# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_2d
_database_code_depnum_ccdc_archive 'CCDC 1942981'
loop_
_audit_author_name
_audit_author_address
'Timo Stein'
;University of Hamburg
Germany
;
_audit_update_record             
;
2019-09-04 deposited with the CCDC.	2019-09-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H13 Cl2 P'
_chemical_formula_weight         331.15

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   8.2413(3)
_cell_length_b                   9.8910(3)
_cell_length_c                   11.4287(3)
_cell_angle_alpha                105.361(3)
_cell_angle_beta                 104.778(3)
_cell_angle_gamma                110.456(3)
_cell_volume                     776.87(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    12940
_cell_measurement_theta_min      4.3240
_cell_measurement_theta_max      76.1160
_cell_oxdiff_length_a            8.2413(3)
_cell_oxdiff_length_b            9.8910(3)
_cell_oxdiff_length_c            11.4287(3)
_cell_oxdiff_angle_alpha         105.361(3)
_cell_oxdiff_angle_beta          104.778(3)
_cell_oxdiff_angle_gamma         110.456(3)
_cell_oxdiff_volume              776.87(4)
_cell_oxdiff_measurement_reflns_used 12940

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.416
_exptl_crystal_F_000             340
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.21
_exptl_absorpt_coefficient_mu    4.631
_shelx_estimated_absorpt_T_min   0.265
_shelx_estimated_absorpt_T_max   0.443
_exptl_absorpt_correction_T_min  0.77706
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.630
_oxdiff_exptl_absorpt_empirical_full_max 4.516
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_ambient_environment      N~2~
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Atlas
_diffrn_detector_area_resol_mean 5.2063
_diffrn_reflns_number            15427
_diffrn_reflns_av_unetI/netI     0.0206
_diffrn_reflns_av_R_equivalents  0.0350
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         4.346
_diffrn_reflns_theta_max         76.453
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0409339000
_diffrn_orient_matrix_UB_12      0.1106575000
_diffrn_orient_matrix_UB_13      -0.0625941000
_diffrn_orient_matrix_UB_21      0.1597415000
_diffrn_orient_matrix_UB_22      0.1426153000
_diffrn_orient_matrix_UB_23      0.1208906000
_diffrn_orient_matrix_UB_31      0.1397526000
_diffrn_orient_matrix_UB_32      -0.0056523000
_diffrn_orient_matrix_UB_33      -0.0663751000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -96.00  -2.00   1.00    1.00    --  -42.35 125.00 120.00   94
  2  ω   -117.00 -18.00   1.00    1.00    --  -42.35 -38.00 -90.00   99
  3  ω    -67.00  32.00   1.00    1.00    --  -42.35  38.00  90.00   99
  4  ω     36.00 140.00   1.00    1.00    --  112.00 -30.00  60.00  104
  5  ω     29.00 109.00   1.00    1.00    --  112.00 -94.00 120.00   80
  6  ω     83.00 178.00   1.00    1.00    --  112.00  61.00  90.00   95
  7  ω     36.00 116.00   1.00    1.00    --  112.00-111.00 -30.00   80
  8  ω     36.00 116.00   1.00    1.00    --  112.00-111.00-120.00   80
  9  ω     57.00 151.00   1.00    1.00    --  112.00 178.00 -30.00   94
 10  ω     36.00 116.00   1.00    1.00    --  112.00-111.00  60.00   80
 11  ω     30.00 165.00   1.00    1.00    --  112.00 -15.00 -90.00  135
 12  ω     40.00 141.00   1.00    1.00    --  112.00 -61.00 -60.00  101
 13  ω     29.00 109.00   1.00    1.00    --  112.00 -94.00-180.00   80
 14  ω     57.00 151.00   1.00    1.00    --  112.00 178.00   0.00   94
 15  ω   -119.00 -10.00   1.00    1.00    --  -42.35 -77.00   0.00  109
 16  ω   -115.00 -14.00   1.00    1.00    --  -42.35 -57.00 150.00  101
 17  ω   -119.00 -10.00   1.00    1.00    --  -42.35 -77.00  90.00  109
 18  ω      1.00  83.00   1.00    1.00    --   42.35 -99.00 -60.00   82
 19  ω     83.00 178.00   1.00    1.00    --  112.00  61.00  60.00   95
 20  ω     83.00 178.00   1.00    1.00    --  112.00  61.00  30.00   95
 21  ω     59.00 178.00   1.00    1.00    --  112.00  15.00-150.00  119
 22  ω     83.00 178.00   1.00    1.00    --  112.00  61.00-150.00   95
 23  ω     59.00 178.00   1.00    1.00    --  112.00  15.00   0.00  119
 24  ω     83.00 178.00   1.00    1.00    --  112.00  61.00 -90.00   95
 25  ω     83.00 178.00   1.00    1.00    --  112.00  61.00   0.00   95
 26  ω     83.00 178.00   1.00    1.00    --  112.00  61.00-180.00   95
 27  ω     83.00 178.00   1.00    1.00    --  112.00  61.00 120.00   95
 28  ω     79.00 178.00   1.00    1.00    --  112.00  77.00 -60.00   99
 29  ω     83.00 178.00   1.00    1.00    --  112.00  61.00 150.00   95
 30  ω     83.00 178.00   1.00    1.00    --  112.00  61.00-120.00   95
 31  ω   -119.00 -10.00   1.00    1.00    --  -42.35 -77.00 -90.00  109
 32  ω   -119.00 -10.00   1.00    1.00    --  -42.35 -77.00-180.00  109
 33  ω   -117.00 -18.00   1.00    1.00    --  -42.35 -38.00  90.00   99
 34  ω   -125.00 -78.00   1.00    1.00    --  -42.35 -87.00  59.00   47
 35  ω     79.00 118.00   1.00    1.00    --  112.00  77.00 -30.00   39
;
_diffrn_measurement_method       'ω scans'
_reflns_number_total             3228
_reflns_number_gt                3145
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_structure_solution    'SUPERFLIP (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0424P)²+0.4588P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3228
_refine_ls_number_parameters     190
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0299
_refine_ls_R_factor_gt           0.0289
_refine_ls_wR_factor_ref         0.0762
_refine_ls_wR_factor_gt          0.0757
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.042
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl10 Cl 0.97017(5) 0.26615(4) 0.86592(3) 0.01803(10) Uani 1 1 d . . . . .
C10 C 0.84755(18) 0.28516(15) 0.62584(13) 0.0132(3) Uani 1 1 d . . . . .
Cl11 Cl 0.75194(5) 0.33926(4) 0.40213(3) 0.01790(10) Uani 1 1 d . . . . .
C11 C 0.9690(2) 0.25048(16) 0.71034(14) 0.0147(3) Uani 1 1 d . . . . .
C12 C 1.1014(2) 0.20806(17) 0.67891(15) 0.0181(3) Uani 1 1 d . . . . .
H12 H 1.178576 0.183160 0.738195 0.022 Uiso 1 1 calc R U . . .
C13 C 1.1203(2) 0.20222(17) 0.56097(15) 0.0194(3) Uani 1 1 d . . . . .
H13 H 1.208762 0.171360 0.538240 0.023 Uiso 1 1 calc R U . . .
C14 C 1.0095(2) 0.24163(17) 0.47621(14) 0.0175(3) Uani 1 1 d . . . . .
H14 H 1.023617 0.241067 0.396164 0.021 Uiso 1 1 calc R U . . .
C15 C 0.87816(19) 0.28175(15) 0.50995(13) 0.0139(3) Uani 1 1 d . . . . .
P40 P 0.65110(5) 0.32862(4) 0.64123(3) 0.01265(10) Uani 1 1 d . . . . .
C40 C 0.7717(2) 0.54295(16) 0.72106(13) 0.0139(3) Uani 1 1 d . . . . .
C41 C 0.6686(2) 0.62407(17) 0.69064(15) 0.0186(3) Uani 1 1 d . . . . .
H41 H 0.542027 0.567545 0.629470 0.022 Uiso 1 1 calc R U . . .
C42 C 0.7503(2) 0.78717(18) 0.74947(16) 0.0214(3) Uani 1 1 d . . . . .
H42 H 0.679242 0.841439 0.728859 0.026 Uiso 1 1 calc R U . . .
C43 C 0.9358(2) 0.87028(17) 0.83832(15) 0.0196(3) Uani 1 1 d . . . . .
H43 H 0.992039 0.981474 0.878162 0.024 Uiso 1 1 calc R U . . .
C44 C 1.0390(2) 0.79031(17) 0.86881(14) 0.0181(3) Uani 1 1 d . . . . .
H44 H 1.165517 0.847202 0.930045 0.022 Uiso 1 1 calc R U . . .
C45 C 0.9583(2) 0.62789(16) 0.81030(14) 0.0151(3) Uani 1 1 d . . . . .
H45 H 1.030169 0.574282 0.831004 0.018 Uiso 1 1 calc R U . . .
C46 C 0.59412(19) 0.27162(16) 0.77095(14) 0.0143(3) Uani 1 1 d . . . . .
C47 C 0.6195(2) 0.37909(16) 0.88964(14) 0.0165(3) Uani 1 1 d . . . . .
H47 H 0.680261 0.488228 0.909376 0.020 Uiso 1 1 calc R U . . .
C48 C 0.5569(2) 0.32804(18) 0.97911(15) 0.0193(3) Uani 1 1 d . . . . .
H48 H 0.576006 0.402388 1.059848 0.023 Uiso 1 1 calc R U . . .
C49 C 0.4664(2) 0.16864(18) 0.95117(15) 0.0202(3) Uani 1 1 d . . . . .
H49 H 0.423984 0.133882 1.012604 0.024 Uiso 1 1 calc R U . . .
C50 C 0.4384(2) 0.06038(17) 0.83246(16) 0.0200(3) Uani 1 1 d . . . . .
H50 H 0.377196 -0.048654 0.813020 0.024 Uiso 1 1 calc R U . . .
C51 C 0.4996(2) 0.11106(16) 0.74244(15) 0.0172(3) Uani 1 1 d . . . . .
H51 H 0.477277 0.036360 0.660801 0.021 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cl10 C11 1.7407(14) . ?
C10 C15 1.404(2) . ?
C10 C11 1.4053(19) . ?
C10 P40 1.8517(14) . ?
Cl11 C15 1.7478(14) . ?
C11 C12 1.391(2) . ?
C12 C13 1.384(2) . ?
C12 H12 0.9500 . ?
C13 C14 1.386(2) . ?
C13 H13 0.9500 . ?
C14 C15 1.382(2) . ?
C14 H14 0.9500 . ?
P40 C46 1.8300(15) . ?
P40 C40 1.8315(14) . ?
C40 C45 1.398(2) . ?
C40 C41 1.4003(19) . ?
C41 C42 1.394(2) . ?
C41 H41 0.9500 . ?
C42 C43 1.390(2) . ?
C42 H42 0.9500 . ?
C43 C44 1.391(2) . ?
C43 H43 0.9500 . ?
C44 C45 1.388(2) . ?
C44 H44 0.9500 . ?
C45 H45 0.9500 . ?
C46 C47 1.396(2) . ?
C46 C51 1.4024(19) . ?
C47 C48 1.388(2) . ?
C47 H47 0.9500 . ?
C48 C49 1.391(2) . ?
C48 H48 0.9500 . ?
C49 C50 1.392(2) . ?
C49 H49 0.9500 . ?
C50 C51 1.387(2) . ?
C50 H50 0.9500 . ?
C51 H51 0.9500 . ?

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
C15 C10 C11 114.19(12) . . ?
C15 C10 P40 115.48(10) . . ?
C11 C10 P40 130.30(11) . . ?
C12 C11 C10 122.98(13) . . ?
C12 C11 Cl10 115.24(11) . . ?
C10 C11 Cl10 121.72(11) . . ?
C13 C12 C11 119.81(13) . . ?
C13 C12 H12 120.1 . . ?
C11 C12 H12 120.1 . . ?
C12 C13 C14 119.68(14) . . ?
C12 C13 H13 120.2 . . ?
C14 C13 H13 120.2 . . ?
C15 C14 C13 118.97(14) . . ?
C15 C14 H14 120.5 . . ?
C13 C14 H14 120.5 . . ?
C14 C15 C10 124.27(13) . . ?
C14 C15 Cl11 116.28(11) . . ?
C10 C15 Cl11 119.39(11) . . ?
C46 P40 C40 102.55(6) . . ?
C46 P40 C10 107.54(6) . . ?
C40 P40 C10 100.91(6) . . ?
C45 C40 C41 119.07(13) . . ?
C45 C40 P40 123.60(10) . . ?
C41 C40 P40 117.32(11) . . ?
C42 C41 C40 120.48(14) . . ?
C42 C41 H41 119.8 . . ?
C40 C41 H41 119.8 . . ?
C43 C42 C41 119.90(14) . . ?
C43 C42 H42 120.1 . . ?
C41 C42 H42 120.1 . . ?
C42 C43 C44 119.87(14) . . ?
C42 C43 H43 120.1 . . ?
C44 C43 H43 120.1 . . ?
C45 C44 C43 120.42(14) . . ?
C45 C44 H44 119.8 . . ?
C43 C44 H44 119.8 . . ?
C44 C45 C40 120.25(13) . . ?
C44 C45 H45 119.9 . . ?
C40 C45 H45 119.9 . . ?
C47 C46 C51 118.63(13) . . ?
C47 C46 P40 123.16(11) . . ?
C51 C46 P40 117.74(11) . . ?
C48 C47 C46 120.66(13) . . ?
C48 C47 H47 119.7 . . ?
C46 C47 H47 119.7 . . ?
C47 C48 C49 120.34(14) . . ?
C47 C48 H48 119.8 . . ?
C49 C48 H48 119.8 . . ?
C48 C49 C50 119.49(14) . . ?
C48 C49 H49 120.3 . . ?
C50 C49 H49 120.3 . . ?
C51 C50 C49 120.28(13) . . ?
C51 C50 H50 119.9 . . ?
C49 C50 H50 119.9 . . ?
C50 C51 C46 120.56(14) . . ?
C50 C51 H51 119.7 . . ?
C46 C51 H51 119.7 . . ?

_refine_diff_density_max         0.350
_refine_diff_density_min         -0.334
_refine_diff_density_rms         0.057

####################################################################### 
# 
# 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_uhm-63
_database_code_depnum_ccdc_archive 'CCDC 1942990'
loop_
_audit_author_name
_audit_author_address
'Timo Stein'
;University of Hamburg
Germany
;
_audit_update_record             
;
2019-09-04 deposited with the CCDC.	2019-09-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
;
(C204 H114 Cu12 O54 P6), 10(O), 2(O), 0.53(O), 0.47(Cl -), 0.47(C2 H8 N +),
24(C3 H7 N O)
;
_chemical_formula_sum            'C276.93 H285.74 Cl0.47 Cu12 N24.47 O90.54 P6'
_chemical_formula_weight         6370.09

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 '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 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           71
_space_group_name_H-M_alt        'I m m m'
_space_group_name_Hall           '-I 2 2'

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

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

_cell_length_a                   18.6420(4)
_cell_length_b                   25.2812(4)
_cell_length_c                   33.3107(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     15699.1(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9786
_cell_measurement_theta_min      3.9330
_cell_measurement_theta_max      69.0350
_cell_oxdiff_length_a            18.6453(5)
_cell_oxdiff_length_b            25.2819(4)
_cell_oxdiff_length_c            33.3039(8)
_cell_oxdiff_angle_alpha         89.9864(16)
_cell_oxdiff_angle_beta          89.970(2)
_cell_oxdiff_angle_gamma         89.9818(18)
_cell_oxdiff_volume              15699.0(6)
_cell_oxdiff_measurement_reflns_used 9786

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.348
_exptl_crystal_F_000             6578
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.08
_exptl_absorpt_coefficient_mu    1.894
_shelx_estimated_absorpt_T_min   0.703
_shelx_estimated_absorpt_T_max   0.863
_exptl_absorpt_correction_T_min  0.81102
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.705
_oxdiff_exptl_absorpt_empirical_full_max 1.412
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_ambient_environment      N~2~
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Atlas
_diffrn_detector_area_resol_mean 10.4127
_diffrn_reflns_number            58750
_diffrn_reflns_av_unetI/netI     0.0490
_diffrn_reflns_av_R_equivalents  0.0770
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_theta_min         3.497
_diffrn_reflns_theta_max         67.491
_diffrn_reflns_theta_full        67.491
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measured_fraction_theta_full 0.962
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_Laue_measured_fraction_full 0.962
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_point_group_measured_fraction_full 0.962
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0545309000
_diffrn_orient_matrix_UB_12      0.0219702000
_diffrn_orient_matrix_UB_13      -0.0304823000
_diffrn_orient_matrix_UB_21      0.0599778000
_diffrn_orient_matrix_UB_22      0.0048443000
_diffrn_orient_matrix_UB_23      -0.0316197000
_diffrn_orient_matrix_UB_31      -0.0159969000
_diffrn_orient_matrix_UB_32      -0.0566301000
_diffrn_orient_matrix_UB_33      -0.0145190000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -104.00 -79.00   1.00   35.00    --  -42.35 -57.00 -60.00   25
  2  ω    -63.00 -10.00   1.00   35.00    --  -42.35 -77.00 -90.00   53
  3  ω   -117.00 -19.00   1.00   35.00    --  -42.35 -38.00  90.00   98
  4  ω    -67.00 -11.00   1.00   35.00    --  -42.35 -77.00 150.00   56
  5  ω    -51.00 -10.00   1.00   35.00    --  -42.35 -77.00  60.00   41
  6  ω    -57.00 -13.00   1.00   35.00    --  -42.35 -77.00-150.00   44
  7  ω    -58.00 -14.00   1.00   35.00    --  -42.35 -57.00 -60.00   44
  8  ω    -95.00  -2.00   1.00   35.00    --  -42.35 125.00-180.00   93
  9  ω   -104.00 -70.00   1.00   35.00    --  -42.35 -77.00  60.00   34
 10  ω   -118.00 -84.00   1.00   35.00    --  -42.35 -77.00   0.00   34
 11  ω   -119.00 -71.00   1.00   35.00    --  -42.35 -77.00 -90.00   48
 12  ω    -43.00 -10.00   1.00   35.00    --  -42.35 -77.00   0.00   33
 13  ω      3.00  56.00   1.00   35.00    --   42.35 -99.00 120.00   53
 14  ω     24.00  85.00   1.00   35.00    --   42.35-125.00   0.00   61
 15  ω      3.00 112.00   1.00   35.00    --   42.35  19.00-120.00  109
 16  ω     18.00 109.00   1.00  140.00    --  100.87 -94.00  30.00   91
 17  ω     72.00 156.00   1.00  140.00    --  100.87  61.00 -90.00   84
 18  ω     71.00 125.00   1.00  140.00    --  100.87  65.00-142.43   54
 19  ω     72.00 172.00   1.00  140.00    --  100.87  61.00-180.00  100
 20  ω     74.00 149.00   1.00  140.00    --  100.87  61.00 150.00   75
 21  ω    120.00 169.00   1.00  140.00    --  100.87  73.00  42.89   49
 22  ω     69.00  95.00   1.00  140.00    --  100.87  73.00 -88.24   26
 23  ω     28.00  73.00   1.00  140.00    --  100.87 -45.00  30.00   45
;
_diffrn_measurement_method       'ω scans'
_reflns_number_total             7346
_reflns_number_gt                3745
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7346
_refine_ls_number_parameters     368
_refine_ls_number_restraints     426
_refine_ls_R_factor_all          0.1552
_refine_ls_R_factor_gt           0.1169
_refine_ls_wR_factor_ref         0.3719
_refine_ls_wR_factor_gt          0.3266
_refine_ls_goodness_of_fit_ref   1.206
_refine_ls_restrained_S_all      1.206
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.000000 0.000000 0.000000 0.106(4) Uiso 0.53(3) 8 d S . P . .
Cl1 Cl 0.000000 0.000000 0.000000 0.106(4) Uiso 0.47(3) 8 d S . P . .
O50 O 0.000000 0.1121(5) 0.000000 0.182(6) Uani 1 4 d S T P . .
O100 O 0.1588(3) 0.1466(2) 0.29992(18) 0.1247(18) Uani 1 1 d . . . . .
O200 O 0.000000 0.000000 0.2229(2) 0.114(4) Uani 1 4 d S T P . .
Cu1 Cu 0.21415(5) 0.21223(4) 0.26925(3) 0.0796(4) Uani 1 1 d . . . . .
Cu2 Cu 0.000000 0.000000 0.15133(5) 0.0972(7) Uani 1 4 d S T P . .
Cu3 Cu 0.000000 0.000000 0.07191(5) 0.0896(7) Uani 1 4 d S T P . .
P40A P 0.5197(3) 0.000000 0.24574(16) 0.101(3) Uani 0.5 2 d DS T P . .
O10A O 0.3091(3) 0.1832(2) 0.27826(14) 0.0957(14) Uani 1 1 d . . . . .
O11A O 0.3705(2) 0.2466(2) 0.24545(15) 0.0906(13) Uani 1 1 d . . . . .
O40A O 0.6000(6) 0.000000 0.2412(8) 0.229(13) Uani 0.5 2 d DS T P . .
C10A C 0.500000 0.1017(3) 0.3009(3) 0.090(2) Uani 1 2 d DS T P . .
C11A C 0.4355(3) 0.1280(3) 0.2934(2) 0.0893(18) Uani 1 1 d D . . . .
H11A H 0.391216 0.111675 0.300224 0.107 Uiso 1 1 calc R U . . .
C12A C 0.4357(3) 0.1775(3) 0.27617(19) 0.0814(16) Uani 1 1 d D . . . .
C13A C 0.500000 0.2022(3) 0.2676(2) 0.077(2) Uani 1 2 d DS T P . .
H13A H 0.500000 0.236371 0.255662 0.093 Uiso 1 2 calc R U P . .
C14A C 0.3673(4) 0.2054(3) 0.2660(2) 0.0856(17) Uani 1 1 d . . . . .
C20A C 0.500000 0.000000 0.2993(3) 0.086(3) Uani 1 4 d DS T P . .
C21A C 0.500000 0.0474(3) 0.3200(3) 0.103(3) Uani 1 2 d DS T P . .
C22A C 0.500000 0.0473(3) 0.3612(3) 0.244(13) Uani 1 2 d DS T P . .
H22A H 0.500000 0.079810 0.375526 0.293 Uiso 1 2 calc R U P . .
C23A C 0.500000 0.000000 0.3820(5) 0.39(4) Uani 1 4 d DS T P . .
H23A H 0.500000 0.000000 0.410546 0.471 Uiso 1 4 calc R U P . .
C40A C 0.4708(9) 0.0513(4) 0.2213(4) 0.136(7) Uani 0.5 1 d DG . P A .
C41A C 0.3974(8) 0.0590(6) 0.2169(5) 0.194(10) Uani 0.5 1 d G . P . .
H41A H 0.364591 0.037123 0.231115 0.233 Uiso 0.5 1 calc R U P . .
C42A C 0.3719(8) 0.0988(7) 0.1919(6) 0.237(13) Uani 0.5 1 d G . P A .
H42A H 0.321675 0.104027 0.188930 0.284 Uiso 0.5 1 calc R U P . .
C43A C 0.4198(13) 0.1308(5) 0.1711(4) 0.225(13) Uani 0.5 1 d G . P . .
H43A H 0.402365 0.157986 0.154023 0.270 Uiso 0.5 1 calc R U P A .
C44A C 0.4932(12) 0.1231(6) 0.1755(5) 0.242(12) Uani 0.5 1 d G . P A -1
H44A H 0.525971 0.145042 0.161302 0.291 Uiso 0.5 1 calc R U P A -1
C45A C 0.5187(7) 0.0834(7) 0.2005(5) 0.204(10) Uani 0.5 1 d G . P . .
H45A H 0.568889 0.078138 0.203487 0.245 Uiso 0.5 1 calc R U P A .
P40B P 0.1614(4) 0.2050(3) 0.000000 0.200(3) Uani 1 2 d DS T P . .
O10B O 0.2752(3) 0.2426(2) 0.18249(14) 0.0997(15) Uani 1 1 d . . . . .
O11B O 0.2133(3) 0.1822(2) 0.21570(15) 0.0965(14) Uani 1 1 d . . . . .
O12B O 0.0740(3) 0.05363(19) 0.14403(14) 0.1085(16) Uani 1 1 d . . . . .
O13B O 0.0717(4) 0.0537(2) 0.07674(14) 0.148(3) Uani 1 1 d . . . . .
O40B O 0.0984(6) 0.1684(6) 0.000000 0.230(6) Uani 1 2 d DS T P . .
C10B C 0.2434(7) 0.1605(5) 0.0745(3) 0.153(4) Uani 1 1 d . . . . .
C11B C 0.2597(5) 0.1871(4) 0.1111(2) 0.124(3) Uani 1 1 d . . . . .
H11B H 0.295819 0.213607 0.111277 0.149 Uiso 1 1 calc R U . . .
C12B C 0.2248(4) 0.1753(3) 0.1458(2) 0.099(2) Uani 1 1 d . . . . .
C13B C 0.1720(5) 0.1353(3) 0.1452(2) 0.109(2) Uani 1 1 d . . . . .
H13B H 0.149460 0.125127 0.169550 0.131 Uiso 1 1 calc R U . . .
C14B C 0.1522(6) 0.1105(3) 0.1093(2) 0.118(3) Uani 1 1 d . . . . .
C15B C 0.1883(6) 0.1227(4) 0.0746(3) 0.143(4) Uani 1 1 d . . . . .
H15B H 0.175816 0.105308 0.050266 0.172 Uiso 1 1 calc R U . . .
C16B C 0.2398(4) 0.2018(3) 0.1842(2) 0.0907(19) Uani 1 1 d . . . . .
C17B C 0.0954(6) 0.0700(3) 0.1096(2) 0.116(3) Uani 1 1 d . . . . .
C20B C 0.2489(5) 0.1749(4) 0.000000 0.117(3) Uani 1 2 d DS T P . .
C21B C 0.2847(5) 0.1698(4) 0.03648(19) 0.179(5) Uani 1 1 d D . . . .
C22B C 0.3590(6) 0.1597(10) 0.0366(2) 0.330(14) Uani 1 1 d D . . . .
H22B H 0.383862 0.154298 0.061188 0.396 Uiso 1 1 calc R U . . .
C23B C 0.3955(8) 0.1576(19) 0.000000 0.51(4) Uani 1 2 d DS T P . .
H23B H 0.446268 0.154741 0.000000 0.613 Uiso 1 2 calc R U P . .
C40B C 0.1633(10) 0.2501(4) 0.0424(3) 0.261(8) Uani 1 1 d DG U . . .
C41B C 0.1050(8) 0.2478(5) 0.0684(5) 0.299(10) Uani 1 1 d G U . . .
H41B H 0.065859 0.225034 0.062611 0.359 Uiso 1 1 calc R U . . .
C42B C 0.1041(7) 0.2789(6) 0.1028(4) 0.414(10) Uani 1 1 d G U . . .
H42B H 0.064286 0.277393 0.120532 0.497 Uiso 1 1 calc R U . . .
C43B C 0.1614(9) 0.3123(5) 0.1112(3) 0.275(9) Uani 1 1 d G U . . .
H43B H 0.160793 0.333553 0.134710 0.330 Uiso 1 1 calc R U . . .
C44B C 0.2197(8) 0.3146(5) 0.0852(4) 0.311(10) Uani 1 1 d G U . . .
H44B H 0.258874 0.337355 0.090967 0.373 Uiso 1 1 calc R U . . .
C45B C 0.2206(8) 0.2835(6) 0.0508(3) 0.246(8) Uani 1 1 d G U . . .
H45B H 0.260449 0.284996 0.033046 0.295 Uiso 1 1 calc R U . . .
C60 C 0.231(4) 0.000000 0.0376(6) 0.46(8) Uani 0.233(15) 2 d DS TU P . .
H60A H 0.200725 0.000000 0.061449 0.695 Uiso 0.233(15) 2 calc R U P . .
H60B H 0.261773 -0.031651 0.037704 0.695 Uiso 0.116(8) 1 calc R U P . .
H60C H 0.261773 0.031651 0.037704 0.695 Uiso 0.116(8) 1 calc R U P . .
N60 N 0.185(4) 0.000000 0.000000 0.14(2) Uani 0.233(15) 4 d DS TU P . .
H60D H 0.156116 0.029142 0.000000 0.162 Uiso 0.116(8) 2 calc R U P . .
H60E H 0.156116 -0.029142 0.000000 0.162 Uiso 0.116(8) 2 calc R U P . .


_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
O1 Cu3 2.3953(17) 9 ?
O1 Cu3 2.3953(17) . ?
O100 Cu1 2.206(5) . ?
O200 Cu2 2.386(8) . ?
Cu1 O11B 1.938(5) . ?
Cu1 O10A 1.940(5) . ?
Cu1 O11A 1.952(5) 13 ?
Cu1 O10B 1.983(5) 13 ?
Cu1 Cu1 2.6603(18) 13 ?
Cu2 O12B 1.950(5) . ?
Cu2 O12B 1.950(5) 2 ?
Cu2 O12B 1.950(5) 12 ?
Cu2 O12B 1.950(5) 11 ?
Cu2 Cu3 2.646(3) . ?
Cu3 O13B 1.911(6) 2 ?
Cu3 O13B 1.911(6) . ?
Cu3 O13B 1.911(6) 12 ?
Cu3 O13B 1.911(6) 11 ?
P40A O40A 1.504(10) . ?
P40A C40A 1.784(8) . ?
P40A C20A 1.821(8) . ?
P40A C41A 2.35(2) 12_655 ?
P40A C41A 2.353(19) 2_655 ?
O10A C14A 1.288(8) . ?
O11A C14A 1.250(8) . ?
O40A H41A 1.20(3) 12_655 ?
C10A C11A 1.397(7) 12_655 ?
C10A C11A 1.397(7) . ?
C10A C21A 1.513(12) . ?
C11A C12A 1.376(8) . ?
C11A H11A 0.9500 . ?
C12A C13A 1.382(7) . ?
C12A C14A 1.495(9) . ?
C13A H13A 0.9500 . ?
C20A C21A 1.384(8) . ?
C20A C21A 1.384(8) 2_655 ?
C21A C22A 1.373(13) . ?
C22A C23A 1.381(11) . ?
C22A H22A 0.9500 . ?
C23A H23A 0.9500 . ?
C40A C41A 1.3900 . ?
C40A C45A 1.3900 . ?
C40A H45A 1.165(17) 12_655 ?
C41A C42A 1.3900 . ?
C41A H41A 0.9500 . ?
C41A H45A 0.911(19) 12_655 ?
C42A C43A 1.3900 . ?
C42A H42A 0.9500 . ?
C42A H45A 1.28(2) 12_655 ?
C43A C44A 1.3900 . ?
C43A H43A 0.9500 . ?
C43A H44A 1.12(5) 12_655 ?
C44A C45A 1.3900 . ?
C44A H44A 0.9500 . ?
C44A H44A 0.81(3) 12_655 ?
C45A H45A 0.9500 . ?
P40B O40B 1.494(9) . ?
P40B C20B 1.801(8) . ?
P40B C40B 1.816(7) 10 ?
P40B C40B 1.816(7) . ?
O10B C16B 1.226(8) . ?
O11B C16B 1.261(9) . ?
O12B C17B 1.284(9) . ?
O13B C17B 1.249(8) . ?
C10B C15B 1.403(12) . ?
C10B C11B 1.425(12) . ?
C10B C21B 1.499(12) . ?
C11B C12B 1.359(11) . ?
C11B H11B 0.9500 . ?
C12B C13B 1.410(10) . ?
C12B C16B 1.472(10) . ?
C13B C14B 1.399(10) . ?
C13B H13B 0.9500 . ?
C14B C15B 1.374(11) . ?
C14B C17B 1.473(12) . ?
C15B H15B 0.9500 . ?
C20B C21B 1.392(7) . ?
C20B C21B 1.392(7) 10 ?
C21B C22B 1.409(9) . ?
C22B C23B 1.398(8) . ?
C22B H22B 0.9500 . ?
C23B H23B 0.9500 . ?
C40B C41B 1.3900 . ?
C40B C45B 1.3900 . ?
C41B C42B 1.3900 . ?
C41B H41B 0.9500 . ?
C42B C43B 1.3900 . ?
C42B H42B 0.9500 . ?
C43B C44B 1.3900 . ?
C43B H43B 0.9500 . ?
C44B C45B 1.3900 . ?
C44B H44B 0.9500 . ?
C45B H45B 0.9500 . ?
C60 N60 1.52(2) . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?
N60 H60D 0.9100 . ?
N60 H60E 0.9100 . ?

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
Cu3 O1 Cu3 180.0 9 . ?
O11B Cu1 O10A 90.1(2) . . ?
O11B Cu1 O11A 88.3(2) . 13 ?
O10A Cu1 O11A 168.0(2) . 13 ?
O11B Cu1 O10B 166.6(2) . 13 ?
O10A Cu1 O10B 90.1(2) . 13 ?
O11A Cu1 O10B 88.7(2) 13 13 ?
O11B Cu1 O100 97.4(2) . . ?
O10A Cu1 O100 94.0(2) . . ?
O11A Cu1 O100 98.0(2) 13 . ?
O10B Cu1 O100 96.0(2) 13 . ?
O11B Cu1 Cu1 80.88(15) . 13 ?
O10A Cu1 Cu1 83.57(15) . 13 ?
O11A Cu1 Cu1 84.41(14) 13 13 ?
O10B Cu1 Cu1 85.80(15) 13 13 ?
O100 Cu1 Cu1 177.01(17) . 13 ?
O12B Cu2 O12B 165.7(3) . 2 ?
O12B Cu2 O12B 90.1(3) . 12 ?
O12B Cu2 O12B 88.1(3) 2 12 ?
O12B Cu2 O12B 88.1(3) . 11 ?
O12B Cu2 O12B 90.1(3) 2 11 ?
O12B Cu2 O12B 165.7(3) 12 11 ?
O12B Cu2 O200 97.17(14) . . ?
O12B Cu2 O200 97.17(15) 2 . ?
O12B Cu2 O200 97.17(14) 12 . ?
O12B Cu2 O200 97.17(14) 11 . ?
O12B Cu2 Cu3 82.83(14) . . ?
O12B Cu2 Cu3 82.83(15) 2 . ?
O12B Cu2 Cu3 82.83(14) 12 . ?
O12B Cu2 Cu3 82.83(14) 11 . ?
O200 Cu2 Cu3 180.0 . . ?
O13B Cu3 O13B 170.3(3) 2 . ?
O13B Cu3 O13B 90.5(5) 2 12 ?
O13B Cu3 O13B 88.7(5) . 12 ?
O13B Cu3 O13B 88.7(5) 2 11 ?
O13B Cu3 O13B 90.5(5) . 11 ?
O13B Cu3 O13B 170.3(3) 12 11 ?
O13B Cu3 O1 94.84(15) 2 . ?
O13B Cu3 O1 94.84(15) . . ?
O13B Cu3 O1 94.84(15) 12 . ?
O13B Cu3 O1 94.84(15) 11 . ?
O13B Cu3 Cu2 85.16(15) 2 . ?
O13B Cu3 Cu2 85.16(15) . . ?
O13B Cu3 Cu2 85.16(15) 12 . ?
O13B Cu3 Cu2 85.16(15) 11 . ?
O1 Cu3 Cu2 180.0 . . ?
O40A P40A C40A 117.6(9) . . ?
O40A P40A C20A 107.4(11) . . ?
C40A P40A C20A 110.1(5) . . ?
O40A P40A C41A 46.0(9) . 12_655 ?
C40A P40A C41A 71.8(13) . 12_655 ?
C20A P40A C41A 122.1(9) . 12_655 ?
O40A P40A C41A 46.0(14) . 2_655 ?
C40A P40A C41A 127.7(14) . 2_655 ?
C20A P40A C41A 122.1(11) . 2_655 ?
C41A P40A C41A 78.7(19) 12_655 2_655 ?
C14A O10A Cu1 123.7(5) . . ?
C14A O11A Cu1 123.0(5) . 13 ?
P40A O40A H41A 125.2(19) . 12_655 ?
C11A C10A C11A 118.9(8) 12_655 . ?
C11A C10A C21A 120.5(4) 12_655 . ?
C11A C10A C21A 120.5(4) . . ?
C12A C11A C10A 120.3(5) . . ?
C12A C11A H11A 119.9 . . ?
C10A C11A H11A 119.9 . . ?
C11A C12A C13A 120.1(5) . . ?
C11A C12A C14A 121.3(5) . . ?
C13A C12A C14A 118.6(6) . . ?
C12A C13A C12A 120.3(8) . 12_655 ?
C12A C13A H13A 119.9 . . ?
C12A C13A H13A 119.9 12_655 . ?
O11A C14A O10A 125.2(7) . . ?
O11A C14A C12A 118.5(6) . . ?
O10A C14A C12A 116.2(6) . . ?
C21A C20A C21A 120.0(9) . 2_655 ?
C21A C20A P40A 119.3(4) . . ?
C21A C20A P40A 119.3(4) 2_655 . ?
C22A C21A C20A 119.8(6) . . ?
C22A C21A C10A 115.1(7) . . ?
C20A C21A C10A 125.1(8) . . ?
C21A C22A C23A 120.2(7) . . ?
C21A C22A H22A 119.9 . . ?
C23A C22A H22A 119.9 . . ?
C22A C23A C22A 119.9(12) 2_655 . ?
C22A C23A H23A 120.1 2_655 . ?
C22A C23A H23A 120.1 . . ?
C41A C40A C45A 120.0 . . ?
C41A C40A P40A 130.8(11) . . ?
C45A C40A P40A 108.8(11) . . ?
C41A C40A H45A 40.6(10) . 12_655 ?
C45A C40A H45A 79.4(10) . 12_655 ?
P40A C40A H45A 168.7(14) . 12_655 ?
C42A C41A C40A 120.0 . . ?
C42A C41A P40A 158.1(7) . 2_655 ?
C40A C41A P40A 38.9(7) . 2_655 ?
C42A C41A H41A 120.0 . . ?
C40A C41A H41A 120.0 . . ?
P40A C41A H41A 81.4 2_655 . ?
C42A C41A H45A 63.7(12) . 12_655 ?
C40A C41A H45A 56.3(12) . 12_655 ?
P40A C41A H45A 94.8(17) 2_655 12_655 ?
H41A C41A H45A 175.9 . 12_655 ?
C41A C42A C43A 120.0 . . ?
C41A C42A H42A 120.0 . . ?
C43A C42A H42A 120.0 . . ?
C41A C42A H45A 39.6(6) . 12_655 ?
C43A C42A H45A 80.4(6) . 12_655 ?
H42A C42A H45A 159.6 . 12_655 ?
C44A C43A C42A 120.0 . . ?
C44A C43A H43A 120.0 . . ?
C42A C43A H43A 120.0 . . ?
C44A C43A H44A 35.7(13) . 12_655 ?
C42A C43A H44A 155.7(13) . 12_655 ?
H43A C43A H44A 84.3 . 12_655 ?
C43A C44A C45A 120.0 . . ?
C43A C44A H44A 120.0 . . ?
C45A C44A H44A 120.0 . . ?
C43A C44A H44A 54(4) . 12_655 ?
C45A C44A H44A 174(4) . 12_655 ?
H44A C44A H44A 66.2 . 12_655 ?
C44A C45A C40A 120.0 . . ?
C44A C45A H45A 120.0 . . ?
C40A C45A H45A 120.0 . . ?
O40B P40B C20B 116.8(8) . . ?
O40B P40B C40B 113.9(8) . 10 ?
C20B P40B C40B 104.3(6) . 10 ?
O40B P40B C40B 113.9(8) . . ?
C20B P40B C40B 104.3(6) . . ?
C40B P40B C40B 102.1(9) 10 . ?
C16B O10B Cu1 120.1(5) . 13 ?
C16B O11B Cu1 127.6(5) . . ?
C17B O12B Cu2 123.7(5) . . ?
C17B O13B Cu3 123.8(6) . . ?
C15B C10B C11B 118.4(9) . . ?
C15B C10B C21B 119.0(8) . . ?
C11B C10B C21B 122.6(9) . . ?
C12B C11B C10B 121.4(9) . . ?
C12B C11B H11B 119.3 . . ?
C10B C11B H11B 119.3 . . ?
C11B C12B C13B 118.7(7) . . ?
C11B C12B C16B 123.2(8) . . ?
C13B C12B C16B 118.1(7) . . ?
C14B C13B C12B 121.1(8) . . ?
C14B C13B H13B 119.4 . . ?
C12B C13B H13B 119.4 . . ?
C15B C14B C13B 119.3(8) . . ?
C15B C14B C17B 120.9(7) . . ?
C13B C14B C17B 119.8(8) . . ?
C14B C15B C10B 120.9(8) . . ?
C14B C15B H15B 119.6 . . ?
C10B C15B H15B 119.6 . . ?
O10B C16B O11B 125.4(7) . . ?
O10B C16B C12B 116.5(7) . . ?
O11B C16B C12B 118.1(7) . . ?
O13B C17B O12B 124.5(9) . . ?
O13B C17B C14B 118.6(8) . . ?
O12B C17B C14B 116.9(7) . . ?
C21B C20B C21B 121.7(9) . 10 ?
C21B C20B P40B 118.2(5) . . ?
C21B C20B P40B 118.2(5) 10 . ?
C20B C21B C22B 119.4(6) . . ?
C20B C21B C10B 120.4(8) . . ?
C22B C21B C10B 118.2(8) . . ?
C23B C22B C21B 118.8(7) . . ?
C23B C22B H22B 120.6 . . ?
C21B C22B H22B 120.6 . . ?
C22B C23B C22B 121.6(11) 10 . ?
C22B C23B H23B 119.2 10 . ?
C22B C23B H23B 119.2 . . ?
C41B C40B C45B 120.0 . . ?
C41B C40B P40B 116.3(12) . . ?
C45B C40B P40B 123.6(12) . . ?
C40B C41B C42B 120.0 . . ?
C40B C41B H41B 120.0 . . ?
C42B C41B H41B 120.0 . . ?
C43B C42B C41B 120.0 . . ?
C43B C42B H42B 120.0 . . ?
C41B C42B H42B 120.0 . . ?
C44B C43B C42B 120.0 . . ?
C44B C43B H43B 120.0 . . ?
C42B C43B H43B 120.0 . . ?
C43B C44B C45B 120.0 . . ?
C43B C44B H44B 120.0 . . ?
C45B C44B H44B 120.0 . . ?
C44B C45B C40B 120.0 . . ?
C44B C45B H45B 120.0 . . ?
C40B C45B H45B 120.0 . . ?
N60 C60 H60A 109.5 . . ?
N60 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
N60 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
C60 N60 C60 110(3) . 4 ?
C60 N60 H60D 109.6 . . ?
C60 N60 H60D 109.6 4 . ?
C60 N60 H60E 109.6 . . ?
C60 N60 H60E 109.6 4 . ?
H60D N60 H60E 108.1 . . ?

_refine_diff_density_max         1.026
_refine_diff_density_min         -1.176
_refine_diff_density_rms         0.114



####################################################################### 
# 
# 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_3c
_database_code_depnum_ccdc_archive 'CCDC 1942984'
loop_
_audit_author_name
_audit_author_address
'Timo Stein'
;University of Hamburg
Germany
;
_audit_update_record             
;
2019-09-04 deposited with the CCDC.	2019-09-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H31 O9 P, C D Cl3'
_chemical_formula_sum            'C31 H31 D Cl3 O9 P'
_chemical_formula_weight         686.89

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
D D 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   10.6082(4)
_cell_length_b                   12.4315(4)
_cell_length_c                   12.9377(5)
_cell_angle_alpha                67.364(3)
_cell_angle_beta                 88.560(3)
_cell_angle_gamma                81.914(3)
_cell_volume                     1558.30(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    44438
_cell_measurement_theta_min      2.9230
_cell_measurement_theta_max      32.4090

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.464
_exptl_crystal_F_000             712
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_exptl_absorpt_coefficient_mu    0.400
_shelx_estimated_absorpt_T_min   0.857
_shelx_estimated_absorpt_T_max   0.939
_exptl_absorpt_correction_T_min  0.95749
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Atlas
_diffrn_detector_area_resol_mean 10.4127
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_number            59878
_diffrn_reflns_av_unetI/netI     0.0217
_diffrn_reflns_av_R_equivalents  0.0320
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.883
_diffrn_reflns_theta_max         32.629
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.948
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             10798
_reflns_number_gt                9368
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_structure_solution    'SUPERFLIP (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0518P)²+0.9005P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10798
_refine_ls_number_parameters     463
_refine_ls_number_restraints     61
_refine_ls_R_factor_all          0.0473
_refine_ls_R_factor_gt           0.0400
_refine_ls_wR_factor_ref         0.1108
_refine_ls_wR_factor_gt          0.1057
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.035
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O10 O 0.81543(9) 0.46685(10) 0.20440(9) 0.0281(2) Uani 1 1 d . . . . .
C10 C 0.42679(10) 0.54656(9) 0.26380(9) 0.01377(18) Uani 1 1 d . . . . .
O11 O 0.75901(8) 0.38341(8) 0.08990(7) 0.01850(16) Uani 1 1 d . . . . .
C11 C 0.55493(10) 0.52979(9) 0.23863(9) 0.01457(18) Uani 1 1 d . . . . .
H11 H 0.614749 0.566172 0.262630 0.017 Uiso 1 1 calc R U . . .
O12 O 0.17206(8) 0.38155(9) 0.14987(8) 0.02434(18) Uani 1 1 d . . . . .
C12 C 0.59564(10) 0.46001(9) 0.17852(9) 0.01419(18) Uani 1 1 d . . . . .
O13 O 0.33055(8) 0.32202(8) 0.05754(8) 0.02123(17) Uani 1 1 d . . . . .
C13 C 0.50825(10) 0.40984(9) 0.13941(9) 0.01441(18) Uani 1 1 d . . . . .
H13 H 0.535448 0.364839 0.095870 0.017 Uiso 1 1 calc R U . . .
C14 C 0.38062(10) 0.42627(9) 0.16473(9) 0.01449(18) Uani 1 1 d . . . . .
C15 C 0.34079(10) 0.49130(9) 0.22909(9) 0.01473(18) Uani 1 1 d . . . . .
H15 H 0.254299 0.498129 0.249573 0.018 Uiso 1 1 calc R U . . .
C16 C 0.73416(10) 0.43826(10) 0.16026(9) 0.01676(19) Uani 1 1 d . . . . .
C17 C 0.89219(11) 0.35258(12) 0.07327(12) 0.0245(2) Uani 1 1 d . . . . .
H17A H 0.934891 0.302972 0.145634 0.037 Uiso 1 1 calc R U . . .
H17B H 0.931686 0.424438 0.039382 0.037 Uiso 1 1 calc R U . . .
H17C H 0.900370 0.309399 0.023498 0.037 Uiso 1 1 calc R U . . .
C18 C 0.28259(10) 0.37519(10) 0.12519(9) 0.01640(19) Uani 1 1 d . . . . .
C19 C 0.23962(12) 0.27068(12) 0.01631(13) 0.0263(3) Uani 1 1 d . . . . .
H19A H 0.171568 0.332486 -0.027283 0.040 Uiso 1 1 calc R U . . .
H19B H 0.203032 0.211854 0.079716 0.040 Uiso 1 1 calc R U . . .
H19C H 0.282508 0.232843 -0.031496 0.040 Uiso 1 1 calc R U . . .
C20 C 0.39914(10) 0.73634(9) 0.30050(8) 0.01293(17) Uani 1 1 d . . . . .
C21 C 0.37224(10) 0.78752(10) 0.38069(9) 0.01412(18) Uani 1 1 d . . . . .
C22 C 0.31768(11) 0.72438(11) 0.48157(9) 0.0175(2) Uani 1 1 d . . . . .
H22 H 0.297430 0.760043 0.534111 0.021 Uiso 1 1 calc R U . . .
C23 C 0.29256(11) 0.61071(11) 0.50639(9) 0.0185(2) Uani 1 1 d . . . . .
H23 H 0.250665 0.570802 0.573152 0.022 Uiso 1 1 calc R U . . .
C24 C 0.32889(11) 0.55590(10) 0.43336(9) 0.01724(19) Uani 1 1 d . . . . .
H24 H 0.316572 0.476401 0.452227 0.021 Uiso 1 1 calc R U . . .
C25 C 0.38375(10) 0.61681(9) 0.33171(9) 0.01380(18) Uani 1 1 d . . . . .
O30 O 0.72011(8) 1.16050(8) 0.32291(7) 0.02114(17) Uani 1 1 d . . . . .
C30 C 0.40307(10) 0.90508(10) 0.36849(9) 0.01465(18) Uani 1 1 d . . . . .
O31 O 0.77448(8) 0.97380(8) 0.33800(9) 0.02497(19) Uani 1 1 d . . . . .
C31 C 0.52800(10) 0.93055(10) 0.35118(9) 0.01530(18) Uani 1 1 d . . . . .
H31 H 0.593026 0.875057 0.340806 0.018 Uiso 1 1 calc R U . . .
O32 O 0.26639(9) 1.26760(8) 0.41695(8) 0.02126(17) Uani 1 1 d . . . . .
C32 C 0.55744(10) 1.03742(10) 0.34911(8) 0.01482(18) Uani 1 1 d . . . . .
O33 O 0.12159(8) 1.16410(8) 0.38947(8) 0.02081(17) Uani 1 1 d . . . . .
C33 C 0.46326(10) 1.12006(10) 0.36351(9) 0.01545(19) Uani 1 1 d . . . . .
H33 H 0.483907 1.192608 0.361874 0.019 Uiso 1 1 calc R U . . .
C34 C 0.33830(10) 1.09549(10) 0.38035(9) 0.01493(18) Uani 1 1 d . . . . .
C35 C 0.30870(10) 0.98829(10) 0.38345(9) 0.01533(19) Uani 1 1 d . . . . .
H35 H 0.223644 0.971642 0.395847 0.018 Uiso 1 1 calc R U . . .
C36 C 0.69048(11) 1.06585(10) 0.33494(9) 0.01651(19) Uani 1 1 d . . . . .
C37 C 0.90530(13) 0.99482(14) 0.32461(15) 0.0352(3) Uani 1 1 d . . . . .
H37A H 0.932944 1.012378 0.387418 0.053 Uiso 1 1 calc R U . . .
H37B H 0.912741 1.061774 0.254184 0.053 Uiso 1 1 calc R U . . .
H37C H 0.959109 0.924595 0.323146 0.053 Uiso 1 1 calc R U . . .
C38 C 0.24077(11) 1.18535(10) 0.39782(9) 0.01657(19) Uani 1 1 d . . . . .
C39 C 0.02228(12) 1.25294(12) 0.39769(13) 0.0272(3) Uani 1 1 d . . . . .
H39A H 0.030684 1.329109 0.337815 0.041 Uiso 1 1 calc R U . . .
H39B H 0.030192 1.258744 0.470614 0.041 Uiso 1 1 calc R U . . .
H39C H -0.061224 1.231055 0.390216 0.041 Uiso 1 1 calc R U . . .
P40 P 0.43629(3) 0.82882(2) 0.15642(2) 0.01227(6) Uani 1 1 d . . . . .
O40 O 0.57308(8) 0.84379(8) 0.14008(7) 0.01797(16) Uani 1 1 d . . . . .
C40 C 0.37602(11) 0.76955(10) 0.06193(9) 0.01594(19) Uani 1 1 d . . . . .
H40A H 0.434559 0.698596 0.065726 0.019 Uiso 1 1 calc R U . . .
H40B H 0.291808 0.745286 0.086988 0.019 Uiso 1 1 calc R U . . .
C41 C 0.36274(13) 0.85837(11) -0.05951(9) 0.0218(2) Uani 1 1 d . . . . .
H41A H 0.296964 0.924439 -0.065445 0.033 Uiso 1 1 calc R U . . .
H41B H 0.338550 0.820013 -0.108046 0.033 Uiso 1 1 calc R U . . .
H41C H 0.444204 0.887553 -0.082859 0.033 Uiso 1 1 calc R U . . .
C42 C 0.33198(11) 0.96748(10) 0.12100(9) 0.01736(19) Uani 1 1 d . . . . .
H42A H 0.357975 1.008384 0.167515 0.021 Uiso 1 1 calc R U . . .
H42B H 0.343828 1.017481 0.041666 0.021 Uiso 1 1 calc R U . . .
C43 C 0.19053(12) 0.95600(12) 0.13750(12) 0.0253(2) Uani 1 1 d . . . . .
H43A H 0.177230 0.907771 0.216079 0.038 Uiso 1 1 calc R U . . .
H43B H 0.162669 0.918510 0.089527 0.038 Uiso 1 1 calc R U . . .
H43C H 0.141048 1.034365 0.117458 0.038 Uiso 1 1 calc R U . . .
C50A C -0.0590(3) 0.6200(2) 0.2933(2) 0.0197(5) Uani 0.4263(9) 1 d D . P A -1
D50A D -0.0676(15) 0.5621(15) 0.2539(13) 0.024 Uiso 0.4263(9) 1 d D U P A -1
Cl1A Cl -0.20405(7) 0.70662(8) 0.28461(10) 0.0353(2) Uani 0.4263(9) 1 d D U P A
-1
Cl2A Cl -0.00304(9) 0.53793(8) 0.43115(8) 0.0391(2) Uani 0.4263(9) 1 d D . P A
-1
Cl3A Cl 0.05476(9) 0.71004(8) 0.21753(9) 0.0384(2) Uani 0.4263(9) 1 d D . P A
-1
C50B C -0.1227(11) 0.7044(15) 0.2319(9) 0.0190(12) Uani 0.2630(14) 1 d D U P B
-2
D50B D -0.1784(18) 0.671(2) 0.1874(18) 0.023 Uiso 0.2630(14) 1 d D U P B -2
Cl1B Cl -0.1965(8) 0.6982(8) 0.3522(5) 0.0199(5) Uani 0.2630(14) 1 d D U P B -2
Cl2B Cl 0.0250(2) 0.6187(2) 0.2614(2) 0.0487(4) Uani 0.2630(14) 1 d D U P B -2
Cl3B Cl -0.111(2) 0.8500(16) 0.1399(18) 0.0283(6) Uani 0.2630(14) 1 d D U P B
-2
C50C C -0.1074(9) 0.6983(12) 0.2514(7) 0.0190(12) Uani 0.3106(15) 1 d D U P C
-3
D50C D -0.1460(17) 0.642(2) 0.2192(17) 0.023 Uiso 0.3106(15) 1 d D U P C -3
Cl1C Cl -0.1897(7) 0.7015(6) 0.3706(4) 0.0199(5) Uani 0.3106(15) 1 d D U P C -3
Cl2C Cl 0.05494(18) 0.64302(19) 0.2911(2) 0.0487(4) Uani 0.3106(15) 1 d D U P C
-3
Cl3C Cl -0.1147(18) 0.8418(13) 0.1462(15) 0.0283(6) Uani 0.3106(15) 1 d D U P C
-3


_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
O10 C16 1.2095(14) . ?
C10 C15 1.3929(15) . ?
C10 C11 1.3956(15) . ?
C10 C25 1.4837(15) . ?
O11 C16 1.3335(14) . ?
O11 C17 1.4439(14) . ?
C11 C12 1.3931(15) . ?
C11 H11 0.9500 . ?
O12 C18 1.2073(14) . ?
C12 C13 1.3905(15) . ?
C12 C16 1.4860(15) . ?
O13 C18 1.3380(14) . ?
O13 C19 1.4435(14) . ?
C13 C14 1.3906(14) . ?
C13 H13 0.9500 . ?
C14 C15 1.3891(15) . ?
C14 C18 1.4862(15) . ?
C15 H15 0.9500 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 C25 1.4145(15) . ?
C20 C21 1.4159(14) . ?
C20 P40 1.8419(10) . ?
C21 C22 1.3986(15) . ?
C21 C30 1.4906(15) . ?
C22 C23 1.3868(17) . ?
C22 H22 0.9500 . ?
C23 C24 1.3816(16) . ?
C23 H23 0.9500 . ?
C24 C25 1.4001(15) . ?
C24 H24 0.9500 . ?
O30 C36 1.2117(14) . ?
C30 C31 1.3984(15) . ?
C30 C35 1.4010(15) . ?
O31 C36 1.3361(15) . ?
O31 C37 1.4419(15) . ?
C31 C32 1.3972(15) . ?
C31 H31 0.9500 . ?
O32 C38 1.2070(14) . ?
C32 C33 1.3919(15) . ?
C32 C36 1.4926(15) . ?
O33 C38 1.3426(14) . ?
O33 C39 1.4485(15) . ?
C33 C34 1.3950(15) . ?
C33 H33 0.9500 . ?
C34 C35 1.3972(15) . ?
C34 C38 1.4921(16) . ?
C35 H35 0.9500 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
P40 O40 1.4884(8) . ?
P40 C42 1.8129(11) . ?
P40 C40 1.8197(11) . ?
C40 C41 1.5296(15) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 C43 1.5291(17) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C50A Cl1A 1.729(3) . ?
C50A Cl2A 1.748(3) . ?
C50A Cl3A 1.774(3) . ?
C50A D50A 1.045(18) . ?
C50B Cl1B 1.703(10) . ?
C50B Cl2B 1.727(10) . ?
C50B Cl3B 1.763(11) . ?
C50B D50B 1.06(2) . ?
C50C Cl1C 1.765(8) . ?
C50C Cl3C 1.772(9) . ?
C50C Cl2C 1.773(8) . ?
C50C D50C 1.067(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
C15 C10 C11 118.95(10) . . ?
C15 C10 C25 120.35(9) . . ?
C11 C10 C25 120.62(10) . . ?
C16 O11 C17 115.76(9) . . ?
C12 C11 C10 120.40(10) . . ?
C12 C11 H11 119.8 . . ?
C10 C11 H11 119.8 . . ?
C13 C12 C11 120.31(10) . . ?
C13 C12 C16 121.23(10) . . ?
C11 C12 C16 118.44(10) . . ?
C18 O13 C19 114.70(9) . . ?
C12 C13 C14 119.27(10) . . ?
C12 C13 H13 120.4 . . ?
C14 C13 H13 120.4 . . ?
C15 C14 C13 120.46(10) . . ?
C15 C14 C18 117.69(9) . . ?
C13 C14 C18 121.84(10) . . ?
C14 C15 C10 120.46(10) . . ?
C14 C15 H15 119.8 . . ?
C10 C15 H15 119.8 . . ?
O10 C16 O11 123.70(10) . . ?
O10 C16 C12 123.83(11) . . ?
O11 C16 C12 112.47(9) . . ?
O11 C17 H17A 109.5 . . ?
O11 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
O11 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
O12 C18 O13 123.50(11) . . ?
O12 C18 C14 124.34(11) . . ?
O13 C18 C14 112.16(9) . . ?
O13 C19 H19A 109.5 . . ?
O13 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
O13 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C25 C20 C21 117.88(9) . . ?
C25 C20 P40 121.93(8) . . ?
C21 C20 P40 119.89(8) . . ?
C22 C21 C20 119.71(10) . . ?
C22 C21 C30 115.66(9) . . ?
C20 C21 C30 124.58(9) . . ?
C23 C22 C21 121.27(10) . . ?
C23 C22 H22 119.4 . . ?
C21 C22 H22 119.4 . . ?
C24 C23 C22 119.54(10) . . ?
C24 C23 H23 120.2 . . ?
C22 C23 H23 120.2 . . ?
C23 C24 C25 120.41(10) . . ?
C23 C24 H24 119.8 . . ?
C25 C24 H24 119.8 . . ?
C24 C25 C20 120.63(10) . . ?
C24 C25 C10 115.53(9) . . ?
C20 C25 C10 123.81(9) . . ?
C31 C30 C35 118.93(10) . . ?
C31 C30 C21 120.77(10) . . ?
C35 C30 C21 120.10(9) . . ?
C36 O31 C37 115.11(10) . . ?
C32 C31 C30 120.16(10) . . ?
C32 C31 H31 119.9 . . ?
C30 C31 H31 119.9 . . ?
C33 C32 C31 120.70(10) . . ?
C33 C32 C36 117.61(10) . . ?
C31 C32 C36 121.66(10) . . ?
C38 O33 C39 114.76(10) . . ?
C32 C33 C34 119.47(10) . . ?
C32 C33 H33 120.3 . . ?
C34 C33 H33 120.3 . . ?
C33 C34 C35 119.99(10) . . ?
C33 C34 C38 117.76(10) . . ?
C35 C34 C38 122.22(10) . . ?
C34 C35 C30 120.74(10) . . ?
C34 C35 H35 119.6 . . ?
C30 C35 H35 119.6 . . ?
O30 C36 O31 123.46(10) . . ?
O30 C36 C32 124.56(11) . . ?
O31 C36 C32 111.98(10) . . ?
O31 C37 H37A 109.5 . . ?
O31 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
O31 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
O32 C38 O33 124.09(11) . . ?
O32 C38 C34 123.78(10) . . ?
O33 C38 C34 112.13(9) . . ?
O33 C39 H39A 109.5 . . ?
O33 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
O33 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
O40 P40 C42 112.88(5) . . ?
O40 P40 C40 112.63(5) . . ?
C42 P40 C40 101.94(5) . . ?
O40 P40 C20 114.29(5) . . ?
C42 P40 C20 106.07(5) . . ?
C40 P40 C20 108.09(5) . . ?
C41 C40 P40 112.57(8) . . ?
C41 C40 H40A 109.1 . . ?
P40 C40 H40A 109.1 . . ?
C41 C40 H40B 109.1 . . ?
P40 C40 H40B 109.1 . . ?
H40A C40 H40B 107.8 . . ?
C40 C41 H41A 109.5 . . ?
C40 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C40 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C43 C42 P40 114.58(8) . . ?
C43 C42 H42A 108.6 . . ?
P40 C42 H42A 108.6 . . ?
C43 C42 H42B 108.6 . . ?
P40 C42 H42B 108.6 . . ?
H42A C42 H42B 107.6 . . ?
C42 C43 H43A 109.5 . . ?
C42 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C42 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
Cl1A C50A Cl2A 113.17(17) . . ?
Cl1A C50A Cl3A 109.47(16) . . ?
Cl2A C50A Cl3A 110.01(15) . . ?
Cl1A C50A D50A 109.2(9) . . ?
Cl2A C50A D50A 108.6(9) . . ?
Cl3A C50A D50A 106.1(9) . . ?
Cl1B C50B Cl2B 110.8(7) . . ?
Cl1B C50B Cl3B 112.4(11) . . ?
Cl2B C50B Cl3B 111.0(10) . . ?
Cl1B C50B D50B 109.2(12) . . ?
Cl2B C50B D50B 107.6(12) . . ?
Cl3B C50B D50B 105.5(11) . . ?
Cl1C C50C Cl3C 110.9(9) . . ?
Cl1C C50C Cl2C 108.4(5) . . ?
Cl3C C50C Cl2C 107.9(8) . . ?
Cl1C C50C D50C 110.4(11) . . ?
Cl3C C50C D50C 109.9(11) . . ?
Cl2C C50C D50C 109.2(11) . . ?

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
C15 C10 C11 C12 0.79(15) . . . . ?
C25 C10 C11 C12 177.52(9) . . . . ?
C10 C11 C12 C13 2.37(16) . . . . ?
C10 C11 C12 C16 -176.00(9) . . . . ?
C11 C12 C13 C14 -2.51(16) . . . . ?
C16 C12 C13 C14 175.81(10) . . . . ?
C12 C13 C14 C15 -0.48(16) . . . . ?
C12 C13 C14 C18 179.85(10) . . . . ?
C13 C14 C15 C10 3.67(16) . . . . ?
C18 C14 C15 C10 -176.65(10) . . . . ?
C11 C10 C15 C14 -3.79(15) . . . . ?
C25 C10 C15 C14 179.47(10) . . . . ?
C17 O11 C16 O10 3.57(17) . . . . ?
C17 O11 C16 C12 -176.30(10) . . . . ?
C13 C12 C16 O10 -170.12(12) . . . . ?
C11 C12 C16 O10 8.23(17) . . . . ?
C13 C12 C16 O11 9.74(15) . . . . ?
C11 C12 C16 O11 -171.91(9) . . . . ?
C19 O13 C18 O12 -0.67(17) . . . . ?
C19 O13 C18 C14 -179.96(10) . . . . ?
C15 C14 C18 O12 -3.83(17) . . . . ?
C13 C14 C18 O12 175.84(11) . . . . ?
C15 C14 C18 O13 175.45(10) . . . . ?
C13 C14 C18 O13 -4.88(15) . . . . ?
C25 C20 C21 C22 -7.55(15) . . . . ?
P40 C20 C21 C22 166.19(8) . . . . ?
C25 C20 C21 C30 169.70(10) . . . . ?
P40 C20 C21 C30 -16.57(14) . . . . ?
C20 C21 C22 C23 1.91(17) . . . . ?
C30 C21 C22 C23 -175.58(10) . . . . ?
C21 C22 C23 C24 3.91(17) . . . . ?
C22 C23 C24 C25 -3.84(17) . . . . ?
C23 C24 C25 C20 -2.03(17) . . . . ?
C23 C24 C25 C10 176.05(10) . . . . ?
C21 C20 C25 C24 7.66(15) . . . . ?
P40 C20 C25 C24 -165.94(8) . . . . ?
C21 C20 C25 C10 -170.25(10) . . . . ?
P40 C20 C25 C10 16.15(14) . . . . ?
C15 C10 C25 C24 58.30(14) . . . . ?
C11 C10 C25 C24 -118.38(11) . . . . ?
C15 C10 C25 C20 -123.69(11) . . . . ?
C11 C10 C25 C20 59.63(14) . . . . ?
C22 C21 C30 C31 120.70(11) . . . . ?
C20 C21 C30 C31 -56.64(15) . . . . ?
C22 C21 C30 C35 -54.03(14) . . . . ?
C20 C21 C30 C35 128.62(11) . . . . ?
C35 C30 C31 C32 0.08(15) . . . . ?
C21 C30 C31 C32 -174.72(10) . . . . ?
C30 C31 C32 C33 -0.38(16) . . . . ?
C30 C31 C32 C36 177.78(9) . . . . ?
C31 C32 C33 C34 0.11(15) . . . . ?
C36 C32 C33 C34 -178.12(9) . . . . ?
C32 C33 C34 C35 0.45(15) . . . . ?
C32 C33 C34 C38 178.75(10) . . . . ?
C33 C34 C35 C30 -0.75(16) . . . . ?
C38 C34 C35 C30 -178.97(10) . . . . ?
C31 C30 C35 C34 0.48(15) . . . . ?
C21 C30 C35 C34 175.31(10) . . . . ?
C37 O31 C36 O30 -0.64(17) . . . . ?
C37 O31 C36 C32 179.89(11) . . . . ?
C33 C32 C36 O30 -8.42(16) . . . . ?
C31 C32 C36 O30 173.37(11) . . . . ?
C33 C32 C36 O31 171.04(10) . . . . ?
C31 C32 C36 O31 -7.17(14) . . . . ?
C39 O33 C38 O32 4.03(17) . . . . ?
C39 O33 C38 C34 -175.81(10) . . . . ?
C33 C34 C38 O32 -12.97(16) . . . . ?
C35 C34 C38 O32 165.29(11) . . . . ?
C33 C34 C38 O33 166.88(9) . . . . ?
C35 C34 C38 O33 -14.87(15) . . . . ?
C25 C20 P40 O40 -100.01(9) . . . . ?
C21 C20 P40 O40 86.52(9) . . . . ?
C25 C20 P40 C42 134.97(9) . . . . ?
C21 C20 P40 C42 -38.51(10) . . . . ?
C25 C20 P40 C40 26.27(10) . . . . ?
C21 C20 P40 C40 -147.21(8) . . . . ?
O40 P40 C40 C41 -70.98(10) . . . . ?
C42 P40 C40 C41 50.26(10) . . . . ?
C20 P40 C40 C41 161.78(8) . . . . ?
O40 P40 C42 C43 -179.54(8) . . . . ?
C40 P40 C42 C43 59.39(9) . . . . ?
C20 P40 C42 C43 -53.65(10) . . . . ?

_refine_diff_density_max         0.751
_refine_diff_density_min         -0.595
_refine_diff_density_rms         0.061

####################################################################### 
# 
# 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_3dtriclinic
_database_code_depnum_ccdc_archive 'CCDC 1942987'
loop_
_audit_author_name
_audit_author_address
'Timo Stein'
;University of Hamburg
Germany
;
_audit_update_record             
;
2019-09-04 deposited with the CCDC.	2019-09-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H31 O9 P'
_chemical_formula_weight         662.60

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   8.2514(4)
_cell_length_b                   11.6965(5)
_cell_length_c                   17.6863(6)
_cell_angle_alpha                101.701(3)
_cell_angle_beta                 97.017(3)
_cell_angle_gamma                102.970(4)
_cell_volume                     1603.49(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    15424
_cell_measurement_theta_min      3.9750
_cell_measurement_theta_max      76.1710
_cell_oxdiff_length_a            8.2514(4)
_cell_oxdiff_length_b            11.6965(5)
_cell_oxdiff_length_c            17.6863(6)
_cell_oxdiff_angle_alpha         101.701(3)
_cell_oxdiff_angle_beta          97.017(3)
_cell_oxdiff_angle_gamma         102.970(4)
_cell_oxdiff_volume              1603.49(11)
_cell_oxdiff_measurement_reflns_used 15424

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_F_000             692
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.250
_exptl_absorpt_coefficient_mu    1.254
_shelx_estimated_absorpt_T_min   0.634
_shelx_estimated_absorpt_T_max   0.745
_exptl_absorpt_correction_T_min  0.64349
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.481
_oxdiff_exptl_absorpt_empirical_full_max 2.439
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Atlas
_diffrn_detector_area_resol_mean 5.2063
_diffrn_reflns_number            32088
_diffrn_reflns_av_unetI/netI     0.0291
_diffrn_reflns_av_R_equivalents  0.0509
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         3.993
_diffrn_reflns_theta_max         77.664
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0862054000
_diffrn_orient_matrix_UB_12      -0.0703452000
_diffrn_orient_matrix_UB_13      -0.0591656000
_diffrn_orient_matrix_UB_21      -0.1388492000
_diffrn_orient_matrix_UB_22      -0.1163280000
_diffrn_orient_matrix_UB_23      -0.0073124000
_diffrn_orient_matrix_UB_31      -0.1056701000
_diffrn_orient_matrix_UB_32      0.0297429000
_diffrn_orient_matrix_UB_33      -0.0679028000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -96.00  -2.00   1.00    1.00    --  -41.85 125.00   0.00   94
  2  ω   -116.00 -17.00   1.00    1.00    --  -41.85 -38.00-150.00   99
  3  ω   -122.00  -1.00   1.00    1.00    --  -41.85 -19.00 -90.00  121
  4  ω     23.00  98.00   1.00    1.00    --   41.85-125.00 -30.00   75
  5  ω      1.00  83.00   1.00    1.00    --   41.85 -99.00  90.00   82
  6  ω      1.00  83.00   1.00    1.00    --   41.85 -99.00-180.00   82
  7  ω     36.00 116.00   1.00    4.00    --  112.00-111.00 -30.00   80
  8  ω     36.00 116.00   1.00    4.00    --  112.00-111.00 120.00   80
  9  ω     40.00 141.00   1.00    4.00    --  112.00 -61.00 -60.00  101
 10  ω    100.00 178.00   1.00    4.00    --  112.00 111.00 -30.00   78
 11  ω     29.00 109.00   1.00    4.00    --  112.00 -94.00 150.00   80
 12  ω     29.00 109.00   1.00    4.00    --  112.00 -94.00-120.00   80
 13  ω     36.00 116.00   1.00    4.00    --  112.00-111.00  30.00   80
 14  ω     86.00 178.00   1.00    4.00    --  112.00  45.00  90.00   92
 15  ω     84.00 178.00   1.00    4.00    --  112.00  30.00   0.00   94
 16  ω    100.00 178.00   1.00    4.00    --  112.00 111.00 -90.00   78
 17  ω    100.00 178.00   1.00    4.00    --  112.00 111.00  30.00   78
 18  ω     29.00 109.00   1.00    4.00    --  112.00 -94.00  60.00   80
 19  ω     39.00 138.00   1.00    4.00    --  112.00 -45.00 120.00   99
 20  ω     29.00 109.00   1.00    4.00    --  112.00 -94.00 120.00   80
 21  ω    100.00 178.00   1.00    4.00    --  112.00 111.00 -60.00   78
 22  ω     36.00 116.00   1.00    4.00    --  112.00-111.00-150.00   80
 23  ω     80.00 178.00   1.00    4.00    --  112.00  75.00   7.16   98
 24  ω     79.00 178.00   1.00    4.00    --  112.00  77.00  90.00   99
 25  ω     29.00 109.00   1.00    4.00    --  112.00 -94.00 -30.00   80
 26  ω     79.00 178.00   1.00    4.00    --  112.00  77.00 -90.00   99
 27  ω     57.00 151.00   1.00    4.00    --  112.00 178.00 -30.00   94
 28  ω   -118.00  -9.00   1.00    1.00    --  -41.85 -77.00  90.00  109
 29  ω   -118.00  -9.00   1.00    1.00    --  -41.85 -77.00 120.00  109
 30  ω   -118.00  -9.00   1.00    1.00    --  -41.85 -77.00-180.00  109
 31  ω    -74.00  34.00   1.00    1.00    --  -41.85  77.00 -30.00  108
 32  ω      9.00 118.00   1.00    1.00    --   41.85  77.00 -60.00  109
 33  ω      9.00 118.00   1.00    1.00    --   41.85  77.00  30.00  109
 34  ω     84.00 178.00   1.00    4.00    --  112.00  30.00-180.00   94
 35  ω     86.00 178.00   1.00    4.00    --  112.00  45.00  60.00   92
 36  ω     79.00 178.00   1.00    4.00    --  112.00  77.00-180.00   99
 37  ω     80.00 160.00   1.00    4.00    --  112.00  73.00 117.95   80
 38  ω     86.00 178.00   1.00    4.00    --  112.00  45.00-120.00   92
;
_diffrn_measurement_method       'ω scans'
_reflns_number_total             6679
_reflns_number_gt                5812
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0795P)²+0.4780P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6679
_refine_ls_number_parameters     437
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0510
_refine_ls_R_factor_gt           0.0450
_refine_ls_wR_factor_ref         0.1275
_refine_ls_wR_factor_gt          0.1206
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.033
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C10 C 0.38912(18) 0.60097(13) 0.72794(9) 0.0219(3) Uani 1 1 d . . . . .
C11 C 0.39450(19) 0.51751(14) 0.77534(9) 0.0235(3) Uani 1 1 d . . . . .
C12 C 0.2864(2) 0.40126(14) 0.75022(9) 0.0277(3) Uani 1 1 d . . . . .
H12 H 0.291799 0.344706 0.781547 0.033 Uiso 1 1 calc R U . . .
C13 C 0.1715(2) 0.36687(15) 0.68044(10) 0.0305(3) Uani 1 1 d . . . . .
H13 H 0.102817 0.286421 0.662760 0.037 Uiso 1 1 calc R U . . .
C14 C 0.1583(2) 0.45162(15) 0.63678(9) 0.0281(3) Uani 1 1 d . . . . .
H14 H 0.076573 0.429395 0.590099 0.034 Uiso 1 1 calc R U . . .
C15 C 0.26229(19) 0.56803(14) 0.66006(9) 0.0239(3) Uani 1 1 d . . . . .
C20 C 0.50679(19) 0.54536(14) 0.85300(9) 0.0237(3) Uani 1 1 d . . . . .
C21 C 0.51672(19) 0.64727(14) 0.91162(9) 0.0240(3) Uani 1 1 d . . . . .
H21 H 0.455622 0.704060 0.901655 0.029 Uiso 1 1 calc R U . . .
C22 C 0.61648(19) 0.66637(14) 0.98525(9) 0.0250(3) Uani 1 1 d . . . . .
C23 C 0.70554(19) 0.58294(14) 1.00030(9) 0.0256(3) Uani 1 1 d . . . . .
H23 H 0.772068 0.595515 1.050484 0.031 Uiso 1 1 calc R U . . .
C24 C 0.69702(19) 0.48168(14) 0.94205(9) 0.0251(3) Uani 1 1 d . . . . .
C25 C 0.59736(19) 0.46268(14) 0.86902(9) 0.0245(3) Uani 1 1 d . . . . .
H25 H 0.590713 0.392578 0.829464 0.029 Uiso 1 1 calc R U . . .
C26 C 0.6292(2) 0.77168(15) 1.05090(10) 0.0281(3) Uani 1 1 d . . . . .
C27 C 0.5497(2) 0.95085(16) 1.09447(11) 0.0373(4) Uani 1 1 d . . . . .
H27A H 0.498619 0.921839 1.136505 0.056 Uiso 1 1 calc R U . . .
H27B H 0.487192 1.003972 1.074855 0.056 Uiso 1 1 calc R U . . .
H27C H 0.667609 0.995788 1.114912 0.056 Uiso 1 1 calc R U . . .
C28 C 0.7924(2) 0.39416(15) 0.96131(10) 0.0285(3) Uani 1 1 d . . . . .
C29 C 0.8669(3) 0.21340(18) 0.91403(13) 0.0434(5) Uani 1 1 d . . . . .
H29A H 0.989148 0.249384 0.926043 0.065 Uiso 1 1 calc R U . . .
H29B H 0.839899 0.146288 0.867375 0.065 Uiso 1 1 calc R U . . .
H29C H 0.830074 0.183321 0.958590 0.065 Uiso 1 1 calc R U . . .
C30 C 0.23052(18) 0.65450(14) 0.61142(9) 0.0241(3) Uani 1 1 d . . . . .
C31 C 0.17460(18) 0.75479(14) 0.64243(9) 0.0245(3) Uani 1 1 d . . . . .
H31 H 0.154587 0.768760 0.694876 0.029 Uiso 1 1 calc R U . . .
C32 C 0.14778(18) 0.83526(14) 0.59617(9) 0.0245(3) Uani 1 1 d . . . . .
C33 C 0.17771(18) 0.81626(14) 0.51955(9) 0.0246(3) Uani 1 1 d . . . . .
H33 H 0.161492 0.871870 0.488764 0.029 Uiso 1 1 calc R U . . .
C34 C 0.23177(19) 0.71478(14) 0.48826(9) 0.0251(3) Uani 1 1 d . . . . .
C35 C 0.25443(19) 0.63311(14) 0.53383(9) 0.0247(3) Uani 1 1 d . . . . .
H35 H 0.286483 0.562282 0.511592 0.030 Uiso 1 1 calc R U . . .
C36 C 0.09555(19) 0.94650(14) 0.62933(9) 0.0263(3) Uani 1 1 d . . . . .
C37 C -0.0109(2) 1.04678(16) 0.73279(10) 0.0335(4) Uani 1 1 d . . . . .
H37A H 0.091502 1.110963 0.757489 0.050 Uiso 1 1 calc R U . . .
H37B H -0.077731 1.027771 0.772871 0.050 Uiso 1 1 calc R U . . .
H37C H -0.077931 1.073918 0.693650 0.050 Uiso 1 1 calc R U . . .
C38 C 0.2735(2) 0.68973(14) 0.40827(9) 0.0263(3) Uani 1 1 d . . . . .
C39 C 0.3195(3) 0.76369(19) 0.29718(11) 0.0448(5) Uani 1 1 d . . . . .
H39A H 0.430969 0.746939 0.300256 0.067 Uiso 1 1 calc R U . . .
H39B H 0.322569 0.836252 0.277182 0.067 Uiso 1 1 calc R U . . .
H39C H 0.235387 0.694887 0.261757 0.067 Uiso 1 1 calc R U . . .
C40 C 0.74342(19) 0.74462(14) 0.79932(9) 0.0241(3) Uani 1 1 d . . . . .
C41 C 0.8275(2) 0.84674(15) 0.85767(10) 0.0282(3) Uani 1 1 d . . . . .
H41 H 0.771374 0.907546 0.874178 0.034 Uiso 1 1 calc R U . . .
C42 C 0.9943(2) 0.86041(16) 0.89220(11) 0.0339(4) Uani 1 1 d . . . . .
H42 H 1.052071 0.930718 0.931783 0.041 Uiso 1 1 calc R U . . .
C43 C 1.0753(2) 0.77116(17) 0.86852(11) 0.0349(4) Uani 1 1 d . . . . .
H43 H 1.189494 0.781101 0.891201 0.042 Uiso 1 1 calc R U . . .
C44 C 0.9905(2) 0.66729(16) 0.81188(10) 0.0317(4) Uani 1 1 d . . . . .
H44 H 1.045636 0.605247 0.797113 0.038 Uiso 1 1 calc R U . . .
C45 C 0.8248(2) 0.65367(15) 0.77659(10) 0.0273(3) Uani 1 1 d . . . . .
H45 H 0.767301 0.582975 0.737274 0.033 Uiso 1 1 calc R U . . .
C46 C 0.59298(18) 0.77179(14) 0.65552(9) 0.0245(3) Uani 1 1 d . . . . .
C47 C 0.5813(2) 0.88024(15) 0.63702(10) 0.0289(3) Uani 1 1 d . . . . .
H47 H 0.540997 0.936826 0.671377 0.035 Uiso 1 1 calc R U . . .
C48 C 0.6287(2) 0.90546(16) 0.56810(11) 0.0343(4) Uani 1 1 d . . . . .
H48 H 0.620624 0.979430 0.555542 0.041 Uiso 1 1 calc R U . . .
C49 C 0.6872(2) 0.82397(18) 0.51799(11) 0.0360(4) Uani 1 1 d . . . . .
H49 H 0.720044 0.842016 0.471209 0.043 Uiso 1 1 calc R U . . .
C50 C 0.6982(2) 0.71472(18) 0.53597(11) 0.0342(4) Uani 1 1 d . . . . .
H50 H 0.737717 0.658186 0.501198 0.041 Uiso 1 1 calc R U . . .
C51 C 0.6515(2) 0.68875(15) 0.60469(10) 0.0282(3) Uani 1 1 d . . . . .
H51 H 0.659328 0.614616 0.617045 0.034 Uiso 1 1 calc R U . . .
O20 O 0.70831(17) 0.78622(12) 1.11585(7) 0.0375(3) Uani 1 1 d . . . . .
O21 O 0.54352(16) 0.84857(11) 1.03099(7) 0.0335(3) Uani 1 1 d . . . . .
O22 O 0.87011(17) 0.40332(12) 1.02563(8) 0.0383(3) Uani 1 1 d . . . . .
O23 O 0.78088(16) 0.30359(11) 0.89939(7) 0.0341(3) Uani 1 1 d . . . . .
O30 O 0.10820(18) 1.03246(12) 0.60044(8) 0.0383(3) Uani 1 1 d . . . . .
O31 O 0.03530(15) 0.94061(10) 0.69517(7) 0.0304(3) Uani 1 1 d . . . . .
O32 O 0.30524(17) 0.59783(11) 0.37700(7) 0.0350(3) Uani 1 1 d . . . . .
O33 O 0.27481(17) 0.78277(11) 0.37406(7) 0.0347(3) Uani 1 1 d . . . . .
O40 O 0.47812(14) 0.84882(10) 0.79152(7) 0.0284(2) Uani 1 1 d . . . . .
P40 P 0.54060(5) 0.74897(3) 0.74893(2) 0.02194(11) 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
C10 C11 1.414(2) . ?
C10 C15 1.418(2) . ?
C10 P40 1.8308(15) . ?
C11 C12 1.398(2) . ?
C11 C20 1.491(2) . ?
C12 C13 1.388(2) . ?
C12 H12 0.9500 . ?
C13 C14 1.389(2) . ?
C13 H13 0.9500 . ?
C14 C15 1.386(2) . ?
C14 H14 0.9500 . ?
C15 C30 1.499(2) . ?
C20 C21 1.392(2) . ?
C20 C25 1.399(2) . ?
C21 C22 1.400(2) . ?
C21 H21 0.9500 . ?
C22 C23 1.394(2) . ?
C22 C26 1.486(2) . ?
C23 C24 1.385(2) . ?
C23 H23 0.9500 . ?
C24 C25 1.391(2) . ?
C24 C28 1.490(2) . ?
C25 H25 0.9500 . ?
C26 O20 1.209(2) . ?
C26 O21 1.336(2) . ?
C27 O21 1.452(2) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 O22 1.207(2) . ?
C28 O23 1.338(2) . ?
C29 O23 1.4443(19) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 C31 1.390(2) . ?
C30 C35 1.391(2) . ?
C31 C32 1.402(2) . ?
C31 H31 0.9500 . ?
C32 C33 1.390(2) . ?
C32 C36 1.492(2) . ?
C33 C34 1.395(2) . ?
C33 H33 0.9500 . ?
C34 C35 1.398(2) . ?
C34 C38 1.484(2) . ?
C35 H35 0.9500 . ?
C36 O30 1.207(2) . ?
C36 O31 1.329(2) . ?
C37 O31 1.4386(19) . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 O32 1.204(2) . ?
C38 O33 1.3468(19) . ?
C39 O33 1.439(2) . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 C41 1.388(2) . ?
C40 C45 1.399(2) . ?
C40 P40 1.8138(15) . ?
C41 C42 1.396(2) . ?
C41 H41 0.9500 . ?
C42 C43 1.384(3) . ?
C42 H42 0.9500 . ?
C43 C44 1.387(3) . ?
C43 H43 0.9500 . ?
C44 C45 1.392(2) . ?
C44 H44 0.9500 . ?
C45 H45 0.9500 . ?
C46 C47 1.393(2) . ?
C46 C51 1.395(2) . ?
C46 P40 1.8136(16) . ?
C47 C48 1.392(2) . ?
C47 H47 0.9500 . ?
C48 C49 1.377(3) . ?
C48 H48 0.9500 . ?
C49 C50 1.397(3) . ?
C49 H49 0.9500 . ?
C50 C51 1.389(2) . ?
C50 H50 0.9500 . ?
C51 H51 0.9500 . ?
O40 P40 1.4850(12) . ?

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
C11 C10 C15 118.64(14) . . ?
C11 C10 P40 123.20(11) . . ?
C15 C10 P40 118.16(11) . . ?
C12 C11 C10 119.39(14) . . ?
C12 C11 C20 116.29(13) . . ?
C10 C11 C20 124.31(14) . . ?
C13 C12 C11 121.32(14) . . ?
C13 C12 H12 119.3 . . ?
C11 C12 H12 119.3 . . ?
C12 C13 C14 119.11(15) . . ?
C12 C13 H13 120.4 . . ?
C14 C13 H13 120.4 . . ?
C15 C14 C13 121.21(14) . . ?
C15 C14 H14 119.4 . . ?
C13 C14 H14 119.4 . . ?
C14 C15 C10 119.93(14) . . ?
C14 C15 C30 116.89(13) . . ?
C10 C15 C30 123.17(14) . . ?
C21 C20 C25 118.96(14) . . ?
C21 C20 C11 122.10(13) . . ?
C25 C20 C11 118.83(14) . . ?
C20 C21 C22 120.20(14) . . ?
C20 C21 H21 119.9 . . ?
C22 C21 H21 119.9 . . ?
C23 C22 C21 120.11(15) . . ?
C23 C22 C26 117.00(14) . . ?
C21 C22 C26 122.87(14) . . ?
C24 C23 C22 119.97(14) . . ?
C24 C23 H23 120.0 . . ?
C22 C23 H23 120.0 . . ?
C23 C24 C25 119.81(14) . . ?
C23 C24 C28 118.00(14) . . ?
C25 C24 C28 122.16(15) . . ?
C24 C25 C20 120.94(14) . . ?
C24 C25 H25 119.5 . . ?
C20 C25 H25 119.5 . . ?
O20 C26 O21 123.33(16) . . ?
O20 C26 C22 123.54(15) . . ?
O21 C26 C22 113.13(14) . . ?
O21 C27 H27A 109.5 . . ?
O21 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
O21 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
O22 C28 O23 123.79(15) . . ?
O22 C28 C24 123.90(16) . . ?
O23 C28 C24 112.31(13) . . ?
O23 C29 H29A 109.5 . . ?
O23 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
O23 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C31 C30 C35 119.47(14) . . ?
C31 C30 C15 120.90(14) . . ?
C35 C30 C15 119.62(14) . . ?
C30 C31 C32 119.90(15) . . ?
C30 C31 H31 120.0 . . ?
C32 C31 H31 120.0 . . ?
C33 C32 C31 120.59(14) . . ?
C33 C32 C36 118.49(13) . . ?
C31 C32 C36 120.84(14) . . ?
C32 C33 C34 119.40(14) . . ?
C32 C33 H33 120.3 . . ?
C34 C33 H33 120.3 . . ?
C33 C34 C35 119.91(15) . . ?
C33 C34 C38 123.17(14) . . ?
C35 C34 C38 116.88(14) . . ?
C30 C35 C34 120.64(14) . . ?
C30 C35 H35 119.7 . . ?
C34 C35 H35 119.7 . . ?
O30 C36 O31 123.82(15) . . ?
O30 C36 C32 124.15(15) . . ?
O31 C36 C32 112.03(13) . . ?
O31 C37 H37A 109.5 . . ?
O31 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
O31 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
O32 C38 O33 123.00(15) . . ?
O32 C38 C34 124.61(14) . . ?
O33 C38 C34 112.38(13) . . ?
O33 C39 H39A 109.5 . . ?
O33 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
O33 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C41 C40 C45 119.78(14) . . ?
C41 C40 P40 115.60(12) . . ?
C45 C40 P40 124.15(12) . . ?
C40 C41 C42 120.23(16) . . ?
C40 C41 H41 119.9 . . ?
C42 C41 H41 119.9 . . ?
C43 C42 C41 119.74(17) . . ?
C43 C42 H42 120.1 . . ?
C41 C42 H42 120.1 . . ?
C42 C43 C44 120.35(15) . . ?
C42 C43 H43 119.8 . . ?
C44 C43 H43 119.8 . . ?
C43 C44 C45 120.20(16) . . ?
C43 C44 H44 119.9 . . ?
C45 C44 H44 119.9 . . ?
C44 C45 C40 119.66(16) . . ?
C44 C45 H45 120.2 . . ?
C40 C45 H45 120.2 . . ?
C47 C46 C51 119.86(15) . . ?
C47 C46 P40 117.34(13) . . ?
C51 C46 P40 122.73(12) . . ?
C48 C47 C46 119.83(16) . . ?
C48 C47 H47 120.1 . . ?
C46 C47 H47 120.1 . . ?
C49 C48 C47 120.47(16) . . ?
C49 C48 H48 119.8 . . ?
C47 C48 H48 119.8 . . ?
C48 C49 C50 119.96(16) . . ?
C48 C49 H49 120.0 . . ?
C50 C49 H49 120.0 . . ?
C51 C50 C49 120.02(17) . . ?
C51 C50 H50 120.0 . . ?
C49 C50 H50 120.0 . . ?
C50 C51 C46 119.85(15) . . ?
C50 C51 H51 120.1 . . ?
C46 C51 H51 120.1 . . ?
C26 O21 C27 114.47(13) . . ?
C28 O23 C29 115.51(14) . . ?
C36 O31 C37 115.47(13) . . ?
C38 O33 C39 114.25(13) . . ?
O40 P40 C46 112.51(7) . . ?
O40 P40 C40 111.72(7) . . ?
C46 P40 C40 101.08(7) . . ?
O40 P40 C10 113.54(7) . . ?
C46 P40 C10 106.42(7) . . ?
C40 P40 C10 110.77(7) . . ?

_refine_diff_density_max         0.565
_refine_diff_density_min         -0.372
_refine_diff_density_rms         0.059

####################################################################### 
# 
# 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_3d
_database_code_depnum_ccdc_archive 'CCDC 1942985'
loop_
_audit_author_name
_audit_author_address
'Timo Stein'
;University of Hamburg
Germany
;
_audit_update_record             
;
2019-09-04 deposited with the CCDC.	2019-09-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C38 H31 O9 P, 2(C H Cl3)'
_chemical_formula_sum            'C40 H33 Cl6 O9 P'
_chemical_formula_weight         901.33

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   10.24130(10)
_cell_length_b                   22.4781(3)
_cell_length_c                   17.7231(2)
_cell_angle_alpha                90
_cell_angle_beta                 94.4590(10)
_cell_angle_gamma                90
_cell_volume                     4067.60(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    26357
_cell_measurement_theta_min      3.4420
_cell_measurement_theta_max      31.9260

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.472
_exptl_crystal_F_000             1848
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.07
_exptl_absorpt_coefficient_mu    0.516
_shelx_estimated_absorpt_T_min   0.904
_shelx_estimated_absorpt_T_max   0.965
_exptl_absorpt_correction_T_min  0.95412
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_ambient_environment      N~2~
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Atlas
_diffrn_detector_area_resol_mean 10.4127
_diffrn_reflns_number            78872
_diffrn_reflns_av_unetI/netI     0.0280
_diffrn_reflns_av_R_equivalents  0.0349
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.870
_diffrn_reflns_theta_max         32.638
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.946
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.946
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_orient_matrix_UB_11      0.0676510000
_diffrn_orient_matrix_UB_12      -0.0070974000
_diffrn_orient_matrix_UB_13      0.0044018000
_diffrn_orient_matrix_UB_21      -0.0019016000
_diffrn_orient_matrix_UB_22      -0.0082823000
_diffrn_orient_matrix_UB_23      -0.0386886000
_diffrn_orient_matrix_UB_31      0.0157006000
_diffrn_orient_matrix_UB_32      0.0296060000
_diffrn_orient_matrix_UB_33      -0.0097784000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -45.00   52.00   1.0000   75.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.3271   38.0000    0.0000 97

#__ type_ start__ end____ width___ exp.time_
  2 omega   -9.00  101.00   1.0000   75.0000
omega____ theta____ kappa____ phi______ frames
    -       22.6396   57.0000   90.0000 110

#__ type_ start__ end____ width___ exp.time_
  3 omega    5.00   93.00   1.0000   75.0000
omega____ theta____ kappa____ phi______ frames
    -       22.6396   57.0000  -30.0000 88

#__ type_ start__ end____ width___ exp.time_
  4 omega  -12.00  104.00   1.0000   75.0000
omega____ theta____ kappa____ phi______ frames
    -       22.6396   77.0000 -150.0000 116

#__ type_ start__ end____ width___ exp.time_
  5 omega  -12.00   67.00   1.0000   75.0000
omega____ theta____ kappa____ phi______ frames
    -       22.6396  -99.0000   90.0000 79

#__ type_ start__ end____ width___ exp.time_
  6 omega  -47.00   64.00   1.0000   75.0000
omega____ theta____ kappa____ phi______ frames
    -       22.6396  -19.0000   90.0000 111

#__ type_ start__ end____ width___ exp.time_
  7 omega   13.00   95.00   1.0000   75.0000
omega____ theta____ kappa____ phi______ frames
    -       22.6396 -145.0000  -44.6969 82

;
_diffrn_measurement_method       'ω scans'
_reflns_number_total             14097
_reflns_number_gt                11252
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_theta     30.44
_reflns_odcompleteness_iscentric 1

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

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_structure_solution    'SUPERFLIP (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0492P)²+3.5090P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         14097
_refine_ls_number_parameters     549
_refine_ls_number_restraints     112
_refine_ls_R_factor_all          0.0639
_refine_ls_R_factor_gt           0.0474
_refine_ls_wR_factor_ref         0.1219
_refine_ls_wR_factor_gt          0.1122
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.061
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O10 O 1.23595(12) 0.51860(6) 0.12882(11) 0.0410(4) Uani 1 1 d . . . . .
C10 C 0.87003(13) 0.64340(6) 0.17321(8) 0.0138(2) Uani 1 1 d . . . . .
O11 O 1.26425(11) 0.61633(5) 0.14548(8) 0.0264(3) Uani 1 1 d . . . . .
C11 C 1.00399(13) 0.63432(6) 0.16758(8) 0.0157(2) Uani 1 1 d . . . . .
H11 H 1.064221 0.665561 0.180275 0.019 Uiso 1 1 calc R U . . .
O12 O 0.77944(11) 0.43990(5) 0.10509(8) 0.0285(3) Uani 1 1 d . . . . .
C12 C 1.04958(13) 0.57960(6) 0.14340(9) 0.0178(3) Uani 1 1 d . . . . .
O13 O 0.61471(10) 0.50555(5) 0.10625(7) 0.0196(2) Uani 1 1 d . . . . .
C13 C 0.96265(14) 0.53348(6) 0.12541(9) 0.0188(3) Uani 1 1 d . . . . .
H13 H 0.994278 0.496187 0.109395 0.023 Uiso 1 1 calc R U . . .
C14 C 0.82915(14) 0.54189(6) 0.13086(8) 0.0163(2) Uani 1 1 d . . . . .
C15 C 0.78301(13) 0.59673(6) 0.15452(8) 0.0150(2) Uani 1 1 d . . . . .
H15 H 0.691742 0.602404 0.157965 0.018 Uiso 1 1 calc R U . . .
C16 C 1.19174(14) 0.56750(7) 0.13804(10) 0.0223(3) Uani 1 1 d . . . . .
C17 C 1.40430(16) 0.60652(8) 0.14937(13) 0.0325(4) Uani 1 1 d . . . . .
H17A H 1.427523 0.574243 0.185094 0.049 Uiso 1 1 calc R U . . .
H17B H 1.449849 0.643000 0.166511 0.049 Uiso 1 1 calc R U . . .
H17C H 1.430343 0.595668 0.099126 0.049 Uiso 1 1 calc R U . . .
C18 C 0.74119(14) 0.49020(6) 0.11263(9) 0.0177(3) Uani 1 1 d . . . . .
C19 C 0.52446(15) 0.45689(7) 0.08980(10) 0.0218(3) Uani 1 1 d . . . . .
H19A H 0.541355 0.439031 0.041065 0.033 Uiso 1 1 calc R U . . .
H19B H 0.434368 0.471866 0.087447 0.033 Uiso 1 1 calc R U . . .
H19C H 0.536529 0.426803 0.129759 0.033 Uiso 1 1 calc R U . . .
C20 C 0.86906(12) 0.75697(6) 0.18446(8) 0.0123(2) Uani 1 1 d . . . . .
C21 C 0.82353(13) 0.70022(6) 0.20538(8) 0.0133(2) Uani 1 1 d . . . . .
C22 C 0.74115(13) 0.69581(6) 0.26457(8) 0.0160(2) Uani 1 1 d . . . . .
H22 H 0.706914 0.658092 0.277022 0.019 Uiso 1 1 calc R U . . .
C23 C 0.70868(14) 0.74570(6) 0.30537(8) 0.0173(3) Uani 1 1 d . . . . .
H23 H 0.648677 0.742457 0.343440 0.021 Uiso 1 1 calc R U . . .
C24 C 0.76430(13) 0.80036(6) 0.29030(8) 0.0158(2) Uani 1 1 d . . . . .
H24 H 0.746984 0.833910 0.320555 0.019 Uiso 1 1 calc R U . . .
C25 C 0.84541(13) 0.80637(6) 0.23104(8) 0.0128(2) Uani 1 1 d . . . . .
O30 O 1.28364(12) 0.98560(6) 0.18615(9) 0.0350(3) Uani 1 1 d . . . . .
C30 C 0.90568(13) 0.86577(6) 0.22039(8) 0.0135(2) Uani 1 1 d . . . . .
O31 O 1.30835(10) 0.89351(5) 0.23349(7) 0.0215(2) Uani 1 1 d . . . . .
C31 C 1.04140(13) 0.87332(6) 0.22239(8) 0.0150(2) Uani 1 1 d . . . . .
H31 H 1.098155 0.840399 0.232737 0.018 Uiso 1 1 calc R U . . .
O32 O 0.82862(12) 1.06958(5) 0.15052(8) 0.0281(3) Uani 1 1 d . . . . .
C32 C 1.09326(13) 0.92962(6) 0.20908(8) 0.0163(2) Uani 1 1 d . . . . .
O33 O 0.66252(10) 1.00808(5) 0.17160(7) 0.0204(2) Uani 1 1 d . . . . .
C33 C 1.01095(14) 0.97776(6) 0.19271(8) 0.0169(3) Uani 1 1 d . . . . .
H33 H 1.046686 1.015520 0.181818 0.020 Uiso 1 1 calc R U . . .
C34 C 0.87584(13) 0.97054(6) 0.19231(8) 0.0148(2) Uani 1 1 d . . . . .
C35 C 0.82408(13) 0.91503(6) 0.20744(8) 0.0147(2) Uani 1 1 d . . . . .
H35 H 0.732083 0.910573 0.208988 0.018 Uiso 1 1 calc R U . . .
C36 C 1.23707(14) 0.94003(7) 0.20805(9) 0.0195(3) Uani 1 1 d . . . . .
C37 C 1.44852(15) 0.90192(8) 0.23534(11) 0.0283(3) Uani 1 1 d . . . . .
H37A H 1.474269 0.907179 0.183651 0.042 Uiso 1 1 calc R U . . .
H37B H 1.492997 0.866976 0.258229 0.042 Uiso 1 1 calc R U . . .
H37C H 1.473308 0.937320 0.265411 0.042 Uiso 1 1 calc R U . . .
C38 C 0.78926(14) 1.02177(6) 0.16966(9) 0.0176(3) Uani 1 1 d . . . . .
C39 C 0.57032(16) 1.05413(7) 0.14700(10) 0.0246(3) Uani 1 1 d . . . . .
H39A H 0.585949 1.089466 0.178809 0.037 Uiso 1 1 calc R U . . .
H39B H 0.480868 1.039773 0.151362 0.037 Uiso 1 1 calc R U . . .
H39C H 0.581634 1.064360 0.094156 0.037 Uiso 1 1 calc R U . . .
P40 P 0.95007(3) 0.76848(2) 0.09743(2) 0.01263(7) Uani 1 1 d . . . . .
O40 O 1.09571(10) 0.76843(5) 0.10819(6) 0.0187(2) Uani 1 1 d . . . . .
C40 C 0.89012(14) 0.71294(6) 0.02968(8) 0.0151(2) Uani 1 1 d . . . . .
C41 C 0.98322(15) 0.68033(7) -0.00629(9) 0.0218(3) Uani 1 1 d . . . . .
H41 H 1.073853 0.687878 0.005215 0.026 Uiso 1 1 calc R U . . .
C42 C 0.94363(18) 0.63680(8) -0.05893(10) 0.0282(3) Uani 1 1 d . . . . .
H42 H 1.007233 0.614393 -0.082956 0.034 Uiso 1 1 calc R U . . .
C43 C 0.81139(19) 0.62608(7) -0.07639(10) 0.0270(3) Uani 1 1 d . . . . .
H43 H 0.784451 0.596011 -0.111922 0.032 Uiso 1 1 calc R U . . .
C44 C 0.71843(16) 0.65925(7) -0.04199(9) 0.0226(3) Uani 1 1 d . . . . .
H44 H 0.627886 0.652305 -0.054694 0.027 Uiso 1 1 calc R U . . .
C45 C 0.75727(14) 0.70262(6) 0.01101(9) 0.0183(3) Uani 1 1 d . . . . .
H45 H 0.693326 0.725211 0.034504 0.022 Uiso 1 1 calc R U . . .
C46 C 0.88773(14) 0.83738(6) 0.05585(8) 0.0148(2) Uani 1 1 d . . . . .
C47 C 0.97824(16) 0.87452(7) 0.02453(9) 0.0217(3) Uani 1 1 d . . . . .
H47 H 1.068087 0.863607 0.026969 0.026 Uiso 1 1 calc R U . . .
C48 C 0.93740(19) 0.92739(8) -0.01022(10) 0.0289(3) Uani 1 1 d . . . . .
H48 H 0.999236 0.952278 -0.032099 0.035 Uiso 1 1 calc R U . . .
C49 C 0.80699(19) 0.94401(7) -0.01312(10) 0.0289(4) Uani 1 1 d . . . . .
H49 H 0.779845 0.980776 -0.035663 0.035 Uiso 1 1 calc R U . . .
C50 C 0.71581(17) 0.90690(7) 0.01696(9) 0.0237(3) Uani 1 1 d . . . . .
H50 H 0.626116 0.918077 0.014348 0.028 Uiso 1 1 calc R U . . .
C51 C 0.75547(14) 0.85348(6) 0.05084(8) 0.0177(3) Uani 1 1 d . . . . .
H51 H 0.692695 0.827877 0.070622 0.021 Uiso 1 1 calc R U . . .
C60A C 0.2617(7) 0.1975(3) 0.1498(6) 0.0211(5) Uiso 0.497(2) 1 d D U P A 1
H60A H 0.208714 0.203248 0.100582 0.025 Uiso 0.497(2) 1 calc R U P A 1
Cl1A Cl 0.20169(15) 0.24561(7) 0.21817(9) 0.02792(19) Uiso 0.497(2) 1 d D U P A
1
Cl2A Cl 0.42773(12) 0.21127(9) 0.13653(7) 0.02435(18) Uiso 0.497(2) 1 d D U P A
1
Cl3A Cl 0.25814(15) 0.12092(7) 0.17518(10) 0.02451(17) Uiso 0.497(2) 1 d D U P
A 1
C60B C 0.2201(12) 0.2164(6) 0.1526(8) 0.0211(5) Uiso 0.0902(7) 1 d D U P B 2
H60B H 0.191927 0.244410 0.110529 0.025 Uiso 0.0902(7) 1 calc R U P B 2
Cl1B Cl 0.2328(5) 0.2550(2) 0.2378(3) 0.02792(19) Uiso 0.0902(7) 1 d D U P B 2
Cl2B Cl 0.3794(5) 0.1884(2) 0.1385(3) 0.02435(18) Uiso 0.0902(7) 1 d D U P B 2
Cl3B Cl 0.1085(4) 0.15657(19) 0.1529(2) 0.02451(17) Uiso 0.0902(7) 1 d D . P B
2
C60C C 0.2633(11) 0.1923(4) 0.1480(8) 0.0211(5) Uiso 0.262(3) 1 d D U P C 3
H60C H 0.222689 0.193374 0.094875 0.025 Uiso 0.262(3) 1 calc R U P C 3
Cl1C Cl 0.1695(3) 0.23864(11) 0.20545(16) 0.02792(19) Uiso 0.262(3) 1 d D U P C
3
Cl2C Cl 0.4268(3) 0.22326(12) 0.1494(2) 0.02435(18) Uiso 0.262(3) 1 d D U P C 3
Cl3C Cl 0.2426(3) 0.12172(13) 0.18454(16) 0.02451(17) Uiso 0.262(3) 1 d D U P C
3
C60D C 0.2632(14) 0.2030(6) 0.1445(10) 0.0211(5) Uiso 0.151(3) 1 d D U P D 4
H60D H 0.229982 0.209096 0.090469 0.025 Uiso 0.151(3) 1 calc R U P D 4
Cl1D Cl 0.1847(5) 0.2519(2) 0.1975(3) 0.02792(19) Uiso 0.151(3) 1 d D U P D 4
Cl3D Cl 0.2265(5) 0.12878(16) 0.1690(3) 0.02451(17) Uiso 0.151(3) 1 d D U P D 4
Cl2D Cl 0.4297(5) 0.2138(3) 0.1505(4) 0.02435(18) Uiso 0.151(3) 1 d D U P D 4
C70A C 0.1365(6) 0.2667(2) 0.4367(3) 0.0206(5) Uiso 0.431(2) 1 d D U P E 5
H70A H 0.220744 0.262658 0.412230 0.025 Uiso 0.431(2) 1 calc R U P E 5
Cl4A Cl 0.00182(15) 0.25997(9) 0.36419(10) 0.01910(16) Uiso 0.431(2) 1 d D U P
E 5
Cl5A Cl 0.1275(2) 0.20933(10) 0.50429(12) 0.02773(15) Uiso 0.431(2) 1 d D U P E
5
Cl6A Cl 0.13547(14) 0.33728(9) 0.48354(15) 0.02965(17) Uiso 0.431(2) 1 d D U P
E 5
C70B C 0.1347(7) 0.2784(3) 0.4285(4) 0.0206(5) Uiso 0.313(2) 1 d D U P F 6
H70B H 0.218386 0.272543 0.403877 0.025 Uiso 0.313(2) 1 calc R U P F 6
Cl4B Cl 0.00450(19) 0.27305(9) 0.35904(12) 0.01910(16) Uiso 0.313(2) 1 d D U P
F 6
Cl5B Cl 0.12840(19) 0.22534(16) 0.50247(11) 0.02773(15) Uiso 0.313(2) 1 d D U P
F 6
Cl6B Cl 0.13194(16) 0.35085(14) 0.46356(16) 0.02965(17) Uiso 0.313(2) 1 d D U P
F 6
C70C C 0.1494(10) 0.2633(4) 0.4534(5) 0.0206(5) Uiso 0.186(2) 1 d D U P G 7
H70C H 0.233655 0.260419 0.428729 0.025 Uiso 0.186(2) 1 calc R U P G 7
Cl4C Cl 0.0205(3) 0.26945(18) 0.3800(2) 0.01910(16) Uiso 0.186(2) 1 d D U P G 7
Cl5C Cl 0.1349(4) 0.19903(15) 0.5076(2) 0.02773(15) Uiso 0.186(2) 1 d D U P G 7
Cl6C Cl 0.1548(3) 0.32811(13) 0.5068(2) 0.02965(17) Uiso 0.186(2) 1 d D U P G 7
C70D C 0.138(2) 0.2951(6) 0.4282(9) 0.0206(5) Uiso 0.0701(14) 1 d D U P H 8
H61D H 0.221470 0.285586 0.405346 0.025 Uiso 0.0701(14) 1 calc R U P H 8
Cl4D Cl 0.0082(9) 0.2546(4) 0.3788(5) 0.01910(16) Uiso 0.0701(14) 1 d D U P H 8
Cl5D Cl 0.1245(6) 0.2494(4) 0.5079(4) 0.02773(15) Uiso 0.0701(14) 1 d D U P H 8
Cl6D Cl 0.1332(6) 0.3711(4) 0.4468(4) 0.02965(17) Uiso 0.0701(14) 1 d D U P H 8


_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
O10 C16 1.2048(19) . ?
C10 C11 1.3983(18) . ?
C10 C15 1.3996(18) . ?
C10 C21 1.4917(18) . ?
O11 C16 1.3259(19) . ?
O11 C17 1.4475(19) . ?
C11 C12 1.3948(19) . ?
C11 H11 0.9500 . ?
O12 C18 1.2076(18) . ?
C12 C13 1.387(2) . ?
C12 C16 1.491(2) . ?
O13 C18 1.3367(17) . ?
O13 C19 1.4470(17) . ?
C13 C14 1.3911(19) . ?
C13 H13 0.9500 . ?
C14 C15 1.3961(19) . ?
C14 C18 1.490(2) . ?
C15 H15 0.9500 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 C25 1.4157(18) . ?
C20 C21 1.4175(18) . ?
C20 P40 1.8258(14) . ?
C21 C22 1.3999(19) . ?
C22 C23 1.389(2) . ?
C22 H22 0.9500 . ?
C23 C24 1.389(2) . ?
C23 H23 0.9500 . ?
C24 C25 1.3952(19) . ?
C24 H24 0.9500 . ?
C25 C30 1.4892(18) . ?
O30 C36 1.2066(19) . ?
C30 C35 1.3954(19) . ?
C30 C31 1.3980(18) . ?
O31 C36 1.3335(19) . ?
O31 C37 1.4458(18) . ?
C31 C32 1.3996(19) . ?
C31 H31 0.9500 . ?
O32 C38 1.2057(18) . ?
C32 C33 1.388(2) . ?
C32 C36 1.493(2) . ?
O33 C38 1.3369(18) . ?
O33 C39 1.4452(18) . ?
C33 C34 1.3926(19) . ?
C33 H33 0.9500 . ?
C34 C35 1.3900(19) . ?
C34 C38 1.489(2) . ?
C35 H35 0.9500 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
P40 O40 1.4888(10) . ?
P40 C40 1.8062(14) . ?
P40 C46 1.8101(14) . ?
C40 C45 1.394(2) . ?
C40 C41 1.396(2) . ?
C41 C42 1.390(2) . ?
C41 H41 0.9500 . ?
C42 C43 1.387(3) . ?
C42 H42 0.9500 . ?
C43 C44 1.387(2) . ?
C43 H43 0.9500 . ?
C44 C45 1.390(2) . ?
C44 H44 0.9500 . ?
C45 H45 0.9500 . ?
C46 C47 1.394(2) . ?
C46 C51 1.398(2) . ?
C47 C48 1.388(2) . ?
C47 H47 0.9500 . ?
C48 C49 1.384(3) . ?
C48 H48 0.9500 . ?
C49 C50 1.389(3) . ?
C49 H49 0.9500 . ?
C50 C51 1.389(2) . ?
C50 H50 0.9500 . ?
C51 H51 0.9500 . ?
C60A Cl2A 1.762(7) . ?
C60A Cl1A 1.769(7) . ?
C60A Cl3A 1.780(6) . ?
C60A H60A 1.0000 . ?
C60B Cl1B 1.737(13) . ?
C60B Cl3B 1.766(13) . ?
C60B Cl2B 1.784(13) . ?
C60B H60B 1.0000 . ?
C60C Cl3C 1.733(10) . ?
C60C Cl1C 1.788(10) . ?
C60C Cl2C 1.812(11) . ?
C60C H60C 1.0000 . ?
C60D Cl1D 1.690(13) . ?
C60D Cl2D 1.718(14) . ?
C60D Cl3D 1.770(14) . ?
C60D H60D 1.0000 . ?
C70A Cl5A 1.768(4) . ?
C70A Cl6A 1.790(5) . ?
C70A Cl4A 1.817(5) . ?
C70A H70A 1.0000 . ?
C70B Cl6B 1.745(6) . ?
C70B Cl4B 1.748(7) . ?
C70B Cl5B 1.777(6) . ?
C70B H70B 1.0000 . ?
C70C Cl6C 1.735(9) . ?
C70C Cl5C 1.747(9) . ?
C70C Cl4C 1.786(9) . ?
C70C H70C 1.0000 . ?
C70D Cl6D 1.741(14) . ?
C70D Cl5D 1.760(14) . ?
C70D Cl4D 1.781(14) . ?
C70D H61D 1.0000 . ?

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
C11 C10 C15 118.95(12) . . ?
C11 C10 C21 119.76(12) . . ?
C15 C10 C21 121.06(12) . . ?
C16 O11 C17 115.08(13) . . ?
C12 C11 C10 120.29(13) . . ?
C12 C11 H11 119.9 . . ?
C10 C11 H11 119.9 . . ?
C13 C12 C11 120.36(13) . . ?
C13 C12 C16 117.46(13) . . ?
C11 C12 C16 122.15(13) . . ?
C18 O13 C19 114.93(11) . . ?
C12 C13 C14 119.94(13) . . ?
C12 C13 H13 120.0 . . ?
C14 C13 H13 120.0 . . ?
C13 C14 C15 119.89(13) . . ?
C13 C14 C18 117.37(12) . . ?
C15 C14 C18 122.72(12) . . ?
C14 C15 C10 120.58(12) . . ?
C14 C15 H15 119.7 . . ?
C10 C15 H15 119.7 . . ?
O10 C16 O11 123.73(14) . . ?
O10 C16 C12 123.65(14) . . ?
O11 C16 C12 112.62(13) . . ?
O11 C17 H17A 109.5 . . ?
O11 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
O11 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
O12 C18 O13 123.56(13) . . ?
O12 C18 C14 123.94(13) . . ?
O13 C18 C14 112.49(12) . . ?
O13 C19 H19A 109.5 . . ?
O13 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
O13 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C25 C20 C21 118.60(12) . . ?
C25 C20 P40 119.42(10) . . ?
C21 C20 P40 121.92(10) . . ?
C22 C21 C20 119.30(12) . . ?
C22 C21 C10 117.05(12) . . ?
C20 C21 C10 123.32(12) . . ?
C23 C22 C21 121.05(13) . . ?
C23 C22 H22 119.5 . . ?
C21 C22 H22 119.5 . . ?
C22 C23 C24 119.72(13) . . ?
C22 C23 H23 120.1 . . ?
C24 C23 H23 120.1 . . ?
C23 C24 C25 120.50(13) . . ?
C23 C24 H24 119.8 . . ?
C25 C24 H24 119.8 . . ?
C24 C25 C20 120.12(12) . . ?
C24 C25 C30 117.33(12) . . ?
C20 C25 C30 122.54(12) . . ?
C35 C30 C31 119.30(12) . . ?
C35 C30 C25 118.91(12) . . ?
C31 C30 C25 121.78(12) . . ?
C36 O31 C37 114.94(12) . . ?
C30 C31 C32 119.67(13) . . ?
C30 C31 H31 120.2 . . ?
C32 C31 H31 120.2 . . ?
C33 C32 C31 120.52(13) . . ?
C33 C32 C36 117.31(13) . . ?
C31 C32 C36 122.10(13) . . ?
C38 O33 C39 116.13(12) . . ?
C32 C33 C34 119.81(13) . . ?
C32 C33 H33 120.1 . . ?
C34 C33 H33 120.1 . . ?
C35 C34 C33 119.82(13) . . ?
C35 C34 C38 121.20(12) . . ?
C33 C34 C38 118.80(12) . . ?
C34 C35 C30 120.76(13) . . ?
C34 C35 H35 119.6 . . ?
C30 C35 H35 119.6 . . ?
O30 C36 O31 123.69(14) . . ?
O30 C36 C32 123.50(14) . . ?
O31 C36 C32 112.81(12) . . ?
O31 C37 H37A 109.5 . . ?
O31 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
O31 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
O32 C38 O33 123.97(14) . . ?
O32 C38 C34 124.04(14) . . ?
O33 C38 C34 111.97(12) . . ?
O33 C39 H39A 109.5 . . ?
O33 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
O33 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
O40 P40 C40 111.72(6) . . ?
O40 P40 C46 111.77(6) . . ?
C40 P40 C46 103.29(6) . . ?
O40 P40 C20 114.09(6) . . ?
C40 P40 C20 108.08(6) . . ?
C46 P40 C20 107.22(6) . . ?
C45 C40 C41 119.53(13) . . ?
C45 C40 P40 123.21(11) . . ?
C41 C40 P40 117.25(11) . . ?
C42 C41 C40 120.15(15) . . ?
C42 C41 H41 119.9 . . ?
C40 C41 H41 119.9 . . ?
C43 C42 C41 120.06(15) . . ?
C43 C42 H42 120.0 . . ?
C41 C42 H42 120.0 . . ?
C42 C43 C44 120.02(15) . . ?
C42 C43 H43 120.0 . . ?
C44 C43 H43 120.0 . . ?
C43 C44 C45 120.25(15) . . ?
C43 C44 H44 119.9 . . ?
C45 C44 H44 119.9 . . ?
C44 C45 C40 119.98(14) . . ?
C44 C45 H45 120.0 . . ?
C40 C45 H45 120.0 . . ?
C47 C46 C51 119.37(13) . . ?
C47 C46 P40 116.74(11) . . ?
C51 C46 P40 123.82(11) . . ?
C48 C47 C46 120.17(15) . . ?
C48 C47 H47 119.9 . . ?
C46 C47 H47 119.9 . . ?
C49 C48 C47 120.28(15) . . ?
C49 C48 H48 119.9 . . ?
C47 C48 H48 119.9 . . ?
C48 C49 C50 119.95(15) . . ?
C48 C49 H49 120.0 . . ?
C50 C49 H49 120.0 . . ?
C51 C50 C49 120.16(15) . . ?
C51 C50 H50 119.9 . . ?
C49 C50 H50 119.9 . . ?
C50 C51 C46 120.03(14) . . ?
C50 C51 H51 120.0 . . ?
C46 C51 H51 120.0 . . ?
Cl2A C60A Cl1A 112.0(4) . . ?
Cl2A C60A Cl3A 104.0(4) . . ?
Cl1A C60A Cl3A 113.8(4) . . ?
Cl2A C60A H60A 108.9 . . ?
Cl1A C60A H60A 108.9 . . ?
Cl3A C60A H60A 108.9 . . ?
Cl1B C60B Cl3B 112.4(8) . . ?
Cl1B C60B Cl2B 106.9(7) . . ?
Cl3B C60B Cl2B 109.3(8) . . ?
Cl1B C60B H60B 109.4 . . ?
Cl3B C60B H60B 109.4 . . ?
Cl2B C60B H60B 109.4 . . ?
Cl3C C60C Cl1C 103.5(6) . . ?
Cl3C C60C Cl2C 119.1(7) . . ?
Cl1C C60C Cl2C 107.8(6) . . ?
Cl3C C60C H60C 108.6 . . ?
Cl1C C60C H60C 108.6 . . ?
Cl2C C60C H60C 108.6 . . ?
Cl1D C60D Cl2D 112.7(9) . . ?
Cl1D C60D Cl3D 110.9(8) . . ?
Cl2D C60D Cl3D 110.3(8) . . ?
Cl1D C60D H60D 107.6 . . ?
Cl2D C60D H60D 107.6 . . ?
Cl3D C60D H60D 107.6 . . ?
Cl5A C70A Cl6A 109.3(3) . . ?
Cl5A C70A Cl4A 110.0(3) . . ?
Cl6A C70A Cl4A 111.8(3) . . ?
Cl5A C70A H70A 108.6 . . ?
Cl6A C70A H70A 108.6 . . ?
Cl4A C70A H70A 108.6 . . ?
Cl6B C70B Cl4B 106.4(3) . . ?
Cl6B C70B Cl5B 111.2(4) . . ?
Cl4B C70B Cl5B 113.8(4) . . ?
Cl6B C70B H70B 108.4 . . ?
Cl4B C70B H70B 108.4 . . ?
Cl5B C70B H70B 108.4 . . ?
Cl6C C70C Cl5C 113.3(5) . . ?
Cl6C C70C Cl4C 108.8(5) . . ?
Cl5C C70C Cl4C 112.1(5) . . ?
Cl6C C70C H70C 107.5 . . ?
Cl5C C70C H70C 107.5 . . ?
Cl4C C70C H70C 107.5 . . ?
Cl6D C70D Cl5D 114.5(10) . . ?
Cl6D C70D Cl4D 124.4(12) . . ?
Cl5D C70D Cl4D 89.8(8) . . ?
Cl6D C70D H61D 108.8 . . ?
Cl5D C70D H61D 108.8 . . ?
Cl4D C70D H61D 108.8 . . ?

_refine_diff_density_max         1.047
_refine_diff_density_min         -0.880
_refine_diff_density_rms         0.070

####################################################################### 
# 
# 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_uhm-62
_database_code_depnum_ccdc_archive 'CCDC 1942989'
loop_
_audit_author_name
_audit_author_address
'Timo Stein'
;University of Hamburg
Germany
;
_audit_update_record             
;
2019-09-04 deposited with the CCDC.	2019-09-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'(C156 H114 Cu12 O54 P6), 10(O), O, (Cl -), (C2 H8 N +), 24(C3 H7 N O)'
_chemical_formula_sum            'C230 H290 Cl Cu12 N25 O89 P6'
_chemical_formula_weight         5812.60

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 '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 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           71
_space_group_name_H-M_alt        'I m m m'
_space_group_name_Hall           '-I 2 2'

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

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

_cell_length_a                   18.3318(4)
_cell_length_b                   25.8343(5)
_cell_length_c                   33.4448(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     15839.1(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    20450
_cell_measurement_theta_min      3.9440
_cell_measurement_theta_max      75.2010
_cell_oxdiff_length_a            18.3350(4)
_cell_oxdiff_length_b            25.8325(6)
_cell_oxdiff_length_c            33.4452(6)
_cell_oxdiff_angle_alpha         90.0234(17)
_cell_oxdiff_angle_beta          89.9865(18)
_cell_oxdiff_angle_gamma         90.0076(19)
_cell_oxdiff_volume              15841.0(6)
_cell_oxdiff_measurement_reflns_used 20453

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.219
_exptl_crystal_F_000             6024
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    1.861
_shelx_estimated_absorpt_T_min   0.808
_shelx_estimated_absorpt_T_max   0.897
_exptl_absorpt_correction_T_min  0.90019
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.682
_oxdiff_exptl_absorpt_empirical_full_max 1.730
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Atlas
_diffrn_detector_area_resol_mean 10.4127
_diffrn_reflns_number            82481
_diffrn_reflns_av_unetI/netI     0.0258
_diffrn_reflns_av_R_equivalents  0.0524
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_theta_min         3.421
_diffrn_reflns_theta_max         67.492
_diffrn_reflns_theta_full        67.492
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0387168000
_diffrn_orient_matrix_UB_12      0.0097672000
_diffrn_orient_matrix_UB_13      -0.0514009000
_diffrn_orient_matrix_UB_21      -0.0650969000
_diffrn_orient_matrix_UB_22      0.0262554000
_diffrn_orient_matrix_UB_23      -0.0163409000
_diffrn_orient_matrix_UB_31      0.0363942000
_diffrn_orient_matrix_UB_32      0.0365650000
_diffrn_orient_matrix_UB_33      0.0254317000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -58.00 -10.00   1.00   30.00    --  -42.10 -77.00  30.00   48
  2  ω   -115.00 -88.00   1.00   30.00    --  -42.10 -38.00 -30.00   27
  3  ω    -87.00 -18.00   1.00   30.00    --  -42.10 -38.00 -30.00   69
  4  ω   -118.00 -10.00   1.00   30.00    --  -42.10 -77.00-150.00  108
  5  ω   -115.00 -10.00   1.00   30.00    --  -42.10 -77.00 -60.00  105
  6  ω    -67.00 -10.00   1.00   30.00    --  -42.10 -77.00 120.00   57
  7  ω   -100.00  -4.00   1.00   30.00    --  -42.10 -19.00  30.00   96
  8  ω    -70.00  29.00   1.00   30.00    --  -42.10  57.00 -30.00   99
  9  ω    -39.00  29.00   1.00   30.00    --  -42.10  38.00  90.00   68
 10  ω    -30.00  70.00   1.00   30.00    --   42.10 -57.00 150.00  100
 11  ω     30.00  97.00   1.00   30.00    --   42.10-125.00  90.00   67
 12  ω     79.00 176.00   1.00  120.00    --  112.00  77.00-150.00   97
 13  ω     79.00 115.00   1.00  120.00    --  112.00  77.00 120.00   36
 14  ω    116.00 172.00   1.00  120.00    --  112.00  77.00 120.00   56
 15  ω     79.00 155.00   1.00  120.00    --  112.00  77.00 -30.00   76
 16  ω     83.00 108.00   1.00  120.00    --  112.00 -94.00 150.00   25
 17  ω     36.00 116.00   1.00  120.00    --  112.00-111.00-120.00   80
 18  ω     82.00 177.00   1.00  120.00    --  112.00  67.00 154.57   95
 19  ω     79.00 105.00   1.00  120.00    --  112.00  77.00  30.00   26
 20  ω     83.00 177.00   1.00  120.00    --  112.00  61.00  90.00   94
 21  ω     83.00 110.00   1.00  120.00    --  112.00  61.00 -30.00   27
 22  ω     29.00  67.00   1.00  120.00    --  112.00 -94.00 150.00   38
 23  ω    112.00 177.00   1.00  120.00    --  112.00  77.00-120.00   65
 24  ω     79.00 149.00   1.00  120.00    --  112.00  77.00 -90.00   70
 25  ω     83.00 109.00   1.00  120.00    --  112.00  61.00 120.00   26
 26  ω     45.00 145.00   1.00  120.00    --  112.00 -77.00-120.00  100
 27  ω     83.00 109.00   1.00  120.00    --  112.00  61.00 -60.00   26
 28  ω     83.00 109.00   1.00  120.00    --  112.00  61.00  30.00   26
 29  ω     83.00 109.00   1.00  120.00    --  112.00  61.00   0.00   26
 30  ω     83.00 140.00   1.00  120.00    --  112.00  61.00  60.00   57
 31  ω     79.00 105.00   1.00  120.00    --  112.00  77.00-180.00   26
 32  ω     79.00  86.00   1.00  120.00    --  112.00 -94.00 -30.00    7
;
_diffrn_measurement_method       'ω scans'
_reflns_number_total             7651
_reflns_number_gt                6192
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1298P)²+9.0209P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7651
_refine_ls_number_parameters     434
_refine_ls_number_restraints     494
_refine_ls_R_factor_all          0.0702
_refine_ls_R_factor_gt           0.0606
_refine_ls_wR_factor_ref         0.1940
_refine_ls_wR_factor_gt          0.1849
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_restrained_S_all      1.063
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C10A C 0.500000 0.1000(2) 0.29921(17) 0.0661(13) Uani 1 2 d S T P . .
C11A C 0.4347(2) 0.12483(15) 0.29058(12) 0.0674(9) Uani 1 1 d . . . . .
H11A H 0.389825 0.108409 0.296894 0.081 Uiso 1 1 calc R U . . .
C12A C 0.4344(2) 0.17338(14) 0.27285(11) 0.0606(9) Uani 1 1 d . . . . .
C13A C 0.500000 0.1974(2) 0.26316(17) 0.0644(13) Uani 1 2 d S T P . .
H13A H 0.500001 0.229937 0.249987 0.077 Uiso 1 2 calc R U P . .
C14A C 0.3649(2) 0.20035(15) 0.26459(11) 0.0614(9) Uani 1 1 d . . . . .
C20A C 0.500000 0.000000 0.2962(2) 0.0650(18) Uani 1 4 d DS T P . .
C21A C 0.500000 0.0465(2) 0.31758(17) 0.0682(13) Uani 1 2 d DS T P . .
C22A C 0.500000 0.0453(2) 0.3577(2) 0.124(3) Uani 1 2 d DS T P . .
H22A H 0.500000 0.077111 0.372038 0.149 Uiso 1 2 calc R U P . .
C23A C 0.500000 0.000000 0.3786(3) 0.178(9) Uani 1 4 d DS T P . .
H23A H 0.500000 0.000000 0.407034 0.213 Uiso 1 4 calc R U P . .
C40A C 0.5757(9) -0.0411(8) 0.2243(6) 0.324(16) Uani 0.5 1 d D U P . .
H40A H 0.600614 -0.058551 0.246852 0.389 Uiso 0.5 1 calc R U P . .
H40B H 0.559699 -0.067212 0.204471 0.389 Uiso 0.5 1 calc R U P . .
C41A C 0.6222(12) 0.000000 0.2058(10) 0.49(2) Uani 1 2 d DS TU P . .
H41A H 0.666597 -0.015710 0.194839 0.733 Uiso 0.5 1 calc R U P . .
H41B H 0.595057 0.017045 0.184265 0.733 Uiso 0.5 1 calc R U P . .
H41C H 0.635496 0.025604 0.226153 0.733 Uiso 0.5 1 calc R U P . .
P40B P 0.2662(3) 0.11904(17) 0.000000 0.0933(11) Uani 0.5 2 d DS T P A 1
O13B O 0.0593(4) 0.0618(2) 0.07912(17) 0.0545(15) Uani 0.5 1 d . . P A 1
O40B O 0.2098(8) 0.0725(5) 0.000000 0.147(5) Uani 0.5 2 d DS T P A 1
C10B C 0.2025(6) 0.1849(3) 0.0751(2) 0.064(2) Uani 0.5 1 d . . P A 1
C11B C 0.2289(7) 0.2048(5) 0.1109(4) 0.063(3) Uani 0.5 1 d . . P A 1
H11B H 0.260410 0.233990 0.111429 0.076 Uiso 0.5 1 calc R U P A 1
C12B C 0.207(2) 0.1797(18) 0.1464(10) 0.062(6) Uani 0.5 1 d . . P A 1
C13B C 0.1588(7) 0.1382(7) 0.1449(5) 0.045(2) Uani 0.5 1 d . . P A 1
H13B H 0.140614 0.123837 0.169076 0.053 Uiso 0.5 1 calc R U P A 1
C14B C 0.1383(7) 0.1190(4) 0.1110(4) 0.049(3) Uani 0.5 1 d . . P A 1
C15B C 0.1535(5) 0.1439(3) 0.0760(2) 0.0604(19) Uani 0.5 1 d . . P A 1
H15B H 0.130411 0.133083 0.051969 0.072 Uiso 0.5 1 calc R U P A 1
C17B C 0.0865(7) 0.0755(4) 0.1130(3) 0.041(2) Uani 0.5 1 d . . P A 1
C20B C 0.2231(6) 0.1858(5) 0.000000 0.075(3) Uani 0.5 2 d DS T P A 1
C21B C 0.2177(4) 0.2122(3) 0.0359(2) 0.070(2) Uani 0.5 1 d D . P A 1
C22B C 0.2063(5) 0.2670(3) 0.03576(19) 0.096(3) Uani 0.5 1 d D . P A 1
H22B H 0.202496 0.285366 0.060292 0.115 Uiso 0.5 1 calc R U P A 1
C23B C 0.2009(7) 0.2931(4) 0.000000 0.133(8) Uani 0.5 2 d DS T P A 1
H23B H 0.193461 0.329507 0.000000 0.159 Uiso 0.5 2 calc R U P A 1
C40B C 0.3230(9) 0.1164(6) 0.0417(3) 0.137(5) Uani 0.5 1 d D . P A 1
H40C H 0.291643 0.117171 0.065739 0.164 Uiso 0.5 1 calc R U P A 1
H40D H 0.347971 0.082463 0.041361 0.164 Uiso 0.5 1 calc R U P A 1
C41B C 0.3812(19) 0.1580(15) 0.0467(10) 0.39(3) Uani 0.5 1 d D U P A 1
H41D H 0.408753 0.151533 0.071363 0.582 Uiso 0.5 1 calc R U P A 1
H41E H 0.414524 0.157217 0.023820 0.582 Uiso 0.5 1 calc R U P A 1
H41F H 0.357907 0.192103 0.048323 0.582 Uiso 0.5 1 calc R U P A 1
P40C P 0.1437(2) 0.19150(15) 0.000000 0.0914(11) Uani 0.5 2 d DS T P A 2
O13C O 0.0898(4) 0.0424(3) 0.07937(19) 0.0554(15) Uani 0.5 1 d . . P A 2
O40C O 0.0819(7) 0.1396(5) 0.000000 0.127(4) Uani 0.5 2 d DS T P A 2
C10C C 0.2449(6) 0.1598(5) 0.0751(2) 0.080(3) Uani 0.5 1 d . . P A 2
C11C C 0.2577(7) 0.1875(5) 0.1099(4) 0.071(3) Uani 0.5 1 d . . P A 2
H11C H 0.290677 0.215785 0.108822 0.085 Uiso 0.5 1 calc R U P A 2
C12C C 0.225(2) 0.1761(18) 0.1461(10) 0.062(6) Uani 0.5 1 d . . P A 2
C13C C 0.1799(7) 0.1333(7) 0.1487(5) 0.045(2) Uani 0.5 1 d . . P A 2
H13C H 0.161178 0.122679 0.173922 0.053 Uiso 0.5 1 calc R U P A 2
C14C C 0.1613(7) 0.1046(5) 0.1124(4) 0.058(3) Uani 0.5 1 d . . P A 2
C15C C 0.1953(5) 0.1191(4) 0.0767(2) 0.072(2) Uani 0.5 1 d . . P A 2
H15C H 0.184168 0.100716 0.052851 0.087 Uiso 0.5 1 calc R U P A 2
C17C C 0.1051(8) 0.0617(4) 0.1117(4) 0.049(2) Uani 0.5 1 d . . P A 2
C20C C 0.2422(7) 0.1719(4) 0.000000 0.075(3) Uani 0.5 2 d DS T P A 2
C21C C 0.2788(5) 0.1729(3) 0.0361(2) 0.096(3) Uani 0.5 1 d D . P A 2
C22C C 0.3558(6) 0.1750(6) 0.0359(2) 0.159(9) Uani 0.5 1 d D . P A 2
H22C H 0.381761 0.175678 0.060485 0.191 Uiso 0.5 1 calc R U P A 2
C23C C 0.3935(8) 0.1761(9) 0.000000 0.175(13) Uani 0.5 2 d DS T P A 2
H23C H 0.445326 0.177626 0.000000 0.210 Uiso 0.5 2 calc R U P A 2
C40C C 0.1288(10) 0.2246(6) 0.0426(3) 0.146(6) Uani 0.5 1 d D . P A 2
H40E H 0.160282 0.209222 0.063495 0.175 Uiso 0.5 1 calc R U P A 2
H40F H 0.146090 0.260447 0.038257 0.175 Uiso 0.5 1 calc R U P A 2
C41C C 0.0458(14) 0.228(2) 0.0609(14) 0.74(5) Uani 0.5 1 d D U P A 2
H41G H 0.046426 0.248602 0.085585 1.115 Uiso 0.5 1 calc R U P A 2
H41H H 0.013581 0.244733 0.041352 1.115 Uiso 0.5 1 calc R U P A 2
H41I H 0.027856 0.193210 0.066738 1.115 Uiso 0.5 1 calc R U P A 2
C16B C 0.2342(2) 0.20429(14) 0.18476(11) 0.0599(9) Uani 1 1 d . . . . .
O10A O 0.30717(15) 0.18066(11) 0.27739(9) 0.0718(7) Uani 1 1 d . . . . .
O11A O 0.36913(14) 0.24192(10) 0.24475(9) 0.0706(7) Uani 1 1 d . . . . .
O10B O 0.27082(16) 0.24494(10) 0.18273(7) 0.0714(8) Uani 1 1 d . . . . .
O11B O 0.20871(16) 0.18404(10) 0.21565(7) 0.0690(7) Uani 1 1 d . . . . .
O12B O 0.07484(15) 0.05341(9) 0.14524(6) 0.0573(6) Uani 1 1 d . . . . .
O100 O 0.14905(19) 0.15364(12) 0.30106(9) 0.0882(9) Uani 1 1 d . . . . .
O200 O 0.000000 0.000000 0.22165(14) 0.0687(14) Uani 1 4 d S T P . .
Cl1 Cl 0.000000 0.000000 0.000000 0.0485(5) Uani 1 8 d S T P A .
P40A P 0.500000 0.000000 0.24124(9) 0.1130(12) Uani 1 4 d DS T P . .
O40A O 0.500000 0.0521(4) 0.2226(3) 0.129(5) Uani 0.5 2 d DS T P . .
Cu1 Cu 0.21264(3) 0.21353(2) 0.26913(2) 0.04868(18) Uani 1 1 d . . . . .
Cu2 Cu 0.000000 0.000000 0.15194(2) 0.0442(2) Uani 1 4 d S T P A .
Cu3 Cu 0.000000 0.000000 0.07207(2) 0.0386(2) Uani 1 4 d S T P . .
O50 O 0.000000 0.1480(7) 0.000000 0.118(5) Uani 0.5 4 d S T P B 3
C60 C 0.237(2) 0.000000 0.0364(5) 0.34(3) Uani 0.5 2 d DS TU P C 3
H60A H 0.208037 0.000000 0.061141 0.510 Uiso 0.5 2 calc R U P C 3
H60B H 0.267402 -0.030973 0.035481 0.510 Uiso 0.25 1 calc R U P C 3
H60C H 0.267402 0.030973 0.035481 0.510 Uiso 0.25 1 calc R U P C 3
N60 N 0.1843(19) 0.000000 0.000000 0.180(12) Uani 0.5 4 d DS TU P C 3
H60D H 0.155448 0.028683 0.000000 0.216 Uiso 0.25 2 calc R U P C 3
H60E H 0.155447 -0.028683 0.000000 0.216 Uiso 0.25 2 calc R U P C 3


_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
C10A C11A 1.388(5) 12_655 ?
C10A C11A 1.388(5) . ?
C10A C21A 1.513(7) . ?
C11A C12A 1.387(5) . ?
C11A H11A 0.9500 . ?
C12A C13A 1.391(5) . ?
C12A C14A 1.478(5) . ?
C13A H13A 0.9500 . ?
C14A O10A 1.249(5) . ?
C14A O11A 1.265(5) . ?
C20A C21A 1.396(6) . ?
C20A C21A 1.396(6) 2_655 ?
C20A P40A 1.839(8) . ?
C21A C22A 1.344(8) . ?
C22A C23A 1.364(8) . ?
C22A H22A 0.9500 . ?
C23A H23A 0.9500 . ?
C40A C41A 1.496(16) . ?
C40A P40A 1.838(14) . ?
C40A H40A 0.9900 . ?
C40A H40B 0.9900 . ?
C40A H41C 1.17(3) 11 ?
C41A H41A 0.9800 . ?
C41A H41B 0.9800 . ?
C41A H41C 0.9800 . ?
C41A H41B 0.9800 11 ?
C41A H41A 0.9800 11 ?
C41A H41C 0.9800 11 ?
P40B O40B 1.587(12) . ?
P40B C40B 1.741(11) . ?
P40B C40B 1.741(11) 10 ?
P40B C20B 1.896(12) . ?
O13B C17B 1.287(13) . ?
O13B Cu3 1.946(6) . ?
C10B C15B 1.388(11) . ?
C10B C11B 1.391(13) . ?
C10B C21B 1.513(10) . ?
C11B C12B 1.41(4) . ?
C11B H11B 0.9500 . ?
C12B C13B 1.39(3) . ?
C12B C16B 1.52(3) . ?
C13B C14B 1.293(19) . ?
C13B H13B 0.9500 . ?
C14B C15B 1.366(14) . ?
C14B C17B 1.473(17) . ?
C15B H15B 0.9500 . ?
C17B O12B 1.240(12) . ?
C20B C21B 1.385(9) . ?
C20B C21B 1.385(9) 10 ?
C21B C22B 1.432(10) . ?
C22B C23B 1.376(9) . ?
C22B H22B 0.9500 . ?
C23B H23B 0.9500 . ?
C40B C41B 1.524(17) . ?
C40B H40C 0.9900 . ?
C40B H40D 0.9900 . ?
C41B H41D 0.9800 . ?
C41B H41E 0.9800 . ?
C41B H41F 0.9800 . ?
P40C C40C 1.683(9) . ?
P40C C40C 1.683(9) 10 ?
P40C O40C 1.756(10) . ?
P40C C20C 1.876(12) . ?
O13C C17C 1.224(14) . ?
O13C Cu3 1.991(7) . ?
C10C C11C 1.388(15) . ?
C10C C15C 1.390(13) . ?
C10C C21C 1.484(11) . ?
C11C C12C 1.38(3) . ?
C11C H11C 0.9500 . ?
C12C C13C 1.38(3) . ?
C12C C16B 1.49(3) . ?
C13C C14C 1.47(2) . ?
C13C H13C 0.9500 . ?
C14C C15C 1.399(17) . ?
C14C C17C 1.51(2) . ?
C15C H15C 0.9500 . ?
C17C O12B 1.271(14) . ?
C20C C21C 1.380(9) . ?
C20C C21C 1.380(9) 10 ?
C21C C22C 1.413(13) . ?
C22C C23C 1.387(11) . ?
C22C H22C 0.9500 . ?
C23C H23C 0.9500 . ?
C40C C41C 1.643(17) . ?
C40C H40E 0.9900 . ?
C40C H40F 0.9900 . ?
C41C H41G 0.9800 . ?
C41C H41H 0.9800 . ?
C41C H41I 0.9800 . ?
C16B O10B 1.248(4) . ?
C16B O11B 1.249(5) . ?
O10A Cu1 1.949(3) . ?
O11A Cu1 1.946(3) 13 ?
O10B Cu1 1.959(2) 13 ?
O11B Cu1 1.945(2) . ?
O12B Cu2 1.959(2) . ?
O100 Cu1 2.212(3) . ?
O200 Cu2 2.332(5) . ?
Cl1 Cu3 2.4105(7) . ?
Cl1 Cu3 2.4105(7) 9 ?
P40A O40A 1.483(9) 2_655 ?
P40A O40A 1.483(9) . ?
Cu1 Cu1 2.6579(9) 13 ?
Cu2 Cu3 2.6710(10) . ?
C60 N60 1.549(18) . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?
N60 H60D 0.9100 . ?
N60 H60E 0.9100 . ?

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
C11A C10A C11A 119.1(5) 12_655 . ?
C11A C10A C21A 120.5(3) 12_655 . ?
C11A C10A C21A 120.5(3) . . ?
C12A C11A C10A 120.7(4) . . ?
C12A C11A H11A 119.6 . . ?
C10A C11A H11A 119.6 . . ?
C11A C12A C13A 119.9(4) . . ?
C11A C12A C14A 120.7(4) . . ?
C13A C12A C14A 119.5(4) . . ?
C12A C13A C12A 119.7(5) . 12_655 ?
C12A C13A H13A 120.2 . . ?
C12A C13A H13A 120.2 12_655 . ?
O10A C14A O11A 125.3(4) . . ?
O10A C14A C12A 118.3(3) . . ?
O11A C14A C12A 116.4(4) . . ?
C21A C20A C21A 118.5(7) . 2_655 ?
C21A C20A P40A 120.8(3) . . ?
C21A C20A P40A 120.8(3) 2_655 . ?
C22A C21A C20A 119.5(5) . . ?
C22A C21A C10A 115.2(5) . . ?
C20A C21A C10A 125.3(5) . . ?
C21A C22A C23A 122.0(6) . . ?
C21A C22A H22A 119.0 . . ?
C23A C22A H22A 119.0 . . ?
C22A C23A C22A 118.4(9) 11 . ?
C22A C23A H23A 120.8 11 . ?
C22A C23A H23A 120.8 . . ?
C41A C40A P40A 98.5(14) . . ?
C41A C40A H40A 112.1 . . ?
P40A C40A H40A 112.1 . . ?
C41A C40A H40B 112.1 . . ?
P40A C40A H40B 112.1 . . ?
H40A C40A H40B 109.7 . . ?
C41A C40A H41B 37.9(5) . 11 ?
P40A C40A H41B 102.2(12) . 11 ?
H40A C40A H41B 138.7 . 11 ?
H40B C40A H41B 76.0 . 11 ?
C41A C40A H41C 40.9(5) . 11 ?
P40A C40A H41C 120(2) . 11 ?
H40A C40A H41C 71.5 . 11 ?
H40B C40A H41C 123.2 . 11 ?
H41B C40A H41C 71.8 11 11 ?
C40A C41A H41A 109.5 . . ?
C40A C41A H41B 109.5 . . ?
H41A C41A H41B 109.5 . . ?
C40A C41A H41C 109.5 . . ?
H41A C41A H41C 109.5 . . ?
H41B C41A H41C 109.5 . . ?
C40A C41A H41B 72.2(18) . 11 ?
H41A C41A H41B 87.8 . 11 ?
H41B C41A H41B 53.4 . 11 ?
H41C C41A H41B 160.0 . 11 ?
C40A C41A H41A 157.2(9) . 11 ?
H41A C41A H41A 48.9 . 11 ?
H41B C41A H41A 87.8 . 11 ?
H41C C41A H41A 77.0 . 11 ?
H41B C41A H41A 109.5 11 11 ?
C40A C41A H41C 51.3(15) . 11 ?
H41A C41A H41C 76.9 . 11 ?
H41B C41A H41C 160.0 . 11 ?
H41C C41A H41C 84.9 . 11 ?
H41B C41A H41C 109.5 11 11 ?
H41A C41A H41C 109.5 11 11 ?
O40B P40B C40B 111.2(6) . . ?
O40B P40B C40B 111.2(6) . 10 ?
C40B P40B C40B 106.3(10) . 10 ?
O40B P40B C20B 114.7(7) . . ?
C40B P40B C20B 106.5(6) . . ?
C40B P40B C20B 106.5(6) 10 . ?
C17B O13B Cu3 123.3(7) . . ?
C15B C10B C11B 119.2(8) . . ?
C15B C10B C21B 119.5(6) . . ?
C11B C10B C21B 120.6(8) . . ?
C10B C11B C12B 117.2(16) . . ?
C10B C11B H11B 121.4 . . ?
C12B C11B H11B 121.4 . . ?
C13B C12B C11B 120(2) . . ?
C13B C12B C16B 124(3) . . ?
C11B C12B C16B 115(2) . . ?
C14B C13B C12B 121(2) . . ?
C14B C13B H13B 119.6 . . ?
C12B C13B H13B 119.6 . . ?
C13B C14B C15B 120.8(13) . . ?
C13B C14B C17B 116.2(13) . . ?
C15B C14B C17B 121.9(10) . . ?
C14B C15B C10B 120.7(8) . . ?
C14B C15B H15B 119.7 . . ?
C10B C15B H15B 119.7 . . ?
O12B C17B O13B 124.9(11) . . ?
O12B C17B C14B 120.1(10) . . ?
O13B C17B C14B 114.9(10) . . ?
C21B C20B C21B 120.2(10) . 10 ?
C21B C20B P40B 118.6(5) . . ?
C21B C20B P40B 118.6(5) 10 . ?
C20B C21B C22B 119.7(7) . . ?
C20B C21B C10B 122.3(7) . . ?
C22B C21B C10B 115.9(6) . . ?
C23B C22B C21B 119.9(6) . . ?
C23B C22B H22B 120.1 . . ?
C21B C22B H22B 120.1 . . ?
C22B C23B C22B 120.7(10) 10 . ?
C22B C23B H23B 119.7 10 . ?
C22B C23B H23B 119.7 . . ?
C41B C40B P40B 118.8(16) . . ?
C41B C40B H40C 107.6 . . ?
P40B C40B H40C 107.6 . . ?
C41B C40B H40D 107.6 . . ?
P40B C40B H40D 107.6 . . ?
H40C C40B H40D 107.1 . . ?
C40B C41B H41D 109.5 . . ?
C40B C41B H41E 109.5 . . ?
H41D C41B H41E 109.5 . . ?
C40B C41B H41F 109.5 . . ?
H41D C41B H41F 109.5 . . ?
H41E C41B H41F 109.5 . . ?
C40C P40C O40C 106.4(6) . . ?
C40C P40C O40C 106.4(6) 10 . ?
C40C P40C C20C 107.1(6) . . ?
C40C P40C C20C 107.1(6) 10 . ?
O40C P40C C20C 114.5(6) . . ?
C17C O13C Cu3 121.5(8) . . ?
C11C C10C C15C 117.9(9) . . ?
C11C C10C C21C 123.3(9) . . ?
C15C C10C C21C 118.7(7) . . ?
C12C C11C C10C 123.5(17) . . ?
C12C C11C H11C 118.2 . . ?
C10C C11C H11C 118.2 . . ?
C11C C12C C13C 119(3) . . ?
C11C C12C C16B 127(2) . . ?
C13C C12C C16B 114(2) . . ?
C12C C13C C14C 119(2) . . ?
C12C C13C H13C 120.3 . . ?
C14C C13C H13C 120.3 . . ?
C15C C14C C13C 117.9(13) . . ?
C15C C14C C17C 119.2(11) . . ?
C13C C14C C17C 122.9(14) . . ?
C10C C15C C14C 121.9(9) . . ?
C10C C15C H15C 119.1 . . ?
C14C C15C H15C 119.1 . . ?
O13C C17C O12B 127.6(13) . . ?
O13C C17C C14C 118.0(12) . . ?
O12B C17C C14C 114.1(11) . . ?
C21C C20C P40C 117.6(5) . . ?
C21C C20C P40C 117.6(5) 10 . ?
C20C C21C C22C 118.9(8) . . ?
C20C C21C C10C 124.1(8) . . ?
C22C C21C C10C 115.5(8) . . ?
C23C C22C C21C 120.2(7) . . ?
C23C C22C H22C 119.9 . . ?
C21C C22C H22C 119.9 . . ?
C22C C23C C22C 120.0(11) 10 . ?
C22C C23C H23C 120.0 10 . ?
C22C C23C H23C 120.0 . . ?
C41C C40C P40C 119.7(19) . . ?
C41C C40C H40E 107.4 . . ?
P40C C40C H40E 107.4 . . ?
C41C C40C H40F 107.4 . . ?
P40C C40C H40F 107.4 . . ?
H40E C40C H40F 106.9 . . ?
C40C C41C H41G 109.5 . . ?
C40C C41C H41H 109.5 . . ?
H41G C41C H41H 109.5 . . ?
C40C C41C H41I 109.5 . . ?
H41G C41C H41I 109.5 . . ?
H41H C41C H41I 109.5 . . ?
O10B C16B O11B 126.8(3) . . ?
O10B C16B C12C 115.1(13) . . ?
O11B C16B C12C 118.0(14) . . ?
O10B C16B C12B 118.9(14) . . ?
O11B C16B C12B 113.7(13) . . ?
C14A O10A Cu1 121.8(3) . . ?
C14A O11A Cu1 125.4(3) . 13 ?
C16B O10B Cu1 120.0(2) . 13 ?
C16B O11B Cu1 125.6(2) . . ?
C17B O12B Cu2 123.0(6) . . ?
C17C O12B Cu2 121.8(7) . . ?
Cu3 Cl1 Cu3 180.0 . 9 ?
O40A P40A O40A 130.3(10) 2_655 . ?
O40A P40A C40A 49.1(7) 2_655 12_655 ?
O40A P40A C40A 113.3(6) . 12_655 ?
O40A P40A C40A 113.3(6) 2_655 11 ?
O40A P40A C40A 49.1(7) . 11 ?
C40A P40A C40A 144.1(12) 12_655 11 ?
O40A P40A C40A 49.1(7) 2_655 . ?
O40A P40A C40A 113.3(6) . . ?
C40A P40A C40A 98.1(15) 12_655 . ?
C40A P40A C40A 70.6(13) 11 . ?
O40A P40A C40A 113.3(6) 2_655 2_655 ?
O40A P40A C40A 49.1(7) . 2_655 ?
C40A P40A C40A 70.6(13) 12_655 2_655 ?
C40A P40A C40A 98.1(15) 11 2_655 ?
C40A P40A C40A 144.1(12) . 2_655 ?
O40A P40A C20A 114.9(5) 2_655 . ?
O40A P40A C20A 114.9(5) . . ?
C40A P40A C20A 108.0(6) 12_655 . ?
C40A P40A C20A 108.0(6) 11 . ?
C40A P40A C20A 108.0(6) . . ?
C40A P40A C20A 108.0(6) 2_655 . ?
C40A O40A C40A 156.5(19) 11 2_655 ?
C40A O40A P40A 78.6(10) 11 . ?
C40A O40A P40A 78.6(10) 2_655 . ?
O11B Cu1 O11A 89.07(13) . 13 ?
O11B Cu1 O10A 89.58(13) . . ?
O11A Cu1 O10A 167.45(11) 13 . ?
O11B Cu1 O10B 167.45(11) . 13 ?
O11A Cu1 O10B 89.50(13) 13 13 ?
O10A Cu1 O10B 89.11(13) . 13 ?
O11B Cu1 O100 98.66(11) . . ?
O11A Cu1 O100 97.06(12) 13 . ?
O10A Cu1 O100 95.47(12) . . ?
O10B Cu1 O100 93.89(11) 13 . ?
O11B Cu1 Cu1 81.61(8) . 13 ?
O11A Cu1 Cu1 82.11(8) 13 13 ?
O10A Cu1 Cu1 85.34(8) . 13 ?
O10B Cu1 Cu1 85.84(8) 13 13 ?
O100 Cu1 Cu1 179.14(10) . 13 ?
O12B Cu2 O12B 89.57(15) 2 12 ?
O12B Cu2 O12B 88.93(15) 2 11 ?
O12B Cu2 O12B 166.87(12) 12 11 ?
O12B Cu2 O12B 166.87(12) 2 . ?
O12B Cu2 O12B 88.93(15) 12 . ?
O12B Cu2 O12B 89.57(15) 11 . ?
O12B Cu2 O200 96.57(6) 2 . ?
O12B Cu2 O200 96.57(6) 12 . ?
O12B Cu2 O200 96.57(6) 11 . ?
O12B Cu2 O200 96.57(6) . . ?
O12B Cu2 Cu3 83.43(6) 2 . ?
O12B Cu2 Cu3 83.43(6) 12 . ?
O12B Cu2 Cu3 83.43(6) 11 . ?
O12B Cu2 Cu3 83.43(6) . . ?
O200 Cu2 Cu3 180.0 . . ?
O13B Cu3 O13B 166.1(3) . 2 ?
O13B Cu3 O13B 68.0(4) . 12 ?
O13B Cu3 O13B 110.2(4) 2 12 ?
O13B Cu3 O13B 110.2(4) . 11 ?
O13B Cu3 O13B 68.0(4) 2 11 ?
O13B Cu3 O13B 166.1(3) 12 11 ?
O13B Cu3 O13C 153.89(18) . 2 ?
O13B Cu3 O13C 21.94(19) 2 2 ?
O13B Cu3 O13C 88.5(3) 12 2 ?
O13B Cu3 O13C 89.8(3) 11 2 ?
O13B Cu3 O13C 88.5(3) . 11 ?
O13B Cu3 O13C 89.8(3) 2 11 ?
O13B Cu3 O13C 153.89(18) 12 11 ?
O13B Cu3 O13C 21.94(19) 11 11 ?
O13B Cu3 O13C 89.8(3) . 12 ?
O13B Cu3 O13C 88.5(3) 2 12 ?
O13B Cu3 O13C 21.94(19) 12 12 ?
O13B Cu3 O13C 153.89(18) 11 12 ?
O13C Cu3 O13C 165.9(4) 2 . ?
O13C Cu3 O13C 66.7(4) 11 . ?
O13C Cu3 O13C 111.4(4) 12 . ?
O13B Cu3 Cl1 96.95(17) . . ?
O13B Cu3 Cl1 96.95(17) 2 . ?
O13B Cu3 Cl1 96.95(17) 12 . ?
O13B Cu3 Cl1 96.95(17) 11 . ?
O13C Cu3 Cl1 97.04(19) 2 . ?
O13C Cu3 Cl1 97.04(19) 11 . ?
O13C Cu3 Cl1 97.04(19) 12 . ?
O13C Cu3 Cl1 97.03(19) . . ?
O13B Cu3 Cu2 83.05(17) . . ?
O13B Cu3 Cu2 83.05(17) 2 . ?
O13B Cu3 Cu2 83.05(17) 12 . ?
O13B Cu3 Cu2 83.05(17) 11 . ?
O13C Cu3 Cu2 82.96(19) 2 . ?
O13C Cu3 Cu2 82.96(19) 11 . ?
O13C Cu3 Cu2 82.96(19) 12 . ?
O13C Cu3 Cu2 82.97(19) . . ?
Cl1 Cu3 Cu2 180.0 . . ?
N60 C60 H60A 109.5 . . ?
N60 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
N60 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
C60 N60 H60D 111.1 . . ?
C60 N60 H60D 111.1 4 . ?
C60 N60 H60E 111.1 . . ?
C60 N60 H60E 111.1 4 . ?
H60D N60 H60E 109.0 . . ?

_refine_diff_density_max         0.841
_refine_diff_density_min         -0.601
_refine_diff_density_rms         0.070



####################################################################### 
# 
# 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_3a
_database_code_depnum_ccdc_archive 'CCDC 1942982'
loop_
_audit_author_name
_audit_author_address
'Timo Stein'
;University of Hamburg
Germany
;
_audit_update_record             
;
2019-09-04 deposited with the CCDC.	2019-09-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H27 O9 P, 1.5(C2 H6 O)'
_chemical_formula_sum            'C31 H36 O10.50 P'
_chemical_formula_weight         607.57

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   10.5051(2)
_cell_length_b                   12.1756(2)
_cell_length_c                   12.9793(3)
_cell_angle_alpha                66.3180(10)
_cell_angle_beta                 88.3110(10)
_cell_angle_gamma                82.6810(10)
_cell_volume                     1507.51(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9902
_cell_measurement_theta_min      2.50
_cell_measurement_theta_max      34.25

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_F_000             642
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_exptl_absorpt_coefficient_mu    0.150
_shelx_estimated_absorpt_T_min   0.979
_shelx_estimated_absorpt_T_max   0.982
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.7098
_exptl_absorpt_correction_T_max  0.7468
_exptl_absorpt_process_details   'SADABS-2012/1 (Bruker AXS Inc., 2012)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Incoatec microfocus'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'Bruker Smart APEX CCD area detector'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_probe          x-ray
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            41778
_diffrn_reflns_av_unetI/netI     0.0182
_diffrn_reflns_av_R_equivalents  0.0190
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.714
_diffrn_reflns_theta_max         33.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             11051
_reflns_number_gt                9904
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'APEX2 v.2014.1-1 (Bruker AXS Inc., 2014)'
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0544P)²+0.6551P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         11051
_refine_ls_number_parameters     400
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0425
_refine_ls_R_factor_gt           0.0382
_refine_ls_wR_factor_ref         0.1081
_refine_ls_wR_factor_gt          0.1043
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.037
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C10 C 0.59836(8) 0.09560(8) 0.12833(7) 0.01218(14) Uani 1 1 d . . . . .
C11 C 0.47147(8) 0.07035(8) 0.14412(7) 0.01284(14) Uani 1 1 d . . . . .
H11 H 0.406238 0.128272 0.151404 0.015 Uiso 1 1 calc R U . . .
C12 C 0.44016(8) -0.04007(8) 0.14924(7) 0.01254(14) Uani 1 1 d . . . . .
C13 C 0.53446(9) -0.12477(8) 0.13632(7) 0.01315(14) Uani 1 1 d . . . . .
H13 H 0.512680 -0.199247 0.139043 0.016 Uiso 1 1 calc R U . . .
C14 C 0.66112(8) -0.09940(8) 0.11935(7) 0.01273(14) Uani 1 1 d . . . . .
C15 C 0.69287(8) 0.00999(8) 0.11555(7) 0.01314(14) Uani 1 1 d . . . . .
H15 H 0.779328 0.026602 0.104201 0.016 Uiso 1 1 calc R U . . .
C16 C 0.30506(9) -0.06841(8) 0.16424(7) 0.01378(15) Uani 1 1 d . . . . .
C17 C 0.08937(10) 0.00643(10) 0.17608(11) 0.0240(2) Uani 1 1 d . . . . .
H17A H 0.038885 0.075650 0.184511 0.036 Uiso 1 1 calc R U . . .
H17B H 0.081141 -0.067180 0.243404 0.036 Uiso 1 1 calc R U . . .
H17C H 0.057650 -0.002494 0.109956 0.036 Uiso 1 1 calc R U . . .
C18 C 0.75908(9) -0.19013(8) 0.10137(8) 0.01425(15) Uani 1 1 d . . . . .
C19 C 0.97938(10) -0.25788(10) 0.10232(10) 0.02309(19) Uani 1 1 d . . . . .
H19A H 1.063604 -0.234429 0.108952 0.035 Uiso 1 1 calc R U . . .
H19B H 0.971472 -0.263433 0.029573 0.035 Uiso 1 1 calc R U . . .
H19C H 0.970652 -0.336563 0.163188 0.035 Uiso 1 1 calc R U . . .
C20 C 0.60387(8) 0.26307(7) 0.19981(7) 0.01115(14) Uani 1 1 d . . . . .
C21 C 0.63225(8) 0.21471(8) 0.11764(7) 0.01188(14) Uani 1 1 d . . . . .
C22 C 0.69122(9) 0.28146(8) 0.01795(7) 0.01424(15) Uani 1 1 d . . . . .
H22 H 0.710997 0.247724 -0.035984 0.017 Uiso 1 1 calc R U . . .
C23 C 0.72130(9) 0.39622(8) -0.00341(8) 0.01506(15) Uani 1 1 d . . . . .
H23 H 0.765371 0.439028 -0.069602 0.018 Uiso 1 1 calc R U . . .
C24 C 0.68654(9) 0.44791(8) 0.07257(8) 0.01423(15) Uani 1 1 d . . . . .
H24 H 0.703479 0.527911 0.056442 0.017 Uiso 1 1 calc R U . . .
C25 C 0.62672(8) 0.38351(8) 0.17289(7) 0.01160(14) Uani 1 1 d . . . . .
C30 C 0.58505(8) 0.45226(7) 0.24297(7) 0.01167(14) Uani 1 1 d . . . . .
C31 C 0.45498(8) 0.47594(8) 0.26200(7) 0.01244(14) Uani 1 1 d . . . . .
H31 H 0.393211 0.443148 0.234463 0.015 Uiso 1 1 calc R U . . .
C32 C 0.41492(8) 0.54744(7) 0.32118(7) 0.01156(14) Uani 1 1 d . . . . .
C33 C 0.50468(8) 0.59464(8) 0.36343(7) 0.01166(14) Uani 1 1 d . . . . .
H33 H 0.477709 0.641772 0.405170 0.014 Uiso 1 1 calc R U . . .
C34 C 0.63451(8) 0.57186(7) 0.34371(7) 0.01126(14) Uani 1 1 d . . . . .
C35 C 0.67439(8) 0.50252(8) 0.28246(7) 0.01250(14) Uani 1 1 d . . . . .
H35 H 0.762863 0.489520 0.267607 0.015 Uiso 1 1 calc R U . . .
C36 C 0.27473(8) 0.57373(8) 0.33509(8) 0.01320(14) Uani 1 1 d . . . . .
C37 C 0.11577(9) 0.65827(10) 0.42256(9) 0.02079(18) Uani 1 1 d . . . . .
H37A H 0.107128 0.700197 0.473436 0.031 Uiso 1 1 calc R U . . .
H37B H 0.073228 0.585033 0.454573 0.031 Uiso 1 1 calc R U . . .
H37C H 0.075751 0.711702 0.349334 0.031 Uiso 1 1 calc R U . . .
C38 C 0.73503(8) 0.62193(8) 0.38416(7) 0.01322(14) Uani 1 1 d . . . . .
C39 C 0.78351(9) 0.72023(9) 0.49872(9) 0.01873(17) Uani 1 1 d . . . . .
H39A H 0.741476 0.757257 0.547468 0.028 Uiso 1 1 calc R U . . .
H39B H 0.823672 0.781204 0.436425 0.028 Uiso 1 1 calc R U . . .
H39C H 0.849324 0.654251 0.542373 0.028 Uiso 1 1 calc R U . . .
P40 P 0.55345(2) 0.16463(2) 0.33966(2) 0.01168(5) Uani 1 1 d . . . . .
C40 C 0.65495(10) 0.02232(9) 0.37935(8) 0.01893(17) Uani 1 1 d . . . . .
H40A H 0.743904 0.037218 0.360423 0.028 Uiso 1 1 calc R U . . .
H40B H 0.626371 -0.023082 0.338682 0.028 Uiso 1 1 calc R U . . .
H40C H 0.649751 -0.024552 0.460535 0.028 Uiso 1 1 calc R U . . .
C41 C 0.60267(10) 0.21441(9) 0.44413(8) 0.01834(17) Uani 1 1 d . . . . .
H41A H 0.691015 0.233718 0.430522 0.028 Uiso 1 1 calc R U . . .
H41B H 0.598165 0.149967 0.519236 0.028 Uiso 1 1 calc R U . . .
H41C H 0.545559 0.286587 0.439394 0.028 Uiso 1 1 calc R U . . .
C50 C 0.14827(12) 0.30733(12) 0.19420(12) 0.0333(3) Uani 1 1 d . . . . .
H50A H 0.170415 0.291197 0.126485 0.040 Uiso 1 1 calc R U . . .
H50B H 0.210068 0.358419 0.202425 0.040 Uiso 1 1 calc R U . . .
C51 C 0.01499(17) 0.37183(17) 0.18110(19) 0.0558(5) Uani 1 1 d . . . . .
H51A H 0.008494 0.446748 0.112819 0.084 Uiso 1 1 calc R U . . .
H51B H -0.004916 0.391118 0.246661 0.084 Uiso 1 1 calc R U . . .
H51C H -0.046015 0.319943 0.175236 0.084 Uiso 1 1 calc R U . . .
C60 C -0.03432(8) 0.05353(12) 0.50987(12) 0.0329(3) Uani 1 1 d D . . . .
H60A H -0.112389 0.029530 0.553556 0.039 Uiso 1 1 calc DR U . . .
H60B H 0.022493 0.077155 0.554913 0.039 Uiso 1 1 calc DR U . . .
O10 O 0.27293(7) -0.16479(6) 0.17594(6) 0.01882(13) Uani 1 1 d . . . . .
O11 O 0.22249(7) 0.02601(7) 0.16191(7) 0.02100(14) Uani 1 1 d . . . . .
O12 O 0.73268(7) -0.27340(6) 0.08142(6) 0.01876(13) Uani 1 1 d . . . . .
O13 O 0.87943(7) -0.16800(6) 0.11009(7) 0.01805(13) Uani 1 1 d . . . . .
O30 O 0.19273(7) 0.54974(7) 0.28651(7) 0.01914(14) Uani 1 1 d . . . . .
O31 O 0.25026(6) 0.62563(6) 0.40830(6) 0.01588(12) Uani 1 1 d . . . . .
O32 O 0.84587(7) 0.61692(8) 0.35718(7) 0.02242(15) Uani 1 1 d . . . . .
O33 O 0.68897(6) 0.67292(6) 0.45422(6) 0.01588(13) Uani 1 1 d . . . . .
O40 O 0.41362(7) 0.15109(7) 0.34561(6) 0.01906(13) Uani 1 1 d . . . . .
O51 O 0.15615(8) 0.19674(8) 0.29067(7) 0.02527(16) Uani 1 1 d . . . . .
H51 H 0.233494 0.171409 0.310344 0.038 Uiso 1 1 calc R U . . .
O61 O -0.06780(18) 0.14932(18) 0.41222(18) 0.0376(4) Uani 0.5 1 d . . P . .
H61 H -0.002029 0.168570 0.374056 0.056 Uiso 0.5 1 calc R U P . .
H61C H -0.05704(16) 0.12147(14) 0.4364(3) 0.030 Uiso 0.5 1 d D U P . .


_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
C10 C11 1.3968(12) . ?
C10 C15 1.4019(12) . ?
C10 C21 1.4888(11) . ?
C11 C12 1.3999(12) . ?
C11 H11 0.9500 . ?
C12 C13 1.3935(12) . ?
C12 C16 1.4919(12) . ?
C13 C14 1.3954(12) . ?
C13 H13 0.9500 . ?
C14 C15 1.3953(12) . ?
C14 C18 1.4956(12) . ?
C15 H15 0.9500 . ?
C16 O10 1.2120(11) . ?
C16 O11 1.3396(11) . ?
C17 O11 1.4425(12) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 O12 1.2078(11) . ?
C18 O13 1.3430(11) . ?
C19 O13 1.4491(12) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 C25 1.4154(11) . ?
C20 C21 1.4192(11) . ?
C20 P40 1.8356(9) . ?
C21 C22 1.3981(12) . ?
C22 C23 1.3875(12) . ?
C22 H22 0.9500 . ?
C23 C24 1.3859(12) . ?
C23 H23 0.9500 . ?
C24 C25 1.4008(12) . ?
C24 H24 0.9500 . ?
C25 C30 1.4880(11) . ?
C30 C35 1.3945(12) . ?
C30 C31 1.3958(12) . ?
C31 C32 1.3964(12) . ?
C31 H31 0.9500 . ?
C32 C33 1.3935(11) . ?
C32 C36 1.4881(12) . ?
C33 C34 1.3938(11) . ?
C33 H33 0.9500 . ?
C34 C35 1.3963(11) . ?
C34 C38 1.4888(12) . ?
C35 H35 0.9500 . ?
C36 O30 1.2120(11) . ?
C36 O31 1.3397(11) . ?
C37 O31 1.4453(11) . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 O32 1.2071(11) . ?
C38 O33 1.3407(11) . ?
C39 O33 1.4487(11) . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
P40 O40 1.4952(7) . ?
P40 C40 1.8026(10) . ?
P40 C41 1.8041(10) . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C50 O51 1.4182(16) . ?
C50 C51 1.494(2) . ?
C50 H50A 0.9900 . ?
C50 H50B 0.9900 . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C60 O61 1.351(2) . ?
C60 C60 1.517(3) 2_556 ?
C60 H60A 0.9900 . ?
C60 H60B 0.9900 . ?
C60 H61C 0.9900(10) . ?
O51 H51 0.8400 . ?
O61 H61 0.8400 . ?
O61 H61C 0.365(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
C11 C10 C15 119.08(8) . . ?
C11 C10 C21 120.81(8) . . ?
C15 C10 C21 119.99(8) . . ?
C10 C11 C12 120.18(8) . . ?
C10 C11 H11 119.9 . . ?
C12 C11 H11 119.9 . . ?
C13 C12 C11 120.48(8) . . ?
C13 C12 C16 118.27(8) . . ?
C11 C12 C16 121.21(8) . . ?
C12 C13 C14 119.52(8) . . ?
C12 C13 H13 120.2 . . ?
C14 C13 H13 120.2 . . ?
C15 C14 C13 120.12(8) . . ?
C15 C14 C18 121.67(8) . . ?
C13 C14 C18 118.18(8) . . ?
C14 C15 C10 120.61(8) . . ?
C14 C15 H15 119.7 . . ?
C10 C15 H15 119.7 . . ?
O10 C16 O11 123.66(8) . . ?
O10 C16 C12 124.32(8) . . ?
O11 C16 C12 112.02(7) . . ?
O11 C17 H17A 109.5 . . ?
O11 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
O11 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
O12 C18 O13 124.15(8) . . ?
O12 C18 C14 123.81(8) . . ?
O13 C18 C14 112.04(7) . . ?
O13 C19 H19A 109.5 . . ?
O13 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
O13 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C25 C20 C21 117.83(7) . . ?
C25 C20 P40 122.58(6) . . ?
C21 C20 P40 119.36(6) . . ?
C22 C21 C20 120.19(8) . . ?
C22 C21 C10 116.07(7) . . ?
C20 C21 C10 123.70(7) . . ?
C23 C22 C21 121.00(8) . . ?
C23 C22 H22 119.5 . . ?
C21 C22 H22 119.5 . . ?
C24 C23 C22 119.49(8) . . ?
C24 C23 H23 120.3 . . ?
C22 C23 H23 120.3 . . ?
C23 C24 C25 120.75(8) . . ?
C23 C24 H24 119.6 . . ?
C25 C24 H24 119.6 . . ?
C24 C25 C20 120.43(8) . . ?
C24 C25 C30 115.50(7) . . ?
C20 C25 C30 124.00(7) . . ?
C35 C30 C31 119.05(8) . . ?
C35 C30 C25 120.34(7) . . ?
C31 C30 C25 120.39(7) . . ?
C30 C31 C32 120.53(8) . . ?
C30 C31 H31 119.7 . . ?
C32 C31 H31 119.7 . . ?
C33 C32 C31 120.31(8) . . ?
C33 C32 C36 121.44(8) . . ?
C31 C32 C36 118.23(7) . . ?
C32 C33 C34 119.21(8) . . ?
C32 C33 H33 120.4 . . ?
C34 C33 H33 120.4 . . ?
C33 C34 C35 120.50(7) . . ?
C33 C34 C38 121.93(7) . . ?
C35 C34 C38 117.56(7) . . ?
C30 C35 C34 120.36(8) . . ?
C30 C35 H35 119.8 . . ?
C34 C35 H35 119.8 . . ?
O30 C36 O31 124.21(8) . . ?
O30 C36 C32 123.73(8) . . ?
O31 C36 C32 112.06(7) . . ?
O31 C37 H37A 109.5 . . ?
O31 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
O31 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
O32 C38 O33 123.68(8) . . ?
O32 C38 C34 123.78(8) . . ?
O33 C38 C34 112.54(7) . . ?
O33 C39 H39A 109.5 . . ?
O33 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
O33 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
O40 P40 C40 112.85(5) . . ?
O40 P40 C41 111.93(5) . . ?
C40 P40 C41 100.63(5) . . ?
O40 P40 C20 113.94(4) . . ?
C40 P40 C20 106.49(4) . . ?
C41 P40 C20 110.08(4) . . ?
P40 C40 H40A 109.5 . . ?
P40 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
P40 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
P40 C41 H41A 109.5 . . ?
P40 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
P40 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
O51 C50 C51 109.38(13) . . ?
O51 C50 H50A 109.8 . . ?
C51 C50 H50A 109.8 . . ?
O51 C50 H50B 109.8 . . ?
C51 C50 H50B 109.8 . . ?
H50A C50 H50B 108.2 . . ?
C50 C51 H51A 109.5 . . ?
C50 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
C50 C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
O61 C60 C60 111.90(18) . 2_556 ?
O61 C60 H60A 109.2 . . ?
C60 C60 H60A 109.2 2_556 . ?
O61 C60 H60B 109.2 . . ?
C60 C60 H60B 109.2 2_556 . ?
H60A C60 H60B 107.9 . . ?
O61 C60 H61C 2.7(2) . . ?
C60 C60 H61C 109.24(11) 2_556 . ?
H60A C60 H61C 110.6 . . ?
H60B C60 H61C 110.6 . . ?
C16 O11 C17 115.74(8) . . ?
C18 O13 C19 114.93(8) . . ?
C36 O31 C37 115.09(7) . . ?
C38 O33 C39 114.91(7) . . ?
C50 O51 H51 109.5 . . ?
C60 O61 H61 109.5 . . ?
C60 O61 H61C 7.2(7) . . ?
H61 O61 H61C 105.4 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C15 C10 C11 C12 1.24(13) . . . . ?
C21 C10 C11 C12 177.28(8) . . . . ?
C10 C11 C12 C13 -1.35(13) . . . . ?
C10 C11 C12 C16 -179.03(8) . . . . ?
C11 C12 C13 C14 0.67(13) . . . . ?
C16 C12 C13 C14 178.42(8) . . . . ?
C12 C13 C14 C15 0.09(13) . . . . ?
C12 C13 C14 C18 -177.69(8) . . . . ?
C13 C14 C15 C10 -0.19(13) . . . . ?
C18 C14 C15 C10 177.51(8) . . . . ?
C11 C10 C15 C14 -0.47(13) . . . . ?
C21 C10 C15 C14 -176.55(8) . . . . ?
C13 C12 C16 O10 6.83(13) . . . . ?
C11 C12 C16 O10 -175.44(9) . . . . ?
C13 C12 C16 O11 -172.41(8) . . . . ?
C11 C12 C16 O11 5.32(12) . . . . ?
C15 C14 C18 O12 -164.51(9) . . . . ?
C13 C14 C18 O12 13.23(14) . . . . ?
C15 C14 C18 O13 15.52(12) . . . . ?
C13 C14 C18 O13 -166.74(8) . . . . ?
C25 C20 C21 C22 5.44(12) . . . . ?
P40 C20 C21 C22 -169.15(7) . . . . ?
C25 C20 C21 C10 -172.18(8) . . . . ?
P40 C20 C21 C10 13.23(11) . . . . ?
C11 C10 C21 C22 -121.28(9) . . . . ?
C15 C10 C21 C22 54.73(11) . . . . ?
C11 C10 C21 C20 56.43(12) . . . . ?
C15 C10 C21 C20 -127.56(9) . . . . ?
C20 C21 C22 C23 -0.96(13) . . . . ?
C10 C21 C22 C23 176.83(8) . . . . ?
C21 C22 C23 C24 -3.29(14) . . . . ?
C22 C23 C24 C25 2.90(14) . . . . ?
C23 C24 C25 C20 1.73(13) . . . . ?
C23 C24 C25 C30 -175.40(8) . . . . ?
C21 C20 C25 C24 -5.82(12) . . . . ?
P40 C20 C25 C24 168.58(7) . . . . ?
C21 C20 C25 C30 171.05(8) . . . . ?
P40 C20 C25 C30 -14.54(12) . . . . ?
C24 C25 C30 C35 -58.96(11) . . . . ?
C20 C25 C30 C35 124.02(9) . . . . ?
C24 C25 C30 C31 115.60(9) . . . . ?
C20 C25 C30 C31 -61.41(12) . . . . ?
C35 C30 C31 C32 -0.95(13) . . . . ?
C25 C30 C31 C32 -175.58(8) . . . . ?
C30 C31 C32 C33 -0.94(13) . . . . ?
C30 C31 C32 C36 177.63(8) . . . . ?
C31 C32 C33 C34 1.43(13) . . . . ?
C36 C32 C33 C34 -177.09(8) . . . . ?
C32 C33 C34 C35 -0.05(13) . . . . ?
C32 C33 C34 C38 178.55(8) . . . . ?
C31 C30 C35 C34 2.33(13) . . . . ?
C25 C30 C35 C34 176.96(8) . . . . ?
C33 C34 C35 C30 -1.84(13) . . . . ?
C38 C34 C35 C30 179.49(8) . . . . ?
C33 C32 C36 O30 168.95(9) . . . . ?
C31 C32 C36 O30 -9.60(13) . . . . ?
C33 C32 C36 O31 -11.72(12) . . . . ?
C31 C32 C36 O31 169.73(8) . . . . ?
C33 C34 C38 O32 -170.49(9) . . . . ?
C35 C34 C38 O32 8.15(14) . . . . ?
C33 C34 C38 O33 9.71(12) . . . . ?
C35 C34 C38 O33 -171.64(8) . . . . ?
C25 C20 P40 O40 102.55(8) . . . . ?
C21 C20 P40 O40 -83.13(8) . . . . ?
C25 C20 P40 C40 -132.39(7) . . . . ?
C21 C20 P40 C40 41.94(8) . . . . ?
C25 C20 P40 C41 -24.14(8) . . . . ?
C21 C20 P40 C41 150.18(7) . . . . ?
O10 C16 O11 C17 0.90(14) . . . . ?
C12 C16 O11 C17 -179.86(8) . . . . ?
O12 C18 O13 C19 -4.57(14) . . . . ?
C14 C18 O13 C19 175.40(8) . . . . ?
O30 C36 O31 C37 -3.08(13) . . . . ?
C32 C36 O31 C37 177.59(8) . . . . ?
O32 C38 O33 C39 -1.43(13) . . . . ?
C34 C38 O33 C39 178.36(8) . . . . ?

_refine_diff_density_max         0.554
_refine_diff_density_min         -0.349
_refine_diff_density_rms         0.059

####################################################################### 
# 
# 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_3b
_database_code_depnum_ccdc_archive 'CCDC 1942983'
loop_
_audit_author_name
_audit_author_address
'Timo Stein'
;University of Hamburg
Germany
;
_audit_update_record             
;
2019-09-04 deposited with the CCDC.	2019-09-27 downloaded from the CCDC.
;
_audit_creation_date             2019-09-02
_audit_creation_method           
;
Olex2 1.3-alpha
(compiled 2019.08.16 svn.r3652 for OlexSys, GUI svn.r5895)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C28 H27 O8 P S'
_chemical_formula_sum            'C28 H27 O8 P S'
_chemical_formula_weight         554.52
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C56 H54 O16 P2 S2 '
_chemical_oxdiff_usercomment     Stein/Froeba
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 '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                   10.9208(4)
_cell_length_b                   11.5897(3)
_cell_length_c                   11.7392(4)
_cell_angle_alpha                100.927(3)
_cell_angle_beta                 109.264(3)
_cell_angle_gamma                103.651(3)
_cell_volume                     1303.80(8)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    22171
_cell_measurement_temperature    99.9(3)
_cell_measurement_theta_max      75.6310
_cell_measurement_theta_min      4.0820
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.119
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.679
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.59a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.413
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             580
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 0 0 0.0851
1 0 0 0.0851
-1 0 2 0.0769
1 0 -2 0.0689
1 -1 0 0.0522
-1 1 0 0.0522

_exptl_crystal_size_max          0.308
_exptl_crystal_size_mid          0.177
_exptl_crystal_size_min          0.104
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-1.0001 0.0001 0.0013 -0.1085 0.0854 -0.0764
1.0001 -0.0001 -0.0013 0.1085 -0.0854 0.0764
-0.9981 -0.0015 1.9996 0.0259 -0.1073 -0.2472
0.9981 0.0015 -1.9996 -0.0259 0.1073 0.2472
1.0003 -0.9993 -0.0015 0.1639 0.0428 0.0461
-1.0003 0.9993 0.0015 -0.1639 -0.0428 -0.0461

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0388
_diffrn_reflns_av_unetI/netI     0.0226
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            37479
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.145
_diffrn_reflns_theta_min         4.104
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.9(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2063
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -87.00  -6.00   1.00    1.50    --  -42.82 125.00   0.00   81
  2  ω   -117.00 -18.00   1.00    1.50    --  -42.82 -38.00-150.00   99
  3  ω   -115.00 -15.00   1.00    1.50    --  -42.82 -57.00 120.00  100
  4  ω      9.00  42.00   1.00    1.50    --   42.82  81.00-123.63   33
  5  ω    -29.00  71.00   1.00    1.50    --   42.82 -57.00 -60.00  100
  6  ω    -21.00  75.00   1.00    1.50    --   42.82 -77.00-180.00   96
  7  ω     28.00 107.00   1.00    6.00    --  111.00 -94.00 -30.00   79
  8  ω     39.00 140.00   1.00    6.00    --  111.00 -61.00 -90.00  101
  9  ω     67.00 178.00   1.00    6.00    --  111.00  18.00  38.06  111
 10  ω     85.00 178.00   1.00    6.00    --  111.00  45.00 150.00   93
 11  ω     38.00 137.00   1.00    6.00    --  111.00 -45.00 150.00   99
 12  ω     38.00 112.00   1.00    6.00    --  111.00-125.00  90.00   74
 13  ω     83.00 178.00   1.00    6.00    --  111.00  55.00  -5.99   95
 14  ω     28.00 107.00   1.00    6.00    --  111.00 -94.00-180.00   79
 15  ω     85.00 178.00   1.00    6.00    --  111.00  45.00  60.00   93
 16  ω     35.00 144.00   1.00    6.00    --  111.00 -77.00  60.00  109
 17  ω     39.00 140.00   1.00    6.00    --  111.00 -61.00 -30.00  101
 18  ω     28.00 107.00   1.00    6.00    --  111.00 -94.00 120.00   79
 19  ω     28.00 107.00   1.00    6.00    --  111.00 -94.00   0.00   79
 20  ω     80.00 178.00   1.00    6.00    --  111.00  70.00 142.38   98
 21  ω     82.00 178.00   1.00    6.00    --  111.00  61.00 -60.00   96
 22  ω     38.00 112.00   1.00    6.00    --  111.00-125.00  60.00   74
 23  ω     28.00 107.00   1.00    6.00    --  111.00 -94.00 -60.00   79
 24  ω     35.00 144.00   1.00    6.00    --  111.00 -77.00 120.00  109
 25  ω     85.00 178.00   1.00    6.00    --  111.00  45.00 120.00   93
 26  ω     82.00 178.00   1.00    6.00    --  111.00  59.00 165.58   96
 27  ω     82.00 178.00   1.00    6.00    --  111.00  61.00-153.05   96
 28  ω     38.00 137.00   1.00    6.00    --  111.00 -45.00-120.00   99
 29  ω     85.00 178.00   1.00    6.00    --  111.00  45.00 -30.00   93
 30  ω     38.00 112.00   1.00    6.00    --  111.00-125.00 -90.00   74
 31  ω    103.00 178.00   1.00    6.00    --  111.00  77.00-120.00   75
 32  ω     38.00 112.00   1.00    6.00    --  111.00-125.00 -60.00   74
 33  ω     38.00 112.00   1.00    6.00    --  111.00-125.00   0.00   74
 34  ω     38.00 112.00   1.00    6.00    --  111.00-125.00 150.00   74
 35  ω    103.00 178.00   1.00    6.00    --  111.00  77.00  60.00   75
 36  ω    103.00 178.00   1.00    6.00    --  111.00  77.00  90.00   75
 37  ω     28.00 107.00   1.00    6.00    --  111.00 -94.00-150.00   79
 38  ω    103.00 178.00   1.00    6.00    --  111.00  77.00 -90.00   75
 39  ω     28.00 107.00   1.00    6.00    --  111.00 -94.00  60.00   79
 40  ω     82.00 178.00   1.00    6.00    --  111.00  61.00-120.00   96
 41  ω     82.00 178.00   1.00    6.00    --  111.00  61.00 120.00   96
 42  ω     38.00 137.00   1.00    6.00    --  111.00 -45.00 -60.00   99
 43  ω     29.00 106.00   1.00    6.00    --  111.00 -96.00 -94.44   77
 44  ω    -67.00  31.00   1.00    1.50    --  -42.82  38.00-180.00   98
 45  ω   -115.00 -15.00   1.00    1.50    --  -42.82 -57.00  60.00  100
 46  ω   -115.00 -15.00   1.00    1.50    --  -42.82 -57.00 -30.00  100
 47  ω     10.00  42.00   1.00    1.50    --   42.82  78.00 108.02   32
 48  ω     10.00  42.00   1.00    1.50    --   42.82  80.00 -75.74   32
 49  ω      9.00  42.00   1.00    1.50    --   42.82  82.00  -0.76   33
 50  ω     10.00  42.00   1.00    1.50    --   42.82  76.00  58.58   32
 51  ω     79.00 178.00   1.00    6.00    --  111.00  74.00   8.28   99
 52  ω     79.00 178.00   1.00    6.00    --  111.00  74.00 -97.61   99
 53  ω     80.00 178.00   1.00    6.00    --  111.00  71.00  74.53   98
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1085529000
_diffrn_orient_matrix_UB_12      -0.0554088000
_diffrn_orient_matrix_UB_13      0.0671134000
_diffrn_orient_matrix_UB_21      -0.0855036000
_diffrn_orient_matrix_UB_22      -0.1282869000
_diffrn_orient_matrix_UB_23      -0.0964511000
_diffrn_orient_matrix_UB_31      0.0762935000
_diffrn_orient_matrix_UB_32      0.0303592000
_diffrn_orient_matrix_UB_33      -0.0855179000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5029
_reflns_number_total             5433
_reflns_odcompleteness_completeness 98.43
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     76.86
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.59a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.59a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.59a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT 2018/3 (Sheldrick, 2015)'
_refine_diff_density_max         0.520
_refine_diff_density_min         -0.347
_refine_diff_density_rms         0.054
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         5433
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0455
_refine_ls_R_factor_gt           0.0419
_refine_ls_restrained_S_all      1.033
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0547P)²+0.8653P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1037
_refine_ls_wR_factor_ref         0.1060
_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 Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C14(H14), C21(H21), C23(H23), C25(H25), C31(H31),
 C33(H33), C35(H35)
2.b Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C29(H29A,H29B,H29C), C37(H37A,H37B,H37C), C39(H39A,H39B,
 H39C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
C10 C 0.24822(16) 0.65332(14) 0.20961(14) 0.0213(3) Uani 1 1 d . . . . .
C11 C 0.17976(16) 0.55885(15) 0.24884(15) 0.0223(3) Uani 1 1 d . . . . .
C12 C 0.11056(17) 0.43913(15) 0.16696(16) 0.0249(3) Uani 1 1 d . . . . .
H12 H 0.067965 0.377380 0.194636 0.030 Uiso 1 1 calc R U . . .
C13 C 0.10451(18) 0.41106(15) 0.04463(16) 0.0268(3) Uani 1 1 d . . . . .
H13 H 0.059192 0.330723 -0.009299 0.032 Uiso 1 1 calc R U . . .
C14 C 0.16654(17) 0.50374(15) 0.00365(15) 0.0254(3) Uani 1 1 d . . . . .
H14 H 0.160601 0.485247 -0.079014 0.030 Uiso 1 1 calc R U . . .
C15 C 0.23770(16) 0.62412(15) 0.08327(15) 0.0222(3) Uani 1 1 d . . . . .
C20 C 0.17522(16) 0.57750(14) 0.37673(15) 0.0224(3) Uani 1 1 d . . . . .
O20 O 0.02568(13) 0.76134(11) 0.68780(11) 0.0306(3) Uani 1 1 d . . . . .
C21 C 0.10828(16) 0.65387(14) 0.41907(15) 0.0227(3) Uani 1 1 d . . . . .
H21 H 0.066427 0.697173 0.367757 0.027 Uiso 1 1 calc R U . . .
O21 O -0.02949(13) 0.79732(11) 0.49840(12) 0.0301(3) Uani 1 1 d . . . . .
O22 O 0.35740(14) 0.38245(13) 0.61070(12) 0.0342(3) Uani 1 1 d . . . . .
C22 C 0.10368(16) 0.66575(14) 0.53843(15) 0.0233(3) Uani 1 1 d . . . . .
C23 C 0.16388(16) 0.59944(14) 0.61519(15) 0.0234(3) Uani 1 1 d . . . . .
H23 H 0.161087 0.607587 0.694568 0.028 Uiso 1 1 calc R U . . .
O23 O 0.26300(14) 0.43998(12) 0.74622(11) 0.0311(3) Uani 1 1 d . . . . .
C24 C 0.22827(17) 0.52088(15) 0.57204(15) 0.0247(3) Uani 1 1 d . . . . .
C25 C 0.23341(17) 0.51040(15) 0.45326(15) 0.0241(3) Uani 1 1 d . . . . .
H25 H 0.276402 0.457758 0.424903 0.029 Uiso 1 1 calc R U . . .
C26 C 0.03109(17) 0.74574(14) 0.58489(15) 0.0243(3) Uani 1 1 d . . . . .
C27 C -0.1015(2) 0.87691(18) 0.5368(2) 0.0364(4) Uani 1 1 d . . . . .
H27A H -0.144640 0.906583 0.468127 0.055 Uiso 1 1 calc R U . . .
H27B H -0.037712 0.946141 0.607670 0.055 Uiso 1 1 calc R U . . .
H27C H -0.169945 0.830832 0.560196 0.055 Uiso 1 1 calc R U . . .
C28 C 0.29115(18) 0.44138(16) 0.64367(16) 0.0274(3) Uani 1 1 d . . . . .
C29 C 0.3233(3) 0.3631(2) 0.81605(19) 0.0432(5) Uani 1 1 d . . . . .
H29A H 0.275643 0.277232 0.769485 0.065 Uiso 1 1 calc R U . . .
H29B H 0.316044 0.378757 0.896480 0.065 Uiso 1 1 calc R U . . .
H29C H 0.418045 0.382354 0.828467 0.065 Uiso 1 1 calc R U . . .
O30 O 0.27188(14) 1.04676(13) -0.16330(14) 0.0387(3) Uani 1 1 d . . . . .
C30 C 0.29431(16) 0.71325(15) 0.02224(14) 0.0230(3) Uani 1 1 d . . . . .
O31 O 0.14196(13) 0.99617(11) -0.05586(12) 0.0300(3) Uani 1 1 d . . . . .
C31 C 0.24587(16) 0.81115(15) 0.00040(15) 0.0243(3) Uani 1 1 d . . . . .
H31 H 0.182504 0.828461 0.032111 0.029 Uiso 1 1 calc R U . . .
O32 O 0.57796(15) 0.64191(14) -0.12870(14) 0.0395(3) Uani 1 1 d . . . . .
C32 C 0.29197(16) 0.88336(15) -0.06883(15) 0.0240(3) Uani 1 1 d . . . . .
O33 O 0.58770(13) 0.81209(13) -0.19504(13) 0.0342(3) Uani 1 1 d . . . . .
C33 C 0.38949(16) 0.86040(15) -0.11465(15) 0.0249(3) Uani 1 1 d . . . . .
H33 H 0.420903 0.909418 -0.159876 0.030 Uiso 1 1 calc R U . . .
C34 C 0.43896(16) 0.76355(16) -0.09189(15) 0.0247(3) Uani 1 1 d . . . . .
C35 C 0.38947(16) 0.68944(15) -0.02646(14) 0.0238(3) Uani 1 1 d . . . . .
H35 H 0.420269 0.622597 -0.014802 0.029 Uiso 1 1 calc R U . . .
C36 C 0.23629(17) 0.98348(16) -0.10221(16) 0.0268(3) Uani 1 1 d . . . . .
C37 C 0.0820(2) 1.0895(2) -0.0885(2) 0.0407(5) Uani 1 1 d . . . . .
H37A H 0.032843 1.066311 -0.178226 0.061 Uiso 1 1 calc R U . . .
H37B H 0.153101 1.167754 -0.061503 0.061 Uiso 1 1 calc R U . . .
H37C H 0.020124 1.096782 -0.047494 0.061 Uiso 1 1 calc R U . . .
C38 C 0.54132(17) 0.73092(17) -0.13968(16) 0.0277(3) Uani 1 1 d . . . . .
C39 C 0.6862(2) 0.7847(2) -0.2449(2) 0.0406(5) Uani 1 1 d . . . . .
H39A H 0.642304 0.709080 -0.313124 0.061 Uiso 1 1 calc R U . . .
H39B H 0.760531 0.775430 -0.179459 0.061 Uiso 1 1 calc R U . . .
H39C H 0.720876 0.851445 -0.275066 0.061 Uiso 1 1 calc R U . . .
S40 S 0.24282(4) 0.91664(4) 0.33517(4) 0.02940(11) Uani 1 1 d . . . . .
C40 C 0.49638(18) 0.87233(17) 0.28498(17) 0.0305(4) Uani 1 1 d . . . . .
H40A H 0.464751 0.899033 0.211110 0.046 Uiso 1 1 calc R U . . .
H40B H 0.538694 0.810645 0.269141 0.046 Uiso 1 1 calc R U . . .
H40C H 0.561921 0.942064 0.354364 0.046 Uiso 1 1 calc R U . . .
P40 P 0.35257(4) 0.80681(4) 0.32332(4) 0.02161(11) Uani 1 1 d . . . . .
C41 C 0.44326(17) 0.78431(16) 0.47257(16) 0.0286(3) Uani 1 1 d . . . . .
H41A H 0.478154 0.716679 0.458135 0.043 Uiso 1 1 calc R U . . .
H41B H 0.381788 0.765678 0.514056 0.043 Uiso 1 1 calc R U . . .
H41C H 0.517990 0.858632 0.524778 0.043 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C10 C11 1.415(2) . ?
C10 C15 1.416(2) . ?
C10 P40 1.8396(16) . ?
C11 C12 1.393(2) . ?
C11 C20 1.495(2) . ?
C12 H12 0.9300 . ?
C12 C13 1.387(2) . ?
C13 H13 0.9300 . ?
C13 C14 1.383(2) . ?
C14 H14 0.9300 . ?
C14 C15 1.392(2) . ?
C15 C30 1.495(2) . ?
C20 C21 1.394(2) . ?
C20 C25 1.392(2) . ?
O20 C26 1.210(2) . ?
C21 H21 0.9300 . ?
C21 C22 1.401(2) . ?
O21 C26 1.341(2) . ?
O21 C27 1.446(2) . ?
O22 C28 1.207(2) . ?
C22 C23 1.395(2) . ?
C22 C26 1.492(2) . ?
C23 H23 0.9300 . ?
C23 C24 1.394(2) . ?
O23 C28 1.339(2) . ?
O23 C29 1.448(2) . ?
C24 C25 1.397(2) . ?
C24 C28 1.496(2) . ?
C25 H25 0.9300 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
O30 C36 1.205(2) . ?
C30 C31 1.392(2) . ?
C30 C35 1.397(2) . ?
O31 C36 1.338(2) . ?
O31 C37 1.439(2) . ?
C31 H31 0.9300 . ?
C31 C32 1.394(2) . ?
O32 C38 1.205(2) . ?
C32 C33 1.397(2) . ?
C32 C36 1.489(2) . ?
O33 C38 1.337(2) . ?
O33 C39 1.451(2) . ?
C33 H33 0.9300 . ?
C33 C34 1.389(2) . ?
C34 C35 1.387(2) . ?
C34 C38 1.497(2) . ?
C35 H35 0.9300 . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?
C39 H39A 0.9600 . ?
C39 H39B 0.9600 . ?
C39 H39C 0.9600 . ?
S40 P40 1.9595(6) . ?
C40 H40A 0.9600 . ?
C40 H40B 0.9600 . ?
C40 H40C 0.9600 . ?
C40 P40 1.8107(17) . ?
P40 C41 1.8079(18) . ?
C41 H41A 0.9600 . ?
C41 H41B 0.9600 . ?
C41 H41C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C11 C10 C15 118.06(14) . . ?
C11 C10 P40 119.93(11) . . ?
C15 C10 P40 121.97(12) . . ?
C10 C11 C20 124.17(14) . . ?
C12 C11 C10 120.52(14) . . ?
C12 C11 C20 115.31(14) . . ?
C11 C12 H12 119.7 . . ?
C13 C12 C11 120.70(15) . . ?
C13 C12 H12 119.7 . . ?
C12 C13 H13 120.3 . . ?
C14 C13 C12 119.31(15) . . ?
C14 C13 H13 120.3 . . ?
C13 C14 H14 119.2 . . ?
C13 C14 C15 121.53(15) . . ?
C15 C14 H14 119.2 . . ?
C10 C15 C30 125.82(14) . . ?
C14 C15 C10 119.80(14) . . ?
C14 C15 C30 114.36(14) . . ?
C21 C20 C11 122.50(14) . . ?
C25 C20 C11 118.49(14) . . ?
C25 C20 C21 118.91(14) . . ?
C20 C21 H21 119.8 . . ?
C20 C21 C22 120.39(15) . . ?
C22 C21 H21 119.8 . . ?
C26 O21 C27 115.33(13) . . ?
C21 C22 C26 121.24(15) . . ?
C23 C22 C21 120.28(14) . . ?
C23 C22 C26 118.46(14) . . ?
C22 C23 H23 120.3 . . ?
C24 C23 C22 119.49(14) . . ?
C24 C23 H23 120.3 . . ?
C28 O23 C29 113.22(14) . . ?
C23 C24 C25 119.84(15) . . ?
C23 C24 C28 124.21(15) . . ?
C25 C24 C28 115.92(14) . . ?
C20 C25 C24 121.06(15) . . ?
C20 C25 H25 119.5 . . ?
C24 C25 H25 119.5 . . ?
O20 C26 O21 123.71(15) . . ?
O20 C26 C22 124.22(15) . . ?
O21 C26 C22 112.06(13) . . ?
O21 C27 H27A 109.5 . . ?
O21 C27 H27B 109.5 . . ?
O21 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
O22 C28 O23 123.65(16) . . ?
O22 C28 C24 123.50(15) . . ?
O23 C28 C24 112.83(14) . . ?
O23 C29 H29A 109.5 . . ?
O23 C29 H29B 109.5 . . ?
O23 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C31 C30 C15 122.70(14) . . ?
C31 C30 C35 118.62(15) . . ?
C35 C30 C15 118.33(14) . . ?
C36 O31 C37 114.45(14) . . ?
C30 C31 H31 119.9 . . ?
C30 C31 C32 120.25(15) . . ?
C32 C31 H31 119.9 . . ?
C31 C32 C33 120.59(15) . . ?
C31 C32 C36 122.27(15) . . ?
C33 C32 C36 117.08(15) . . ?
C38 O33 C39 114.97(14) . . ?
C32 C33 H33 120.4 . . ?
C34 C33 C32 119.24(15) . . ?
C34 C33 H33 120.4 . . ?
C33 C34 C38 122.75(15) . . ?
C35 C34 C33 119.93(15) . . ?
C35 C34 C38 117.27(15) . . ?
C30 C35 H35 119.3 . . ?
C34 C35 C30 121.30(15) . . ?
C34 C35 H35 119.3 . . ?
O30 C36 O31 123.39(16) . . ?
O30 C36 C32 124.37(16) . . ?
O31 C36 C32 112.24(14) . . ?
O31 C37 H37A 109.5 . . ?
O31 C37 H37B 109.5 . . ?
O31 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
O32 C38 O33 124.08(15) . . ?
O32 C38 C34 123.63(16) . . ?
O33 C38 C34 112.28(15) . . ?
O33 C39 H39A 109.5 . . ?
O33 C39 H39B 109.5 . . ?
O33 C39 H39C 109.5 . . ?
H39A C39 H39B 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
P40 C40 H40A 109.5 . . ?
P40 C40 H40B 109.5 . . ?
P40 C40 H40C 109.5 . . ?
C10 P40 S40 112.02(5) . . ?
C40 P40 C10 109.53(7) . . ?
C40 P40 S40 113.18(6) . . ?
C41 P40 C10 108.19(8) . . ?
C41 P40 S40 113.55(6) . . ?
C41 P40 C40 99.62(8) . . ?
P40 C41 H41A 109.5 . . ?
P40 C41 H41B 109.5 . . ?
P40 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 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
C10 C11 C12 C13 -1.6(2) . . . . ?
C10 C11 C20 C21 65.9(2) . . . . ?
C10 C11 C20 C25 -117.85(17) . . . . ?
C10 C15 C30 C31 -66.2(2) . . . . ?
C10 C15 C30 C35 120.69(17) . . . . ?
C11 C10 C15 C14 -2.8(2) . . . . ?
C11 C10 C15 C30 175.52(14) . . . . ?
C11 C10 P40 S40 -86.55(12) . . . . ?
C11 C10 P40 C40 147.01(13) . . . . ?
C11 C10 P40 C41 39.36(14) . . . . ?
C11 C12 C13 C14 -0.8(2) . . . . ?
C11 C20 C21 C22 178.26(14) . . . . ?
C11 C20 C25 C24 -177.86(14) . . . . ?
C12 C11 C20 C21 -114.10(17) . . . . ?
C12 C11 C20 C25 62.1(2) . . . . ?
C12 C13 C14 C15 1.5(3) . . . . ?
C13 C14 C15 C10 0.4(2) . . . . ?
C13 C14 C15 C30 -178.11(15) . . . . ?
C14 C15 C30 C31 112.24(17) . . . . ?
C14 C15 C30 C35 -60.92(19) . . . . ?
C15 C10 C11 C12 3.4(2) . . . . ?
C15 C10 C11 C20 -176.59(14) . . . . ?
C15 C10 P40 S40 95.89(13) . . . . ?
C15 C10 P40 C40 -30.55(15) . . . . ?
C15 C10 P40 C41 -138.20(13) . . . . ?
C15 C30 C31 C32 -173.10(15) . . . . ?
C15 C30 C35 C34 175.52(14) . . . . ?
C20 C11 C12 C13 178.37(15) . . . . ?
C20 C21 C22 C23 -1.2(2) . . . . ?
C20 C21 C22 C26 -179.23(14) . . . . ?
C21 C20 C25 C24 -1.5(2) . . . . ?
C21 C22 C23 C24 -0.2(2) . . . . ?
C21 C22 C26 O20 -178.65(16) . . . . ?
C21 C22 C26 O21 2.2(2) . . . . ?
C22 C23 C24 C25 0.8(2) . . . . ?
C22 C23 C24 C28 -177.38(15) . . . . ?
C23 C22 C26 O20 3.3(2) . . . . ?
C23 C22 C26 O21 -175.84(14) . . . . ?
C23 C24 C25 C20 0.1(2) . . . . ?
C23 C24 C28 O22 -172.99(17) . . . . ?
C23 C24 C28 O23 8.7(2) . . . . ?
C25 C20 C21 C22 2.0(2) . . . . ?
C25 C24 C28 O22 8.8(3) . . . . ?
C25 C24 C28 O23 -169.53(15) . . . . ?
C26 C22 C23 C24 177.86(14) . . . . ?
C27 O21 C26 O20 1.2(2) . . . . ?
C27 O21 C26 C22 -179.68(14) . . . . ?
C28 C24 C25 C20 178.40(15) . . . . ?
C29 O23 C28 O22 1.6(3) . . . . ?
C29 O23 C28 C24 179.90(16) . . . . ?
C30 C31 C32 C33 -1.5(2) . . . . ?
C30 C31 C32 C36 175.73(15) . . . . ?
C31 C30 C35 C34 2.1(2) . . . . ?
C31 C32 C33 C34 0.8(2) . . . . ?
C31 C32 C36 O30 -178.92(17) . . . . ?
C31 C32 C36 O31 1.5(2) . . . . ?
C32 C33 C34 C35 1.3(2) . . . . ?
C32 C33 C34 C38 178.75(15) . . . . ?
C33 C32 C36 O30 -1.6(3) . . . . ?
C33 C32 C36 O31 178.76(14) . . . . ?
C33 C34 C35 C30 -2.8(2) . . . . ?
C33 C34 C38 O32 -174.46(17) . . . . ?
C33 C34 C38 O33 5.9(2) . . . . ?
C35 C30 C31 C32 0.0(2) . . . . ?
C35 C34 C38 O32 3.1(3) . . . . ?
C35 C34 C38 O33 -176.54(15) . . . . ?
C36 C32 C33 C34 -176.52(15) . . . . ?
C37 O31 C36 O30 2.0(3) . . . . ?
C37 O31 C36 C32 -178.34(15) . . . . ?
C38 C34 C35 C30 179.62(14) . . . . ?
C39 O33 C38 O32 1.1(3) . . . . ?
C39 O33 C38 C34 -179.26(15) . . . . ?
P40 C10 C11 C12 -174.23(12) . . . . ?
P40 C10 C11 C20 5.8(2) . . . . ?
P40 C10 C15 C14 174.81(12) . . . . ?
P40 C10 C15 C30 -6.9(2) . . . . ?

_olex2_date_sample_data_collection 2019-08-30
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.603
_oxdiff_exptl_absorpt_empirical_full_min 0.721
####################################################################### 
# 
# 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_3dmonoclinic
_database_code_depnum_ccdc_archive 'CCDC 1942986'
loop_
_audit_author_name
_audit_author_address
'Timo Stein'
;University of Hamburg
Germany
;
_audit_update_record             
;
2019-09-04 deposited with the CCDC.	2019-09-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H31 O9 P'
_chemical_formula_weight         662.60

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   36.1084(4)
_cell_length_b                   12.08210(10)
_cell_length_c                   15.1558(2)
_cell_angle_alpha                90
_cell_angle_beta                 99.4400(10)
_cell_angle_gamma                90
_cell_volume                     6522.41(13)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    28734
_cell_measurement_theta_min      3.8440
_cell_measurement_theta_max      76.4130
_cell_oxdiff_length_a            36.1015(7)
_cell_oxdiff_length_b            12.0845(2)
_cell_oxdiff_length_c            15.1557(3)
_cell_oxdiff_angle_alpha         89.9404(15)
_cell_oxdiff_angle_beta          99.4413(16)
_cell_oxdiff_angle_gamma         89.9949(15)
_cell_oxdiff_volume              6522.4(2)
_cell_oxdiff_measurement_reflns_used 28834

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.350
_exptl_crystal_F_000             2768
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_exptl_absorpt_coefficient_mu    1.233
_shelx_estimated_absorpt_T_min   0.724
_shelx_estimated_absorpt_T_max   0.964
_exptl_absorpt_correction_T_min  0.75542
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.42b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.178
_oxdiff_exptl_absorpt_empirical_full_max 1.490
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_ambient_environment      N~2~
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Atlas
_diffrn_detector_area_resol_mean 10.4127
_diffrn_reflns_number            66459
_diffrn_reflns_av_unetI/netI     0.0227
_diffrn_reflns_av_R_equivalents  0.0596
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.863
_diffrn_reflns_theta_max         72.484
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0265707000
_diffrn_orient_matrix_UB_12      -0.1005188000
_diffrn_orient_matrix_UB_13      0.0138784000
_diffrn_orient_matrix_UB_21      0.0181646000
_diffrn_orient_matrix_UB_22      0.0370187000
_diffrn_orient_matrix_UB_23      -0.0803400000
_diffrn_orient_matrix_UB_31      0.0289076000
_diffrn_orient_matrix_UB_32      0.0691201000
_diffrn_orient_matrix_UB_33      0.0630176000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -50.00  15.00   1.00    3.50    --  -42.10  38.00-120.00   65
  2  ω    -50.00 -14.00   1.00    3.50    --  -42.10 -57.00-150.00   36
  3  ω    -50.00 -10.00   1.00    3.50    --  -42.10 -77.00 -90.00   40
  4  ω    -71.00 -10.00   1.00    3.50    --  -42.10 -77.00-180.00   61
  5  ω    -75.00 -14.00   1.00    3.50    --  -42.10 -57.00   0.00   61
  6  ω      1.00  69.00   1.00    3.50    --   42.10 -99.00 120.00   68
  7  ω      3.00  49.00   1.00    3.50    --   42.10 -99.00  60.00   46
  8  ω      1.00  44.00   1.00    3.50    --   42.10 -99.00   0.00   43
  9  ω     37.00  83.00   1.00   14.00    --  112.00-111.00   0.00   46
 10  ω     77.00 114.00   1.00   14.00    --  112.00-111.00  30.00   37
 11  ω    110.00 145.00   1.00   14.00    --  112.00 -77.00   0.00   35
 12  ω     91.00 116.00   1.00   14.00    --  112.00-111.00 120.00   25
 13  ω     37.00  72.00   1.00   14.00    --  112.00-111.00 120.00   35
 14  ω     37.00 114.00   1.00   14.00    --  112.00-111.00  90.00   77
 15  ω     50.00 116.00   1.00   14.00    --  112.00-111.00 -30.00   66
 16  ω     87.00 116.00   1.00   14.00    --  112.00-111.00 -90.00   29
 17  ω     53.00 139.00   1.00   14.00    --  112.00 -61.00-180.00   86
 18  ω     82.00 114.00   1.00   14.00    --  112.00  64.00 -51.62   32
 19  ω    122.00 178.00   1.00   14.00    --  112.00  77.00 -60.00   56
 20  ω    146.00 173.00   1.00   14.00    --  112.00  77.00   0.00   27
 21  ω    141.00 168.00   1.00   14.00    --  112.00  61.00   7.16   27
 22  ω    134.00 160.00   1.00   14.00    --  112.00  62.00  43.04   26
 23  ω    113.00 176.00   1.00   14.00    --  112.00  77.00  30.00   63
 24  ω    121.00 176.00   1.00   14.00    --  112.00  73.00 -72.45   55
 25  ω    131.00 177.00   1.00   14.00    --  112.00  77.00-120.00   46
 26  ω    114.00 166.00   1.00   14.00    --  112.00  73.00-149.49   52
 27  ω    110.00 176.00   1.00   14.00    --  112.00  77.00-180.00   66
 28  ω     80.00 106.00   1.00   14.00    --  112.00  73.00 -72.45   26
 29  ω     79.00 174.00   1.00   14.00    --  112.00  77.00 -30.00   95
 30  ω    115.00 141.00   1.00   14.00    --  112.00  77.00  60.00   26
 31  ω    109.00 178.00   1.00   14.00    --  112.00  77.00 150.00   69
 32  ω    127.00 163.00   1.00   14.00    --  112.00  60.00 164.26   36
 33  ω     80.00 106.00   1.00   14.00    --  112.00  76.00  49.26   26
 34  ω     79.00 126.00   1.00   14.00    --  112.00  77.00  90.00   47
 35  ω     82.00 173.00   1.00   14.00    --  112.00  67.00 123.37   91
 36  ω     83.00 178.00   1.00   14.00    --  112.00  61.00  60.00   95
 37  ω     83.00 175.00   1.00   14.00    --  112.00  61.00  90.00   92
 38  ω     83.00 120.00   1.00   14.00    --  112.00  61.00 120.00   37
 39  ω     79.00 104.00   1.00   14.00    --  112.00  77.00 150.00   25
 40  ω     83.00 109.00   1.00   14.00    --  112.00  60.00 164.26   26
 41  ω     83.00 145.00   1.00   14.00    --  112.00  61.00 150.00   62
 42  ω     79.00 106.00   1.00   14.00    --  112.00  77.00  30.00   27
 43  ω     79.00 105.00   1.00   14.00    --  112.00  77.00   0.00   26
 44  ω     83.00 165.00   1.00   14.00    --  112.00  61.00   0.00   82
 45  ω     80.00 111.00   1.00   14.00    --  112.00  73.00-149.49   31
 46  ω     83.00 109.00   1.00   14.00    --  112.00  61.00-150.00   26
 47  ω     83.00 149.00   1.00   14.00    --  112.00  61.00-120.00   66
 48  ω     83.00 159.00   1.00   14.00    --  112.00  61.00 -90.00   76
 49  ω     80.00 105.00   1.00   14.00    --  112.00  76.00 -43.98   25
 50  ω     83.00 115.00   1.00   14.00    --  112.00  61.00 -30.00   32
 51  ω     83.00 129.00   1.00   14.00    --  112.00  61.00  30.00   46
 52  ω     79.00 106.00   1.00   14.00    --  112.00  77.00 -60.00   27
 53  ω     82.00 108.00   1.00   14.00    --  112.00  64.00 -77.00   26
 54  ω     79.00 105.00   1.00   14.00    --  112.00  77.00-120.00   26
 55  ω     80.00 107.00   1.00   14.00    --  112.00  77.00-150.00   27
 56  ω     83.00 109.00   1.00   14.00    --  112.00  61.00-180.00   26
 57  ω     79.00 105.00   1.00   14.00    --  112.00  77.00-180.00   26
 58  ω     83.00 109.00   1.00   14.00    --  112.00  61.00   7.16   26
 59  ω     83.00 109.00   1.00   14.00    --  112.00  62.00  43.04   26
 60  ω     79.00 105.00   1.00   14.00    --  112.00  77.00  60.00   26
 61  ω     79.00 105.00   1.00   14.00    --  112.00  77.00 120.00   26
 62  ω     81.00 112.00   1.00   14.00    --  112.00  70.00 178.61   31
 63  ω      7.00  33.00   1.00    3.50    --   42.10  86.00  60.00   26
 64  ω     37.00  91.00   1.00   14.00    --  112.00 -77.00   0.00   54
 65  ω     41.00  66.00   1.00   14.00    --  112.00-111.00 -90.00   25
 66  ω     40.00 112.00   1.00   14.00    --  112.00-111.00-150.00   72
 67  ω     33.00  96.00   1.00   14.00    --  112.00 -94.00 150.00   63
 68  ω    -95.00  -2.00   1.00    3.50    --  -42.10 125.00-150.00   93
 69  ω   -114.00 -88.00   1.00    3.50    --  -42.10 -57.00-150.00   26
 70  ω   -118.00 -79.00   1.00    3.50    --  -42.10 -77.00 -90.00   39
 71  ω   -118.00 -10.00   1.00    3.50    --  -42.10 -77.00 -30.00  108
 72  ω   -103.00 -10.00   1.00    3.50    --  -42.10 -77.00  90.00   93
 73  ω   -116.00 -18.00   1.00    3.50    --  -42.10 -38.00 120.00   98
;
_diffrn_measurement_method       'ω scans'
_reflns_number_total             6465
_reflns_number_gt                5841
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_theta     74.33
_reflns_odcompleteness_iscentric 1
_computing_data_collection       'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_computing_structure_solution    'SUPERFLIP (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0529P)²+6.5889P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6465
_refine_ls_number_parameters     437
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_gt           0.0381
_refine_ls_wR_factor_ref         0.0980
_refine_ls_wR_factor_gt          0.0937
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.029
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C10 C 0.60534(3) 0.46070(10) 0.43044(8) 0.0120(2) Uani 1 1 d . . . . .
C11 C 0.62389(3) 0.56219(10) 0.42079(8) 0.0134(2) Uani 1 1 d . . . . .
C12 C 0.60894(4) 0.63411(10) 0.35166(9) 0.0155(3) Uani 1 1 d . . . . .
H12 H 0.621032 0.702970 0.345971 0.019 Uiso 1 1 calc R U . . .
C13 C 0.57712(4) 0.60790(11) 0.29141(9) 0.0157(3) Uani 1 1 d . . . . .
H13 H 0.566599 0.659967 0.247357 0.019 Uiso 1 1 calc R U . . .
C14 C 0.56074(4) 0.50478(11) 0.29602(9) 0.0150(2) Uani 1 1 d . . . . .
H14 H 0.539824 0.484443 0.252495 0.018 Uiso 1 1 calc R U . . .
C15 C 0.57462(3) 0.43069(10) 0.36373(8) 0.0127(2) Uani 1 1 d . . . . .
O20 O 0.78147(3) 0.51488(11) 0.64220(11) 0.0474(4) Uani 1 1 d . . . . .
C20 C 0.65956(3) 0.59816(11) 0.47720(8) 0.0135(2) Uani 1 1 d . . . . .
O21 O 0.74562(3) 0.38040(9) 0.57172(8) 0.0274(2) Uani 1 1 d . . . . .
C21 C 0.68913(4) 0.52531(11) 0.50506(9) 0.0147(2) Uani 1 1 d . . . . .
H21 H 0.686812 0.449597 0.488137 0.018 Uiso 1 1 calc R U . . .
O22 O 0.73158(4) 0.90469(10) 0.61604(10) 0.0442(4) Uani 1 1 d . . . . .
C22 C 0.72213(4) 0.56291(11) 0.55767(9) 0.0178(3) Uani 1 1 d . . . . .
O23 O 0.67332(3) 0.92894(8) 0.54333(8) 0.0263(2) Uani 1 1 d . . . . .
C23 C 0.72645(4) 0.67436(12) 0.58004(10) 0.0199(3) Uani 1 1 d . . . . .
H23 H 0.749062 0.699917 0.615122 0.024 Uiso 1 1 calc R U . . .
C24 C 0.69754(4) 0.74802(11) 0.55084(9) 0.0166(3) Uani 1 1 d . . . . .
C25 C 0.66423(4) 0.70981(11) 0.50078(9) 0.0147(3) Uani 1 1 d . . . . .
H25 H 0.644327 0.760404 0.482310 0.018 Uiso 1 1 calc R U . . .
C26 C 0.75304(4) 0.48594(13) 0.59501(11) 0.0247(3) Uani 1 1 d . . . . .
C27 C 0.77263(5) 0.30019(15) 0.61428(14) 0.0394(4) Uani 1 1 d . . . . .
H27A H 0.796954 0.313102 0.595370 0.059 Uiso 1 1 calc R U . . .
H27B H 0.763870 0.225331 0.596857 0.059 Uiso 1 1 calc R U . . .
H27C H 0.775335 0.307885 0.679392 0.059 Uiso 1 1 calc R U . . .
C28 C 0.70311(4) 0.86730(12) 0.57501(10) 0.0212(3) Uani 1 1 d . . . . .
C29 C 0.67747(5) 1.04629(13) 0.56157(14) 0.0366(4) Uani 1 1 d . . . . .
H29A H 0.679440 1.059094 0.626028 0.055 Uiso 1 1 calc R U . . .
H29B H 0.655556 1.085788 0.529827 0.055 Uiso 1 1 calc R U . . .
H29C H 0.700214 1.073432 0.541220 0.055 Uiso 1 1 calc R U . . .
O30 O 0.56644(3) -0.07579(8) 0.34440(8) 0.0288(3) Uani 1 1 d . . . . .
C30 C 0.55613(4) 0.31988(10) 0.36056(8) 0.0131(2) Uani 1 1 d . . . . .
O31 O 0.61103(3) 0.03517(8) 0.30609(7) 0.0197(2) Uani 1 1 d . . . . .
C31 C 0.57564(4) 0.22322(11) 0.34779(8) 0.0139(2) Uani 1 1 d . . . . .
H31 H 0.601216 0.227236 0.340281 0.017 Uiso 1 1 calc R U . . .
O32 O 0.44369(3) 0.29234(8) 0.39639(8) 0.0247(2) Uani 1 1 d . . . . .
C32 C 0.55782(4) 0.12057(10) 0.34599(9) 0.0145(3) Uani 1 1 d . . . . .
O33 O 0.44725(3) 0.10737(8) 0.38974(8) 0.0227(2) Uani 1 1 d . . . . .
C33 C 0.52052(4) 0.11316(11) 0.35831(9) 0.0155(3) Uani 1 1 d . . . . .
H33 H 0.508733 0.042973 0.359289 0.019 Uiso 1 1 calc R U . . .
C34 C 0.50068(4) 0.20959(11) 0.36916(8) 0.0143(3) Uani 1 1 d . . . . .
C35 C 0.51818(4) 0.31210(10) 0.36796(8) 0.0134(2) Uani 1 1 d . . . . .
H35 H 0.504093 0.377733 0.372226 0.016 Uiso 1 1 calc R U . . .
C36 C 0.57807(4) 0.01580(11) 0.33268(9) 0.0165(3) Uani 1 1 d . . . . .
C37 C 0.63300(4) -0.06174(12) 0.29385(11) 0.0233(3) Uani 1 1 d . . . . .
H37A H 0.640291 -0.099204 0.351430 0.035 Uiso 1 1 calc R U . . .
H37B H 0.655577 -0.039608 0.270214 0.035 Uiso 1 1 calc R U . . .
H37C H 0.618040 -0.112225 0.251591 0.035 Uiso 1 1 calc R U . . .
C38 C 0.46120(4) 0.20944(11) 0.38596(9) 0.0161(3) Uani 1 1 d . . . . .
C39 C 0.40983(4) 0.10311(13) 0.41239(12) 0.0277(3) Uani 1 1 d . . . . .
H39A H 0.410552 0.129185 0.473878 0.042 Uiso 1 1 calc R U . . .
H39B H 0.400593 0.026722 0.407299 0.042 Uiso 1 1 calc R U . . .
H39C H 0.393014 0.150531 0.371311 0.042 Uiso 1 1 calc R U . . .
P40 P 0.61688(2) 0.36620(2) 0.52529(2) 0.01160(9) Uani 1 1 d . . . . .
O40 O 0.63906(3) 0.26814(8) 0.50541(6) 0.0178(2) Uani 1 1 d . . . . .
C40 C 0.63977(4) 0.43851(11) 0.62361(9) 0.0155(3) Uani 1 1 d . . . . .
C41 C 0.66996(4) 0.38365(13) 0.67440(10) 0.0224(3) Uani 1 1 d . . . . .
H41 H 0.677040 0.312217 0.656940 0.027 Uiso 1 1 calc R U . . .
C42 C 0.68970(4) 0.43345(16) 0.75057(10) 0.0322(4) Uani 1 1 d . . . . .
H42 H 0.710197 0.396052 0.785426 0.039 Uiso 1 1 calc R U . . .
C43 C 0.67938(5) 0.53754(16) 0.77531(10) 0.0353(4) Uani 1 1 d . . . . .
H43 H 0.693332 0.572562 0.826301 0.042 Uiso 1 1 calc R U . . .
C44 C 0.64872(5) 0.59157(14) 0.72621(10) 0.0289(3) Uani 1 1 d . . . . .
H44 H 0.641530 0.662546 0.744424 0.035 Uiso 1 1 calc R U . . .
C45 C 0.62862(4) 0.54186(12) 0.65062(9) 0.0193(3) Uani 1 1 d . . . . .
H45 H 0.607416 0.578029 0.617530 0.023 Uiso 1 1 calc R U . . .
C46 C 0.57211(4) 0.32833(10) 0.55629(8) 0.0131(2) Uani 1 1 d . . . . .
C47 C 0.56701(4) 0.21703(11) 0.57600(9) 0.0173(3) Uani 1 1 d . . . . .
H47 H 0.586209 0.164919 0.570536 0.021 Uiso 1 1 calc R U . . .
C48 C 0.53408(4) 0.18189(12) 0.60354(10) 0.0217(3) Uani 1 1 d . . . . .
H48 H 0.530956 0.106158 0.617499 0.026 Uiso 1 1 calc R U . . .
C49 C 0.50571(4) 0.25749(12) 0.61068(9) 0.0203(3) Uani 1 1 d . . . . .
H49 H 0.483068 0.233536 0.628898 0.024 Uiso 1 1 calc R U . . .
C50 C 0.51067(4) 0.36870(11) 0.59096(9) 0.0168(3) Uani 1 1 d . . . . .
H50 H 0.491230 0.420354 0.595419 0.020 Uiso 1 1 calc R U . . .
C51 C 0.54383(4) 0.40470(11) 0.56482(8) 0.0142(2) Uani 1 1 d . . . . .
H51 H 0.547237 0.480870 0.552819 0.017 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C10 C11 1.4162(17) . ?
C10 C15 1.4198(17) . ?
C10 P40 1.8296(12) . ?
C11 C12 1.3995(18) . ?
C11 C20 1.4893(17) . ?
C12 C13 1.3821(19) . ?
C12 H12 0.9500 . ?
C13 C14 1.3859(18) . ?
C13 H13 0.9500 . ?
C14 C15 1.3917(18) . ?
C14 H14 0.9500 . ?
C15 C30 1.4932(17) . ?
O20 C26 1.203(2) . ?
C20 C21 1.3947(18) . ?
C20 C25 1.3987(18) . ?
O21 C26 1.3384(19) . ?
O21 C27 1.4491(18) . ?
C21 C22 1.3965(18) . ?
C21 H21 0.9500 . ?
O22 C28 1.1993(19) . ?
C22 C23 1.391(2) . ?
C22 C26 1.4912(19) . ?
O23 C28 1.3313(18) . ?
O23 C29 1.4476(17) . ?
C23 C24 1.3878(19) . ?
C23 H23 0.9500 . ?
C24 C25 1.3913(18) . ?
C24 C28 1.4924(18) . ?
C25 H25 0.9500 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
O30 C36 1.2070(17) . ?
C30 C31 1.3937(18) . ?
C30 C35 1.3964(18) . ?
O31 C36 1.3383(16) . ?
O31 C37 1.4432(16) . ?
C31 C32 1.3954(17) . ?
C31 H31 0.9500 . ?
O32 C38 1.2087(17) . ?
C32 C33 1.3928(18) . ?
C32 C36 1.4919(18) . ?
O33 C38 1.3370(16) . ?
O33 C39 1.4486(16) . ?
C33 C34 1.3915(18) . ?
C33 H33 0.9500 . ?
C34 C35 1.3918(17) . ?
C34 C38 1.4885(18) . ?
C35 H35 0.9500 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
P40 O40 1.4884(9) . ?
P40 C40 1.8063(13) . ?
P40 C46 1.8144(13) . ?
C40 C45 1.394(2) . ?
C40 C41 1.3947(19) . ?
C41 C42 1.390(2) . ?
C41 H41 0.9500 . ?
C42 C43 1.381(3) . ?
C42 H42 0.9500 . ?
C43 C44 1.391(3) . ?
C43 H43 0.9500 . ?
C44 C45 1.388(2) . ?
C44 H44 0.9500 . ?
C45 H45 0.9500 . ?
C46 C47 1.3962(18) . ?
C46 C51 1.3980(18) . ?
C47 C48 1.390(2) . ?
C47 H47 0.9500 . ?
C48 C49 1.390(2) . ?
C48 H48 0.9500 . ?
C49 C50 1.394(2) . ?
C49 H49 0.9500 . ?
C50 C51 1.3911(18) . ?
C50 H50 0.9500 . ?
C51 H51 0.9500 . ?

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
C11 C10 C15 118.36(11) . . ?
C11 C10 P40 124.81(9) . . ?
C15 C10 P40 116.79(9) . . ?
C12 C11 C10 118.95(11) . . ?
C12 C11 C20 116.07(11) . . ?
C10 C11 C20 124.93(11) . . ?
C13 C12 C11 121.94(12) . . ?
C13 C12 H12 119.0 . . ?
C11 C12 H12 119.0 . . ?
C12 C13 C14 119.21(12) . . ?
C12 C13 H13 120.4 . . ?
C14 C13 H13 120.4 . . ?
C13 C14 C15 120.69(12) . . ?
C13 C14 H14 119.7 . . ?
C15 C14 H14 119.7 . . ?
C14 C15 C10 120.37(11) . . ?
C14 C15 C30 116.61(11) . . ?
C10 C15 C30 123.01(11) . . ?
C21 C20 C25 118.50(12) . . ?
C21 C20 C11 122.47(11) . . ?
C25 C20 C11 119.00(11) . . ?
C26 O21 C27 115.39(13) . . ?
C20 C21 C22 120.44(12) . . ?
C20 C21 H21 119.8 . . ?
C22 C21 H21 119.8 . . ?
C23 C22 C21 120.34(12) . . ?
C23 C22 C26 117.66(12) . . ?
C21 C22 C26 121.95(13) . . ?
C28 O23 C29 115.28(12) . . ?
C24 C23 C22 119.65(12) . . ?
C24 C23 H23 120.2 . . ?
C22 C23 H23 120.2 . . ?
C23 C24 C25 119.92(12) . . ?
C23 C24 C28 118.48(12) . . ?
C25 C24 C28 121.59(12) . . ?
C24 C25 C20 121.10(12) . . ?
C24 C25 H25 119.4 . . ?
C20 C25 H25 119.4 . . ?
O20 C26 O21 123.24(14) . . ?
O20 C26 C22 123.85(14) . . ?
O21 C26 C22 112.90(12) . . ?
O21 C27 H27A 109.5 . . ?
O21 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
O21 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
O22 C28 O23 123.33(13) . . ?
O22 C28 C24 124.09(14) . . ?
O23 C28 C24 112.54(12) . . ?
O23 C29 H29A 109.5 . . ?
O23 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
O23 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C31 C30 C35 118.67(11) . . ?
C31 C30 C15 121.49(11) . . ?
C35 C30 C15 119.82(11) . . ?
C36 O31 C37 115.57(10) . . ?
C30 C31 C32 120.37(12) . . ?
C30 C31 H31 119.8 . . ?
C32 C31 H31 119.8 . . ?
C33 C32 C31 120.50(12) . . ?
C33 C32 C36 118.01(11) . . ?
C31 C32 C36 121.48(12) . . ?
C38 O33 C39 114.57(11) . . ?
C34 C33 C32 119.34(12) . . ?
C34 C33 H33 120.3 . . ?
C32 C33 H33 120.3 . . ?
C33 C34 C35 120.00(12) . . ?
C33 C34 C38 123.03(11) . . ?
C35 C34 C38 116.93(11) . . ?
C34 C35 C30 120.97(12) . . ?
C34 C35 H35 119.5 . . ?
C30 C35 H35 119.5 . . ?
O30 C36 O31 123.55(12) . . ?
O30 C36 C32 124.61(12) . . ?
O31 C36 C32 111.84(11) . . ?
O31 C37 H37A 109.5 . . ?
O31 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
O31 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
O32 C38 O33 123.35(12) . . ?
O32 C38 C34 123.89(12) . . ?
O33 C38 C34 112.75(11) . . ?
O33 C39 H39A 109.5 . . ?
O33 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
O33 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
O40 P40 C40 111.31(6) . . ?
O40 P40 C46 112.56(6) . . ?
C40 P40 C46 102.41(6) . . ?
O40 P40 C10 113.48(6) . . ?
C40 P40 C10 111.15(6) . . ?
C46 P40 C10 105.25(6) . . ?
C45 C40 C41 120.06(13) . . ?
C45 C40 P40 124.08(10) . . ?
C41 C40 P40 115.85(11) . . ?
C42 C41 C40 120.04(15) . . ?
C42 C41 H41 120.0 . . ?
C40 C41 H41 120.0 . . ?
C43 C42 C41 119.67(15) . . ?
C43 C42 H42 120.2 . . ?
C41 C42 H42 120.2 . . ?
C42 C43 C44 120.58(14) . . ?
C42 C43 H43 119.7 . . ?
C44 C43 H43 119.7 . . ?
C45 C44 C43 120.06(15) . . ?
C45 C44 H44 120.0 . . ?
C43 C44 H44 120.0 . . ?
C44 C45 C40 119.52(14) . . ?
C44 C45 H45 120.2 . . ?
C40 C45 H45 120.2 . . ?
C47 C46 C51 119.47(12) . . ?
C47 C46 P40 116.91(10) . . ?
C51 C46 P40 123.56(10) . . ?
C48 C47 C46 120.52(13) . . ?
C48 C47 H47 119.7 . . ?
C46 C47 H47 119.7 . . ?
C49 C48 C47 120.03(13) . . ?
C49 C48 H48 120.0 . . ?
C47 C48 H48 120.0 . . ?
C48 C49 C50 119.63(13) . . ?
C48 C49 H49 120.2 . . ?
C50 C49 H49 120.2 . . ?
C51 C50 C49 120.61(13) . . ?
C51 C50 H50 119.7 . . ?
C49 C50 H50 119.7 . . ?
C50 C51 C46 119.73(12) . . ?
C50 C51 H51 120.1 . . ?
C46 C51 H51 120.1 . . ?

_refine_diff_density_max         0.382
_refine_diff_density_min         -0.496
_refine_diff_density_rms         0.051

