 . ?
C30 C31 1.396(4) . ?
C30 C33 1.487(5) . ?
C31 C32 1.391(5) . ?
C31 H31 0.95 . ?
C32 H32 0.95 . ?
C33 C38 1.392(5) . ?
C33 C34 1.405(5) . ?
C34 C35 1.388(5) . ?
C34 H34 0.95 . ?
C35 C36 1.373(5) . ?
C35 H35 0.95 . ?
C36 C37 1.393(5) . ?
C36 H36 0.95 . ?
C37 C38 1.390(5) . ?
C37 H37 0.95 . ?
C38 H38 0.95 . ?
C39 C40 1.394(5) . ?
C39 C44 1.398(5) . ?
C40 C41 1.397(5) . ?
C40 H40 0.95 . ?
C41 C42 1.392(5) . ?
C41 H41 0.95 . ?
C42 C43 1.397(5) . ?
C42 C45 1.484(5) . ?
C43 C44 1.391(5) . ?
C43 H43 0.95 . ?
C44 H44 0.95 . ?
C45 C50 1.395(5) . ?
C45 C46 1.395(5) . ?
C46 C47 1.381(5) . ?
C46 H46 0.95 . ?
C47 C48 1.386(6) . ?
C47 H47 0.95 . ?
C48 C49 1.376(6) . ?
C48 H48 0.95 . ?
C49 C50 1.382(6) . ?
C49 H49 0.95 . ?
C50 H50 0.95 . ?
C51 N1 1.470(5) . ?
C51 C52 1.511(6) . ?
C51 H51A 0.99 . ?
C51 H51B 0.99 . ?
C52 H52A 0.98 . ?
C52 H52B 0.98 . ?
C52 H52C 0.98 . ?
C53 N1 1.468(5) . ?
C53 C54 1.514(6) . ?
C53 H53A 0.99 . ?
C53 H53B 0.99 . ?
C54 H54A 0.98 . ?
C54 H54B 0.98 . ?
C54 H54C 0.98 . ?
C55 N2 1.474(5) . ?
C55 C56 1.516(6) . ?
C55 H55A 0.99 . ?
C55 H55B 0.99 . ?
C56 H56A 0.98 . ?
C56 H56B 0.98 . ?
C56 H56C 0.98 . ?
C57 N2 1.464(5) . ?
C57 C58 1.510(5) . ?
C57 H57A 0.99 . ?
C57 H57B 0.99 . ?
C58 H58A 0.98 . ?
C58 H58B 0.98 . ?
C58 H58C 0.98 . ?
C59 N3 1.481(5) . ?
C59 C60 1.507(6) . ?
C59 H59A 0.99 . ?
C59 H59B 0.99 . ?
C60 H60A 0.98 . ?
C60 H60B 0.98 . ?
C60 H60C 0.98 . ?
C61 N3 1.465(5) . ?
C61 C62 1.522(5) . ?
C61 H61A 0.99 . ?
C61 H61B 0.99 . ?
C62 H62A 0.98 . ?
C62 H62B 0.98 . ?
C62 H62C 0.98 . ?
C63 N4 1.471(5) . ?
C63 C64 1.515(6) . ?
C63 H63A 0.99 . ?
C63 H63B 0.99 . ?
C64 H64A 0.98 . ?
C64 H64B 0.98 . ?
C64 H64C 0.98 . ?
C65 N4 1.463(5) . ?
C65 C66 1.534(5) . ?
C65 H65A 0.99 . ?
C65 H65B 0.99 . ?
C66 H66A 0.98 . ?
C66 H66B 0.98 . ?
C66 H66C 0.98 . ?
C67 C68 1.471(7) . ?
C67 H67A 0.98 . ?
C67 H67B 0.98 . ?
C67 H67C 0.98 . ?
C68 C69 1.513(7) . ?
C68 H68A 0.99 . ?
C68 H68B 0.99 . ?
C69 C70 1.509(7) . ?
C69 H69A 0.99 . ?
C69 H69B 0.99 . ?
C70 C71 1.505(7) . ?
C70 H70A 0.99 . ?
C70 H70B 0.99 . ?
C71 H71A 0.98 . ?
C71 H71B 0.98 . ?
C71 H71C 0.98 . ?
N1 P1 1.700(3) . ?
N2 P1 1.697(3) . ?
N3 P4 1.703(3) . ?
N4 P4 1.691(3) . ?
P1 P2 2.2639(13) . ?
P2 P3 2.2087(13) . ?
P3 P4 2.2473(13) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C14 109.1(3) . . ?
C2 C1 C26 117.2(3) . . ?
C14 C1 C26 112.5(3) . . ?
C2 C1 P2 109.0(2) . . ?
C14 C1 P2 111.7(2) . . ?
C26 C1 P2 96.8(2) . . ?
C7 C2 C3 117.5(3) . . ?
C7 C2 C1 123.8(3) . . ?
C3 C2 C1 118.4(3) . . ?
C4 C3 C2 121.3(3) . . ?
C4 C3 H3 119.4 . . ?
C2 C3 H3 119.4 . . ?
C3 C4 C5 121.3(3) . . ?
C3 C4 H4 119.4 . . ?
C5 C4 H4 119.4 . . ?
C4 C5 C6 117.4(3) . . ?
C4 C5 C8 121.9(3) . . ?
C6 C5 C8 120.7(3) . . ?
C7 C6 C5 121.4(3) . . ?
C7 C6 H6 119.3 . . ?
C5 C6 H6 119.3 . . ?
C6 C7 C2 121.1(3) . . ?
C6 C7 H7 119.4 . . ?
C2 C7 H7 119.4 . . ?
C9 C8 C13 118.3(3) . . ?
C9 C8 C5 121.0(3) . . ?
C13 C8 C5 120.7(3) . . ?
C10 C9 C8 120.7(4) . . ?
C10 C9 H9 119.7 . . ?
C8 C9 H9 119.7 . . ?
C11 C10 C9 120.5(4) . . ?
C11 C10 H10 119.8 . . ?
C9 C10 H10 119.8 . . ?
C10 C11 C12 119.5(4) . . ?
C10 C11 H11 120.2 . . ?
C12 C11 H11 120.2 . . ?
C11 C12 C13 120.5(4) . . ?
C11 C12 H12 119.7 . . ?
C13 C12 H12 119.7 . . ?
C12 C13 C8 120.5(4) . . ?
C12 C13 H13 119.7 . . ?
C8 C13 H13 119.7 . . ?
C15 C14 C19 116.6(3) . . ?
C15 C14 C1 122.4(3) . . ?
C19 C14 C1 120.9(3) . . ?
C14 C15 C16 121.8(3) . . ?
C14 C15 H15 119.1 . . ?
C16 C15 H15 119.1 . . ?
C15 C16 C17 121.5(3) . . ?
C15 C16 H16 119.2 . . ?
C17 C16 H16 119.2 . . ?
C18 C17 C16 116.9(3) . . ?
C18 C17 C20 121.5(3) . . ?
C16 C17 C20 121.6(3) . . ?
C19 C18 C17 121.1(3) . . ?
C19 C18 H18 119.5 . . ?
C17 C18 H18 119.5 . . ?
C18 C19 C14 122.1(3) . . ?
C18 C19 H19 118.9 . . ?
C14 C19 H19 118.9 . . ?
C25 C20 C21 117.9(3) . . ?
C25 C20 C17 121.1(3) . . ?
C21 C20 C17 121.0(3) . . ?
C22 C21 C20 121.3(4) . . ?
C22 C21 H21 119.3 . . ?
C20 C21 H21 119.3 . . ?
C23 C22 C21 120.2(4) . . ?
C23 C22 H22 119.9 . . ?
C21 C22 H22 119.9 . . ?
C22 C23 C24 119.0(4) . . ?
C22 C23 H23 120.5 . . ?
C24 C23 H23 120.5 . . ?
C25 C24 C23 120.8(4) . . ?
C25 C24 H24 119.6 . . ?
C23 C24 H24 119.6 . . ?
C24 C25 C20 120.8(4) . . ?
C24 C25 H25 119.6 . . ?
C20 C25 H25 119.6 . . ?
C27 C26 C39 110.2(3) . . ?
C27 C26 C1 113.6(3) . . ?
C39 C26 C1 115.3(3) . . ?
C27 C26 P3 110.9(2) . . ?
C39 C26 P3 110.1(2) . . ?
C1 C26 P3 96.0(2) . . ?
C28 C27 C32 116.5(3) . . ?
C28 C27 C26 121.2(3) . . ?
C32 C27 C26 122.3(3) . . ?
C29 C28 C27 121.8(3) . . ?
C29 C28 H28 119.1 . . ?
C27 C28 H28 119.1 . . ?
C28 C29 C30 121.3(3) . . ?
C28 C29 H29 119.3 . . ?
C30 C29 H29 119.3 . . ?
C29 C30 C31 117.6(3) . . ?
C29 C30 C33 120.7(3) . . ?
C31 C30 C33 121.8(3) . . ?
C32 C31 C30 120.5(3) . . ?
C32 C31 H31 119.7 . . ?
C30 C31 H31 119.7 . . ?
C31 C32 C27 122.1(3) . . ?
C31 C32 H32 118.9 . . ?
C27 C32 H32 118.9 . . ?
C38 C33 C34 118.8(3) . . ?
C38 C33 C30 121.7(3) . . ?
C34 C33 C30 119.5(3) . . ?
C35 C34 C33 120.2(4) . . ?
C35 C34 H34 119.9 . . ?
C33 C34 H34 119.9 . . ?
C36 C35 C34 120.6(4) . . ?
C36 C35 H35 119.7 . . ?
C34 C35 H35 119.7 . . ?
C35 C36 C37 120.0(4) . . ?
C35 C36 H36 120 . . ?
C37 C36 H36 120 . . ?
C38 C37 C36 119.9(4) . . ?
C38 C37 H37 120.1 . . ?
C36 C37 H37 120.1 . . ?
C37 C38 C33 120.6(3) . . ?
C37 C38 H38 119.7 . . ?
C33 C38 H38 119.7 . . ?
C40 C39 C44 116.8(3) . . ?
C40 C39 C26 121.4(3) . . ?
C44 C39 C26 121.8(3) . . ?
C39 C40 C41 121.6(3) . . ?
C39 C40 H40 119.2 . . ?
C41 C40 H40 119.2 . . ?
C42 C41 C40 121.3(3) . . ?
C42 C41 H41 119.4 . . ?
C40 C41 H41 119.4 . . ?
C41 C42 C43 117.3(3) . . ?
C41 C42 C45 121.3(3) . . ?
C43 C42 C45 121.4(3) . . ?
C44 C43 C42 121.2(3) . . ?
C44 C43 H43 119.4 . . ?
C42 C43 H43 119.4 . . ?
C43 C44 C39 121.7(3) . . ?
C43 C44 H44 119.1 . . ?
C39 C44 H44 119.1 . . ?
C50 C45 C46 117.1(3) . . ?
C50 C45 C42 120.5(3) . . ?
C46 C45 C42 122.4(3) . . ?
C47 C46 C45 122.2(4) . . ?
C47 C46 H46 118.9 . . ?
C45 C46 H46 118.9 . . ?
C46 C47 C48 119.4(4) . . ?
C46 C47 H47 120.3 . . ?
C48 C47 H47 120.3 . . ?
C49 C48 C47 119.6(4) . . ?
C49 C48 H48 120.2 . . ?
C47 C48 H48 120.2 . . ?
C48 C49 C50 120.7(4) . . ?
C48 C49 H49 119.7 . . ?
C50 C49 H49 119.7 . . ?
C49 C50 C45 121.0(4) . . ?
C49 C50 H50 119.5 . . ?
C45 C50 H50 119.5 . . ?
N1 C51 C52 114.8(3) . . ?
N1 C51 H51A 108.6 . . ?
C52 C51 H51A 108.6 . . ?
N1 C51 H51B 108.6 . . ?
C52 C51 H51B 108.6 . . ?
H51A C51 H51B 107.5 . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
N1 C53 C54 113.6(3) . . ?
N1 C53 H53A 108.8 . . ?
C54 C53 H53A 108.8 . . ?
N1 C53 H53B 108.8 . . ?
C54 C53 H53B 108.8 . . ?
H53A C53 H53B 107.7 . . ?
C53 C54 H54A 109.5 . . ?
C53 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C53 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
N2 C55 C56 114.8(4) . . ?
N2 C55 H55A 108.6 . . ?
C56 C55 H55A 108.6 . . ?
N2 C55 H55B 108.6 . . ?
C56 C55 H55B 108.6 . . ?
H55A C55 H55B 107.5 . . ?
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 . . ?
N2 C57 C58 115.7(4) . . ?
N2 C57 H57A 108.4 . . ?
C58 C57 H57A 108.4 . . ?
N2 C57 H57B 108.4 . . ?
C58 C57 H57B 108.4 . . ?
H57A C57 H57B 107.4 . . ?
C57 C58 H58A 109.5 . . ?
C57 C58 H58B 109.5 . . ?
H58A C58 H58B 109.5 . . ?
C57 C58 H58C 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
N3 C59 C60 115.0(3) . . ?
N3 C59 H59A 108.5 . . ?
C60 C59 H59A 108.5 . . ?
N3 C59 H59B 108.5 . . ?
C60 C59 H59B 108.5 . . ?
H59A C59 H59B 107.5 . . ?
C59 C60 H60A 109.5 . . ?
C59 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
C59 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
N3 C61 C62 114.7(3) . . ?
N3 C61 H61A 108.6 . . ?
C62 C61 H61A 108.6 . . ?
N3 C61 H61B 108.6 . . ?
C62 C61 H61B 108.6 . . ?
H61A C61 H61B 107.6 . . ?
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 . . ?
N4 C63 C64 114.2(4) . . ?
N4 C63 H63A 108.7 . . ?
C64 C63 H63A 108.7 . . ?
N4 C63 H63B 108.7 . . ?
C64 C63 H63B 108.7 . . ?
H63A C63 H63B 107.6 . . ?
C63 C64 H64A 109.5 . . ?
C63 C64 H64B 109.5 . . ?
H64A C64 H64B 109.5 . . ?
C63 C64 H64C 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
N4 C65 C66 113.2(3) . . ?
N4 C65 H65A 108.9 . . ?
C66 C65 H65A 108.9 . . ?
N4 C65 H65B 108.9 . . ?
C66 C65 H65B 108.9 . . ?
H65A C65 H65B 107.7 . . ?
C65 C66 H66A 109.5 . . ?
C65 C66 H66B 109.5 . . ?
H66A C66 H66B 109.5 . . ?
C65 C66 H66C 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?
C68 C67 H67A 109.5 . . ?
C68 C67 H67B 109.5 . . ?
H67A C67 H67B 109.5 . . ?
C68 C67 H67C 109.5 . . ?
H67A C67 H67C 109.5 . . ?
H67B C67 H67C 109.5 . . ?
C67 C68 C69 114.3(5) . . ?
C67 C68 H68A 108.7 . . ?
C69 C68 H68A 108.7 . . ?
C67 C68 H68B 108.7 . . ?
C69 C68 H68B 108.7 . . ?
H68A C68 H68B 107.6 . . ?
C70 C69 C68 116.0(4) . . ?
C70 C69 H69A 108.3 . . ?
C68 C69 H69A 108.3 . . ?
C70 C69 H69B 108.3 . . ?
C68 C69 H69B 108.3 . . ?
H69A C69 H69B 107.4 . . ?
C71 C70 C69 112.7(4) . . ?
C71 C70 H70A 109.1 . . ?
C69 C70 H70A 109.1 . . ?
C71 C70 H70B 109.1 . . ?
C69 C70 H70B 109.1 . . ?
H70A C70 H70B 107.8 . . ?
C70 C71 H71A 109.5 . . ?
C70 C71 H71B 109.5 . . ?
H71A C71 H71B 109.5 . . ?
C70 C71 H71C 109.5 . . ?
H71A C71 H71C 109.5 . . ?
H71B C71 H71C 109.5 . . ?
C53 N1 C51 115.4(3) . . ?
C53 N1 P1 126.1(3) . . ?
C51 N1 P1 114.1(3) . . ?
C57 N2 C55 115.7(3) . . ?
C57 N2 P1 123.6(3) . . ?
C55 N2 P1 115.3(3) . . ?
C61 N3 C59 113.8(3) . . ?
C61 N3 P4 125.2(3) . . ?
C59 N3 P4 117.6(3) . . ?
C65 N4 C63 116.2(3) . . ?
C65 N4 P4 127.2(3) . . ?
C63 N4 P4 113.7(3) . . ?
N2 P1 N1 109.61(16) . . ?
N2 P1 P2 105.88(12) . . ?
N1 P1 P2 93.96(12) . . ?
C1 P2 P3 79.48(10) . . ?
C1 P2 P1 104.34(11) . . ?
P3 P2 P1 111.67(5) . . ?
C26 P3 P2 79.80(11) . . ?
C26 P3 P4 107.54(11) . . ?
P2 P3 P4 94.93(5) . . ?
N4 P4 N3 112.47(16) . . ?
N4 P4 P3 102.42(12) . . ?
N3 P4 P3 94.89(12) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C14 C1 C2 C7 -94.4(4) . . . . ?
C26 C1 C2 C7 34.9(4) . . . . ?
P2 C1 C2 C7 143.3(3) . . . . ?
C14 C1 C2 C3 79.7(4) . . . . ?
C26 C1 C2 C3 -151.0(3) . . . . ?
P2 C1 C2 C3 -42.5(4) . . . . ?
C7 C2 C3 C4 -0.5(5) . . . . ?
C1 C2 C3 C4 -175.0(3) . . . . ?
C2 C3 C4 C5 0.8(5) . . . . ?
C3 C4 C5 C6 -0.8(5) . . . . ?
C3 C4 C5 C8 179.7(3) . . . . ?
C4 C5 C6 C7 0.6(5) . . . . ?
C8 C5 C6 C7 -179.9(3) . . . . ?
C5 C6 C7 C2 -0.3(5) . . . . ?
C3 C2 C7 C6 0.2(5) . . . . ?
C1 C2 C7 C6 174.4(3) . . . . ?
C4 C5 C8 C9 39.1(5) . . . . ?
C6 C5 C8 C9 -140.4(4) . . . . ?
C4 C5 C8 C13 -142.5(3) . . . . ?
C6 C5 C8 C13 38.0(5) . . . . ?
C13 C8 C9 C10 0.0(5) . . . . ?
C5 C8 C9 C10 178.5(3) . . . . ?
C8 C9 C10 C11 0.5(6) . . . . ?
C9 C10 C11 C12 -0.2(6) . . . . ?
C10 C11 C12 C13 -0.6(6) . . . . ?
C11 C12 C13 C8 1.1(6) . . . . ?
C9 C8 C13 C12 -0.8(5) . . . . ?
C5 C8 C13 C12 -179.3(3) . . . . ?
C2 C1 C14 C15 -2.9(4) . . . . ?
C26 C1 C14 C15 -134.7(3) . . . . ?
P2 C1 C14 C15 117.7(3) . . . . ?
C2 C1 C14 C19 -180.0(3) . . . . ?
C26 C1 C14 C19 48.2(4) . . . . ?
P2 C1 C14 C19 -59.4(4) . . . . ?
C19 C14 C15 C16 0.3(5) . . . . ?
C1 C14 C15 C16 -176.9(3) . . . . ?
C14 C15 C16 C17 1.1(6) . . . . ?
C15 C16 C17 C18 -1.5(5) . . . . ?
C15 C16 C17 C20 177.6(3) . . . . ?
C16 C17 C18 C19 0.6(5) . . . . ?
C20 C17 C18 C19 -178.5(3) . . . . ?
C17 C18 C19 C14 0.8(5) . . . . ?
C15 C14 C19 C18 -1.3(5) . . . . ?
C1 C14 C19 C18 176.0(3) . . . . ?
C18 C17 C20 C25 -26.8(5) . . . . ?
C16 C17 C20 C25 154.1(4) . . . . ?
C18 C17 C20 C21 152.9(4) . . . . ?
C16 C17 C20 C21 -26.1(5) . . . . ?
C25 C20 C21 C22 -1.2(6) . . . . ?
C17 C20 C21 C22 179.0(4) . . . . ?
C20 C21 C22 C23 1.1(6) . . . . ?
C21 C22 C23 C24 -0.4(6) . . . . ?
C22 C23 C24 C25 -0.1(6) . . . . ?
C23 C24 C25 C20 0.0(6) . . . . ?
C21 C20 C25 C24 0.7(6) . . . . ?
C17 C20 C25 C24 -179.5(4) . . . . ?
C2 C1 C26 C27 -104.5(3) . . . . ?
C14 C1 C26 C27 23.2(4) . . . . ?
P2 C1 C26 C27 140.1(2) . . . . ?
C2 C1 C26 C39 24.1(4) . . . . ?
C14 C1 C26 C39 151.7(3) . . . . ?
P2 C1 C26 C39 -91.4(3) . . . . ?
C2 C1 C26 P3 139.6(2) . . . . ?
C14 C1 C26 P3 -92.7(3) . . . . ?
P2 C1 C26 P3 24.18(18) . . . . ?
C39 C26 C27 C28 -83.3(4) . . . . ?
C1 C26 C27 C28 47.9(4) . . . . ?
P3 C26 C27 C28 154.6(3) . . . . ?
C39 C26 C27 C32 95.4(4) . . . . ?
C1 C26 C27 C32 -133.5(3) . . . . ?
P3 C26 C27 C32 -26.8(4) . . . . ?
C32 C27 C28 C29 2.6(5) . . . . ?
C26 C27 C28 C29 -178.7(3) . . . . ?
C27 C28 C29 C30 0.2(5) . . . . ?
C28 C29 C30 C31 -3.5(5) . . . . ?
C28 C29 C30 C33 175.8(3) . . . . ?
C29 C30 C31 C32 3.9(5) . . . . ?
C33 C30 C31 C32 -175.4(3) . . . . ?
C30 C31 C32 C27 -1.2(5) . . . . ?
C28 C27 C32 C31 -2.1(5) . . . . ?
C26 C27 C32 C31 179.2(3) . . . . ?
C29 C30 C33 C38 148.2(3) . . . . ?
C31 C30 C33 C38 -32.5(5) . . . . ?
C29 C30 C33 C34 -33.5(5) . . . . ?
C31 C30 C33 C34 145.8(3) . . . . ?
C38 C33 C34 C35 -0.7(5) . . . . ?
C30 C33 C34 C35 -179.0(3) . . . . ?
C33 C34 C35 C36 0.3(6) . . . . ?
C34 C35 C36 C37 0.6(6) . . . . ?
C35 C36 C37 C38 -0.9(6) . . . . ?
C36 C37 C38 C33 0.5(6) . . . . ?
C34 C33 C38 C37 0.3(5) . . . . ?
C30 C33 C38 C37 178.5(3) . . . . ?
C27 C26 C39 C40 -11.4(4) . . . . ?
C1 C26 C39 C40 -141.6(3) . . . . ?
P3 C26 C39 C40 111.2(3) . . . . ?
C27 C26 C39 C44 172.3(3) . . . . ?
C1 C26 C39 C44 42.1(4) . . . . ?
P3 C26 C39 C44 -65.1(4) . . . . ?
C44 C39 C40 C41 2.1(5) . . . . ?
C26 C39 C40 C41 -174.3(3) . . . . ?
C39 C40 C41 C42 0.3(5) . . . . ?
C40 C41 C42 C43 -2.7(5) . . . . ?
C40 C41 C42 C45 176.3(3) . . . . ?
C41 C42 C43 C44 2.8(5) . . . . ?
C45 C42 C43 C44 -176.3(3) . . . . ?
C42 C43 C44 C39 -0.4(5) . . . . ?
C40 C39 C44 C43 -2.1(5) . . . . ?
C26 C39 C44 C43 174.3(3) . . . . ?
C41 C42 C45 C50 -147.3(4) . . . . ?
C43 C42 C45 C50 31.8(5) . . . . ?
C41 C42 C45 C46 32.6(5) . . . . ?
C43 C42 C45 C46 -148.3(4) . . . . ?
C50 C45 C46 C47 0.2(6) . . . . ?
C42 C45 C46 C47 -179.7(4) . . . . ?
C45 C46 C47 C48 -0.4(6) . . . . ?
C46 C47 C48 C49 0.0(7) . . . . ?
C47 C48 C49 C50 0.6(7) . . . . ?
C48 C49 C50 C45 -0.8(7) . . . . ?
C46 C45 C50 C49 0.4(6) . . . . ?
C42 C45 C50 C49 -179.7(4) . . . . ?
C67 C68 C69 C70 -174.4(5) . . . . ?
C68 C69 C70 C71 175.8(4) . . . . ?
C54 C53 N1 C51 -54.2(4) . . . . ?
C54 C53 N1 P1 151.1(3) . . . . ?
C52 C51 N1 C53 -62.1(5) . . . . ?
C52 C51 N1 P1 95.6(4) . . . . ?
C58 C57 N2 C55 -43.6(5) . . . . ?
C58 C57 N2 P1 163.6(3) . . . . ?
C56 C55 N2 C57 -59.6(5) . . . . ?
C56 C55 N2 P1 95.5(4) . . . . ?
C62 C61 N3 C59 -60.5(5) . . . . ?
C62 C61 N3 P4 98.0(4) . . . . ?
C60 C59 N3 C61 -155.2(4) . . . . ?
C60 C59 N3 P4 44.6(5) . . . . ?
C66 C65 N4 C63 -64.0(4) . . . . ?
C66 C65 N4 P4 137.1(3) . . . . ?
C64 C63 N4 C65 -78.7(4) . . . . ?
C64 C63 N4 P4 83.1(4) . . . . ?
C57 N2 P1 N1 -69.0(4) . . . . ?
C55 N2 P1 N1 138.1(3) . . . . ?
C57 N2 P1 P2 31.2(4) . . . . ?
C55 N2 P1 P2 -121.7(3) . . . . ?
C53 N1 P1 N2 48.3(3) . . . . ?
C51 N1 P1 N2 -106.7(3) . . . . ?
C53 N1 P1 P2 -60.2(3) . . . . ?
C51 N1 P1 P2 144.9(2) . . . . ?
C65 N4 P4 N3 56.6(3) . . . . ?
C63 N4 P4 N3 -102.8(3) . . . . ?
C65 N4 P4 P3 -44.1(3) . . . . ?
C63 N4 P4 P3 156.6(2) . . . . ?
C61 N3 P4 N4 -41.3(4) . . . . ?
C59 N3 P4 N4 116.4(3) . . . . ?
C61 N3 P4 P3 64.3(3) . . . . ?
C59 N3 P4 P3 -138.0(3) . . . . ?



# END of CIF
####################################################################### 
# 
# 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_shelx_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2386110'
loop_
_audit_author_name
_audit_author_address
'Lukasz Ponikiewski'
;Gdansk University of Technology
Poland
;
_audit_update_record             
;
2024-09-23 deposited with the CCDC.	2024-11-13 downloaded from the CCDC.
;

_audit_creation_date             2024-07-18T13:39:06-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_moiety         'C18 H34 Cl3 N2 P Ru'
_chemical_formula_sum            'C18 H34 Cl3 N2 P Ru'
_chemical_formula_weight         516.86

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.4357(4)
_cell_length_b                   11.5604(6)
_cell_length_c                   13.4708(6)
_cell_angle_alpha                94.140(4)
_cell_angle_beta                 94.656(4)
_cell_angle_gamma                98.498(4)
_cell_volume                     1137.28(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    22948
_cell_measurement_theta_min      3.30
_cell_measurement_theta_max      67.54
_cell_measurement_wavelength     1.54186

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       plate
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.07
_exptl_crystal_density_diffrn    1.509
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             532

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    9.512
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in: F. R. Ahmed (Editor), "Crystallographic
Computing", Munksgaard, Copenhagen (1970), 255 - 270. Afterwards scaling of
reflection intensities was performed within STOE LANA. J. Koziskova, F. Hahn,
J. Richter, J. Kozisek, Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136-140.
;
_exptl_absorpt_correction_T_min  0.1879
_exptl_absorpt_correction_T_max  0.5888
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
3 5 2 0.0480
-2 -6 -1 0.0250
-3 5 -2 0.0380
3 -4 2 0.0650
-1 0 4 0.0320
1 0 -3 0.0150


#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     1.54186
_diffrn_radiation_type           CuK\a
_diffrn_radiation_probe          x-ray
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_type            'STOE Imaging Plate'
_diffrn_detector_area_resol_mean 6.67
_diffrn_source                   'GeniX Cu, 0.05 x 0.05 mm2 microfocus'
_diffrn_source_type              ?
_diffrn_source_target            ?
_diffrn_source_voltage           50
_diffrn_source_current           0.600
_diffrn_source_power             0.030
_diffrn_radiation_monochromator  'parabolic x-ray mirror'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_collimation    '0.6 mm diameter'
_diffrn_measurement_method       'rotation method, ω scans'
_diffrn_measurement_details      
; 1311 frames, detector distance = 45 mm
;
_diffrn_reflns_av_R_equivalents  0.0304
_diffrn_reflns_av_unetI/netI     0.0239
_diffrn_reflns_number            12033
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.304
_diffrn_reflns_theta_max         65.994
_diffrn_reflns_theta_full        65.994
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.961
_diffrn_reflns_Laue_measured_fraction_full 0.961
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_point_group_measured_fraction_full 0.961
_diffrn_reflns_point_group_measured_fraction_max 0.961
_reflns_Friedel_coverage         0
_reflns_number_total             3811
_reflns_number_gt                3378
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       
;
X-Area WinXpose 2.0.22.0 (STOE, 2016)
;
_computing_cell_refinement       
;
X-Area Recipe 1.34.0.0 (STOE, 2019)
;
_computing_data_reduction        
;
X-Area Integrate 1.77.0.0 (STOE, 2019)
X-Area LANA 1.77.1.0 (STOE, 2019)
;
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0614P)²+9.7638P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2018/1 (Sheldrick 2018)'
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_coef       0.0025(3)
_refine_ls_number_reflns         3811
_refine_ls_number_parameters     205
_refine_ls_number_restraints     0
_refine_ls_number_constraints    0
_refine_ls_R_factor_all          0.0644
_refine_ls_R_factor_gt           0.0544
_refine_ls_wR_factor_ref         0.1528
_refine_ls_wR_factor_gt          0.1403
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_restrained_S_all      1.131
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_diff_density_max         1.061
_refine_diff_density_min         -1.186
_refine_diff_density_rms         0.167

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru 0.0552 3.296 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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
Ru1 Ru 0.34491(6) 0.61755(4) 0.33635(4) 0.0250(2) Uani 1 1 d . . . . .
Cl1 Cl 0.5861(2) 0.54588(17) 0.25251(15) 0.0388(5) Uani 1 1 d . . . . .
Cl2 Cl 0.5889(2) 0.74042(16) 0.44111(14) 0.0408(5) Uani 1 1 d . . . . .
Cl3 Cl 0.1277(2) 0.74894(15) 0.12999(12) 0.0337(4) Uani 1 1 d . . . . .
P1 P 0.3584(2) 0.77255(15) 0.23586(12) 0.0253(4) Uani 1 1 d . . . . .
N1 N 0.5152(9) 0.7945(6) 0.1561(5) 0.0422(16) Uani 1 1 d . . . . .
N2 N 0.3594(8) 0.9025(5) 0.2896(4) 0.0307(13) Uani 1 1 d . . . . .
C1 C 0.1634(9) 0.4496(6) 0.2853(5) 0.0274(6) Uani 1 1 d . . . . .
C2 C 0.0582(9) 0.5423(6) 0.2838(5) 0.0274(6) Uani 1 1 d . . . . .
H2 H -0.013255 0.552858 0.224427 0.033 Uiso 1 1 calc R U . . .
C3 C 0.0595(9) 0.6201(6) 0.3717(5) 0.0274(6) Uani 1 1 d . . . . .
H3 H -0.01109 0.682091 0.36932 0.033 Uiso 1 1 calc R U . . .
C4 C 0.1621(8) 0.6072(6) 0.4614(5) 0.0274(6) Uani 1 1 d . . . . .
C5 C 0.2619(9) 0.5093(6) 0.4647(5) 0.0274(6) Uani 1 1 d . . . . .
H5 H 0.328022 0.496509 0.525208 0.033 Uiso 1 1 calc R U . . .
C6 C 0.2616(9) 0.4330(6) 0.3788(5) 0.0274(6) Uani 1 1 d . . . . .
H6 H 0.327605 0.368833 0.382277 0.033 Uiso 1 1 calc R U . . .
C7 C 0.1681(10) 0.3664(6) 0.1958(5) 0.0325(16) Uani 1 1 d . . . . .
H7 H 0.296118 0.34958 0.194804 0.039 Uiso 1 1 calc R U . . .
C8 C 0.0443(12) 0.2494(7) 0.2074(6) 0.045(2) Uani 1 1 d . . . . .
H8A H 0.081176 0.219469 0.270945 0.067 Uiso 1 1 calc R U . . .
H8B H 0.056304 0.191959 0.15206 0.067 Uiso 1 1 calc R U . . .
H8C H -0.083026 0.262437 0.206477 0.067 Uiso 1 1 calc R U . . .
C9 C 0.1157(12) 0.4116(7) 0.0963(5) 0.0419(19) Uani 1 1 d . . . . .
H9A H -0.013114 0.421863 0.092402 0.063 Uiso 1 1 calc R U . . .
H9B H 0.134426 0.354985 0.041846 0.063 Uiso 1 1 calc R U . . .
H9C H 0.191805 0.487107 0.090435 0.063 Uiso 1 1 calc R U . . .
C10 C 0.1719(11) 0.6891(7) 0.5528(6) 0.043(2) Uani 1 1 d . . . . .
H10A H 0.296157 0.732425 0.56673 0.065 Uiso 1 1 calc R U . . .
H10B H 0.140235 0.644332 0.609681 0.065 Uiso 1 1 calc R U . . .
H10C H 0.085871 0.744595 0.542319 0.065 Uiso 1 1 calc R U . . .
C11 C 0.5082(14) 0.7095(8) 0.0672(7) 0.054(2) Uani 1 1 d . . . . .
H11A H 0.415035 0.640519 0.073794 0.065 Uiso 1 1 calc R U . . .
H11B H 0.627872 0.681875 0.065618 0.065 Uiso 1 1 calc R U . . .
C12 C 0.4630(18) 0.7609(10) -0.0311(8) 0.075(3) Uani 1 1 d . . . . .
H12A H 0.340577 0.782979 -0.032237 0.112 Uiso 1 1 calc R U . . .
H12B H 0.466527 0.702274 -0.086915 0.112 Uiso 1 1 calc R U . . .
H12C H 0.552667 0.830532 -0.037378 0.112 Uiso 1 1 calc R U . . .
C13 C 0.7003(11) 0.8478(8) 0.1988(9) 0.060(3) Uani 1 1 d . . . . .
H13A H 0.775347 0.785119 0.20986 0.073 Uiso 1 1 calc R U . . .
H13B H 0.692926 0.890661 0.264291 0.073 Uiso 1 1 calc R U . . .
C14 C 0.7932(13) 0.9339(10) 0.1279(11) 0.089(5) Uani 1 1 d . . . . .
H14A H 0.813684 0.889899 0.065995 0.133 Uiso 1 1 calc R U . . .
H14B H 0.910459 0.97404 0.16085 0.133 Uiso 1 1 calc R U . . .
H14C H 0.7139 0.992016 0.112312 0.133 Uiso 1 1 calc R U . . .
C15 C 0.3651(10) 1.0072(6) 0.2290(5) 0.0336(16) Uani 1 1 d . . . . .
H15A H 0.240784 1.027867 0.218717 0.04 Uiso 1 1 calc R U . . .
H15B H 0.405291 0.986759 0.16257 0.04 Uiso 1 1 calc R U . . .
C16 C 0.4939(14) 1.1124(7) 0.2802(6) 0.051(2) Uani 1 1 d . . . . .
H16A H 0.448574 1.137025 0.343438 0.076 Uiso 1 1 calc R U . . .
H16B H 0.500579 1.177034 0.23678 0.076 Uiso 1 1 calc R U . . .
H16C H 0.615768 1.091012 0.293476 0.076 Uiso 1 1 calc R U . . .
C17 C 0.2939(15) 0.9210(8) 0.3884(6) 0.055(3) Uani 1 1 d . . . . .
H17A H 0.376995 0.986197 0.427599 0.066 Uiso 1 1 calc R U . . .
H17B H 0.298238 0.84936 0.423958 0.066 Uiso 1 1 calc R U . . .
C18 C 0.102(2) 0.9495(12) 0.3835(10) 0.107(6) Uani 1 1 d . . . . .
H18A H 0.100806 1.027828 0.360357 0.161 Uiso 1 1 calc R U . . .
H18B H 0.057721 0.947681 0.450147 0.161 Uiso 1 1 calc R U . . .
H18C H 0.021568 0.891293 0.336936 0.161 Uiso 1 1 calc R U . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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
Ru1 C3 2.217(7) . ?
Ru1 C2 2.218(6) . ?
Ru1 C1 2.224(6) . ?
Ru1 C4 2.248(6) . ?
Ru1 C6 2.260(7) . ?
Ru1 C5 2.279(7) . ?
Ru1 P1 2.3179(17) . ?
Ru1 Cl1 2.4106(18) . ?
Ru1 Cl2 2.4154(16) . ?
Cl3 P1 2.112(2) . ?
P1 N2 1.619(6) . ?
P1 N1 1.653(6) . ?
N1 C13 1.474(11) . ?
N1 C11 1.486(11) . ?
N2 C17 1.466(10) . ?
N2 C15 1.506(9) . ?
C1 C2 1.417(10) . ?
C1 C6 1.444(10) . ?
C1 C7 1.493(10) . ?
C2 C3 1.433(10) . ?
C2 H2 0.95 . ?
C3 C4 1.405(10) . ?
C3 H3 0.95 . ?
C4 C5 1.443(10) . ?
C4 C10 1.489(10) . ?
C5 C6 1.403(10) . ?
C5 H5 0.95 . ?
C6 H6 0.95 . ?
C7 C9 1.515(10) . ?
C7 C8 1.545(10) . ?
C7 H7 1 . ?
C8 H8A 0.98 . ?
C8 H8B 0.98 . ?
C8 H8C 0.98 . ?
C9 H9A 0.98 . ?
C9 H9B 0.98 . ?
C9 H9C 0.98 . ?
C10 H10A 0.98 . ?
C10 H10B 0.98 . ?
C10 H10C 0.98 . ?
C11 C12 1.523(13) . ?
C11 H11A 0.99 . ?
C11 H11B 0.99 . ?
C12 H12A 0.98 . ?
C12 H12B 0.98 . ?
C12 H12C 0.98 . ?
C13 C14 1.556(12) . ?
C13 H13A 0.99 . ?
C13 H13B 0.99 . ?
C14 H14A 0.98 . ?
C14 H14B 0.98 . ?
C14 H14C 0.98 . ?
C15 C16 1.516(10) . ?
C15 H15A 0.99 . ?
C15 H15B 0.99 . ?
C16 H16A 0.98 . ?
C16 H16B 0.98 . ?
C16 H16C 0.98 . ?
C17 C18 1.511(17) . ?
C17 H17A 0.99 . ?
C17 H17B 0.99 . ?
C18 H18A 0.98 . ?
C18 H18B 0.98 . ?
C18 H18C 0.98 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C3 Ru1 C2 37.7(2) . . ?
C3 Ru1 C1 67.6(2) . . ?
C2 Ru1 C1 37.2(3) . . ?
C3 Ru1 C4 36.7(2) . . ?
C2 Ru1 C4 67.5(2) . . ?
C1 Ru1 C4 80.4(2) . . ?
C3 Ru1 C6 77.8(3) . . ?
C2 Ru1 C6 66.3(2) . . ?
C1 Ru1 C6 37.6(2) . . ?
C4 Ru1 C6 66.4(2) . . ?
C3 Ru1 C5 65.8(2) . . ?
C2 Ru1 C5 78.4(2) . . ?
C1 Ru1 C5 67.0(2) . . ?
C4 Ru1 C5 37.2(3) . . ?
C6 Ru1 C5 36.0(2) . . ?
C3 Ru1 P1 96.04(19) . . ?
C2 Ru1 P1 95.14(18) . . ?
C1 Ru1 P1 119.53(18) . . ?
C4 Ru1 P1 120.73(19) . . ?
C6 Ru1 P1 156.94(18) . . ?
C5 Ru1 P1 157.79(18) . . ?
C3 Ru1 Cl1 155.69(18) . . ?
C2 Ru1 Cl1 118.35(18) . . ?
C1 Ru1 Cl1 89.03(18) . . ?
C4 Ru1 Cl1 149.20(19) . . ?
C6 Ru1 Cl1 87.69(18) . . ?
C5 Ru1 Cl1 112.18(18) . . ?
P1 Ru1 Cl1 89.66(6) . . ?
C3 Ru1 Cl2 118.78(18) . . ?
C2 Ru1 Cl2 156.46(19) . . ?
C1 Ru1 Cl2 154.51(19) . . ?
C4 Ru1 Cl2 92.05(17) . . ?
C6 Ru1 Cl2 117.26(17) . . ?
C5 Ru1 Cl2 92.36(17) . . ?
P1 Ru1 Cl2 85.29(6) . . ?
Cl1 Ru1 Cl2 85.17(7) . . ?
N2 P1 N1 103.2(3) . . ?
N2 P1 Cl3 103.6(2) . . ?
N1 P1 Cl3 97.2(3) . . ?
N2 P1 Ru1 117.6(2) . . ?
N1 P1 Ru1 121.7(2) . . ?
Cl3 P1 Ru1 110.43(9) . . ?
C13 N1 C11 115.1(7) . . ?
C13 N1 P1 116.5(6) . . ?
C11 N1 P1 119.3(6) . . ?
C17 N2 C15 114.1(6) . . ?
C17 N2 P1 122.1(5) . . ?
C15 N2 P1 120.6(5) . . ?
C2 C1 C6 117.9(6) . . ?
C2 C1 C7 122.5(6) . . ?
C6 C1 C7 119.6(6) . . ?
C2 C1 Ru1 71.2(4) . . ?
C6 C1 Ru1 72.6(4) . . ?
C7 C1 Ru1 129.7(5) . . ?
C1 C2 C3 120.2(6) . . ?
C1 C2 Ru1 71.6(4) . . ?
C3 C2 Ru1 71.1(4) . . ?
C1 C2 H2 119.9 . . ?
C3 C2 H2 119.9 . . ?
Ru1 C2 H2 129.8 . . ?
C4 C3 C2 121.9(7) . . ?
C4 C3 Ru1 72.9(4) . . ?
C2 C3 Ru1 71.2(4) . . ?
C4 C3 H3 119.1 . . ?
C2 C3 H3 119.1 . . ?
Ru1 C3 H3 129.4 . . ?
C3 C4 C5 118.1(6) . . ?
C3 C4 C10 123.2(7) . . ?
C5 C4 C10 118.7(6) . . ?
C3 C4 Ru1 70.4(4) . . ?
C5 C4 Ru1 72.6(4) . . ?
C10 C4 Ru1 128.3(5) . . ?
C6 C5 C4 120.3(6) . . ?
C6 C5 Ru1 71.3(4) . . ?
C4 C5 Ru1 70.3(4) . . ?
C6 C5 H5 119.9 . . ?
C4 C5 H5 119.9 . . ?
Ru1 C5 H5 131.4 . . ?
C5 C6 C1 121.6(7) . . ?
C5 C6 Ru1 72.7(4) . . ?
C1 C6 Ru1 69.9(4) . . ?
C5 C6 H6 119.2 . . ?
C1 C6 H6 119.2 . . ?
Ru1 C6 H6 131 . . ?
C1 C7 C9 115.1(6) . . ?
C1 C7 C8 109.2(6) . . ?
C9 C7 C8 109.9(7) . . ?
C1 C7 H7 107.5 . . ?
C9 C7 H7 107.5 . . ?
C8 C7 H7 107.5 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C4 C10 H10A 109.5 . . ?
C4 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C4 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N1 C11 C12 113.3(8) . . ?
N1 C11 H11A 108.9 . . ?
C12 C11 H11A 108.9 . . ?
N1 C11 H11B 108.9 . . ?
C12 C11 H11B 108.9 . . ?
H11A C11 H11B 107.7 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N1 C13 C14 111.1(9) . . ?
N1 C13 H13A 109.4 . . ?
C14 C13 H13A 109.4 . . ?
N1 C13 H13B 109.4 . . ?
C14 C13 H13B 109.4 . . ?
H13A C13 H13B 108 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N2 C15 C16 111.7(6) . . ?
N2 C15 H15A 109.3 . . ?
C16 C15 H15A 109.3 . . ?
N2 C15 H15B 109.3 . . ?
C16 C15 H15B 109.3 . . ?
H15A C15 H15B 107.9 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N2 C17 C18 113.1(8) . . ?
N2 C17 H17A 109 . . ?
C18 C17 H17A 109 . . ?
N2 C17 H17B 109 . . ?
C18 C17 H17B 109 . . ?
H17A C17 H17B 107.8 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 P1 N1 C13 57.6(6) . . . . ?
Cl3 P1 N1 C13 163.5(6) . . . . ?
Ru1 P1 N1 C13 -77.1(6) . . . . ?
N2 P1 N1 C11 -156.9(6) . . . . ?
Cl3 P1 N1 C11 -51.0(6) . . . . ?
Ru1 P1 N1 C11 68.4(7) . . . . ?
N1 P1 N2 C17 -157.3(7) . . . . ?
Cl3 P1 N2 C17 101.8(6) . . . . ?
Ru1 P1 N2 C17 -20.3(7) . . . . ?
N1 P1 N2 C15 43.9(6) . . . . ?
Cl3 P1 N2 C15 -57.0(5) . . . . ?
Ru1 P1 N2 C15 -179.1(4) . . . . ?
C6 C1 C2 C3 3.4(9) . . . . ?
C7 C1 C2 C3 -179.6(6) . . . . ?
Ru1 C1 C2 C3 -54.0(5) . . . . ?
C6 C1 C2 Ru1 57.4(5) . . . . ?
C7 C1 C2 Ru1 -125.6(6) . . . . ?
C1 C2 C3 C4 -0.5(9) . . . . ?
Ru1 C2 C3 C4 -54.7(5) . . . . ?
C1 C2 C3 Ru1 54.3(5) . . . . ?
C2 C3 C4 C5 -2.7(9) . . . . ?
Ru1 C3 C4 C5 -56.6(5) . . . . ?
C2 C3 C4 C10 177.6(6) . . . . ?
Ru1 C3 C4 C10 123.6(6) . . . . ?
C2 C3 C4 Ru1 54.0(5) . . . . ?
C3 C4 C5 C6 2.8(9) . . . . ?
C10 C4 C5 C6 -177.5(6) . . . . ?
Ru1 C4 C5 C6 -52.8(5) . . . . ?
C3 C4 C5 Ru1 55.6(5) . . . . ?
C10 C4 C5 Ru1 -124.7(6) . . . . ?
C4 C5 C6 C1 0.2(9) . . . . ?
Ru1 C5 C6 C1 -52.1(5) . . . . ?
C4 C5 C6 Ru1 52.3(5) . . . . ?
C2 C1 C6 C5 -3.3(9) . . . . ?
C7 C1 C6 C5 179.6(6) . . . . ?
Ru1 C1 C6 C5 53.4(5) . . . . ?
C2 C1 C6 Ru1 -56.7(5) . . . . ?
C7 C1 C6 Ru1 126.2(6) . . . . ?
C2 C1 C7 C9 22.1(9) . . . . ?
C6 C1 C7 C9 -161.0(6) . . . . ?
Ru1 C1 C7 C9 -69.7(9) . . . . ?
C2 C1 C7 C8 -102.0(8) . . . . ?
C6 C1 C7 C8 74.9(8) . . . . ?
Ru1 C1 C7 C8 166.3(6) . . . . ?
C13 N1 C11 C12 -101.5(10) . . . . ?
P1 N1 C11 C12 112.5(8) . . . . ?
C11 N1 C13 C14 69.9(10) . . . . ?
P1 N1 C13 C14 -143.1(8) . . . . ?
C17 N2 C15 C16 61.5(9) . . . . ?
P1 N2 C15 C16 -138.2(6) . . . . ?
C15 N2 C17 C18 60.5(10) . . . . ?
P1 N2 C17 C18 -99.5(9) . . . . ?



# END of CIF
####################################################################### 
# 
# 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_shelx_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 2386112'
loop_
_audit_author_name
_audit_author_address
'Lukasz Ponikiewski'
;Gdansk University of Technology
Poland
;
_audit_update_record             
;
2024-09-23 deposited with the CCDC.	2024-11-13 downloaded from the CCDC.
;

_audit_creation_date             2021-04-01T09:25:10-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_moiety         'C42 H60 N4 P4'
_chemical_formula_sum            'C42 H60 N4 P4'
_chemical_formula_weight         744.82

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_Int_Tables_number      15
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   17.1259(16)
_cell_length_b                   10.8384(7)
_cell_length_c                   23.062(2)
_cell_angle_alpha                90
_cell_angle_beta                 106.613(8)
_cell_angle_gamma                90
_cell_volume                     4102.0(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    5682
_cell_measurement_theta_min      2.29
_cell_measurement_theta_max      27.80
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.1
_exptl_crystal_density_diffrn    1.206
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1600

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.218
_exptl_absorpt_correction_type   none
_shelx_estimated_absorpt_T_min   0.97
_shelx_estimated_absorpt_T_max   0.978

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_standards_number         0
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_type            'STOE Imaging Plate'
_diffrn_detector_area_resol_mean 6.67
_diffrn_source                   'GeniX Mo, 0.05 x 0.05 mm2 microfocus'
_diffrn_source_type              ?
_diffrn_source_target            ?
_diffrn_source_voltage           50
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_radiation_monochromator  'parabolic x-ray mirror'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_collimation    '0.6 mm diameter'
_diffrn_measurement_method       'rotation method, ω scans'
_diffrn_measurement_details      
; 148 frames, detector distance = 100 mm
;
_diffrn_reflns_av_R_equivalents  0.1029
_diffrn_reflns_av_unetI/netI     0.1184
_diffrn_reflns_number            10355
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.295
_diffrn_reflns_theta_max         26.994
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.995
_reflns_Friedel_coverage         0
_reflns_number_total             4450
_reflns_number_gt                2405
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#
_computing_data_collection       
;
X-Area WinXpose 2.0.22.0 (STOE, 2016)
;
_computing_cell_refinement       
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
;
_computing_data_reduction        
;
X-Area Integrate 1.72.0.0 (STOE, 2018)
X-Area X-Red32 1.63.4.0 (STOE, 2017) 
;
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1985P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         4450
_refine_ls_number_parameters     231
_refine_ls_number_restraints     0
_refine_ls_number_constraints    0
_refine_ls_R_factor_all          0.179
_refine_ls_R_factor_gt           0.1031
_refine_ls_wR_factor_ref         0.3186
_refine_ls_wR_factor_gt          0.2545
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_restrained_S_all      1.012
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         1.107
_refine_diff_density_min         -0.715
_refine_diff_density_rms         0.121

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.5349(3) 0.2420(4) 0.2822(2) 0.0348(12) Uani 1 1 d . . . . .
C2 C 0.6096(3) 0.1625(5) 0.2851(2) 0.0373(12) Uani 1 1 d . . . . .
C3 C 0.6857(3) 0.2029(5) 0.3189(3) 0.0479(15) Uani 1 1 d . . . . .
H3 H 0.690555 0.279005 0.34007 0.057 Uiso 1 1 calc R U . . .
C4 C 0.7556(4) 0.1329(6) 0.3224(4) 0.0631(19) Uani 1 1 d . . . . .
H4 H 0.806875 0.161408 0.346905 0.076 Uiso 1 1 calc R U . . .
C5 C 0.7521(4) 0.0254(6) 0.2916(3) 0.0592(18) Uani 1 1 d . . . . .
H5 H 0.800183 -0.019697 0.29311 0.071 Uiso 1 1 calc R U . . .
C6 C 0.6762(4) -0.0170(5) 0.2578(3) 0.0506(16) Uani 1 1 d . . . . .
H6 H 0.672083 -0.09202 0.235902 0.061 Uiso 1 1 calc R U . . .
C7 C 0.6065(4) 0.0492(5) 0.2559(3) 0.0429(13) Uani 1 1 d . . . . .
H7 H 0.555007 0.01652 0.234088 0.051 Uiso 1 1 calc R U . . .
C8 C 0.5015(3) 0.2105(5) 0.3364(2) 0.0361(12) Uani 1 1 d . . . . .
C9 C 0.5453(3) 0.1396(5) 0.3844(3) 0.0404(13) Uani 1 1 d . . . . .
H9 H 0.598207 0.111659 0.385279 0.048 Uiso 1 1 calc R U . . .
C10 C 0.5138(4) 0.1087(5) 0.4311(3) 0.0470(14) Uani 1 1 d . . . . .
H10 H 0.544861 0.058346 0.463169 0.056 Uiso 1 1 calc R U . . .
C11 C 0.4374(4) 0.1497(5) 0.4321(3) 0.0475(15) Uani 1 1 d . . . . .
H11 H 0.415922 0.128422 0.464503 0.057 Uiso 1 1 calc R U . . .
C12 C 0.3937(4) 0.2217(5) 0.3851(3) 0.0439(14) Uani 1 1 d . . . . .
H12 H 0.341038 0.249988 0.384687 0.053 Uiso 1 1 calc R U . . .
C13 C 0.4254(3) 0.2538(5) 0.3383(3) 0.0401(13) Uani 1 1 d . . . . .
H13 H 0.394833 0.306184 0.306974 0.048 Uiso 1 1 calc R U . . .
C14 C 0.7038(3) 0.4809(5) 0.4183(3) 0.0425(13) Uani 1 1 d . . . . .
H14A H 0.717979 0.564592 0.435191 0.051 Uiso 1 1 calc R U . . .
H14B H 0.70755 0.481201 0.37629 0.051 Uiso 1 1 calc R U . . .
C15 C 0.7656(4) 0.3897(6) 0.4553(3) 0.0554(16) Uani 1 1 d . . . . .
H15A H 0.769061 0.39881 0.498259 0.083 Uiso 1 1 calc R U . . .
H15B H 0.819041 0.40598 0.449381 0.083 Uiso 1 1 calc R U . . .
H15C H 0.748446 0.305466 0.442155 0.083 Uiso 1 1 calc R U . . .
C16 C 0.6062(4) 0.4300(5) 0.4761(3) 0.0457(14) Uani 1 1 d . . . . .
H16A H 0.639782 0.358313 0.494943 0.055 Uiso 1 1 calc R U . . .
H16B H 0.54836 0.407363 0.469706 0.055 Uiso 1 1 calc R U . . .
C17 C 0.6265(4) 0.5379(6) 0.5200(3) 0.0558(16) Uani 1 1 d . . . . .
H17A H 0.684456 0.558189 0.528722 0.084 Uiso 1 1 calc R U . . .
H17B H 0.614389 0.515441 0.557728 0.084 Uiso 1 1 calc R U . . .
H17C H 0.593666 0.609684 0.501985 0.084 Uiso 1 1 calc R U . . .
C18 C 0.6141(3) 0.7148(5) 0.3325(3) 0.0435(13) Uani 1 1 d . . . . .
H18A H 0.594877 0.759919 0.29366 0.052 Uiso 1 1 calc R U . . .
H18B H 0.654184 0.652355 0.328086 0.052 Uiso 1 1 calc R U . . .
C19 C 0.6559(4) 0.8052(5) 0.3822(3) 0.0487(15) Uani 1 1 d . . . . .
H19A H 0.61589 0.864979 0.388077 0.073 Uiso 1 1 calc R U . . .
H19B H 0.699215 0.848734 0.370537 0.073 Uiso 1 1 calc R U . . .
H19C H 0.679391 0.759988 0.419964 0.073 Uiso 1 1 calc R U . . .
C20 C 0.4744(4) 0.7319(5) 0.3414(3) 0.0457(14) Uani 1 1 d . . . . .
H20A H 0.424227 0.688662 0.318247 0.055 Uiso 1 1 calc R U . . .
H20B H 0.479678 0.807341 0.318538 0.055 Uiso 1 1 calc R U . . .
C21 C 0.4650(4) 0.7689(6) 0.4010(3) 0.0586(17) Uani 1 1 d . . . . .
H21A H 0.455999 0.69538 0.422922 0.088 Uiso 1 1 calc R U . . .
H21B H 0.418362 0.824743 0.394886 0.088 Uiso 1 1 calc R U . . .
H21C H 0.514598 0.811121 0.424513 0.088 Uiso 1 1 calc R U . . .
N2 N 0.5445(3) 0.6518(4) 0.3448(2) 0.0424(11) Uani 1 1 d . . . . .
N1 N 0.6195(3) 0.4536(4) 0.4171(2) 0.0410(11) Uani 1 1 d . . . . .
P1 P 0.56203(8) 0.41613(12) 0.28148(6) 0.0351(4) Uani 1 1 d . . . A 1
P2 P 0.53562(8) 0.50096(12) 0.36217(7) 0.0364(4) Uani 1 1 d . . . A 1



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.528(7) . ?
C1 C8 1.555(7) . ?
C1 C1 1.619(10) 2_655 ?
C1 P1 1.945(5) . ?
C2 C3 1.384(8) . ?
C2 C7 1.394(8) . ?
C3 C4 1.400(8) . ?
C3 H3 0.95 . ?
C4 C5 1.356(10) . ?
C4 H4 0.95 . ?
C5 C6 1.389(9) . ?
C5 H5 0.95 . ?
C6 C7 1.382(8) . ?
C6 H6 0.95 . ?
C7 H7 0.95 . ?
C8 C9 1.380(8) . ?
C8 C13 1.398(7) . ?
C9 C10 1.376(8) . ?
C9 H9 0.95 . ?
C10 C11 1.389(8) . ?
C10 H10 0.95 . ?
C11 C12 1.371(8) . ?
C11 H11 0.95 . ?
C12 C13 1.383(7) . ?
C12 H12 0.95 . ?
C13 H13 0.95 . ?
C14 N1 1.465(7) . ?
C14 C15 1.519(8) . ?
C14 H14A 0.99 . ?
C14 H14B 0.99 . ?
C15 H15A 0.98 . ?
C15 H15B 0.98 . ?
C15 H15C 0.98 . ?
C16 N1 1.465(7) . ?
C16 C17 1.521(8) . ?
C16 H16A 0.99 . ?
C16 H16B 0.99 . ?
C17 H17A 0.98 . ?
C17 H17B 0.98 . ?
C17 H17C 0.98 . ?
C18 N2 1.470(7) . ?
C18 C19 1.522(8) . ?
C18 H18A 0.99 . ?
C18 H18B 0.99 . ?
C19 H19A 0.98 . ?
C19 H19B 0.98 . ?
C19 H19C 0.98 . ?
C20 N2 1.466(7) . ?
C20 C21 1.484(8) . ?
C20 H20A 0.99 . ?
C20 H20B 0.99 . ?
C21 H21A 0.98 . ?
C21 H21B 0.98 . ?
C21 H21C 0.98 . ?
N2 P2 1.700(5) . ?
N1 P2 1.701(5) . ?
P1 P1 2.204(3) 2_655 ?
P1 P2 2.2346(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
C2 C1 C8 109.7(4) . . ?
C2 C1 C1 115.4(4) . 2_655 ?
C8 C1 C1 113.2(5) . 2_655 ?
C2 C1 P1 110.4(3) . . ?
C8 C1 P1 111.3(3) . . ?
C1 C1 P1 96.18(18) 2_655 . ?
C3 C2 C7 116.8(5) . . ?
C3 C2 C1 119.2(5) . . ?
C7 C2 C1 124.0(5) . . ?
C2 C3 C4 120.8(6) . . ?
C2 C3 H3 119.6 . . ?
C4 C3 H3 119.6 . . ?
C5 C4 C3 121.7(7) . . ?
C5 C4 H4 119.1 . . ?
C3 C4 H4 119.1 . . ?
C4 C5 C6 118.2(6) . . ?
C4 C5 H5 120.9 . . ?
C6 C5 H5 120.9 . . ?
C7 C6 C5 120.5(6) . . ?
C7 C6 H6 119.7 . . ?
C5 C6 H6 119.7 . . ?
C6 C7 C2 121.9(6) . . ?
C6 C7 H7 119.1 . . ?
C2 C7 H7 119.1 . . ?
C9 C8 C13 117.4(5) . . ?
C9 C8 C1 121.8(4) . . ?
C13 C8 C1 120.9(5) . . ?
C10 C9 C8 121.2(5) . . ?
C10 C9 H9 119.4 . . ?
C8 C9 H9 119.4 . . ?
C9 C10 C11 121.2(6) . . ?
C9 C10 H10 119.4 . . ?
C11 C10 H10 119.4 . . ?
C12 C11 C10 118.2(5) . . ?
C12 C11 H11 120.9 . . ?
C10 C11 H11 120.9 . . ?
C11 C12 C13 120.9(5) . . ?
C11 C12 H12 119.6 . . ?
C13 C12 H12 119.6 . . ?
C12 C13 C8 121.1(5) . . ?
C12 C13 H13 119.4 . . ?
C8 C13 H13 119.4 . . ?
N1 C14 C15 113.8(5) . . ?
N1 C14 H14A 108.8 . . ?
C15 C14 H14A 108.8 . . ?
N1 C14 H14B 108.8 . . ?
C15 C14 H14B 108.8 . . ?
H14A C14 H14B 107.7 . . ?
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 . . ?
N1 C16 C17 114.7(5) . . ?
N1 C16 H16A 108.6 . . ?
C17 C16 H16A 108.6 . . ?
N1 C16 H16B 108.6 . . ?
C17 C16 H16B 108.6 . . ?
H16A C16 H16B 107.6 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N2 C18 C19 112.7(5) . . ?
N2 C18 H18A 109.1 . . ?
C19 C18 H18A 109.1 . . ?
N2 C18 H18B 109.1 . . ?
C19 C18 H18B 109.1 . . ?
H18A C18 H18B 107.8 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N2 C20 C21 114.4(5) . . ?
N2 C20 H20A 108.7 . . ?
C21 C20 H20A 108.7 . . ?
N2 C20 H20B 108.7 . . ?
C21 C20 H20B 108.7 . . ?
H20A C20 H20B 107.6 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 N2 C18 114.3(4) . . ?
C20 N2 P2 117.1(4) . . ?
C18 N2 P2 128.6(4) . . ?
C14 N1 C16 115.6(5) . . ?
C14 N1 P2 124.8(4) . . ?
C16 N1 P2 115.0(4) . . ?
C1 P1 P1 79.51(16) . 2_655 ?
C1 P1 P2 106.64(16) . . ?
P1 P1 P2 99.34(8) 2_655 . ?
N2 P2 N1 110.6(2) . . ?
N2 P2 P1 98.43(17) . . ?
N1 P2 P1 99.64(16) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C8 C1 C2 C3 -86.9(6) . . . . ?
C1 C1 C2 C3 143.9(5) 2_655 . . . ?
P1 C1 C2 C3 36.2(6) . . . . ?
C8 C1 C2 C7 92.5(6) . . . . ?
C1 C1 C2 C7 -36.8(6) 2_655 . . . ?
P1 C1 C2 C7 -144.4(4) . . . . ?
C7 C2 C3 C4 0.9(8) . . . . ?
C1 C2 C3 C4 -179.6(5) . . . . ?
C2 C3 C4 C5 1.9(10) . . . . ?
C3 C4 C5 C6 -2.4(10) . . . . ?
C4 C5 C6 C7 0.0(10) . . . . ?
C5 C6 C7 C2 2.9(9) . . . . ?
C3 C2 C7 C6 -3.3(8) . . . . ?
C1 C2 C7 C6 177.3(5) . . . . ?
C2 C1 C8 C9 11.8(7) . . . . ?
C1 C1 C8 C9 142.3(4) 2_655 . . . ?
P1 C1 C8 C9 -110.7(5) . . . . ?
C2 C1 C8 C13 -168.4(5) . . . . ?
C1 C1 C8 C13 -37.9(5) 2_655 . . . ?
P1 C1 C8 C13 69.2(6) . . . . ?
C13 C8 C9 C10 2.6(8) . . . . ?
C1 C8 C9 C10 -177.6(5) . . . . ?
C8 C9 C10 C11 -1.3(9) . . . . ?
C9 C10 C11 C12 0.3(9) . . . . ?
C10 C11 C12 C13 -0.7(9) . . . . ?
C11 C12 C13 C8 2.2(9) . . . . ?
C9 C8 C13 C12 -3.0(8) . . . . ?
C1 C8 C13 C12 177.1(5) . . . . ?
C21 C20 N2 C18 -103.4(6) . . . . ?
C21 C20 N2 P2 76.7(6) . . . . ?
C19 C18 N2 C20 69.3(6) . . . . ?
C19 C18 N2 P2 -110.7(5) . . . . ?
C15 C14 N1 C16 49.0(7) . . . . ?
C15 C14 N1 P2 -156.4(4) . . . . ?
C17 C16 N1 C14 62.1(7) . . . . ?
C17 C16 N1 P2 -95.0(6) . . . . ?
C20 N2 P2 N1 -132.6(4) . . . . ?
C18 N2 P2 N1 47.5(5) . . . . ?
C20 N2 P2 P1 123.8(4) . . . . ?
C18 N2 P2 P1 -56.2(5) . . . . ?
C14 N1 P2 N2 -44.9(5) . . . . ?
C16 N1 P2 N2 109.7(4) . . . . ?
C14 N1 P2 P1 57.9(4) . . . . ?
C16 N1 P2 P1 -147.4(4) . . . . ?



# END of CIF
####################################################################### 
# 
# 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_shelx_CCDC3
_database_code_depnum_ccdc_archive 'CCDC 2386111'
loop_
_audit_author_name
_audit_author_address
'Lukasz Ponikiewski'
;Gdansk University of Technology
Poland
;
_audit_update_record             
;
2024-09-23 deposited with the CCDC.	2024-11-13 downloaded from the CCDC.
;

_audit_creation_date             2024-05-16T11:30:48-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_moiety         'C30 H74 Li2 N4 O2 P4 Si2'
_chemical_formula_sum            'C30 H74 Li2 N4 O2 P4 Si2'
_chemical_formula_weight         716.87

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_Int_Tables_number      15
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   19.6660(9)
_cell_length_b                   9.8948(3)
_cell_length_c                   23.2825(11)
_cell_angle_alpha                90
_cell_angle_beta                 104.656(4)
_cell_angle_gamma                90
_cell_volume                     4383.2(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9384
_cell_measurement_theta_min      2.32
_cell_measurement_theta_max      29.54
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.16
_exptl_crystal_density_diffrn    1.086
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1568

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.255
_exptl_absorpt_correction_type   none
_shelx_estimated_absorpt_T_min   0.958
_shelx_estimated_absorpt_T_max   0.96

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_type            'STOE Imaging Plate'
_diffrn_detector_area_resol_mean 6.67
_diffrn_source                   'GeniX Mo, 0.05 x 0.05 mm2 microfocus'
_diffrn_source_target            ?
_diffrn_source_voltage           50
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_radiation_monochromator  'parabolic x-ray mirror'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_collimation    '0.6 mm diameter'
_diffrn_measurement_method       'rotation method, ω scans'
_diffrn_measurement_details      
; 175 frames, detector distance = 100 mm
;
_diffrn_reflns_av_R_equivalents  0.0406
_diffrn_reflns_av_unetI/netI     0.0653
_diffrn_reflns_number            12015
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         2.32
_diffrn_reflns_theta_max         27.994
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.99
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.99
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.99
_reflns_Friedel_coverage         0
_reflns_number_total             5238
_reflns_number_gt                3321
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       
;
X-Area WinXpose 2.0.22.0 (STOE, 2016)
;
_computing_cell_refinement       
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
;
_computing_data_reduction        
;
X-Area Integrate 1.72.0.0 (STOE, 2018)
X-Area X-Red32 1.63.4.0 (STOE, 2017) 
;
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0548P)²+0.0593P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         5238
_refine_ls_number_parameters     206
_refine_ls_number_restraints     0
_refine_ls_number_constraints    0
_refine_ls_R_factor_all          0.0907
_refine_ls_R_factor_gt           0.0444
_refine_ls_wR_factor_ref         0.1113
_refine_ls_wR_factor_gt          0.0976
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_restrained_S_all      1.027
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.261
_refine_diff_density_min         -0.232
_refine_diff_density_rms         0.055

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li -0.0003 0.0001 '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 0.006 '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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.35049(13) 1.0164(2) 0.36353(10) 0.0393(5) Uani 1 1 d . . . . .
H1A H 0.40237 1.022971 0.372884 0.047 Uiso 1 1 calc R U . . .
H1B H 0.336367 1.026839 0.401196 0.047 Uiso 1 1 calc R U . . .
C2 C 0.31951(18) 1.1306(3) 0.32283(13) 0.0662(9) Uani 1 1 d . . . . .
H2A H 0.335265 1.124166 0.286218 0.099 Uiso 1 1 calc R U . . .
H2B H 0.334921 1.216904 0.342457 0.099 Uiso 1 1 calc R U . . .
H2C H 0.268104 1.125158 0.313245 0.099 Uiso 1 1 calc R U . . .
C3 C 0.35119(11) 0.8466(3) 0.28545(9) 0.0371(5) Uani 1 1 d . . . . .
H3A H 0.335515 0.91884 0.255594 0.045 Uiso 1 1 calc R U . . .
H3B H 0.326874 0.762287 0.268939 0.045 Uiso 1 1 calc R U . . .
C4 C 0.42967(13) 0.8266(3) 0.29467(11) 0.0563(8) Uani 1 1 d . . . . .
H4A H 0.454314 0.910439 0.309721 0.084 Uiso 1 1 calc R U . . .
H4B H 0.439681 0.802537 0.256807 0.084 Uiso 1 1 calc R U . . .
H4C H 0.44572 0.753774 0.323448 0.084 Uiso 1 1 calc R U . . .
C5 C 0.38786(11) 0.7566(2) 0.47588(9) 0.0332(5) Uani 1 1 d . . . . .
H5A H 0.395772 0.701741 0.512541 0.04 Uiso 1 1 calc R U . . .
H5B H 0.361748 0.838522 0.482114 0.04 Uiso 1 1 calc R U . . .
C6 C 0.45912(11) 0.8007(2) 0.46832(10) 0.0405(6) Uani 1 1 d . . . . .
H6A H 0.487924 0.720839 0.466456 0.061 Uiso 1 1 calc R U . . .
H6B H 0.482686 0.857111 0.502109 0.061 Uiso 1 1 calc R U . . .
H6C H 0.452676 0.852763 0.43151 0.061 Uiso 1 1 calc R U . . .
C7 C 0.37912(11) 0.5645(2) 0.40632(10) 0.0350(5) Uani 1 1 d . . . . .
H7A H 0.42143 0.599385 0.395538 0.042 Uiso 1 1 calc R U . . .
H7B H 0.347746 0.524708 0.370212 0.042 Uiso 1 1 calc R U . . .
C8 C 0.40087(12) 0.4553(2) 0.45299(11) 0.0413(6) Uani 1 1 d . . . . .
H8A H 0.435054 0.492315 0.487575 0.062 Uiso 1 1 calc R U . . .
H8B H 0.422197 0.379937 0.436524 0.062 Uiso 1 1 calc R U . . .
H8C H 0.359442 0.423063 0.46505 0.062 Uiso 1 1 calc R U . . .
C9 C 0.13275(13) 0.9173(3) 0.27409(9) 0.0465(6) Uani 1 1 d . . . . .
H9A H 0.090563 0.895839 0.242712 0.07 Uiso 1 1 calc R U . . .
H9B H 0.173901 0.876138 0.264587 0.07 Uiso 1 1 calc R U . . .
H9C H 0.138915 1.01556 0.277016 0.07 Uiso 1 1 calc R U . . .
C10 C 0.05168(12) 0.9499(3) 0.36735(10) 0.0437(6) Uani 1 1 d . . . . .
H10A H 0.065852 1.044961 0.372439 0.066 Uiso 1 1 calc R U . . .
H10B H 0.043843 0.915124 0.404564 0.066 Uiso 1 1 calc R U . . .
H10C H 0.008176 0.942125 0.335758 0.066 Uiso 1 1 calc R U . . .
C11 C 0.08921(14) 0.6715(3) 0.33303(12) 0.0531(7) Uani 1 1 d . . . . .
H11A H 0.044695 0.671805 0.302333 0.08 Uiso 1 1 calc R U . . .
H11B H 0.081634 0.633662 0.369814 0.08 Uiso 1 1 calc R U . . .
H11C H 0.123686 0.616246 0.319735 0.08 Uiso 1 1 calc R U . . .
C12 C 0.21508(13) 0.3875(2) 0.38680(9) 0.0405(6) Uani 1 1 d . . . . .
H12A H 0.258431 0.332705 0.392844 0.049 Uiso 1 1 calc R U . . .
H12B H 0.213598 0.452314 0.354102 0.049 Uiso 1 1 calc R U . . .
C14 C 0.15114(14) 0.2982(3) 0.37260(11) 0.0465(6) Uani 1 1 d . . . . .
H14A H 0.158546 0.2171 0.350022 0.056 Uiso 1 1 calc R U . . .
H14B H 0.109129 0.347533 0.349845 0.056 Uiso 1 1 calc R U . . .
C15 C 0.14458(14) 0.2612(3) 0.43424(11) 0.0449(6) Uani 1 1 d . . . . .
H15A H 0.095901 0.234274 0.433553 0.054 Uiso 1 1 calc R U . . .
H15B H 0.17706 0.186935 0.45152 0.054 Uiso 1 1 calc R U . . .
C16 C 0.16458(13) 0.3901(2) 0.46790(10) 0.0411(6) Uani 1 1 d . . . . .
H16A H 0.122502 0.446862 0.465544 0.049 Uiso 1 1 calc R U . . .
H16B H 0.186987 0.370899 0.510191 0.049 Uiso 1 1 calc R U . . .
Li1 Li 0.25842(18) 0.6269(4) 0.46640(15) 0.0308(8) Uani 1 1 d . . . . .
N1 N 0.32941(9) 0.88253(18) 0.33932(7) 0.0314(4) Uani 1 1 d . . . . .
N2 N 0.34246(8) 0.67804(18) 0.42693(7) 0.0272(4) Uani 1 1 d . . . . .
O1 O 0.21330(8) 0.45821(15) 0.44061(6) 0.0340(4) Uani 1 1 d . . . . .
P2 P 0.28454(3) 0.76326(6) 0.36727(2) 0.02661(14) Uani 1 1 d . . . . .
P1 P 0.22175(3) 0.86973(6) 0.41766(2) 0.02688(14) Uani 1 1 d . . . . .
Si1 Si 0.12292(3) 0.84904(6) 0.34680(3) 0.03250(16) Uani 1 1 d . . . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.458(3) . ?
C1 C2 1.501(3) . ?
C1 H1A 0.99 . ?
C1 H1B 0.99 . ?
C2 H2A 0.98 . ?
C2 H2B 0.98 . ?
C2 H2C 0.98 . ?
C3 N1 1.468(2) . ?
C3 C4 1.516(3) . ?
C3 H3A 0.99 . ?
C3 H3B 0.99 . ?
C4 H4A 0.98 . ?
C4 H4B 0.98 . ?
C4 H4C 0.98 . ?
C5 N2 1.478(3) . ?
C5 C6 1.520(3) . ?
C5 H5A 0.99 . ?
C5 H5B 0.99 . ?
C6 H6A 0.98 . ?
C6 H6B 0.98 . ?
C6 H6C 0.98 . ?
C7 N2 1.479(3) . ?
C7 C8 1.515(3) . ?
C7 H7A 0.99 . ?
C7 H7B 0.99 . ?
C8 H8A 0.98 . ?
C8 H8B 0.98 . ?
C8 H8C 0.98 . ?
C9 Si1 1.878(2) . ?
C9 H9A 0.98 . ?
C9 H9B 0.98 . ?
C9 H9C 0.98 . ?
C10 Si1 1.878(2) . ?
C10 H10A 0.98 . ?
C10 H10B 0.98 . ?
C10 H10C 0.98 . ?
C11 Si1 1.877(3) . ?
C11 H11A 0.98 . ?
C11 H11B 0.98 . ?
C11 H11C 0.98 . ?
C12 O1 1.443(2) . ?
C12 C14 1.504(3) . ?
C12 H12A 0.99 . ?
C12 H12B 0.99 . ?
C14 C15 1.518(3) . ?
C14 H14A 0.99 . ?
C14 H14B 0.99 . ?
C15 C16 1.496(3) . ?
C15 H15A 0.99 . ?
C15 H15B 0.99 . ?
C16 O1 1.444(2) . ?
C16 H16A 0.99 . ?
C16 H16B 0.99 . ?
Li1 O1 1.914(4) . ?
Li1 N2 2.145(4) . ?
Li1 P1 2.628(3) 7_566 ?
Li1 P1 2.677(4) . ?
Li1 P2 2.830(3) . ?
Li1 Li1 2.959(7) 7_566 ?
N1 P2 1.6987(18) . ?
N2 P2 1.7712(17) . ?
P2 P1 2.1781(7) . ?
P1 Si1 2.2178(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
N1 C1 C2 114.2(2) . . ?
N1 C1 H1A 108.7 . . ?
C2 C1 H1A 108.7 . . ?
N1 C1 H1B 108.7 . . ?
C2 C1 H1B 108.7 . . ?
H1A C1 H1B 107.6 . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N1 C3 C4 114.66(19) . . ?
N1 C3 H3A 108.6 . . ?
C4 C3 H3A 108.6 . . ?
N1 C3 H3B 108.6 . . ?
C4 C3 H3B 108.6 . . ?
H3A C3 H3B 107.6 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N2 C5 C6 117.17(18) . . ?
N2 C5 H5A 108 . . ?
C6 C5 H5A 108 . . ?
N2 C5 H5B 108 . . ?
C6 C5 H5B 108 . . ?
H5A C5 H5B 107.2 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N2 C7 C8 112.42(17) . . ?
N2 C7 H7A 109.1 . . ?
C8 C7 H7A 109.1 . . ?
N2 C7 H7B 109.1 . . ?
C8 C7 H7B 109.1 . . ?
H7A C7 H7B 107.9 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
Si1 C9 H9A 109.5 . . ?
Si1 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
Si1 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
Si1 C10 H10A 109.5 . . ?
Si1 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
Si1 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
Si1 C11 H11A 109.5 . . ?
Si1 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
Si1 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
O1 C12 C14 105.85(17) . . ?
O1 C12 H12A 110.6 . . ?
C14 C12 H12A 110.6 . . ?
O1 C12 H12B 110.6 . . ?
C14 C12 H12B 110.6 . . ?
H12A C12 H12B 108.7 . . ?
C12 C14 C15 101.55(19) . . ?
C12 C14 H14A 111.5 . . ?
C15 C14 H14A 111.5 . . ?
C12 C14 H14B 111.5 . . ?
C15 C14 H14B 111.5 . . ?
H14A C14 H14B 109.3 . . ?
C16 C15 C14 102.47(19) . . ?
C16 C15 H15A 111.3 . . ?
C14 C15 H15A 111.3 . . ?
C16 C15 H15B 111.3 . . ?
C14 C15 H15B 111.3 . . ?
H15A C15 H15B 109.2 . . ?
O1 C16 C15 106.44(17) . . ?
O1 C16 H16A 110.4 . . ?
C15 C16 H16A 110.4 . . ?
O1 C16 H16B 110.4 . . ?
C15 C16 H16B 110.4 . . ?
H16A C16 H16B 108.6 . . ?
O1 Li1 N2 114.68(17) . . ?
O1 Li1 P1 105.66(15) . 7_566 ?
N2 Li1 P1 120.45(16) . 7_566 ?
O1 Li1 P1 126.58(17) . . ?
N2 Li1 P1 76.15(11) . . ?
P1 Li1 P1 112.21(13) 7_566 . ?
O1 Li1 P2 108.98(14) . . ?
N2 Li1 P2 38.71(7) . . ?
P1 Li1 P2 145.19(15) 7_566 . ?
P1 Li1 P2 46.49(6) . . ?
O1 Li1 Li1 141.2(2) . 7_566 ?
N2 Li1 Li1 103.51(19) . 7_566 ?
P1 Li1 Li1 56.90(11) 7_566 7_566 ?
P1 Li1 Li1 55.31(11) . 7_566 ?
P2 Li1 Li1 96.10(16) . 7_566 ?
C1 N1 C3 115.73(18) . . ?
C1 N1 P2 127.41(14) . . ?
C3 N1 P2 116.84(15) . . ?
C5 N2 C7 113.61(16) . . ?
C5 N2 P2 119.83(14) . . ?
C7 N2 P2 112.13(13) . . ?
C5 N2 Li1 100.04(15) . . ?
C7 N2 Li1 116.84(16) . . ?
P2 N2 Li1 92.06(12) . . ?
C12 O1 C16 108.69(16) . . ?
C12 O1 Li1 125.73(16) . . ?
C16 O1 Li1 125.13(16) . . ?
N1 P2 N2 109.75(9) . . ?
N1 P2 P1 106.89(7) . . ?
N2 P2 P1 98.49(6) . . ?
N1 P2 Li1 149.62(10) . . ?
N2 P2 Li1 49.23(9) . . ?
P1 P2 Li1 63.05(7) . . ?
P2 P1 Si1 93.68(3) . . ?
P2 P1 Li1 127.04(8) . 7_566 ?
Si1 P1 Li1 129.76(8) . 7_566 ?
P2 P1 Li1 70.46(7) . . ?
Si1 P1 Li1 108.89(8) . . ?
Li1 P1 Li1 67.79(13) 7_566 . ?
C11 Si1 C9 107.17(13) . . ?
C11 Si1 C10 106.67(12) . . ?
C9 Si1 C10 106.99(11) . . ?
C11 Si1 P1 114.76(8) . . ?
C9 Si1 P1 111.52(8) . . ?
C10 Si1 P1 109.35(8) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C12 C14 C15 -33.6(3) . . . . ?
C12 C14 C15 C16 38.0(3) . . . . ?
C14 C15 C16 O1 -29.6(3) . . . . ?
C2 C1 N1 C3 62.8(3) . . . . ?
C2 C1 N1 P2 -118.8(2) . . . . ?
C4 C3 N1 C1 68.8(3) . . . . ?
C4 C3 N1 P2 -109.8(2) . . . . ?
C6 C5 N2 C7 48.4(2) . . . . ?
C6 C5 N2 P2 -88.1(2) . . . . ?
C6 C5 N2 Li1 173.68(19) . . . . ?
C8 C7 N2 C5 66.6(2) . . . . ?
C8 C7 N2 P2 -153.60(16) . . . . ?
C8 C7 N2 Li1 -49.2(2) . . . . ?
C14 C12 O1 C16 15.9(3) . . . . ?
C14 C12 O1 Li1 -156.7(2) . . . . ?
C15 C16 O1 C12 8.9(3) . . . . ?
C15 C16 O1 Li1 -178.4(2) . . . . ?
C1 N1 P2 N2 -79.25(19) . . . . ?
C3 N1 P2 N2 99.15(16) . . . . ?
C1 N1 P2 P1 26.59(19) . . . . ?
C3 N1 P2 P1 -155.02(13) . . . . ?
C1 N1 P2 Li1 -38.7(3) . . . . ?
C3 N1 P2 Li1 139.73(19) . . . . ?
C5 N2 P2 N1 51.44(16) . . . . ?
C7 N2 P2 N1 -85.59(15) . . . . ?
Li1 N2 P2 N1 154.25(12) . . . . ?
C5 N2 P2 P1 -60.01(14) . . . . ?
C7 N2 P2 P1 162.96(13) . . . . ?
Li1 N2 P2 P1 42.80(11) . . . . ?
C5 N2 P2 Li1 -102.81(17) . . . . ?
C7 N2 P2 Li1 120.15(18) . . . . ?

# END of CIF
####################################################################### 
# 
# 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_shelx_CCDC4
_database_code_depnum_ccdc_archive 'CCDC 2386114'
loop_
_audit_author_name
_audit_author_address
'Lukasz Ponikiewski'
;Gdansk University of Technology
Poland
;
_audit_update_record             
;
2024-09-23 deposited with the CCDC.	2024-11-13 downloaded from the CCDC.
;

_audit_creation_date             2024-06-19T10:55:39-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_moiety         'C33 H36 P2'
_chemical_formula_sum            'C33 H36 P2'
_chemical_formula_weight         494.56

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P b c n'
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_Int_Tables_number      60
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   9.8631(4)
_cell_length_b                   20.3925(11)
_cell_length_c                   28.0508(14)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5641.9(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    13822
_cell_measurement_theta_min      2.41
_cell_measurement_theta_max      29.39
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_exptl_crystal_density_diffrn    1.164
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2112

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.173
_shelx_estimated_absorpt_T_min   0.974
_shelx_estimated_absorpt_T_max   0.976
_exptl_absorpt_correction_type   none

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_type            'STOE Imaging Plate'
_diffrn_detector_area_resol_mean 6.67
_diffrn_source                   'GeniX Mo, 0.05 x 0.05 mm2 microfocus'
_diffrn_source_type              ?
_diffrn_source_target            ?
_diffrn_source_voltage           50
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_radiation_monochromator  'parabolic x-ray mirror'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_collimation    '0.6 mm diameter'
_diffrn_measurement_method       'rotation method, ω scans'
_diffrn_measurement_details      
; 197 frames, detector distance = 100 mm
;
_diffrn_reflns_av_R_equivalents  0.1007
_diffrn_reflns_av_unetI/netI     0.0888
_diffrn_reflns_number            21111
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_theta_min         2.406
_diffrn_reflns_theta_max         26.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.99
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.99
_diffrn_reflns_point_group_measured_fraction_max 0.991
_reflns_Friedel_coverage         0
_reflns_number_total             6100
_reflns_number_gt                3550
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       
;
X-Area WinXpose 2.0.22.0 (STOE, 2016)
;
_computing_cell_refinement       
;
X-Area Recipe 1.34.0.0 (STOE, 2019)
;
_computing_data_reduction        
;
X-Area Integrate 1.77.0.0 (STOE, 2019)
X-Area LANA 1.77.1.0 (STOE, 2019)
;
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0036P)²+21.9318P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         6100
_refine_ls_number_parameters     323
_refine_ls_number_restraints     0
_refine_ls_number_constraints    0
_refine_ls_R_factor_all          0.188
_refine_ls_R_factor_gt           0.0998
_refine_ls_wR_factor_ref         0.1932
_refine_ls_wR_factor_gt          0.1532
_refine_ls_goodness_of_fit_ref   1.209
_refine_ls_restrained_S_all      1.209
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.361
_refine_diff_density_min         -0.363
_refine_diff_density_rms         0.089

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.7176(5) 0.4344(2) 0.27772(16) 0.0276(10) Uani 1 1 d . . . . .
C2 C 0.7247(5) 0.4704(2) 0.23181(15) 0.0249(10) Uani 1 1 d . . . . .
C3 C 0.6834(5) 0.5361(2) 0.22855(17) 0.0311(11) Uani 1 1 d . . . . .
H3 H 0.656203 0.558556 0.256626 0.037 Uiso 1 1 calc R U . . .
C4 C 0.6814(5) 0.5687(2) 0.18539(16) 0.0302(11) Uani 1 1 d . . . . .
H4 H 0.651847 0.613049 0.184318 0.036 Uiso 1 1 calc R U . . .
C5 C 0.7222(5) 0.5375(2) 0.14297(16) 0.0255(10) Uani 1 1 d . . . . .
C6 C 0.7679(5) 0.4730(2) 0.14681(17) 0.0275(10) Uani 1 1 d . . . . .
H6 H 0.799345 0.451098 0.119037 0.033 Uiso 1 1 calc R U . . .
C7 C 0.7687(5) 0.4400(2) 0.18992(16) 0.0289(11) Uani 1 1 d . . . . .
H7 H 0.799686 0.395884 0.191059 0.035 Uiso 1 1 calc R U . . .
C8 C 0.7164(5) 0.5712(2) 0.09600(16) 0.0267(10) Uani 1 1 d . . . . .
C9 C 0.7291(5) 0.6386(2) 0.09252(18) 0.0320(11) Uani 1 1 d . . . . .
H9 H 0.742855 0.663851 0.120583 0.038 Uiso 1 1 calc R U . . .
C10 C 0.7220(6) 0.6701(3) 0.04850(18) 0.0387(13) Uani 1 1 d . . . . .
H10 H 0.730154 0.716461 0.046776 0.046 Uiso 1 1 calc R U . . .
C11 C 0.7033(6) 0.6341(3) 0.00748(18) 0.0390(13) Uani 1 1 d . . . . .
H11 H 0.699582 0.655387 -0.022632 0.047 Uiso 1 1 calc R U . . .
C12 C 0.6900(6) 0.5671(3) 0.01052(18) 0.0387(13) Uani 1 1 d . . . . .
H12 H 0.675954 0.541965 -0.017584 0.046 Uiso 1 1 calc R U . . .
C13 C 0.6969(5) 0.5360(2) 0.05437(17) 0.0332(12) Uani 1 1 d . . . . .
H13 H 0.687999 0.489635 0.055915 0.04 Uiso 1 1 calc R U . . .
C14 C 0.7370(5) 0.4740(2) 0.32189(16) 0.0266(10) Uani 1 1 d . . . . .
C15 C 0.6296(5) 0.4840(2) 0.35312(17) 0.0288(11) Uani 1 1 d . . . . .
H15 H 0.542799 0.46653 0.345879 0.035 Uiso 1 1 calc R U . . .
C16 C 0.6484(5) 0.5196(2) 0.39486(17) 0.0304(11) Uani 1 1 d . . . . .
H16 H 0.573425 0.526714 0.415466 0.036 Uiso 1 1 calc R U . . .
C17 C 0.7741(5) 0.5449(2) 0.40712(16) 0.0264(10) Uani 1 1 d . . . . .
C18 C 0.8814(5) 0.5356(2) 0.37525(17) 0.0302(11) Uani 1 1 d . . . . .
H18 H 0.968478 0.552747 0.382599 0.036 Uiso 1 1 calc R U . . .
C19 C 0.8616(5) 0.5015(2) 0.33276(18) 0.0319(11) Uani 1 1 d . . . . .
H19 H 0.934728 0.496972 0.310948 0.038 Uiso 1 1 calc R U . . .
C20 C 0.7942(5) 0.5794(2) 0.45322(16) 0.0264(10) Uani 1 1 d . . . . .
C21 C 0.6882(5) 0.6136(2) 0.47424(17) 0.0308(11) Uani 1 1 d . . . . .
H21 H 0.602597 0.614814 0.458754 0.037 Uiso 1 1 calc R U . . .
C22 C 0.7046(6) 0.6459(2) 0.51746(18) 0.0354(12) Uani 1 1 d . . . . .
H22 H 0.631442 0.669793 0.531024 0.043 Uiso 1 1 calc R U . . .
C23 C 0.8293(5) 0.6431(2) 0.54074(19) 0.0363(12) Uani 1 1 d . . . . .
H23 H 0.841213 0.664545 0.570497 0.044 Uiso 1 1 calc R U . . .
C24 C 0.9352(6) 0.6090(2) 0.52048(18) 0.0360(12) Uani 1 1 d . . . . .
H24 H 1.020326 0.60716 0.536263 0.043 Uiso 1 1 calc R U . . .
C25 C 0.9182(5) 0.5775(2) 0.47736(18) 0.0324(12) Uani 1 1 d . . . . .
H25 H 0.992035 0.554022 0.463844 0.039 Uiso 1 1 calc R U . . .
C26 C 0.5602(5) 0.2665(2) 0.35758(17) 0.0326(12) Uani 1 1 d . . . . .
P1 P 0.68450(15) 0.35299(7) 0.27581(5) 0.0345(3) Uani 1 1 d . . . . .
P2 P 0.71483(14) 0.31945(6) 0.35040(5) 0.0318(3) Uani 1 1 d . . . . .
C27 C 0.5314(6) 0.2149(3) 0.3196(2) 0.062(2) Uani 1 1 d . . . A 1
H27A H 0.598237 0.1795 0.322013 0.093 Uiso 1 1 calc R U . A 1
H27B H 0.53724 0.235064 0.287908 0.093 Uiso 1 1 calc R U . A 1
H27C H 0.44019 0.196977 0.324291 0.093 Uiso 1 1 calc R U . A 1
C28 C 0.5668(6) 0.2325(3) 0.40650(19) 0.0435(14) Uani 1 1 d . . . B 1
H28A H 0.48034 0.210519 0.412918 0.065 Uiso 1 1 calc R U . B 1
H28B H 0.584042 0.26533 0.43129 0.065 Uiso 1 1 calc R U . B 1
H28C H 0.6401 0.200096 0.406445 0.065 Uiso 1 1 calc R U . B 1
C29 C 0.4412(6) 0.3148(3) 0.3589(2) 0.0539(17) Uani 1 1 d . . . C 1
H29A H 0.357682 0.291168 0.366888 0.081 Uiso 1 1 calc R U . C 1
H29B H 0.431219 0.335555 0.327582 0.081 Uiso 1 1 calc R U . C 1
H29C H 0.458579 0.348477 0.383026 0.081 Uiso 1 1 calc R U . C 1
C30 C 0.8699(6) 0.2668(3) 0.3405(2) 0.0492(16) Uani 1 1 d . . . D 1
C31 C 0.8620(7) 0.2153(4) 0.3010(4) 0.102(3) Uani 1 1 d . . . D 1
H31A H 0.829806 0.235935 0.271559 0.154 Uiso 1 1 calc R U . D 1
H31B H 0.799065 0.180525 0.310487 0.154 Uiso 1 1 calc R U . D 1
H31C H 0.952223 0.196547 0.295687 0.154 Uiso 1 1 calc R U . D 1
C32 C 0.9036(7) 0.2334(5) 0.3883(3) 0.113(4) Uani 1 1 d . . . D 1
H32A H 0.997028 0.217087 0.387514 0.17 Uiso 1 1 calc R U . D 1
H32B H 0.841281 0.196741 0.393604 0.17 Uiso 1 1 calc R U . D 1
H32C H 0.894042 0.265302 0.414253 0.17 Uiso 1 1 calc R U . D 1
C33 C 0.9835(5) 0.3147(3) 0.3293(2) 0.0489(15) Uani 1 1 d . . . D 1
H33A H 0.986291 0.348912 0.353769 0.073 Uiso 1 1 calc R U . D 1
H33B H 0.967212 0.334804 0.29805 0.073 Uiso 1 1 calc R U . D 1
H33C H 1.070225 0.291261 0.328723 0.073 Uiso 1 1 calc R U . D 1



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.485(6) . ?
C1 C14 1.491(6) . ?
C1 P1 1.692(5) . ?
C2 C7 1.398(6) . ?
C2 C3 1.402(6) . ?
C3 C4 1.382(6) . ?
C3 H3 0.95 . ?
C4 C5 1.409(6) . ?
C4 H4 0.95 . ?
C5 C6 1.395(6) . ?
C5 C8 1.488(6) . ?
C6 C7 1.384(6) . ?
C6 H6 0.95 . ?
C7 H7 0.95 . ?
C8 C9 1.383(6) . ?
C8 C13 1.385(6) . ?
C9 C10 1.393(7) . ?
C9 H9 0.95 . ?
C10 C11 1.377(7) . ?
C10 H10 0.95 . ?
C11 C12 1.377(7) . ?
C11 H11 0.95 . ?
C12 C13 1.385(7) . ?
C12 H12 0.95 . ?
C13 H13 0.95 . ?
C14 C19 1.385(7) . ?
C14 C15 1.389(6) . ?
C15 C16 1.389(7) . ?
C15 H15 0.95 . ?
C16 C17 1.386(7) . ?
C16 H16 0.95 . ?
C17 C18 1.398(6) . ?
C17 C20 1.486(6) . ?
C18 C19 1.394(7) . ?
C18 H18 0.95 . ?
C19 H19 0.95 . ?
C20 C21 1.387(6) . ?
C20 C25 1.398(7) . ?
C21 C22 1.390(7) . ?
C21 H21 0.95 . ?
C22 C23 1.394(7) . ?
C22 H22 0.95 . ?
C23 C24 1.377(7) . ?
C23 H23 0.95 . ?
C24 C25 1.380(7) . ?
C24 H24 0.95 . ?
C25 H25 0.95 . ?
C26 C27 1.524(7) . ?
C26 C29 1.533(7) . ?
C26 C28 1.538(7) . ?
C26 P2 1.880(5) . ?
P1 P2 2.2216(18) . ?
P2 C30 1.889(6) . ?
C27 H27A 0.98 . ?
C27 H27B 0.98 . ?
C27 H27C 0.98 . ?
C28 H28A 0.98 . ?
C28 H28B 0.98 . ?
C28 H28C 0.98 . ?
C29 H29A 0.98 . ?
C29 H29B 0.98 . ?
C29 H29C 0.98 . ?
C30 C33 1.520(7) . ?
C30 C31 1.527(10) . ?
C30 C32 1.540(9) . ?
C31 H31A 0.98 . ?
C31 H31B 0.98 . ?
C31 H31C 0.98 . ?
C32 H32A 0.98 . ?
C32 H32B 0.98 . ?
C32 H32C 0.98 . ?
C33 H33A 0.98 . ?
C33 H33B 0.98 . ?
C33 H33C 0.98 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C14 116.5(4) . . ?
C2 C1 P1 117.9(4) . . ?
C14 C1 P1 125.6(4) . . ?
C7 C2 C3 117.3(4) . . ?
C7 C2 C1 121.6(4) . . ?
C3 C2 C1 121.0(4) . . ?
C4 C3 C2 121.4(4) . . ?
C4 C3 H3 119.3 . . ?
C2 C3 H3 119.3 . . ?
C3 C4 C5 121.2(4) . . ?
C3 C4 H4 119.4 . . ?
C5 C4 H4 119.4 . . ?
C6 C5 C4 117.0(4) . . ?
C6 C5 C8 121.1(4) . . ?
C4 C5 C8 121.9(4) . . ?
C7 C6 C5 121.9(5) . . ?
C7 C6 H6 119.1 . . ?
C5 C6 H6 119.1 . . ?
C6 C7 C2 121.1(5) . . ?
C6 C7 H7 119.5 . . ?
C2 C7 H7 119.5 . . ?
C9 C8 C13 118.0(5) . . ?
C9 C8 C5 121.2(4) . . ?
C13 C8 C5 120.8(4) . . ?
C8 C9 C10 121.0(5) . . ?
C8 C9 H9 119.5 . . ?
C10 C9 H9 119.5 . . ?
C11 C10 C9 120.1(5) . . ?
C11 C10 H10 119.9 . . ?
C9 C10 H10 119.9 . . ?
C12 C11 C10 119.4(5) . . ?
C12 C11 H11 120.3 . . ?
C10 C11 H11 120.3 . . ?
C11 C12 C13 120.3(5) . . ?
C11 C12 H12 119.8 . . ?
C13 C12 H12 119.8 . . ?
C8 C13 C12 121.2(5) . . ?
C8 C13 H13 119.4 . . ?
C12 C13 H13 119.4 . . ?
C19 C14 C15 118.5(4) . . ?
C19 C14 C1 121.1(4) . . ?
C15 C14 C1 120.4(4) . . ?
C14 C15 C16 120.5(5) . . ?
C14 C15 H15 119.8 . . ?
C16 C15 H15 119.8 . . ?
C17 C16 C15 121.5(5) . . ?
C17 C16 H16 119.3 . . ?
C15 C16 H16 119.3 . . ?
C16 C17 C18 117.9(4) . . ?
C16 C17 C20 120.8(4) . . ?
C18 C17 C20 121.3(5) . . ?
C19 C18 C17 120.6(5) . . ?
C19 C18 H18 119.7 . . ?
C17 C18 H18 119.7 . . ?
C14 C19 C18 121.0(5) . . ?
C14 C19 H19 119.5 . . ?
C18 C19 H19 119.5 . . ?
C21 C20 C25 117.9(4) . . ?
C21 C20 C17 120.5(4) . . ?
C25 C20 C17 121.6(4) . . ?
C20 C21 C22 121.4(5) . . ?
C20 C21 H21 119.3 . . ?
C22 C21 H21 119.3 . . ?
C21 C22 C23 119.4(5) . . ?
C21 C22 H22 120.3 . . ?
C23 C22 H22 120.3 . . ?
C24 C23 C22 119.8(5) . . ?
C24 C23 H23 120.1 . . ?
C22 C23 H23 120.1 . . ?
C23 C24 C25 120.3(5) . . ?
C23 C24 H24 119.8 . . ?
C25 C24 H24 119.8 . . ?
C24 C25 C20 121.1(5) . . ?
C24 C25 H25 119.4 . . ?
C20 C25 H25 119.4 . . ?
C27 C26 C29 108.5(5) . . ?
C27 C26 C28 108.8(5) . . ?
C29 C26 C28 107.5(4) . . ?
C27 C26 P2 118.2(4) . . ?
C29 C26 P2 104.7(4) . . ?
C28 C26 P2 108.7(4) . . ?
C1 P1 P2 104.26(17) . . ?
C26 P2 C30 110.2(2) . . ?
C26 P2 P1 99.70(16) . . ?
C30 P2 P1 98.4(2) . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C26 C29 H29A 109.5 . . ?
C26 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C26 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C33 C30 C31 109.2(6) . . ?
C33 C30 C32 107.7(5) . . ?
C31 C30 C32 109.8(6) . . ?
C33 C30 P2 105.2(4) . . ?
C31 C30 P2 117.1(5) . . ?
C32 C30 P2 107.3(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 . . ?
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 . . ?
C30 C33 H33A 109.5 . . ?
C30 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C30 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C14 C1 C2 C7 150.8(4) . . . . ?
P1 C1 C2 C7 -30.7(6) . . . . ?
C14 C1 C2 C3 -31.2(7) . . . . ?
P1 C1 C2 C3 147.3(4) . . . . ?
C7 C2 C3 C4 2.3(7) . . . . ?
C1 C2 C3 C4 -175.7(5) . . . . ?
C2 C3 C4 C5 -0.7(8) . . . . ?
C3 C4 C5 C6 -1.6(7) . . . . ?
C3 C4 C5 C8 178.0(5) . . . . ?
C4 C5 C6 C7 2.3(7) . . . . ?
C8 C5 C6 C7 -177.3(5) . . . . ?
C5 C6 C7 C2 -0.7(8) . . . . ?
C3 C2 C7 C6 -1.7(7) . . . . ?
C1 C2 C7 C6 176.4(5) . . . . ?
C6 C5 C8 C9 -151.8(5) . . . . ?
C4 C5 C8 C9 28.6(8) . . . . ?
C6 C5 C8 C13 28.8(7) . . . . ?
C4 C5 C8 C13 -150.8(5) . . . . ?
C13 C8 C9 C10 0.2(8) . . . . ?
C5 C8 C9 C10 -179.2(5) . . . . ?
C8 C9 C10 C11 -0.5(9) . . . . ?
C9 C10 C11 C12 0.8(9) . . . . ?
C10 C11 C12 C13 -0.7(9) . . . . ?
C9 C8 C13 C12 -0.1(8) . . . . ?
C5 C8 C13 C12 179.3(5) . . . . ?
C11 C12 C13 C8 0.4(9) . . . . ?
C2 C1 C14 C19 -68.4(6) . . . . ?
P1 C1 C14 C19 113.2(5) . . . . ?
C2 C1 C14 C15 111.6(5) . . . . ?
P1 C1 C14 C15 -66.8(6) . . . . ?
C19 C14 C15 C16 -1.6(7) . . . . ?
C1 C14 C15 C16 178.4(4) . . . . ?
C14 C15 C16 C17 -1.2(7) . . . . ?
C15 C16 C17 C18 2.3(7) . . . . ?
C15 C16 C17 C20 -176.5(4) . . . . ?
C16 C17 C18 C19 -0.6(7) . . . . ?
C20 C17 C18 C19 178.2(4) . . . . ?
C15 C14 C19 C18 3.3(7) . . . . ?
C1 C14 C19 C18 -176.7(5) . . . . ?
C17 C18 C19 C14 -2.3(8) . . . . ?
C16 C17 C20 C21 -29.9(7) . . . . ?
C18 C17 C20 C21 151.4(5) . . . . ?
C16 C17 C20 C25 148.4(5) . . . . ?
C18 C17 C20 C25 -30.3(7) . . . . ?
C25 C20 C21 C22 1.2(7) . . . . ?
C17 C20 C21 C22 179.6(4) . . . . ?
C20 C21 C22 C23 -1.3(8) . . . . ?
C21 C22 C23 C24 0.8(8) . . . . ?
C22 C23 C24 C25 -0.3(8) . . . . ?
C23 C24 C25 C20 0.2(8) . . . . ?
C21 C20 C25 C24 -0.7(7) . . . . ?
C17 C20 C25 C24 -179.1(5) . . . . ?
C2 C1 P1 P2 171.8(3) . . . . ?
C14 C1 P1 P2 -9.9(5) . . . . ?
C27 C26 P2 C30 -52.1(5) . . . . ?
C29 C26 P2 C30 -173.0(4) . . . . ?
C28 C26 P2 C30 72.4(4) . . . . ?
C27 C26 P2 P1 50.6(5) . . . . ?
C29 C26 P2 P1 -70.3(4) . . . . ?
C28 C26 P2 P1 175.1(3) . . . . ?
C26 P2 C30 C33 173.3(4) . . . . ?
P1 P2 C30 C33 69.7(4) . . . . ?
C26 P2 C30 C31 51.8(6) . . . . ?
P1 P2 C30 C31 -51.8(5) . . . . ?
C26 P2 C30 C32 -72.2(5) . . . . ?
P1 P2 C30 C32 -175.8(5) . . . . ?



# END of CIF
####################################################################### 
# 
# 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_za19
_database_code_depnum_ccdc_archive 'CCDC 2386109'
loop_
_audit_author_name
_audit_author_address
'Lukasz Ponikiewski'
;Gdansk University of Technology
Poland
;
_audit_update_record             
;
2024-09-23 deposited with the CCDC.	2024-11-13 downloaded from the CCDC.
;

_audit_creation_date             2024-04-05T10:03:03-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_moiety         'C33 H38 Cl3 P Ru2, C7 H8'
_chemical_formula_sum            'C40 H46 Cl3 P Ru2'
_chemical_formula_weight         866.23

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.1085(4)
_cell_length_b                   14.1466(6)
_cell_length_c                   14.9037(7)
_cell_angle_alpha                66.843(3)
_cell_angle_beta                 72.498(3)
_cell_angle_gamma                83.439(3)
_cell_volume                     1868.80(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    24745
_cell_measurement_theta_min      2.24
_cell_measurement_theta_max      29.66
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       plate
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.07
_exptl_crystal_density_diffrn    1.539
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             880

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    1.093
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in: F. R. Ahmed (Editor), "Crystallographic
Computing", Munksgaard, Copenhagen (1970), 255 - 270. Afterwards scaling of
reflection intensities was performed within STOE LANA. J. Koziskova, F. Hahn,
J. Richter, J. Kozisek, Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136-140.
;
_exptl_absorpt_correction_T_min  0.2623
_exptl_absorpt_correction_T_max  0.7363
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 1 1 0.1810
0 1 0 0.1910
-1 0 1 0.1830
0 -1 0 0.3010
3 0 -4 0.1230
-1 0 -1 0.1130
1 1 1 0.1860
1 0 1 0.1800
-3 -3 -2 0.2740
2 -3 -2 0.2990

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_standards_number         0
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_type            'STOE Imaging Plate'
_diffrn_detector_area_resol_mean 6.67
_diffrn_source                   'GeniX Mo, 0.05 x 0.05 mm2 microfocus'
_diffrn_source_type              ?
_diffrn_source_target            ?
_diffrn_source_voltage           50
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_radiation_monochromator  'parabolic x-ray mirror'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_collimation    '0.6 mm diameter'
_diffrn_measurement_method       'rotation method, ω scans'
_diffrn_measurement_details      
; 216 frames, detector distance = 100 mm
;
_diffrn_reflns_av_unetI/netI     0.0569
_diffrn_reflns_number            9036
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.548
_diffrn_reflns_theta_max         29.321
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.887
_diffrn_measured_fraction_theta_max 0.885
_diffrn_reflns_Laue_measured_fraction_full 0.887
_diffrn_reflns_Laue_measured_fraction_max 0.885
_diffrn_reflns_point_group_measured_fraction_full 0.887
_diffrn_reflns_point_group_measured_fraction_max 0.885
_reflns_Friedel_coverage         0
_reflns_number_total             9036
_reflns_number_gt                7414
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       
;
X-Area WinXpose 2.0.22.0 (STOE, 2016)
;
_computing_cell_refinement       
;
X-Area Recipe 1.34.0.0 (STOE, 2019)
;
_computing_data_reduction        
;
X-Area Integrate 1.77.0.0 (STOE, 2019)
X-Area LANA 1.77.1.0 (STOE, 2019)
;
_computing_structure_solution    'SUPERFLIP (Palatinus & Chapuis,2007)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     'iterative - e.g. charge flipping method'
_atom_sites_solution_secondary   'iterative - e.g. charge flipping method'
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
The crystal was twinned and has been refined as a 2-component twin with the following matrix using ROTAX (Parsons 1
Gould; Cooper et al., 2002): 180.0 degree rotation about 0. 0. 1. direct lattice direction: [ -1.000 0.000 0.000] [ 0.000
-1.000 0.000] [ -0.765 -0.766 1.000] BASF = 0.0.43725.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1002P)²+20.1480P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         9036
_refine_ls_number_parameters     423
_refine_ls_number_restraints     0
_refine_ls_number_constraints    0
_refine_ls_R_factor_all          0.0896
_refine_ls_R_factor_gt           0.0702
_refine_ls_wR_factor_ref         0.2326
_refine_ls_wR_factor_gt          0.2138
_refine_ls_goodness_of_fit_ref   1.09
_refine_ls_restrained_S_all      1.09
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         2.571
_refine_diff_density_min         -1.711
_refine_diff_density_rms         0.244

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.9269(8) 0.6947(6) 0.0216(6) 0.0172(14) Uani 1 1 d . . . . .
C2 C 0.9544(8) 0.6371(6) 0.1217(6) 0.0173(14) Uani 1 1 d . . . . .
C3 C 0.8980(9) 0.6705(6) 0.2046(7) 0.0221(16) Uani 1 1 d . . . . .
H3 H 0.845039 0.731811 0.195505 0.027 Uiso 1 1 calc R U . . .
C4 C 0.9212(9) 0.6129(7) 0.2981(7) 0.0259(17) Uani 1 1 d . . . . .
H4 H 0.880347 0.633261 0.354063 0.031 Uiso 1 1 calc R U . . .
C5 C 1.0038(9) 0.5258(7) 0.3107(7) 0.0236(16) Uani 1 1 d . . . . .
H5 H 1.021681 0.488024 0.374425 0.028 Uiso 1 1 calc R U . . .
C6 C 1.0606(9) 0.4937(6) 0.2296(7) 0.0232(16) Uani 1 1 d . . . . .
H6 H 1.115235 0.43321 0.238715 0.028 Uiso 1 1 calc R U . . .
C7 C 1.0374(8) 0.5501(6) 0.1359(7) 0.0208(15) Uani 1 1 d . . . . .
H7 H 1.078725 0.528867 0.080611 0.025 Uiso 1 1 calc R U . . .
C8 C 1.0474(8) 0.7165(6) -0.0707(6) 0.0182(14) Uani 1 1 d . . . . .
C9 C 1.1715(9) 0.7558(6) -0.0750(7) 0.0225(16) Uani 1 1 d . . . . .
H9 H 1.17839 0.766485 -0.017511 0.027 Uiso 1 1 calc R U . . .
C10 C 1.2828(10) 0.7790(7) -0.1595(7) 0.0274(18) Uani 1 1 d . . . . .
H10 H 1.365844 0.805091 -0.160361 0.033 Uiso 1 1 calc R U . . .
C11 C 1.2734(9) 0.7639(7) -0.2457(7) 0.0263(17) Uani 1 1 d . . . . .
H11 H 1.349317 0.781203 -0.305456 0.032 Uiso 1 1 calc R U . . .
C12 C 1.1522(10) 0.7235(7) -0.2420(7) 0.0260(17) Uani 1 1 d . . . . .
H12 H 1.14543 0.712088 -0.299194 0.031 Uiso 1 1 calc R U . . .
C13 C 1.0415(8) 0.6999(6) -0.1554(7) 0.0220(16) Uani 1 1 d . . . . .
H13 H 0.959376 0.671747 -0.15366 0.026 Uiso 1 1 calc R U . . .
C14 C 0.5615(9) 0.5278(6) 0.1475(7) 0.0247(17) Uani 1 1 d . . . . .
C15 C 0.4284(9) 0.5726(6) 0.1482(7) 0.0244(17) Uani 1 1 d . . . . .
H15 H 0.388498 0.577 0.096597 0.029 Uiso 1 1 calc R U . . .
C16 C 0.3529(9) 0.6111(7) 0.2242(7) 0.0260(17) Uani 1 1 d . . . . .
H16 H 0.260493 0.634209 0.22598 0.031 Uiso 1 1 calc R U . . .
C17 C 0.4109(9) 0.6156(6) 0.2947(7) 0.0237(16) Uani 1 1 d . . . . .
C18 C 0.5516(9) 0.5805(6) 0.2891(6) 0.0220(16) Uani 1 1 d . . . . .
H18 H 0.596694 0.58824 0.333313 0.026 Uiso 1 1 calc R U . . .
C19 C 0.6238(9) 0.5351(6) 0.2195(7) 0.0239(17) Uani 1 1 d . . . . .
H19 H 0.714527 0.509038 0.220134 0.029 Uiso 1 1 calc R U . . .
C20 C 0.6367(10) 0.4830(7) 0.0714(8) 0.031(2) Uani 1 1 d . . . . .
H20A H 0.602622 0.413025 0.093421 0.046 Uiso 1 1 calc R U . . .
H20B H 0.736191 0.481014 0.065114 0.046 Uiso 1 1 calc R U . . .
H20C H 0.620859 0.525354 0.005449 0.046 Uiso 1 1 calc R U . . .
C21 C 0.3402(10) 0.6631(8) 0.3726(7) 0.031(2) Uani 1 1 d . . . . .
H21 H 0.409313 0.708565 0.372161 0.037 Uiso 1 1 calc R U . . .
C22 C 0.2150(12) 0.7282(9) 0.3502(9) 0.037(2) Uani 1 1 d . . . . .
H22A H 0.138204 0.683409 0.364 0.056 Uiso 1 1 calc R U . . .
H22B H 0.238996 0.774993 0.27862 0.056 Uiso 1 1 calc R U . . .
H22C H 0.18696 0.768318 0.393534 0.056 Uiso 1 1 calc R U . . .
C23 C 0.3007(15) 0.5783(11) 0.4768(9) 0.052(3) Uani 1 1 d . . . . .
H23A H 0.223856 0.538049 0.482388 0.078 Uiso 1 1 calc R U . . .
H23B H 0.271995 0.608509 0.52871 0.078 Uiso 1 1 calc R U . . .
H23C H 0.380666 0.533449 0.487068 0.078 Uiso 1 1 calc R U . . .
C24 C 0.8127(10) 0.9839(7) -0.1292(7) 0.0262(18) Uani 1 1 d . . . . .
C25 C 0.6843(9) 1.0156(6) -0.1522(7) 0.0226(16) Uani 1 1 d . . . . .
H25 H 0.614683 1.042715 -0.109887 0.027 Uiso 1 1 calc R U . . .
C26 C 0.6577(9) 1.0074(6) -0.2380(7) 0.0231(16) Uani 1 1 d . . . . .
H26 H 0.572206 1.03179 -0.252868 0.028 Uiso 1 1 calc R U . . .
C27 C 0.7519(9) 0.9657(6) -0.2986(7) 0.0219(16) Uani 1 1 d . . . . .
C28 C 0.8774(8) 0.9240(6) -0.2695(7) 0.0228(16) Uani 1 1 d . . . . .
H28 H 0.940086 0.887051 -0.305482 0.027 Uiso 1 1 calc R U . . .
C29 C 0.9077(9) 0.9369(6) -0.1905(7) 0.0251(17) Uani 1 1 d . . . . .
H29 H 0.99428 0.91365 -0.177106 0.03 Uiso 1 1 calc R U . . .
C30 C 0.8457(11) 1.0020(7) -0.0469(8) 0.031(2) Uani 1 1 d . . . . .
H30A H 0.892074 1.068779 -0.074806 0.046 Uiso 1 1 calc R U . . .
H30B H 0.907054 0.94754 -0.017395 0.046 Uiso 1 1 calc R U . . .
H30C H 0.75976 1.001662 0.005865 0.046 Uiso 1 1 calc R U . . .
C31 C 0.7308(10) 0.9555(6) -0.3919(7) 0.0237(16) Uani 1 1 d . . . . .
H31 H 0.784984 0.894577 -0.400889 0.028 Uiso 1 1 calc R U . . .
C32 C 0.7912(15) 1.0507(10) -0.4860(8) 0.047(3) Uani 1 1 d . . . . .
H32A H 0.735602 1.111022 -0.481599 0.071 Uiso 1 1 calc R U . . .
H32B H 0.789759 1.04068 -0.547101 0.071 Uiso 1 1 calc R U . . .
H32C H 0.88707 1.061445 -0.489555 0.071 Uiso 1 1 calc R U . . .
C33 C 0.5806(12) 0.9386(9) -0.3822(8) 0.038(2) Uani 1 1 d . . . . .
H33A H 0.5413 0.881496 -0.318112 0.057 Uiso 1 1 calc R U . . .
H33B H 0.57608 0.922235 -0.439242 0.057 Uiso 1 1 calc R U . . .
H33C H 0.527446 1.001223 -0.382854 0.057 Uiso 1 1 calc R U . . .
C34 C 0.7589(11) 0.8303(8) 0.3962(9) 0.033(2) Uani 1 1 d . . . . .
C35 C 0.8520(15) 0.8014(10) 0.4541(12) 0.051(3) Uani 1 1 d . . . . .
H35 H 0.938057 0.836809 0.428433 0.061 Uiso 1 1 calc R U . . .
C36 C 0.823(2) 0.7251(11) 0.5449(15) 0.074(6) Uani 1 1 d . . . . .
H36 H 0.890136 0.705528 0.582013 0.089 Uiso 1 1 calc R U . . .
C37 C 0.697(3) 0.6735(10) 0.5863(11) 0.088(7) Uani 1 1 d . . . . .
H37 H 0.676383 0.619677 0.651701 0.106 Uiso 1 1 calc R U . . .
C38 C 0.6010(19) 0.7023(11) 0.5300(10) 0.064(5) Uani 1 1 d . . . . .
H38 H 0.513535 0.668508 0.557841 0.077 Uiso 1 1 calc R U . . .
C39 C 0.6312(13) 0.7795(8) 0.4340(9) 0.039(2) Uani 1 1 d . . . . .
H39 H 0.566833 0.797571 0.394846 0.046 Uiso 1 1 calc R U . . .
C40 C 0.7907(17) 0.9191(11) 0.2943(9) 0.059(4) Uani 1 1 d . . . . .
H40A H 0.801895 0.982222 0.303669 0.088 Uiso 1 1 calc R U . . .
H40B H 0.71428 0.927493 0.264113 0.088 Uiso 1 1 calc R U . . .
H40C H 0.876649 0.905057 0.249203 0.088 Uiso 1 1 calc R U . . .
Cl1 Cl 0.5985(2) 0.83145(15) 0.17491(16) 0.0233(4) Uani 1 1 d . . . . .
Cl2 Cl 0.4851(2) 0.81291(15) -0.00653(15) 0.0211(4) Uani 1 1 d . . . . .
Cl3 Cl 0.6790(2) 0.71283(16) -0.17480(16) 0.0236(4) Uani 1 1 d . . . . .
P1 P 0.7669(2) 0.73547(15) 0.01041(16) 0.0165(4) Uani 1 1 d . . . . .
Ru1 Ru 0.56067(6) 0.68875(5) 0.13776(5) 0.01676(16) Uani 1 1 d . . . . .
Ru2 Ru 0.71456(6) 0.85397(5) -0.13275(5) 0.01626(15) Uani 1 1 d . . . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.487(11) . ?
C1 C8 1.488(11) . ?
C1 P1 1.689(8) . ?
C2 C7 1.389(10) . ?
C2 C3 1.430(12) . ?
C3 C4 1.387(12) . ?
C4 C5 1.389(12) . ?
C5 C6 1.396(13) . ?
C6 C7 1.385(12) . ?
C8 C13 1.391(12) . ?
C8 C9 1.403(11) . ?
C9 C10 1.366(13) . ?
C10 C11 1.413(13) . ?
C11 C12 1.388(13) . ?
C12 C13 1.382(12) . ?
C14 C15 1.419(12) . ?
C14 C19 1.438(14) . ?
C14 C20 1.484(13) . ?
C14 Ru1 2.223(8) . ?
C15 C16 1.425(13) . ?
C15 Ru1 2.165(8) . ?
C16 C17 1.372(13) . ?
C16 Ru1 2.250(8) . ?
C17 C18 1.441(12) . ?
C17 C21 1.522(13) . ?
C17 Ru1 2.271(8) . ?
C18 C19 1.408(13) . ?
C18 Ru1 2.152(8) . ?
C19 Ru1 2.164(8) . ?
C21 C23 1.511(15) . ?
C21 C22 1.519(15) . ?
C24 C29 1.416(14) . ?
C24 C25 1.420(12) . ?
C24 C30 1.481(12) . ?
C24 Ru2 2.211(8) . ?
C25 C26 1.431(13) . ?
C25 Ru2 2.185(8) . ?
C26 C27 1.359(12) . ?
C26 Ru2 2.254(8) . ?
C27 C28 1.451(12) . ?
C27 C31 1.529(12) . ?
C27 Ru2 2.292(8) . ?
C28 C29 1.382(14) . ?
C28 Ru2 2.147(8) . ?
C29 Ru2 2.155(9) . ?
C31 C33 1.519(14) . ?
C31 C32 1.530(14) . ?
C34 C35 1.386(16) . ?
C34 C39 1.398(15) . ?
C34 C40 1.511(16) . ?
C35 C36 1.33(2) . ?
C36 C37 1.39(3) . ?
C37 C38 1.39(3) . ?
C38 C39 1.385(17) . ?
Cl1 Ru1 2.390(2) . ?
Cl2 Ru1 2.450(2) . ?
Cl2 Ru2 2.466(2) . ?
Cl3 Ru2 2.407(2) . ?
P1 Ru2 2.303(2) . ?
P1 Ru1 2.309(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C8 117.3(7) . . ?
C2 C1 P1 122.4(6) . . ?
C8 C1 P1 120.2(6) . . ?
C7 C2 C3 118.8(7) . . ?
C7 C2 C1 120.2(8) . . ?
C3 C2 C1 121.0(7) . . ?
C4 C3 C2 119.6(7) . . ?
C3 C4 C5 120.5(9) . . ?
C4 C5 C6 120.0(8) . . ?
C7 C6 C5 120.1(8) . . ?
C6 C7 C2 120.9(8) . . ?
C13 C8 C9 117.7(7) . . ?
C13 C8 C1 121.8(7) . . ?
C9 C8 C1 120.5(8) . . ?
C10 C9 C8 121.9(8) . . ?
C9 C10 C11 119.5(8) . . ?
C12 C11 C10 119.3(8) . . ?
C13 C12 C11 120.1(9) . . ?
C12 C13 C8 121.5(8) . . ?
C15 C14 C19 116.3(8) . . ?
C15 C14 C20 121.8(9) . . ?
C19 C14 C20 121.8(8) . . ?
C15 C14 Ru1 68.9(5) . . ?
C19 C14 Ru1 68.7(5) . . ?
C20 C14 Ru1 129.5(6) . . ?
C14 C15 C16 122.0(9) . . ?
C14 C15 Ru1 73.4(5) . . ?
C16 C15 Ru1 74.4(5) . . ?
C17 C16 C15 121.4(8) . . ?
C17 C16 Ru1 73.2(5) . . ?
C15 C16 Ru1 68.0(5) . . ?
C16 C17 C18 117.7(8) . . ?
C16 C17 C21 124.0(8) . . ?
C18 C17 C21 118.0(8) . . ?
C16 C17 Ru1 71.5(5) . . ?
C18 C17 Ru1 66.6(4) . . ?
C21 C17 Ru1 129.2(6) . . ?
C19 C18 C17 121.4(8) . . ?
C19 C18 Ru1 71.4(5) . . ?
C17 C18 Ru1 75.5(5) . . ?
C18 C19 C14 120.7(8) . . ?
C18 C19 Ru1 70.5(5) . . ?
C14 C19 Ru1 73.1(5) . . ?
C23 C21 C22 110.9(9) . . ?
C23 C21 C17 108.8(9) . . ?
C22 C21 C17 113.7(9) . . ?
C29 C24 C25 116.5(8) . . ?
C29 C24 C30 122.2(9) . . ?
C25 C24 C30 121.3(9) . . ?
C29 C24 Ru2 69.0(5) . . ?
C25 C24 Ru2 70.2(4) . . ?
C30 C24 Ru2 132.9(6) . . ?
C24 C25 C26 121.3(8) . . ?
C24 C25 Ru2 72.1(5) . . ?
C26 C25 Ru2 73.8(5) . . ?
C27 C26 C25 121.6(8) . . ?
C27 C26 Ru2 74.2(5) . . ?
C25 C26 Ru2 68.6(5) . . ?
C26 C27 C28 117.2(8) . . ?
C26 C27 C31 124.3(8) . . ?
C28 C27 C31 118.4(8) . . ?
C26 C27 Ru2 71.1(5) . . ?
C28 C27 Ru2 65.6(5) . . ?
C31 C27 Ru2 132.3(6) . . ?
C29 C28 C27 121.4(8) . . ?
C29 C28 Ru2 71.6(5) . . ?
C27 C28 Ru2 76.4(5) . . ?
C28 C29 C24 121.6(8) . . ?
C28 C29 Ru2 70.9(5) . . ?
C24 C29 Ru2 73.2(5) . . ?
C33 C31 C27 113.7(8) . . ?
C33 C31 C32 110.8(9) . . ?
C27 C31 C32 109.0(8) . . ?
C35 C34 C39 119.8(12) . . ?
C35 C34 C40 120.9(12) . . ?
C39 C34 C40 119.3(10) . . ?
C36 C35 C34 121.2(15) . . ?
C35 C36 C37 121.1(14) . . ?
C36 C37 C38 118.5(13) . . ?
C39 C38 C37 121.0(15) . . ?
C38 C39 C34 118.3(13) . . ?
Ru1 Cl2 Ru2 98.07(7) . . ?
C1 P1 Ru2 126.3(3) . . ?
C1 P1 Ru1 126.4(3) . . ?
Ru2 P1 Ru1 107.21(8) . . ?
C18 Ru1 C19 38.1(3) . . ?
C18 Ru1 C15 80.4(3) . . ?
C19 Ru1 C15 68.2(3) . . ?
C18 Ru1 C14 68.8(3) . . ?
C19 Ru1 C14 38.2(3) . . ?
C15 Ru1 C14 37.7(3) . . ?
C18 Ru1 C16 66.3(3) . . ?
C19 Ru1 C16 79.2(3) . . ?
C15 Ru1 C16 37.6(3) . . ?
C14 Ru1 C16 67.5(3) . . ?
C18 Ru1 C17 37.9(3) . . ?
C19 Ru1 C17 68.1(3) . . ?
C15 Ru1 C17 66.7(3) . . ?
C14 Ru1 C17 80.2(3) . . ?
C16 Ru1 C17 35.3(3) . . ?
C18 Ru1 P1 122.4(2) . . ?
C19 Ru1 P1 96.3(2) . . ?
C15 Ru1 P1 120.4(3) . . ?
C14 Ru1 P1 95.4(2) . . ?
C16 Ru1 P1 157.7(3) . . ?
C17 Ru1 P1 160.0(2) . . ?
C18 Ru1 Cl1 92.9(3) . . ?
C19 Ru1 Cl1 121.2(3) . . ?
C15 Ru1 Cl1 151.8(3) . . ?
C14 Ru1 Cl1 159.4(3) . . ?
C16 Ru1 Cl1 114.8(3) . . ?
C17 Ru1 Cl1 91.3(2) . . ?
P1 Ru1 Cl1 86.31(8) . . ?
C18 Ru1 Cl2 160.2(2) . . ?
C19 Ru1 Cl2 150.6(3) . . ?
C15 Ru1 Cl2 90.0(3) . . ?
C14 Ru1 Cl2 113.0(3) . . ?
C16 Ru1 Cl2 95.6(2) . . ?
C17 Ru1 Cl2 122.3(2) . . ?
P1 Ru1 Cl2 77.46(7) . . ?
Cl1 Ru1 Cl2 87.41(7) . . ?
C28 Ru2 C29 37.5(4) . . ?
C28 Ru2 C25 79.6(3) . . ?
C29 Ru2 C25 67.5(3) . . ?
C28 Ru2 C24 68.1(4) . . ?
C29 Ru2 C24 37.8(4) . . ?
C25 Ru2 C24 37.7(3) . . ?
C28 Ru2 C26 66.0(3) . . ?
C29 Ru2 C26 78.7(3) . . ?
C25 Ru2 C26 37.6(3) . . ?
C24 Ru2 C26 67.6(3) . . ?
C28 Ru2 C27 38.0(3) . . ?
C29 Ru2 C27 67.4(3) . . ?
C25 Ru2 C27 65.9(3) . . ?
C24 Ru2 C27 79.6(3) . . ?
C26 Ru2 C27 34.8(3) . . ?
C28 Ru2 P1 120.2(2) . . ?
C29 Ru2 P1 94.7(2) . . ?
C25 Ru2 P1 120.4(2) . . ?
C24 Ru2 P1 94.2(2) . . ?
C26 Ru2 P1 157.9(2) . . ?
C27 Ru2 P1 158.1(2) . . ?
C28 Ru2 Cl3 94.9(3) . . ?
C29 Ru2 Cl3 123.8(3) . . ?
C25 Ru2 Cl3 149.7(2) . . ?
C24 Ru2 Cl3 161.6(3) . . ?
C26 Ru2 Cl3 113.1(2) . . ?
C27 Ru2 Cl3 91.5(2) . . ?
P1 Ru2 Cl3 88.18(7) . . ?
C28 Ru2 Cl2 162.4(2) . . ?
C29 Ru2 Cl2 147.9(3) . . ?
C25 Ru2 Cl2 89.6(2) . . ?
C24 Ru2 Cl2 111.0(3) . . ?
C26 Ru2 Cl2 97.1(2) . . ?
C27 Ru2 Cl2 124.7(2) . . ?
P1 Ru2 Cl2 77.25(7) . . ?
Cl3 Ru2 Cl2 87.42(7) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C8 C1 C2 C7 -45.8(10) . . . . ?
P1 C1 C2 C7 134.7(7) . . . . ?
C8 C1 C2 C3 133.4(8) . . . . ?
P1 C1 C2 C3 -46.2(10) . . . . ?
C7 C2 C3 C4 -3.3(12) . . . . ?
C1 C2 C3 C4 177.6(8) . . . . ?
C2 C3 C4 C5 2.9(13) . . . . ?
C3 C4 C5 C6 -2.0(13) . . . . ?
C4 C5 C6 C7 1.5(13) . . . . ?
C5 C6 C7 C2 -1.9(13) . . . . ?
C3 C2 C7 C6 2.8(12) . . . . ?
C1 C2 C7 C6 -178.0(7) . . . . ?
C2 C1 C8 C13 133.7(8) . . . . ?
P1 C1 C8 C13 -46.8(10) . . . . ?
C2 C1 C8 C9 -46.9(10) . . . . ?
P1 C1 C8 C9 132.7(7) . . . . ?
C13 C8 C9 C10 1.1(12) . . . . ?
C1 C8 C9 C10 -178.4(8) . . . . ?
C8 C9 C10 C11 0.4(13) . . . . ?
C9 C10 C11 C12 -1.4(14) . . . . ?
C10 C11 C12 C13 1.0(14) . . . . ?
C11 C12 C13 C8 0.6(13) . . . . ?
C9 C8 C13 C12 -1.6(12) . . . . ?
C1 C8 C13 C12 177.9(8) . . . . ?
C19 C14 C15 C16 -7.7(12) . . . . ?
C20 C14 C15 C16 176.8(8) . . . . ?
Ru1 C14 C15 C16 -58.9(7) . . . . ?
C19 C14 C15 Ru1 51.3(7) . . . . ?
C20 C14 C15 Ru1 -124.2(8) . . . . ?
C14 C15 C16 C17 6.2(13) . . . . ?
Ru1 C15 C16 C17 -52.2(8) . . . . ?
C14 C15 C16 Ru1 58.4(7) . . . . ?
C15 C16 C17 C18 0.4(13) . . . . ?
Ru1 C16 C17 C18 -49.5(7) . . . . ?
C15 C16 C17 C21 175.2(8) . . . . ?
Ru1 C16 C17 C21 125.3(8) . . . . ?
C15 C16 C17 Ru1 49.9(8) . . . . ?
C16 C17 C18 C19 -5.3(12) . . . . ?
C21 C17 C18 C19 179.6(8) . . . . ?
Ru1 C17 C18 C19 -57.1(7) . . . . ?
C16 C17 C18 Ru1 51.8(7) . . . . ?
C21 C17 C18 Ru1 -123.3(7) . . . . ?
C17 C18 C19 C14 3.7(12) . . . . ?
Ru1 C18 C19 C14 -55.4(7) . . . . ?
C17 C18 C19 Ru1 59.0(7) . . . . ?
C15 C14 C19 C18 2.7(12) . . . . ?
C20 C14 C19 C18 178.2(8) . . . . ?
Ru1 C14 C19 C18 54.2(7) . . . . ?
C15 C14 C19 Ru1 -51.4(7) . . . . ?
C20 C14 C19 Ru1 124.1(8) . . . . ?
C16 C17 C21 C23 110.1(11) . . . . ?
C18 C17 C21 C23 -75.1(11) . . . . ?
Ru1 C17 C21 C23 -156.7(9) . . . . ?
C16 C17 C21 C22 -14.0(13) . . . . ?
C18 C17 C21 C22 160.8(8) . . . . ?
Ru1 C17 C21 C22 79.2(11) . . . . ?
C29 C24 C25 C26 -4.7(12) . . . . ?
C30 C24 C25 C26 173.7(8) . . . . ?
Ru2 C24 C25 C26 -57.4(7) . . . . ?
C29 C24 C25 Ru2 52.7(7) . . . . ?
C30 C24 C25 Ru2 -128.9(8) . . . . ?
C24 C25 C26 C27 2.5(13) . . . . ?
Ru2 C25 C26 C27 -54.2(7) . . . . ?
C24 C25 C26 Ru2 56.6(7) . . . . ?
C25 C26 C27 C28 3.5(12) . . . . ?
Ru2 C26 C27 C28 -48.1(7) . . . . ?
C25 C26 C27 C31 -179.4(8) . . . . ?
Ru2 C26 C27 C31 128.9(8) . . . . ?
C25 C26 C27 Ru2 51.7(7) . . . . ?
C26 C27 C28 C29 -7.4(12) . . . . ?
C31 C27 C28 C29 175.4(8) . . . . ?
Ru2 C27 C28 C29 -58.1(7) . . . . ?
C26 C27 C28 Ru2 50.7(7) . . . . ?
C31 C27 C28 Ru2 -126.5(7) . . . . ?
C27 C28 C29 C24 5.2(13) . . . . ?
Ru2 C28 C29 C24 -55.2(7) . . . . ?
C27 C28 C29 Ru2 60.4(7) . . . . ?
C25 C24 C29 C28 0.9(12) . . . . ?
C30 C24 C29 C28 -177.5(8) . . . . ?
Ru2 C24 C29 C28 54.2(7) . . . . ?
C25 C24 C29 Ru2 -53.3(7) . . . . ?
C30 C24 C29 Ru2 128.3(8) . . . . ?
C26 C27 C31 C33 -32.2(12) . . . . ?
C28 C27 C31 C33 144.8(8) . . . . ?
Ru2 C27 C31 C33 63.0(11) . . . . ?
C26 C27 C31 C32 92.0(11) . . . . ?
C28 C27 C31 C32 -91.0(10) . . . . ?
Ru2 C27 C31 C32 -172.8(8) . . . . ?
C39 C34 C35 C36 0.9(18) . . . . ?
C40 C34 C35 C36 178.3(13) . . . . ?
C34 C35 C36 C37 -2(2) . . . . ?
C35 C36 C37 C38 1(3) . . . . ?
C36 C37 C38 C39 1(2) . . . . ?
C37 C38 C39 C34 -2(2) . . . . ?
C35 C34 C39 C38 1.1(17) . . . . ?
C40 C34 C39 C38 -176.4(12) . . . . ?
C2 C1 P1 Ru2 165.6(5) . . . . ?
C8 C1 P1 Ru2 -14.0(8) . . . . ?
C2 C1 P1 Ru1 -11.3(8) . . . . ?
C8 C1 P1 Ru1 169.1(5) . . . . ?


# start Validation Reply Form
_vrf_PLAT029_za19                
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.887 Why?
RESPONSE: The crystal was twinned and has been refined as a 2-component twin with the following matrix using ROTAX (Parsons 1
Gould; Cooper et al., 2002): 180.0 degree rotation about 0. 0. 1. direct lattice direction: [ -1.000 0.000 0.000] [ 0.000
-1.000 0.000] [ -0.765 -0.766 1.000] BASF = 0.0.43725.
;
_vrf_PLAT911_za19                
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        772 Report
RESPONSE: This alert is affected by two factors: 1) The crystal was twinned and has been refined as a 2-component twin with 
the following matrix using ROTAX;  2) Beamstop theta-min limit set too high.
;
# end Validation Reply Form 
# END of CIF
####################################################################### 
# 
# 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_za13_2024
_database_code_depnum_ccdc_archive 'CCDC 2386113'
loop_
_audit_author_name
_audit_author_address
'Lukasz Ponikiewski'
;Gdansk University of Technology
Poland
;
_audit_update_record             
;
2024-09-23 deposited with the CCDC.	2024-11-13 downloaded from the CCDC.
;
_audit_creation_date             2024-05-17
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C45 H46 Cl3 P Ru2'
_chemical_formula_sum            'C45 H46 Cl3 P Ru2'
_chemical_formula_weight         926.28
_chemical_melting_point          ?
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'
Cl Cl 0.1484 0.1585 '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'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   16.3325(5)
_cell_length_b                   16.6265(5)
_cell_length_c                   16.9118(5)
_cell_angle_alpha                74.161(2)
_cell_angle_beta                 78.653(2)
_cell_angle_gamma                87.765(2)
_cell_volume                     4331.2(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    111251
_cell_measurement_temperature    120
_cell_measurement_theta_max      29.77
_cell_measurement_theta_min      1.97
_shelx_estimated_absorpt_T_max   0.887
_shelx_estimated_absorpt_T_min   0.871
_exptl_absorpt_coefficient_mu    0.948
_exptl_absorpt_correction_T_max  0.7363
_exptl_absorpt_correction_T_min  0.1623
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in: F. R. Ahmed (Editor), "Crystallographic
Computing", Munksgaard, Copenhagen (1970), 255 - 270. Afterwards scaling of
reflection intensities was performed within STOE LANA. J. Koziskova, F. Hahn,
J. Richter, J. Kozisek, Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136-140.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.421
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1880
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 1 1 0.1810
0 1 0 0.1910
-1 0 1 0.1830
0 -1 0 0.3010
3 0 -4 0.1230
-1 0 -1 0.1130
1 1 1 0.1860
1 0 1 0.1800
-3 -3 -2 0.2740
2 -3 -2 0.2990

_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0313
_diffrn_reflns_av_unetI/netI     0.0342
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            51776
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.636
_diffrn_reflns_theta_min         1.968
_diffrn_ambient_temperature      120
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE Imaging Plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_details      '409 frames, detector distance = 100 mm'
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method, ω scans'
_diffrn_radiation_collimation    '0.6 mm diameter'
_diffrn_radiation_monochromator  'parabolic x-ray mirror'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'GeniX Mo, 0.05 x 0.05 mm2 microfocus'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_reflns_d_resolution_high        0.719
_reflns_d_resolution_low         10.347
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_limit_h_max              22
_reflns_limit_h_min              -22
_reflns_limit_k_max              22
_reflns_limit_k_min              -23
_reflns_limit_l_max              23
_reflns_limit_l_min              -23
_reflns_number_gt                18255
_reflns_number_total             23279
_reflns_special_details          'reflections have not been merged'
_reflns_threshold_expression     I>4u(I)
_computing_cell_refinement       
;
X-Area Recipe 1.34.0.0 (STOE, 2019)
;
_computing_data_collection       
;
X-Area WinXpose 2.0.22.0 (STOE, 2016)
;
_computing_data_reduction        
;
X-Area Integrate 1.77.0.0 (STOE, 2019)
X-Area LANA 1.77.1.0 (STOE, 2019)
;
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 1.88, Darmstadt 2019
;
_computing_structure_refinement  'SHELXL 2018/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.863
_refine_diff_density_min         -1.556
_refine_diff_density_rms         0.113
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     931
_refine_ls_number_reflns         23279
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0655
_refine_ls_R_factor_gt           0.0481
_refine_ls_restrained_S_all      1.015
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0636P)²+8.8334P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1186
_refine_ls_wR_factor_ref         0.1327
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C33(H33), C43(H43), C78(H78), C88(H88)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C15(H15), C16(H16), C18(H18), C19(H19), C21(H21), C22(H22), C23(H23),
  C24(H24), C25(H25), C27(H27), C28(H28), C30(H30), C31(H31), C37(H37),
 C38(H38), C40(H40), C41(H41), C48(H48), C49(H49), C51(H51), C52(H52), C54(H54),
  C55(H55), C56(H56), C57(H57), C58(H58), C60(H60), C61(H61), C63(H63),
 C64(H64), C66(H66), C67(H67), C68(H68), C69(H69), C70(H70), C72(H72), C73(H73),
  C75(H75), C76(H76), C82(H82), C83(H83), C85(H85), C86(H86)
2.c Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C42(H42A,H42B,
 H42C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C77(H77A,H77B,H77C), C79(H79A,
 H79B,H79C), C80(H80A,H80B,H80C), C87(H87A,H87B,H87C), C89(H89A,H89B,H89C),
 C90(H90A,H90B,H90C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.4808(2) 0.0760(2) 0.81754(19) 0.0273(6) Uani 1 1 d . . . . .
C2 C 0.4020(2) 0.1068(2) 0.85942(18) 0.0280(6) Uani 1 1 d . . . . .
C3 C 0.3284(2) 0.0578(2) 0.88771(19) 0.0289(7) Uani 1 1 d . . . . .
H3 H 0.327402 0.004907 0.876561 0.035 Uiso 1 1 calc R U . . .
C4 C 0.2569(2) 0.0857(2) 0.9319(2) 0.0309(7) Uani 1 1 d . . . . .
H4 H 0.207651 0.051813 0.949876 0.037 Uiso 1 1 calc R U . . .
C5 C 0.2565(2) 0.1624(2) 0.95003(19) 0.0297(7) Uani 1 1 d . . . . .
C6 C 0.3290(2) 0.2122(2) 0.9209(2) 0.0315(7) Uani 1 1 d . . . . .
H6 H 0.329677 0.265411 0.931539 0.038 Uiso 1 1 calc R U . . .
C7 C 0.4001(2) 0.1844(2) 0.8764(2) 0.0300(7) Uani 1 1 d . . . . .
H7 H 0.448764 0.219184 0.856985 0.036 Uiso 1 1 calc R U . . .
C8 C 0.1811(2) 0.1898(2) 1.0007(2) 0.0331(7) Uani 1 1 d . . . . .
C9 C 0.1347(3) 0.1326(3) 1.0696(2) 0.0433(9) Uani 1 1 d . . . . .
H9 H 0.152034 0.076111 1.084545 0.052 Uiso 1 1 calc R U . . .
C10 C 0.0634(3) 0.1571(3) 1.1167(3) 0.0565(12) Uani 1 1 d . . . . .
H10 H 0.032443 0.117090 1.163329 0.068 Uiso 1 1 calc R U . . .
C11 C 0.0372(3) 0.2382(3) 1.0969(3) 0.0550(12) Uani 1 1 d . . . . .
H11 H -0.011584 0.254550 1.129463 0.066 Uiso 1 1 calc R U . . .
C12 C 0.0824(3) 0.2957(3) 1.0293(3) 0.0528(11) Uani 1 1 d . . . . .
H12 H 0.064458 0.352000 1.014956 0.063 Uiso 1 1 calc R U . . .
C13 C 0.1544(3) 0.2724(3) 0.9814(2) 0.0414(9) Uani 1 1 d . . . . .
H13 H 0.185323 0.312943 0.935317 0.050 Uiso 1 1 calc R U . . .
C14 C 0.5602(2) 0.09757(19) 0.83828(19) 0.0263(6) Uani 1 1 d . . . . .
C15 C 0.5648(2) 0.08894(19) 0.92206(19) 0.0277(6) Uani 1 1 d . . . . .
H15 H 0.515620 0.075261 0.964098 0.033 Uiso 1 1 calc R U . . .
C16 C 0.6397(2) 0.1000(2) 0.94456(19) 0.0296(7) Uani 1 1 d . . . . .
H16 H 0.641156 0.093545 1.001845 0.035 Uiso 1 1 calc R U . . .
C17 C 0.7139(2) 0.1208(2) 0.8840(2) 0.0302(7) Uani 1 1 d . . . . .
C18 C 0.7071(2) 0.1351(2) 0.80000(19) 0.0297(7) Uani 1 1 d . . . . .
H18 H 0.754975 0.153274 0.757280 0.036 Uiso 1 1 calc R U . . .
C19 C 0.6320(2) 0.1234(2) 0.77774(19) 0.0286(7) Uani 1 1 d . . . . .
H19 H 0.629613 0.133078 0.720228 0.034 Uiso 1 1 calc R U . . .
C20 C 0.7956(2) 0.1230(2) 0.9095(2) 0.0351(7) Uani 1 1 d . . . . .
C21 C 0.8015(3) 0.1460(3) 0.9822(2) 0.0410(8) Uani 1 1 d . . . . .
H21 H 0.753085 0.164067 1.013760 0.049 Uiso 1 1 calc R U . . .
C22 C 0.8770(3) 0.1427(3) 1.0084(3) 0.0532(11) Uani 1 1 d . . . . .
H22 H 0.879767 0.158532 1.057672 0.064 Uiso 1 1 calc R U . . .
C23 C 0.9485(3) 0.1165(3) 0.9636(3) 0.0564(12) Uani 1 1 d . . . . .
H23 H 1.000106 0.113928 0.982119 0.068 Uiso 1 1 calc R U . . .
C24 C 0.9437(3) 0.0942(3) 0.8919(3) 0.0551(11) Uani 1 1 d . . . . .
H24 H 0.992471 0.075912 0.861063 0.066 Uiso 1 1 calc R U . . .
C25 C 0.8691(3) 0.0979(3) 0.8641(2) 0.0423(9) Uani 1 1 d . . . . .
H25 H 0.867453 0.083374 0.813902 0.051 Uiso 1 1 calc R U . . .
C26 C 0.3738(2) 0.1086(2) 0.6022(2) 0.0302(7) Uani 1 1 d . . . . .
C27 C 0.3207(2) 0.1073(2) 0.6802(2) 0.0313(7) Uani 1 1 d . . . . .
H27 H 0.328931 0.148023 0.707985 0.038 Uiso 1 1 calc R U . . .
C28 C 0.2565(2) 0.0473(2) 0.7167(2) 0.0328(7) Uani 1 1 d . . . . .
H28 H 0.222939 0.047041 0.769537 0.039 Uiso 1 1 calc R U . . .
C29 C 0.2407(2) -0.0139(2) 0.6752(2) 0.0322(7) Uani 1 1 d . . . . .
C30 C 0.2940(2) -0.0148(2) 0.6007(2) 0.0334(7) Uani 1 1 d . . . . .
H30 H 0.285201 -0.054901 0.572441 0.040 Uiso 1 1 calc R U . . .
C31 C 0.3618(2) 0.0437(2) 0.56603(19) 0.0306(7) Uani 1 1 d . . . . .
H31 H 0.399953 0.038919 0.517328 0.037 Uiso 1 1 calc R U . . .
C32 C 0.4416(3) 0.1727(2) 0.5606(2) 0.0417(9) Uani 1 1 d . . . . .
H32A H 0.489262 0.146929 0.532127 0.063 Uiso 1 1 calc R U . . .
H32B H 0.459203 0.194797 0.602806 0.063 Uiso 1 1 calc R U . . .
H32C H 0.420717 0.218354 0.519507 0.063 Uiso 1 1 calc R U . . .
C33 C 0.1681(3) -0.0748(3) 0.7140(2) 0.0458(10) Uani 1 1 d . . . . .
H33 H 0.154322 -0.079335 0.775402 0.055 Uiso 1 1 calc R U . . .
C34 C 0.0922(3) -0.0382(4) 0.6760(3) 0.0659(14) Uani 1 1 d . . . . .
H34A H 0.079519 0.016543 0.686337 0.099 Uiso 1 1 calc R U . . .
H34B H 0.043939 -0.075960 0.701890 0.099 Uiso 1 1 calc R U . . .
H34C H 0.104827 -0.031907 0.615496 0.099 Uiso 1 1 calc R U . . .
C35 C 0.1860(3) -0.1619(3) 0.7034(3) 0.0597(13) Uani 1 1 d . . . . .
H35A H 0.197015 -0.159369 0.643707 0.090 Uiso 1 1 calc R U . . .
H35B H 0.137525 -0.198612 0.732392 0.090 Uiso 1 1 calc R U . . .
H35C H 0.234893 -0.183991 0.727377 0.090 Uiso 1 1 calc R U . . .
C36 C 0.5995(2) -0.1531(2) 0.8286(2) 0.0327(7) Uani 1 1 d . . . . .
C37 C 0.6523(2) -0.0831(2) 0.8177(2) 0.0348(8) Uani 1 1 d . . . . .
H37 H 0.644462 -0.053256 0.859108 0.042 Uiso 1 1 calc R U . . .
C38 C 0.7163(2) -0.0576(2) 0.7460(2) 0.0341(7) Uani 1 1 d . . . . .
H38 H 0.748349 -0.008573 0.738015 0.041 Uiso 1 1 calc R U . . .
C39 C 0.7338(2) -0.1045(2) 0.6849(2) 0.0329(7) Uani 1 1 d . . . . .
C40 C 0.6804(2) -0.1702(2) 0.6936(2) 0.0331(7) Uani 1 1 d . . . . .
H40 H 0.689263 -0.200704 0.652770 0.040 Uiso 1 1 calc R U . . .
C41 C 0.6117(2) -0.1929(2) 0.7634(2) 0.0321(7) Uani 1 1 d . . . . .
H41 H 0.573690 -0.235700 0.765709 0.039 Uiso 1 1 calc R U . . .
C42 C 0.5314(3) -0.1826(3) 0.9046(2) 0.0448(9) Uani 1 1 d . . . . .
H42A H 0.489115 -0.214283 0.891259 0.067 Uiso 1 1 calc R U . . .
H42B H 0.505473 -0.134180 0.921533 0.067 Uiso 1 1 calc R U . . .
H42C H 0.555285 -0.218504 0.950566 0.067 Uiso 1 1 calc R U . . .
C43 C 0.8052(2) -0.0756(3) 0.6101(3) 0.0426(9) Uani 1 1 d . . . . .
H43 H 0.793298 -0.017231 0.579376 0.051 Uiso 1 1 calc R U . . .
C44 C 0.8871(3) -0.0733(5) 0.6399(4) 0.0805(18) Uani 1 1 d . . . . .
H44A H 0.898167 -0.128953 0.674086 0.121 Uiso 1 1 calc R U . . .
H44B H 0.882962 -0.033132 0.673471 0.121 Uiso 1 1 calc R U . . .
H44C H 0.932763 -0.056171 0.591298 0.121 Uiso 1 1 calc R U . . .
C45 C 0.8143(3) -0.1289(3) 0.5485(3) 0.0582(12) Uani 1 1 d . . . . .
H45A H 0.825607 -0.186735 0.577054 0.087 Uiso 1 1 calc R U . . .
H45B H 0.860556 -0.106903 0.501703 0.087 Uiso 1 1 calc R U . . .
H45C H 0.762402 -0.127257 0.527242 0.087 Uiso 1 1 calc R U . . .
C46 C 0.4964(2) 0.4257(2) 0.67889(18) 0.0269(6) Uani 1 1 d . . . . .
C47 C 0.5752(2) 0.39729(19) 0.63471(18) 0.0270(6) Uani 1 1 d . . . . .
C48 C 0.6413(2) 0.4522(2) 0.5903(2) 0.0326(7) Uani 1 1 d . . . . .
H48 H 0.637518 0.509389 0.590277 0.039 Uiso 1 1 calc R U . . .
C49 C 0.7126(2) 0.4245(2) 0.5462(2) 0.0341(7) Uani 1 1 d . . . . .
H49 H 0.756600 0.463301 0.516250 0.041 Uiso 1 1 calc R U . . .
C50 C 0.7212(2) 0.3408(2) 0.5449(2) 0.0317(7) Uani 1 1 d . . . . .
C51 C 0.6552(2) 0.2858(2) 0.58984(19) 0.0307(7) Uani 1 1 d . . . . .
H51 H 0.659229 0.228597 0.590114 0.037 Uiso 1 1 calc R U . . .
C52 C 0.5840(2) 0.3132(2) 0.63404(19) 0.0279(6) Uani 1 1 d . . . . .
H52 H 0.540258 0.274303 0.664442 0.034 Uiso 1 1 calc R U . . .
C53 C 0.7967(2) 0.3109(2) 0.4966(2) 0.0351(8) Uani 1 1 d . . . . .
C54 C 0.8444(3) 0.3659(3) 0.4255(2) 0.0435(9) Uani 1 1 d . . . . .
H54 H 0.827912 0.422340 0.407769 0.052 Uiso 1 1 calc R U . . .
C55 C 0.9155(3) 0.3380(3) 0.3809(3) 0.0529(11) Uani 1 1 d . . . . .
H55 H 0.947542 0.375956 0.333288 0.063 Uiso 1 1 calc R U . . .
C56 C 0.9403(3) 0.2557(3) 0.4051(3) 0.0549(12) Uani 1 1 d . . . . .
H56 H 0.989161 0.237217 0.374763 0.066 Uiso 1 1 calc R U . . .
C57 C 0.8927(3) 0.2008(3) 0.4743(3) 0.0511(11) Uani 1 1 d . . . . .
H57 H 0.908408 0.143941 0.490808 0.061 Uiso 1 1 calc R U . . .
C58 C 0.8222(3) 0.2284(3) 0.5197(3) 0.0418(9) Uani 1 1 d . . . . .
H58 H 0.790706 0.190138 0.567413 0.050 Uiso 1 1 calc R U . . .
C59 C 0.4180(2) 0.39471(19) 0.66493(19) 0.0272(6) Uani 1 1 d . . . . .
C60 C 0.4106(2) 0.3918(2) 0.58453(19) 0.0292(7) Uani 1 1 d . . . . .
H60 H 0.455905 0.410973 0.539018 0.035 Uiso 1 1 calc R U . . .
C61 C 0.3389(2) 0.3615(2) 0.56994(19) 0.0304(7) Uani 1 1 d . . . . .
H61 H 0.335919 0.360402 0.514709 0.036 Uiso 1 1 calc R U . . .
C62 C 0.2703(2) 0.3324(2) 0.6355(2) 0.0295(7) Uani 1 1 d . . . . .
C63 C 0.2782(2) 0.3350(2) 0.7155(2) 0.0321(7) Uani 1 1 d . . . . .
H63 H 0.232999 0.315486 0.761108 0.038 Uiso 1 1 calc R U . . .
C64 C 0.3500(2) 0.3650(2) 0.73027(19) 0.0288(7) Uani 1 1 d . . . . .
H64 H 0.353250 0.365519 0.785622 0.035 Uiso 1 1 calc R U . . .
C65 C 0.1931(2) 0.3001(2) 0.6195(2) 0.0347(7) Uani 1 1 d . . . . .
C66 C 0.1401(3) 0.2432(3) 0.6825(3) 0.0429(9) Uani 1 1 d . . . . .
H66 H 0.154270 0.223046 0.736182 0.051 Uiso 1 1 calc R U . . .
C67 C 0.0668(3) 0.2154(3) 0.6683(3) 0.0542(11) Uani 1 1 d . . . . .
H67 H 0.031275 0.176553 0.712201 0.065 Uiso 1 1 calc R U . . .
C68 C 0.0454(3) 0.2440(4) 0.5906(3) 0.0605(13) Uani 1 1 d . . . . .
H68 H -0.004932 0.224996 0.580965 0.073 Uiso 1 1 calc R U . . .
C69 C 0.0970(3) 0.3001(3) 0.5272(3) 0.0587(13) Uani 1 1 d . . . . .
H69 H 0.082194 0.319794 0.473699 0.070 Uiso 1 1 calc R U . . .
C70 C 0.1706(3) 0.3283(3) 0.5408(3) 0.0450(9) Uani 1 1 d . . . . .
H70 H 0.205973 0.366837 0.496464 0.054 Uiso 1 1 calc R U . . .
C71 C 0.3658(2) 0.6456(2) 0.6762(2) 0.0349(8) Uani 1 1 d . . . . .
C72 C 0.3175(2) 0.5714(2) 0.6935(2) 0.0351(8) Uani 1 1 d . . . . .
H72 H 0.323917 0.540324 0.653188 0.042 Uiso 1 1 calc R U . . .
C73 C 0.2601(2) 0.5432(2) 0.7697(2) 0.0370(8) Uani 1 1 d . . . . .
H73 H 0.231293 0.491384 0.781580 0.044 Uiso 1 1 calc R U . . .
C74 C 0.2444(2) 0.5914(2) 0.8296(2) 0.0376(8) Uani 1 1 d . . . . .
C75 C 0.2934(2) 0.6618(2) 0.8141(2) 0.0364(8) Uani 1 1 d . . . . .
H75 H 0.285491 0.694144 0.853368 0.044 Uiso 1 1 calc R U . . .
C76 C 0.3559(3) 0.6866(2) 0.7395(2) 0.0363(8) Uani 1 1 d . . . . .
H76 H 0.391988 0.732423 0.732691 0.044 Uiso 1 1 calc R U . . .
C77 C 0.4276(3) 0.6761(3) 0.5962(2) 0.0510(11) Uani 1 1 d . . . . .
H77A H 0.402716 0.720704 0.557389 0.077 Uiso 1 1 calc R U . . .
H77B H 0.442903 0.629787 0.570924 0.077 Uiso 1 1 calc R U . . .
H77C H 0.477599 0.697838 0.607704 0.077 Uiso 1 1 calc R U . . .
C78 C 0.1801(3) 0.5589(3) 0.9094(3) 0.0560(12) Uani 1 1 d . . . . .
H78 H 0.192668 0.498936 0.934112 0.067 Uiso 1 1 calc R U . . .
C79 C 0.1814(4) 0.6054(4) 0.9750(3) 0.0778(19) Uani 1 1 d . . . . .
H79A H 0.238466 0.607030 0.984658 0.117 Uiso 1 1 calc R U . . .
H79B H 0.144452 0.576595 1.027466 0.117 Uiso 1 1 calc R U . . .
H79C H 0.162095 0.662618 0.955225 0.117 Uiso 1 1 calc R U . . .
C80 C 0.0929(3) 0.5619(4) 0.8855(4) 0.0782(18) Uani 1 1 d . . . . .
H80A H 0.050646 0.539545 0.936100 0.117 Uiso 1 1 calc R U . . .
H80B H 0.093087 0.528063 0.846216 0.117 Uiso 1 1 calc R U . . .
H80C H 0.079901 0.619846 0.859150 0.117 Uiso 1 1 calc R U . . .
C81 C 0.6286(2) 0.3965(2) 0.8608(2) 0.0351(7) Uani 1 1 d . . . . .
C82 C 0.6238(2) 0.4499(2) 0.9127(2) 0.0361(8) Uani 1 1 d . . . . .
H82 H 0.582889 0.439100 0.962967 0.043 Uiso 1 1 calc R U . . .
C83 C 0.6790(2) 0.5201(2) 0.8919(2) 0.0347(8) Uani 1 1 d . . . . .
H83 H 0.675589 0.553632 0.929739 0.042 Uiso 1 1 calc R U . . .
C84 C 0.7377(2) 0.5408(2) 0.8175(2) 0.0324(7) Uani 1 1 d . . . . .
C85 C 0.7377(2) 0.4898(2) 0.7608(2) 0.0344(7) Uani 1 1 d . . . . .
H85 H 0.772998 0.505401 0.707003 0.041 Uiso 1 1 calc R U . . .
C86 C 0.6871(2) 0.4180(2) 0.7830(2) 0.0352(8) Uani 1 1 d . . . . .
H86 H 0.691647 0.383266 0.746086 0.042 Uiso 1 1 calc R U . . .
C87 C 0.5727(3) 0.3199(2) 0.8833(3) 0.0493(10) Uani 1 1 d . . . . .
H87A H 0.597897 0.272619 0.918592 0.074 Uiso 1 1 calc R U . . .
H87B H 0.566082 0.306415 0.831931 0.074 Uiso 1 1 calc R U . . .
H87C H 0.517855 0.331115 0.913778 0.074 Uiso 1 1 calc R U . . .
C88 C 0.7950(3) 0.6171(3) 0.7912(3) 0.0441(9) Uani 1 1 d . . . . .
H88 H 0.792662 0.647313 0.731882 0.053 Uiso 1 1 calc R U . . .
C89 C 0.7698(3) 0.6776(3) 0.8451(3) 0.0508(10) Uani 1 1 d . . . . .
H89A H 0.711107 0.692576 0.845321 0.076 Uiso 1 1 calc R U . . .
H89B H 0.804980 0.728124 0.822027 0.076 Uiso 1 1 calc R U . . .
H89C H 0.776988 0.650798 0.902535 0.076 Uiso 1 1 calc R U . . .
C90 C 0.8850(3) 0.5890(3) 0.7950(4) 0.0651(14) Uani 1 1 d . . . . .
H90A H 0.888713 0.559651 0.852947 0.098 Uiso 1 1 calc R U . . .
H90B H 0.922473 0.638002 0.775357 0.098 Uiso 1 1 calc R U . . .
H90C H 0.901414 0.551278 0.759270 0.098 Uiso 1 1 calc R U . . .
Cl1 Cl 0.34189(6) -0.13174(5) 0.81817(5) 0.03194(17) Uani 1 1 d . . . . .
Cl2 Cl 0.48921(5) -0.09726(5) 0.64018(5) 0.02960(16) Uani 1 1 d . . . . .
Cl3 Cl 0.63477(6) 0.06092(5) 0.58896(5) 0.03116(16) Uani 1 1 d . . . . .
Cl4 Cl 0.36351(6) 0.43527(5) 0.91493(5) 0.03280(17) Uani 1 1 d . . . . .
Cl5 Cl 0.49470(6) 0.60347(5) 0.85138(5) 0.03097(16) Uani 1 1 d . . . . .
Cl6 Cl 0.63326(6) 0.64178(5) 0.66421(5) 0.03408(18) Uani 1 1 d . . . . .
P1 P 0.48374(6) 0.01417(5) 0.75210(5) 0.02610(16) Uani 1 1 d . . . . .
P2 P 0.49643(6) 0.49045(5) 0.74044(5) 0.02585(16) Uani 1 1 d . . . . .
Ru1 Ru 0.37439(2) -0.01497(2) 0.69486(2) 0.02567(6) Uani 1 1 d . . . . .
Ru2 Ru 0.59838(2) -0.06008(2) 0.70655(2) 0.02600(6) Uani 1 1 d . . . . .
Ru3 Ru 0.38155(2) 0.55701(2) 0.79635(2) 0.02641(7) Uani 1 1 d . . . . .
Ru4 Ru 0.60935(2) 0.52582(2) 0.78907(2) 0.02635(7) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.487(4) . ?
C1 C14 1.489(5) . ?
C1 P1 1.697(3) . ?
C2 C3 1.405(5) . ?
C2 C7 1.393(4) . ?
C3 H3 0.9500 . ?
C3 C4 1.393(5) . ?
C4 H4 0.9500 . ?
C4 C5 1.391(5) . ?
C5 C6 1.398(5) . ?
C5 C8 1.487(5) . ?
C6 H6 0.9500 . ?
C6 C7 1.391(5) . ?
C7 H7 0.9500 . ?
C8 C9 1.393(5) . ?
C8 C13 1.395(5) . ?
C9 H9 0.9500 . ?
C9 C10 1.391(6) . ?
C10 H10 0.9500 . ?
C10 C11 1.371(7) . ?
C11 H11 0.9500 . ?
C11 C12 1.376(7) . ?
C12 H12 0.9500 . ?
C12 C13 1.396(5) . ?
C13 H13 0.9500 . ?
C14 C15 1.401(4) . ?
C14 C19 1.391(5) . ?
C15 H15 0.9500 . ?
C15 C16 1.384(5) . ?
C16 H16 0.9500 . ?
C16 C17 1.411(5) . ?
C17 C18 1.400(4) . ?
C17 C20 1.485(5) . ?
C18 H18 0.9500 . ?
C18 C19 1.386(5) . ?
C19 H19 0.9500 . ?
C20 C21 1.405(5) . ?
C20 C25 1.406(5) . ?
C21 H21 0.9500 . ?
C21 C22 1.384(6) . ?
C22 H22 0.9500 . ?
C22 C23 1.386(7) . ?
C23 H23 0.9500 . ?
C23 C24 1.378(7) . ?
C24 H24 0.9500 . ?
C24 C25 1.384(6) . ?
C25 H25 0.9500 . ?
C26 C27 1.423(5) . ?
C26 C31 1.415(5) . ?
C26 C32 1.495(5) . ?
C26 Ru1 2.218(3) . ?
C27 H27 0.9500 . ?
C27 C28 1.403(5) . ?
C27 Ru1 2.154(3) . ?
C28 H28 0.9500 . ?
C28 C29 1.442(5) . ?
C28 Ru1 2.167(3) . ?
C29 C30 1.386(5) . ?
C29 C33 1.511(5) . ?
C29 Ru1 2.272(4) . ?
C30 H30 0.9500 . ?
C30 C31 1.426(5) . ?
C30 Ru1 2.254(3) . ?
C31 H31 0.9500 . ?
C31 Ru1 2.177(3) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33 1.0000 . ?
C33 C34 1.537(6) . ?
C33 C35 1.518(7) . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 C37 1.425(5) . ?
C36 C41 1.413(5) . ?
C36 C42 1.506(5) . ?
C36 Ru2 2.218(3) . ?
C37 H37 0.9500 . ?
C37 C38 1.414(5) . ?
C37 Ru2 2.165(3) . ?
C38 H38 0.9500 . ?
C38 C39 1.435(5) . ?
C38 Ru2 2.164(4) . ?
C39 C40 1.382(5) . ?
C39 C43 1.525(5) . ?
C39 Ru2 2.296(3) . ?
C40 H40 0.9500 . ?
C40 C41 1.436(5) . ?
C40 Ru2 2.259(3) . ?
C41 H41 0.9500 . ?
C41 Ru2 2.176(3) . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 H43 1.0000 . ?
C43 C44 1.524(7) . ?
C43 C45 1.524(6) . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 C47 1.486(4) . ?
C46 C59 1.482(5) . ?
C46 P2 1.689(3) . ?
C47 C48 1.395(5) . ?
C47 C52 1.402(4) . ?
C48 H48 0.9500 . ?
C48 C49 1.388(5) . ?
C49 H49 0.9500 . ?
C49 C50 1.399(5) . ?
C50 C51 1.396(5) . ?
C50 C53 1.488(5) . ?
C51 H51 0.9500 . ?
C51 C52 1.387(5) . ?
C52 H52 0.9500 . ?
C53 C54 1.405(6) . ?
C53 C58 1.391(5) . ?
C54 H54 0.9500 . ?
C54 C55 1.392(6) . ?
C55 H55 0.9500 . ?
C55 C56 1.385(7) . ?
C56 H56 0.9500 . ?
C56 C57 1.386(7) . ?
C57 H57 0.9500 . ?
C57 C58 1.389(5) . ?
C58 H58 0.9500 . ?
C59 C60 1.403(4) . ?
C59 C64 1.400(5) . ?
C60 H60 0.9500 . ?
C60 C61 1.383(5) . ?
C61 H61 0.9500 . ?
C61 C62 1.407(5) . ?
C62 C63 1.397(4) . ?
C62 C65 1.489(5) . ?
C63 H63 0.9500 . ?
C63 C64 1.386(5) . ?
C64 H64 0.9500 . ?
C65 C66 1.389(6) . ?
C65 C70 1.401(5) . ?
C66 H66 0.9500 . ?
C66 C67 1.385(6) . ?
C67 H67 0.9500 . ?
C67 C68 1.379(7) . ?
C68 H68 0.9500 . ?
C68 C69 1.376(8) . ?
C69 H69 0.9500 . ?
C69 C70 1.389(6) . ?
C70 H70 0.9500 . ?
C71 C72 1.421(5) . ?
C71 C76 1.399(5) . ?
C71 C77 1.495(5) . ?
C71 Ru3 2.215(3) . ?
C72 H72 0.9500 . ?
C72 C73 1.410(5) . ?
C72 Ru3 2.156(3) . ?
C73 H73 0.9500 . ?
C73 C74 1.436(5) . ?
C73 Ru3 2.153(4) . ?
C74 C75 1.378(6) . ?
C74 C78 1.518(5) . ?
C74 Ru3 2.289(4) . ?
C75 H75 0.9500 . ?
C75 C76 1.431(5) . ?
C75 Ru3 2.263(3) . ?
C76 H76 0.9500 . ?
C76 Ru3 2.167(3) . ?
C77 H77A 0.9800 . ?
C77 H77B 0.9800 . ?
C77 H77C 0.9800 . ?
C78 H78 1.0000 . ?
C78 C79 1.520(8) . ?
C78 C80 1.550(8) . ?
C79 H79A 0.9800 . ?
C79 H79B 0.9800 . ?
C79 H79C 0.9800 . ?
C80 H80A 0.9800 . ?
C80 H80B 0.9800 . ?
C80 H80C 0.9800 . ?
C81 C82 1.399(5) . ?
C81 C86 1.432(5) . ?
C81 C87 1.513(5) . ?
C81 Ru4 2.206(3) . ?
C82 H82 0.9500 . ?
C82 C83 1.426(5) . ?
C82 Ru4 2.180(3) . ?
C83 H83 0.9500 . ?
C83 C84 1.390(5) . ?
C83 Ru4 2.237(3) . ?
C84 C85 1.443(5) . ?
C84 C88 1.518(5) . ?
C84 Ru4 2.278(4) . ?
C85 H85 0.9500 . ?
C85 C86 1.400(5) . ?
C85 Ru4 2.156(4) . ?
C86 H86 0.9500 . ?
C86 Ru4 2.170(3) . ?
C87 H87A 0.9800 . ?
C87 H87B 0.9800 . ?
C87 H87C 0.9800 . ?
C88 H88 1.0000 . ?
C88 C89 1.527(6) . ?
C88 C90 1.534(6) . ?
C89 H89A 0.9800 . ?
C89 H89B 0.9800 . ?
C89 H89C 0.9800 . ?
C90 H90A 0.9800 . ?
C90 H90B 0.9800 . ?
C90 H90C 0.9800 . ?
Cl1 Ru1 2.4154(8) . ?
Cl2 Ru1 2.4599(8) . ?
Cl2 Ru2 2.4645(8) . ?
Cl3 Ru2 2.4083(8) . ?
Cl4 Ru3 2.4089(8) . ?
Cl5 Ru3 2.4614(9) . ?
Cl5 Ru4 2.4621(8) . ?
Cl6 Ru4 2.4167(8) . ?
P1 Ru1 2.3163(9) . ?
P1 Ru2 2.3226(9) . ?
P2 Ru3 2.3131(9) . ?
P2 Ru4 2.3170(9) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C14 117.4(3) . . ?
C2 C1 P1 123.4(3) . . ?
C14 C1 P1 119.2(2) . . ?
C3 C2 C1 121.9(3) . . ?
C7 C2 C1 120.5(3) . . ?
C7 C2 C3 117.5(3) . . ?
C2 C3 H3 119.5 . . ?
C4 C3 C2 120.9(3) . . ?
C4 C3 H3 119.5 . . ?
C3 C4 H4 119.5 . . ?
C5 C4 C3 121.0(3) . . ?
C5 C4 H4 119.5 . . ?
C4 C5 C6 118.5(3) . . ?
C4 C5 C8 120.5(3) . . ?
C6 C5 C8 121.0(3) . . ?
C5 C6 H6 119.8 . . ?
C7 C6 C5 120.4(3) . . ?
C7 C6 H6 119.8 . . ?
C2 C7 H7 119.1 . . ?
C6 C7 C2 121.7(3) . . ?
C6 C7 H7 119.1 . . ?
C9 C8 C5 120.2(3) . . ?
C9 C8 C13 117.9(3) . . ?
C13 C8 C5 121.8(3) . . ?
C8 C9 H9 119.6 . . ?
C10 C9 C8 120.8(4) . . ?
C10 C9 H9 119.6 . . ?
C9 C10 H10 119.5 . . ?
C11 C10 C9 120.9(5) . . ?
C11 C10 H10 119.5 . . ?
C10 C11 H11 120.4 . . ?
C10 C11 C12 119.1(4) . . ?
C12 C11 H11 120.4 . . ?
C11 C12 H12 119.6 . . ?
C11 C12 C13 120.8(4) . . ?
C13 C12 H12 119.6 . . ?
C8 C13 C12 120.5(4) . . ?
C8 C13 H13 119.8 . . ?
C12 C13 H13 119.8 . . ?
C15 C14 C1 119.5(3) . . ?
C19 C14 C1 122.6(3) . . ?
C19 C14 C15 117.9(3) . . ?
C14 C15 H15 119.5 . . ?
C16 C15 C14 121.1(3) . . ?
C16 C15 H15 119.5 . . ?
C15 C16 H16 119.4 . . ?
C15 C16 C17 121.2(3) . . ?
C17 C16 H16 119.4 . . ?
C16 C17 C20 120.7(3) . . ?
C18 C17 C16 116.9(3) . . ?
C18 C17 C20 122.3(3) . . ?
C17 C18 H18 119.2 . . ?
C19 C18 C17 121.6(3) . . ?
C19 C18 H18 119.2 . . ?
C14 C19 H19 119.5 . . ?
C18 C19 C14 121.1(3) . . ?
C18 C19 H19 119.5 . . ?
C21 C20 C17 121.2(3) . . ?
C21 C20 C25 117.6(4) . . ?
C25 C20 C17 121.1(3) . . ?
C20 C21 H21 119.6 . . ?
C22 C21 C20 120.8(4) . . ?
C22 C21 H21 119.6 . . ?
C21 C22 H22 119.6 . . ?
C21 C22 C23 120.9(4) . . ?
C23 C22 H22 119.6 . . ?
C22 C23 H23 120.5 . . ?
C24 C23 C22 119.0(4) . . ?
C24 C23 H23 120.5 . . ?
C23 C24 H24 119.5 . . ?
C23 C24 C25 121.1(4) . . ?
C25 C24 H24 119.5 . . ?
C20 C25 H25 119.7 . . ?
C24 C25 C20 120.7(4) . . ?
C24 C25 H25 119.7 . . ?
C27 C26 C32 122.8(3) . . ?
C27 C26 Ru1 68.56(18) . . ?
C31 C26 C27 116.9(3) . . ?
C31 C26 C32 120.3(3) . . ?
C31 C26 Ru1 69.66(18) . . ?
C32 C26 Ru1 131.1(3) . . ?
C26 C27 H27 119.3 . . ?
C26 C27 Ru1 73.47(18) . . ?
C28 C27 C26 121.4(3) . . ?
C28 C27 H27 119.3 . . ?
C28 C27 Ru1 71.55(19) . . ?
Ru1 C27 H27 127.9 . . ?
C27 C28 H28 119.6 . . ?
C27 C28 C29 120.8(3) . . ?
C27 C28 Ru1 70.55(19) . . ?
C29 C28 H28 119.6 . . ?
C29 C28 Ru1 75.06(19) . . ?
Ru1 C28 H28 126.8 . . ?
C28 C29 C33 119.5(3) . . ?
C28 C29 Ru1 67.12(19) . . ?
C30 C29 C28 118.0(3) . . ?
C30 C29 C33 122.5(3) . . ?
C30 C29 Ru1 71.4(2) . . ?
C33 C29 Ru1 132.7(2) . . ?
C29 C30 H30 119.6 . . ?
C29 C30 C31 120.9(3) . . ?
C29 C30 Ru1 72.9(2) . . ?
C31 C30 H30 119.6 . . ?
C31 C30 Ru1 68.34(19) . . ?
Ru1 C30 H30 132.3 . . ?
C26 C31 C30 121.7(3) . . ?
C26 C31 H31 119.1 . . ?
C26 C31 Ru1 72.80(18) . . ?
C30 C31 H31 119.1 . . ?
C30 C31 Ru1 74.16(19) . . ?
Ru1 C31 H31 125.7 . . ?
C26 C32 H32A 109.5 . . ?
C26 C32 H32B 109.5 . . ?
C26 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C29 C33 H33 108.0 . . ?
C29 C33 C34 108.3(4) . . ?
C29 C33 C35 113.9(4) . . ?
C34 C33 H33 108.0 . . ?
C35 C33 H33 108.0 . . ?
C35 C33 C34 110.5(4) . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C33 C35 H35A 109.5 . . ?
C33 C35 H35B 109.5 . . ?
C33 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C37 C36 C42 122.1(3) . . ?
C37 C36 Ru2 69.03(19) . . ?
C41 C36 C37 117.2(3) . . ?
C41 C36 C42 120.6(4) . . ?
C41 C36 Ru2 69.64(19) . . ?
C42 C36 Ru2 131.0(3) . . ?
C36 C37 H37 119.6 . . ?
C36 C37 Ru2 73.04(19) . . ?
C38 C37 C36 120.7(3) . . ?
C38 C37 H37 119.6 . . ?
C38 C37 Ru2 70.9(2) . . ?
Ru2 C37 H37 128.7 . . ?
C37 C38 H38 119.4 . . ?
C37 C38 C39 121.2(3) . . ?
C37 C38 Ru2 71.0(2) . . ?
C39 C38 H38 119.4 . . ?
C39 C38 Ru2 76.3(2) . . ?
Ru2 C38 H38 125.0 . . ?
C38 C39 C43 119.0(3) . . ?
C38 C39 Ru2 66.31(19) . . ?
C40 C39 C38 117.9(3) . . ?
C40 C39 C43 122.9(3) . . ?
C40 C39 Ru2 70.9(2) . . ?
C43 C39 Ru2 130.4(2) . . ?
C39 C40 H40 119.5 . . ?
C39 C40 C41 121.1(3) . . ?
C39 C40 Ru2 73.80(19) . . ?
C41 C40 H40 119.5 . . ?
C41 C40 Ru2 68.01(18) . . ?
Ru2 C40 H40 131.6 . . ?
C36 C41 C40 121.4(3) . . ?
C36 C41 H41 119.3 . . ?
C36 C41 Ru2 72.87(19) . . ?
C40 C41 H41 119.3 . . ?
C40 C41 Ru2 74.28(19) . . ?
Ru2 C41 H41 125.3 . . ?
C36 C42 H42A 109.5 . . ?
C36 C42 H42B 109.5 . . ?
C36 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C39 C43 H43 107.6 . . ?
C44 C43 C39 110.2(4) . . ?
C44 C43 H43 107.6 . . ?
C45 C43 C39 113.3(4) . . ?
C45 C43 H43 107.6 . . ?
C45 C43 C44 110.2(4) . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C43 C45 H45A 109.5 . . ?
C43 C45 H45B 109.5 . . ?
C43 C45 H45C 109.5 . . ?
H45A C45 H45B 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C47 C46 P2 121.8(3) . . ?
C59 C46 C47 116.0(3) . . ?
C59 C46 P2 122.2(2) . . ?
C48 C47 C46 122.3(3) . . ?
C48 C47 C52 117.6(3) . . ?
C52 C47 C46 120.0(3) . . ?
C47 C48 H48 119.5 . . ?
C49 C48 C47 121.0(3) . . ?
C49 C48 H48 119.5 . . ?
C48 C49 H49 119.3 . . ?
C48 C49 C50 121.5(3) . . ?
C50 C49 H49 119.3 . . ?
C49 C50 C53 121.9(3) . . ?
C51 C50 C49 117.5(3) . . ?
C51 C50 C53 120.6(3) . . ?
C50 C51 H51 119.4 . . ?
C52 C51 C50 121.2(3) . . ?
C52 C51 H51 119.4 . . ?
C47 C52 H52 119.4 . . ?
C51 C52 C47 121.2(3) . . ?
C51 C52 H52 119.4 . . ?
C54 C53 C50 120.4(3) . . ?
C58 C53 C50 121.6(4) . . ?
C58 C53 C54 117.9(3) . . ?
C53 C54 H54 119.8 . . ?
C55 C54 C53 120.4(4) . . ?
C55 C54 H54 119.8 . . ?
C54 C55 H55 119.6 . . ?
C56 C55 C54 120.8(4) . . ?
C56 C55 H55 119.6 . . ?
C55 C56 H56 120.4 . . ?
C55 C56 C57 119.1(4) . . ?
C57 C56 H56 120.4 . . ?
C56 C57 H57 119.8 . . ?
C56 C57 C58 120.4(4) . . ?
C58 C57 H57 119.8 . . ?
C53 C58 H58 119.3 . . ?
C57 C58 C53 121.4(4) . . ?
C57 C58 H58 119.3 . . ?
C60 C59 C46 120.3(3) . . ?
C64 C59 C46 122.4(3) . . ?
C64 C59 C60 117.3(3) . . ?
C59 C60 H60 119.2 . . ?
C61 C60 C59 121.6(3) . . ?
C61 C60 H60 119.2 . . ?
C60 C61 H61 119.4 . . ?
C60 C61 C62 121.1(3) . . ?
C62 C61 H61 119.4 . . ?
C61 C62 C65 121.0(3) . . ?
C63 C62 C61 117.1(3) . . ?
C63 C62 C65 122.0(3) . . ?
C62 C63 H63 119.1 . . ?
C64 C63 C62 121.9(3) . . ?
C64 C63 H63 119.1 . . ?
C59 C64 H64 119.5 . . ?
C63 C64 C59 121.0(3) . . ?
C63 C64 H64 119.5 . . ?
C66 C65 C62 121.2(3) . . ?
C66 C65 C70 118.0(4) . . ?
C70 C65 C62 120.7(4) . . ?
C65 C66 H66 119.4 . . ?
C67 C66 C65 121.2(4) . . ?
C67 C66 H66 119.4 . . ?
C66 C67 H67 120.0 . . ?
C68 C67 C66 120.1(5) . . ?
C68 C67 H67 120.0 . . ?
C67 C68 H68 120.1 . . ?
C69 C68 C67 119.8(4) . . ?
C69 C68 H68 120.1 . . ?
C68 C69 H69 119.8 . . ?
C68 C69 C70 120.5(5) . . ?
C70 C69 H69 119.8 . . ?
C65 C70 H70 119.8 . . ?
C69 C70 C65 120.4(5) . . ?
C69 C70 H70 119.8 . . ?
C72 C71 C77 121.8(3) . . ?
C72 C71 Ru3 68.76(19) . . ?
C76 C71 C72 116.7(3) . . ?
C76 C71 C77 121.4(4) . . ?
C76 C71 Ru3 69.53(19) . . ?
C77 C71 Ru3 130.0(3) . . ?
C71 C72 H72 119.5 . . ?
C71 C72 Ru3 73.3(2) . . ?
C73 C72 C71 120.9(3) . . ?
C73 C72 H72 119.5 . . ?
C73 C72 Ru3 70.8(2) . . ?
Ru3 C72 H72 128.7 . . ?
C72 C73 H73 119.5 . . ?
C72 C73 C74 121.1(3) . . ?
C72 C73 Ru3 71.0(2) . . ?
C74 C73 H73 119.5 . . ?
C74 C73 Ru3 76.4(2) . . ?
Ru3 C73 H73 124.8 . . ?
C73 C74 C78 118.6(4) . . ?
C73 C74 Ru3 66.1(2) . . ?
C75 C74 C73 117.7(3) . . ?
C75 C74 C78 123.5(4) . . ?
C75 C74 Ru3 71.3(2) . . ?
C78 C74 Ru3 130.2(3) . . ?
C74 C75 H75 119.7 . . ?
C74 C75 C76 120.6(3) . . ?
C74 C75 Ru3 73.4(2) . . ?
C76 C75 H75 119.7 . . ?
C76 C75 Ru3 67.58(19) . . ?
Ru3 C75 H75 132.3 . . ?
C71 C76 C75 122.3(4) . . ?
C71 C76 H76 118.8 . . ?
C71 C76 Ru3 73.3(2) . . ?
C75 C76 H76 118.8 . . ?
C75 C76 Ru3 74.8(2) . . ?
Ru3 C76 H76 124.8 . . ?
C71 C77 H77A 109.5 . . ?
C71 C77 H77B 109.5 . . ?
C71 C77 H77C 109.5 . . ?
H77A C77 H77B 109.5 . . ?
H77A C77 H77C 109.5 . . ?
H77B C77 H77C 109.5 . . ?
C74 C78 H78 107.8 . . ?
C74 C78 C79 113.5(4) . . ?
C74 C78 C80 108.2(4) . . ?
C79 C78 H78 107.8 . . ?
C79 C78 C80 111.5(4) . . ?
C80 C78 H78 107.8 . . ?
C78 C79 H79A 109.5 . . ?
C78 C79 H79B 109.5 . . ?
C78 C79 H79C 109.5 . . ?
H79A C79 H79B 109.5 . . ?
H79A C79 H79C 109.5 . . ?
H79B C79 H79C 109.5 . . ?
C78 C80 H80A 109.5 . . ?
C78 C80 H80B 109.5 . . ?
C78 C80 H80C 109.5 . . ?
H80A C80 H80B 109.5 . . ?
H80A C80 H80C 109.5 . . ?
H80B C80 H80C 109.5 . . ?
C82 C81 C86 117.7(3) . . ?
C82 C81 C87 122.3(4) . . ?
C82 C81 Ru4 70.41(19) . . ?
C86 C81 C87 120.1(4) . . ?
C86 C81 Ru4 69.56(19) . . ?
C87 C81 Ru4 129.8(3) . . ?
C81 C82 H82 119.3 . . ?
C81 C82 C83 121.4(3) . . ?
C81 C82 Ru4 72.39(19) . . ?
C83 C82 H82 119.3 . . ?
C83 C82 Ru4 73.35(19) . . ?
Ru4 C82 H82 127.0 . . ?
C82 C83 H83 119.1 . . ?
C82 C83 Ru4 69.0(2) . . ?
C84 C83 C82 121.7(3) . . ?
C84 C83 H83 119.1 . . ?
C84 C83 Ru4 73.7(2) . . ?
Ru4 C83 H83 131.0 . . ?
C83 C84 C85 116.8(3) . . ?
C83 C84 C88 123.3(3) . . ?
C83 C84 Ru4 70.5(2) . . ?
C85 C84 C88 119.7(3) . . ?
C85 C84 Ru4 66.5(2) . . ?
C88 C84 Ru4 129.9(3) . . ?
C84 C85 H85 119.2 . . ?
C84 C85 Ru4 75.7(2) . . ?
C86 C85 C84 121.6(3) . . ?
C86 C85 H85 119.2 . . ?
C86 C85 Ru4 71.7(2) . . ?
Ru4 C85 H85 125.2 . . ?
C81 C86 H86 119.8 . . ?
C81 C86 Ru4 72.26(19) . . ?
C85 C86 C81 120.5(3) . . ?
C85 C86 H86 119.8 . . ?
C85 C86 Ru4 70.6(2) . . ?
Ru4 C86 H86 130.0 . . ?
C81 C87 H87A 109.5 . . ?
C81 C87 H87B 109.5 . . ?
C81 C87 H87C 109.5 . . ?
H87A C87 H87B 109.5 . . ?
H87A C87 H87C 109.5 . . ?
H87B C87 H87C 109.5 . . ?
C84 C88 H88 108.2 . . ?
C84 C88 C89 112.8(4) . . ?
C84 C88 C90 109.4(4) . . ?
C89 C88 H88 108.2 . . ?
C89 C88 C90 109.8(4) . . ?
C90 C88 H88 108.2 . . ?
C88 C89 H89A 109.5 . . ?
C88 C89 H89B 109.5 . . ?
C88 C89 H89C 109.5 . . ?
H89A C89 H89B 109.5 . . ?
H89A C89 H89C 109.5 . . ?
H89B C89 H89C 109.5 . . ?
C88 C90 H90A 109.5 . . ?
C88 C90 H90B 109.5 . . ?
C88 C90 H90C 109.5 . . ?
H90A C90 H90B 109.5 . . ?
H90A C90 H90C 109.5 . . ?
H90B C90 H90C 109.5 . . ?
Ru1 Cl2 Ru2 98.77(3) . . ?
Ru3 Cl5 Ru4 98.11(3) . . ?
C1 P1 Ru1 126.74(12) . . ?
C1 P1 Ru2 125.85(12) . . ?
Ru1 P1 Ru2 107.38(3) . . ?
C46 P2 Ru3 126.11(13) . . ?
C46 P2 Ru4 126.98(12) . . ?
Ru3 P2 Ru4 106.88(3) . . ?
C26 Ru1 C29 79.90(13) . . ?
C26 Ru1 C30 67.40(13) . . ?
C26 Ru1 Cl1 163.30(9) . . ?
C26 Ru1 Cl2 108.58(9) . . ?
C26 Ru1 P1 96.85(9) . . ?
C27 Ru1 C26 37.97(12) . . ?
C27 Ru1 C28 37.90(14) . . ?
C27 Ru1 C29 67.92(13) . . ?
C27 Ru1 C30 79.26(13) . . ?
C27 Ru1 C31 67.88(12) . . ?
C27 Ru1 Cl1 125.51(9) . . ?
C27 Ru1 Cl2 145.28(10) . . ?
C27 Ru1 P1 95.13(10) . . ?
C28 Ru1 C26 68.39(13) . . ?
C28 Ru1 C29 37.82(13) . . ?
C28 Ru1 C30 66.48(13) . . ?
C28 Ru1 C31 80.09(13) . . ?
C28 Ru1 Cl1 95.79(10) . . ?
C28 Ru1 Cl2 163.34(9) . . ?
C28 Ru1 P1 119.33(10) . . ?
C29 Ru1 Cl1 90.82(9) . . ?
C29 Ru1 Cl2 126.20(9) . . ?
C29 Ru1 P1 156.51(9) . . ?
C30 Ru1 C29 35.67(12) . . ?
C30 Ru1 Cl1 112.19(10) . . ?
C30 Ru1 Cl2 97.04(9) . . ?
C30 Ru1 P1 160.78(10) . . ?
C31 Ru1 C26 37.54(12) . . ?
C31 Ru1 C29 66.68(13) . . ?
C31 Ru1 C30 37.50(13) . . ?
C31 Ru1 Cl1 148.40(10) . . ?
C31 Ru1 Cl2 88.09(9) . . ?
C31 Ru1 P1 123.38(10) . . ?
Cl1 Ru1 Cl2 88.11(3) . . ?
P1 Ru1 Cl1 86.11(3) . . ?
P1 Ru1 Cl2 77.02(3) . . ?
C36 Ru2 C39 79.49(13) . . ?
C36 Ru2 C40 67.40(12) . . ?
C36 Ru2 Cl2 110.20(10) . . ?
C36 Ru2 Cl3 160.38(10) . . ?
C36 Ru2 P1 96.99(9) . . ?
C37 Ru2 C36 37.93(14) . . ?
C37 Ru2 C39 67.54(13) . . ?
C37 Ru2 C40 79.07(12) . . ?
C37 Ru2 C41 67.84(13) . . ?
C37 Ru2 Cl2 147.34(11) . . ?
C37 Ru2 Cl3 122.60(11) . . ?
C37 Ru2 P1 96.97(9) . . ?
C38 Ru2 C36 68.53(14) . . ?
C38 Ru2 C37 38.11(14) . . ?
C38 Ru2 C39 37.41(12) . . ?
C38 Ru2 C40 66.09(13) . . ?
C38 Ru2 C41 80.15(14) . . ?
C38 Ru2 Cl2 160.97(9) . . ?
C38 Ru2 Cl3 93.06(10) . . ?
C38 Ru2 P1 122.13(9) . . ?
C39 Ru2 Cl2 123.83(9) . . ?
C39 Ru2 Cl3 89.96(9) . . ?
C39 Ru2 P1 159.12(9) . . ?
C40 Ru2 C39 35.31(13) . . ?
C40 Ru2 Cl2 95.54(10) . . ?
C40 Ru2 Cl3 112.30(9) . . ?
C40 Ru2 P1 159.43(10) . . ?
C41 Ru2 C36 37.50(12) . . ?
C41 Ru2 C39 66.47(14) . . ?
C41 Ru2 C40 37.71(13) . . ?
C41 Ru2 Cl2 88.11(10) . . ?
C41 Ru2 Cl3 149.28(9) . . ?
C41 Ru2 P1 122.08(10) . . ?
Cl3 Ru2 Cl2 89.42(3) . . ?
P1 Ru2 Cl2 76.82(3) . . ?
P1 Ru2 Cl3 86.97(3) . . ?
C71 Ru3 C74 79.59(13) . . ?
C71 Ru3 C75 67.22(13) . . ?
C71 Ru3 Cl4 160.55(11) . . ?
C71 Ru3 Cl5 111.18(11) . . ?
C71 Ru3 P2 96.06(9) . . ?
C72 Ru3 C71 37.92(14) . . ?
C72 Ru3 C74 67.68(14) . . ?
C72 Ru3 C75 78.89(13) . . ?
C72 Ru3 C76 67.48(14) . . ?
C72 Ru3 Cl4 122.67(11) . . ?
C72 Ru3 Cl5 148.26(11) . . ?
C72 Ru3 P2 95.81(10) . . ?
C73 Ru3 C71 68.64(14) . . ?
C73 Ru3 C72 38.20(15) . . ?
C73 Ru3 C74 37.55(14) . . ?
C73 Ru3 C75 66.07(14) . . ?
C73 Ru3 C76 79.96(15) . . ?
C73 Ru3 Cl4 93.62(10) . . ?
C73 Ru3 Cl5 161.31(10) . . ?
C73 Ru3 P2 121.13(10) . . ?
C74 Ru3 Cl4 91.17(9) . . ?
C74 Ru3 Cl5 123.89(11) . . ?
C74 Ru3 P2 158.37(11) . . ?
C75 Ru3 C74 35.25(14) . . ?
C75 Ru3 Cl4 113.84(9) . . ?
C75 Ru3 Cl5 96.21(11) . . ?
C75 Ru3 P2 159.01(10) . . ?
C76 Ru3 C71 37.20(13) . . ?
C76 Ru3 C74 66.37(14) . . ?
C76 Ru3 C75 37.62(13) . . ?
C76 Ru3 Cl4 150.76(10) . . ?
C76 Ru3 Cl5 89.40(11) . . ?
C76 Ru3 P2 121.60(10) . . ?
Cl4 Ru3 Cl5 88.19(3) . . ?
P2 Ru3 Cl4 86.22(3) . . ?
P2 Ru3 Cl5 77.54(3) . . ?
C81 Ru4 C83 67.34(14) . . ?
C81 Ru4 C84 80.10(14) . . ?
C81 Ru4 Cl5 117.22(10) . . ?
C81 Ru4 Cl6 153.08(10) . . ?
C81 Ru4 P2 94.12(10) . . ?
C82 Ru4 C81 37.21(14) . . ?
C82 Ru4 C83 37.63(14) . . ?
C82 Ru4 C84 66.93(13) . . ?
C82 Ru4 Cl5 91.18(10) . . ?
C82 Ru4 Cl6 157.53(11) . . ?
C82 Ru4 P2 115.52(11) . . ?
C83 Ru4 C84 35.86(13) . . ?
C83 Ru4 Cl5 91.82(9) . . ?
C83 Ru4 Cl6 119.90(10) . . ?
C83 Ru4 P2 151.68(10) . . ?
C84 Ru4 Cl5 116.59(9) . . ?
C84 Ru4 Cl6 92.92(9) . . ?
C84 Ru4 P2 165.95(9) . . ?
C85 Ru4 C81 68.61(14) . . ?
C85 Ru4 C82 80.16(14) . . ?
C85 Ru4 C83 66.62(13) . . ?
C85 Ru4 C84 37.87(12) . . ?
C85 Ru4 C86 37.78(14) . . ?
C85 Ru4 Cl5 154.33(10) . . ?
C85 Ru4 Cl6 89.90(10) . . ?
C85 Ru4 P2 128.08(10) . . ?
C86 Ru4 C81 38.19(14) . . ?
C86 Ru4 C82 67.68(13) . . ?
C86 Ru4 C83 79.15(13) . . ?
C86 Ru4 C84 67.82(14) . . ?
C86 Ru4 Cl5 155.39(10) . . ?
C86 Ru4 Cl6 115.18(10) . . ?
C86 Ru4 P2 99.76(11) . . ?
Cl6 Ru4 Cl5 89.22(3) . . ?
P2 Ru4 Cl5 77.45(3) . . ?
P2 Ru4 Cl6 86.48(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 175.5(3) . . . . ?
C1 C2 C7 C6 -175.2(3) . . . . ?
C1 C14 C15 C16 173.2(3) . . . . ?
C1 C14 C19 C18 -173.6(3) . . . . ?
C2 C1 C14 C15 45.1(4) . . . . ?
C2 C1 C14 C19 -137.4(3) . . . . ?
C2 C1 P1 Ru1 12.1(3) . . . . ?
C2 C1 P1 Ru2 -166.0(2) . . . . ?
C2 C3 C4 C5 -0.7(5) . . . . ?
C3 C2 C7 C6 1.2(5) . . . . ?
C3 C4 C5 C6 1.8(5) . . . . ?
C3 C4 C5 C8 -177.0(3) . . . . ?
C4 C5 C6 C7 -1.4(5) . . . . ?
C4 C5 C8 C9 39.9(5) . . . . ?
C4 C5 C8 C13 -139.9(4) . . . . ?
C5 C6 C7 C2 -0.1(5) . . . . ?
C5 C8 C9 C10 -179.0(4) . . . . ?
C5 C8 C13 C12 178.8(4) . . . . ?
C6 C5 C8 C9 -138.9(4) . . . . ?
C6 C5 C8 C13 41.3(5) . . . . ?
C7 C2 C3 C4 -0.8(5) . . . . ?
C8 C5 C6 C7 177.4(3) . . . . ?
C8 C9 C10 C11 -0.3(7) . . . . ?
C9 C8 C13 C12 -1.0(6) . . . . ?
C9 C10 C11 C12 0.1(7) . . . . ?
C10 C11 C12 C13 -0.3(7) . . . . ?
C11 C12 C13 C8 0.8(7) . . . . ?
C13 C8 C9 C10 0.8(6) . . . . ?
C14 C1 C2 C3 -140.9(3) . . . . ?
C14 C1 C2 C7 35.3(4) . . . . ?
C14 C1 P1 Ru1 -171.13(18) . . . . ?
C14 C1 P1 Ru2 10.8(3) . . . . ?
C14 C15 C16 C17 0.3(5) . . . . ?
C15 C14 C19 C18 4.0(5) . . . . ?
C15 C16 C17 C18 4.2(5) . . . . ?
C15 C16 C17 C20 -172.9(3) . . . . ?
C16 C17 C18 C19 -4.6(5) . . . . ?
C16 C17 C20 C21 -32.1(5) . . . . ?
C16 C17 C20 C25 144.6(4) . . . . ?
C17 C18 C19 C14 0.6(5) . . . . ?
C17 C20 C21 C22 175.8(4) . . . . ?
C17 C20 C25 C24 -175.1(4) . . . . ?
C18 C17 C20 C21 151.0(4) . . . . ?
C18 C17 C20 C25 -32.3(5) . . . . ?
C19 C14 C15 C16 -4.4(5) . . . . ?
C20 C17 C18 C19 172.4(3) . . . . ?
C20 C21 C22 C23 -0.1(7) . . . . ?
C21 C20 C25 C24 1.7(6) . . . . ?
C21 C22 C23 C24 0.4(7) . . . . ?
C22 C23 C24 C25 0.3(8) . . . . ?
C23 C24 C25 C20 -1.3(7) . . . . ?
C25 C20 C21 C22 -1.0(6) . . . . ?
C26 C27 C28 C29 -1.7(5) . . . . ?
C26 C27 C28 Ru1 56.3(3) . . . . ?
C27 C26 C31 C30 6.8(5) . . . . ?
C27 C26 C31 Ru1 -51.3(3) . . . . ?
C27 C28 C29 C30 3.8(5) . . . . ?
C27 C28 C29 C33 -176.8(3) . . . . ?
C27 C28 C29 Ru1 55.9(3) . . . . ?
C28 C29 C30 C31 -0.6(5) . . . . ?
C28 C29 C30 Ru1 50.0(3) . . . . ?
C28 C29 C33 C34 93.8(4) . . . . ?
C28 C29 C33 C35 -142.9(4) . . . . ?
C29 C30 C31 C26 -4.9(5) . . . . ?
C29 C30 C31 Ru1 52.7(3) . . . . ?
C30 C29 C33 C34 -86.9(5) . . . . ?
C30 C29 C33 C35 36.5(5) . . . . ?
C31 C26 C27 C28 -3.5(5) . . . . ?
C31 C26 C27 Ru1 51.9(3) . . . . ?
C32 C26 C27 C28 178.6(3) . . . . ?
C32 C26 C27 Ru1 -126.0(3) . . . . ?
C32 C26 C31 C30 -175.3(3) . . . . ?
C32 C26 C31 Ru1 126.6(3) . . . . ?
C33 C29 C30 C31 -180.0(3) . . . . ?
C33 C29 C30 Ru1 -129.3(3) . . . . ?
C36 C37 C38 C39 -4.3(5) . . . . ?
C36 C37 C38 Ru2 55.6(3) . . . . ?
C37 C36 C41 C40 6.9(5) . . . . ?
C37 C36 C41 Ru2 -51.7(3) . . . . ?
C37 C38 C39 C40 6.9(5) . . . . ?
C37 C38 C39 C43 -178.2(3) . . . . ?
C37 C38 C39 Ru2 57.3(3) . . . . ?
C38 C39 C40 C41 -2.5(5) . . . . ?
C38 C39 C40 Ru2 48.4(3) . . . . ?
C38 C39 C43 C44 58.5(5) . . . . ?
C38 C39 C43 C45 -177.5(3) . . . . ?
C39 C40 C41 C36 -4.4(5) . . . . ?
C39 C40 C41 Ru2 53.5(3) . . . . ?
C40 C39 C43 C44 -126.8(4) . . . . ?
C40 C39 C43 C45 -2.8(5) . . . . ?
C41 C36 C37 C38 -2.6(5) . . . . ?
C41 C36 C37 Ru2 52.0(3) . . . . ?
C42 C36 C37 C38 179.3(3) . . . . ?
C42 C36 C37 Ru2 -126.1(3) . . . . ?
C42 C36 C41 C40 -174.9(3) . . . . ?
C42 C36 C41 Ru2 126.4(3) . . . . ?
C43 C39 C40 C41 -177.3(3) . . . . ?
C43 C39 C40 Ru2 -126.4(3) . . . . ?
C46 C47 C48 C49 -176.8(3) . . . . ?
C46 C47 C52 C51 176.8(3) . . . . ?
C46 C59 C60 C61 178.7(3) . . . . ?
C46 C59 C64 C63 -178.8(3) . . . . ?
C47 C46 C59 C60 -41.9(4) . . . . ?
C47 C46 C59 C64 136.1(3) . . . . ?
C47 C46 P2 Ru3 169.67(19) . . . . ?
C47 C46 P2 Ru4 -12.8(3) . . . . ?
C47 C48 C49 C50 -0.4(5) . . . . ?
C48 C47 C52 C51 -0.9(5) . . . . ?
C48 C49 C50 C51 -0.1(5) . . . . ?
C48 C49 C50 C53 178.9(3) . . . . ?
C49 C50 C51 C52 0.0(5) . . . . ?
C49 C50 C53 C54 -26.8(5) . . . . ?
C49 C50 C53 C58 153.5(4) . . . . ?
C50 C51 C52 C47 0.5(5) . . . . ?
C50 C53 C54 C55 179.3(4) . . . . ?
C50 C53 C58 C57 180.0(4) . . . . ?
C51 C50 C53 C54 152.1(4) . . . . ?
C51 C50 C53 C58 -27.6(5) . . . . ?
C52 C47 C48 C49 0.9(5) . . . . ?
C53 C50 C51 C52 -179.0(3) . . . . ?
C53 C54 C55 C56 0.6(7) . . . . ?
C54 C53 C58 C57 0.2(6) . . . . ?
C54 C55 C56 C57 0.5(7) . . . . ?
C55 C56 C57 C58 -1.3(7) . . . . ?
C56 C57 C58 C53 0.9(6) . . . . ?
C58 C53 C54 C55 -1.0(6) . . . . ?
C59 C46 C47 C48 133.1(3) . . . . ?
C59 C46 C47 C52 -44.5(4) . . . . ?
C59 C46 P2 Ru3 -9.6(3) . . . . ?
C59 C46 P2 Ru4 167.92(19) . . . . ?
C59 C60 C61 C62 0.0(5) . . . . ?
C60 C59 C64 C63 -0.7(5) . . . . ?
C60 C61 C62 C63 -0.4(5) . . . . ?
C60 C61 C62 C65 179.9(3) . . . . ?
C61 C62 C63 C64 0.3(5) . . . . ?
C61 C62 C65 C66 154.6(3) . . . . ?
C61 C62 C65 C70 -27.4(5) . . . . ?
C62 C63 C64 C59 0.3(5) . . . . ?
C62 C65 C66 C67 177.7(4) . . . . ?
C62 C65 C70 C69 -177.6(4) . . . . ?
C63 C62 C65 C66 -25.0(5) . . . . ?
C63 C62 C65 C70 153.0(3) . . . . ?
C64 C59 C60 C61 0.6(5) . . . . ?
C65 C62 C63 C64 179.9(3) . . . . ?
C65 C66 C67 C68 0.1(6) . . . . ?
C66 C65 C70 C69 0.5(6) . . . . ?
C66 C67 C68 C69 0.1(7) . . . . ?
C67 C68 C69 C70 0.0(7) . . . . ?
C68 C69 C70 C65 -0.3(7) . . . . ?
C70 C65 C66 C67 -0.4(6) . . . . ?
C71 C72 C73 C74 4.3(5) . . . . ?
C71 C72 C73 Ru3 -55.7(3) . . . . ?
C72 C71 C76 C75 -7.4(5) . . . . ?
C72 C71 C76 Ru3 51.6(3) . . . . ?
C72 C73 C74 C75 -6.4(5) . . . . ?
C72 C73 C74 C78 178.3(3) . . . . ?
C72 C73 C74 Ru3 -57.5(3) . . . . ?
C73 C74 C75 C76 1.7(5) . . . . ?
C73 C74 C75 Ru3 -48.6(3) . . . . ?
C73 C74 C78 C79 168.5(4) . . . . ?
C73 C74 C78 C80 -67.1(5) . . . . ?
C74 C75 C76 C71 5.4(5) . . . . ?
C74 C75 C76 Ru3 -52.9(3) . . . . ?
C75 C74 C78 C79 -6.6(6) . . . . ?
C75 C74 C78 C80 117.9(5) . . . . ?
C76 C71 C72 C73 2.6(5) . . . . ?
C76 C71 C72 Ru3 -52.0(3) . . . . ?
C77 C71 C72 C73 179.4(3) . . . . ?
C77 C71 C72 Ru3 124.8(3) . . . . ?
C77 C71 C76 C75 175.7(3) . . . . ?
C77 C71 C76 Ru3 -125.2(3) . . . . ?
C78 C74 C75 C76 176.7(4) . . . . ?
C78 C74 C75 Ru3 126.4(4) . . . . ?
C81 C82 C83 C84 2.7(6) . . . . ?
C81 C82 C83 Ru4 56.5(3) . . . . ?
C82 C81 C86 C85 0.4(5) . . . . ?
C82 C81 C86 Ru4 -53.2(3) . . . . ?
C82 C83 C84 C85 2.5(5) . . . . ?
C82 C83 C84 C88 177.3(3) . . . . ?
C82 C83 C84 Ru4 51.7(3) . . . . ?
C83 C84 C85 C86 -6.3(5) . . . . ?
C83 C84 C85 Ru4 51.1(3) . . . . ?
C83 C84 C88 C89 -11.7(5) . . . . ?
C83 C84 C88 C90 110.7(4) . . . . ?
C84 C85 C86 C81 4.9(5) . . . . ?
C84 C85 C86 Ru4 59.3(3) . . . . ?
C85 C84 C88 C89 162.9(3) . . . . ?
C85 C84 C88 C90 -74.6(5) . . . . ?
C86 C81 C82 C83 -4.2(5) . . . . ?
C86 C81 C82 Ru4 52.8(3) . . . . ?
C87 C81 C82 C83 177.8(3) . . . . ?
C87 C81 C82 Ru4 -125.3(3) . . . . ?
C87 C81 C86 C85 178.5(3) . . . . ?
C87 C81 C86 Ru4 124.9(3) . . . . ?
C88 C84 C85 C86 178.7(3) . . . . ?
C88 C84 C85 Ru4 -123.9(3) . . . . ?
P1 C1 C2 C3 35.9(4) . . . . ?
P1 C1 C2 C7 -147.9(3) . . . . ?
P1 C1 C14 C15 -131.9(3) . . . . ?
P1 C1 C14 C19 45.6(4) . . . . ?
P2 C46 C47 C48 -46.3(4) . . . . ?
P2 C46 C47 C52 136.1(3) . . . . ?
P2 C46 C59 C60 137.4(3) . . . . ?
P2 C46 C59 C64 -44.6(4) . . . . ?
Ru1 C26 C27 C28 -55.4(3) . . . . ?
Ru1 C26 C31 C30 58.2(3) . . . . ?
Ru1 C27 C28 C29 -58.0(3) . . . . ?
Ru1 C28 C29 C30 -52.1(3) . . . . ?
Ru1 C28 C29 C33 127.3(3) . . . . ?
Ru1 C29 C30 C31 -50.6(3) . . . . ?
Ru1 C29 C33 C34 178.8(3) . . . . ?
Ru1 C29 C33 C35 -57.8(5) . . . . ?
Ru1 C30 C31 C26 -57.5(3) . . . . ?
Ru2 C36 C37 C38 -54.6(3) . . . . ?
Ru2 C36 C41 C40 58.6(3) . . . . ?
Ru2 C37 C38 C39 -59.9(3) . . . . ?
Ru2 C38 C39 C40 -50.5(3) . . . . ?
Ru2 C38 C39 C43 124.5(3) . . . . ?
Ru2 C39 C40 C41 -50.9(3) . . . . ?
Ru2 C39 C43 C44 140.9(4) . . . . ?
Ru2 C39 C43 C45 -95.1(4) . . . . ?
Ru2 C40 C41 C36 -58.0(3) . . . . ?
Ru3 C71 C72 C73 54.6(3) . . . . ?
Ru3 C71 C76 C75 -59.1(3) . . . . ?
Ru3 C72 C73 C74 60.1(3) . . . . ?
Ru3 C73 C74 C75 51.1(3) . . . . ?
Ru3 C73 C74 C78 -124.3(3) . . . . ?
Ru3 C74 C75 C76 50.3(3) . . . . ?
Ru3 C74 C78 C79 86.7(5) . . . . ?
Ru3 C74 C78 C80 -148.9(3) . . . . ?
Ru3 C75 C76 C71 58.3(3) . . . . ?
Ru4 C81 C82 C83 -56.9(3) . . . . ?
Ru4 C81 C86 C85 53.6(3) . . . . ?
Ru4 C82 C83 C84 -53.8(3) . . . . ?
Ru4 C83 C84 C85 -49.2(3) . . . . ?
Ru4 C83 C84 C88 125.6(4) . . . . ?
Ru4 C84 C85 C86 -57.4(3) . . . . ?
Ru4 C84 C88 C89 79.9(4) . . . . ?
Ru4 C84 C88 C90 -157.6(3) . . . . ?
Ru4 C85 C86 C81 -54.4(3) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.500 0.500 421.9 94.9 '2 C4H8O1'
2 0.353 0.708 -0.039 12.0 0.0 '1 ?'
3 0.647 0.292 0.039 12.0 0.0 '1 ?'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
