# Electronic Supplementary Material (ESI) for Chemical Science.
# 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. 
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data_exp_2558
_database_code_depnum_ccdc_archive 'CCDC 1872113'
_audit_update_record             
;
2018-10-09 deposited with the CCDC.
2019-01-17 downloaded from the CCDC.
;
_audit_creation_date             2018-04-18
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.04.03 svn.r3497 for OlexSys, GUI svn.r5486)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C35 H27 O P Sn'
_chemical_formula_sum            'C35 H27 O P Sn'
_chemical_formula_weight         613.22
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 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'
Sn Sn 0.0259 5.4591 '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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   9.93270(10)
_cell_length_b                   18.4467(3)
_cell_length_c                   15.8535(2)
_cell_angle_alpha                90
_cell_angle_beta                 104.801(2)
_cell_angle_gamma                90
_cell_volume                     2808.38(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6399
_cell_measurement_temperature    149.93(15)
_cell_measurement_theta_max      74.1950
_cell_measurement_theta_min      3.7330
_shelx_estimated_absorpt_T_max   0.448
_shelx_estimated_absorpt_T_min   0.381
_exptl_absorpt_coefficient_mu    7.969
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60110
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.44a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear whiteish white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.450
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0213
_diffrn_reflns_av_unetI/netI     0.0266
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            10059
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.095
_diffrn_reflns_theta_min         3.749
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.93(15)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6525
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -66.00  26.00   1.00    1.00    --  -41.14  38.00-120.00   92
  2  ω   -113.00 -20.00   1.00    1.00    --  -41.14 -38.00  60.00   93
  3  ω     61.00 100.00   1.00    1.00    --   41.14 178.00   0.00   39
  4  ω     83.00 109.00   1.00    1.50    --  107.98  45.00  60.00   26
  5  ω     32.00 132.00   1.00    1.50    --  107.98 -30.00-120.00  100
  6  ω     36.00 123.00   1.00    1.50    --  107.98 -45.00  30.00   87
  7  ω     38.00  74.00   1.00    1.50    --  107.98 -95.00  30.00   36
  8  ω     99.00 138.00   1.00    1.50    --  107.98 125.00 -60.00   39
  9  ω    129.00 171.00   1.00    1.50    --  107.98  45.00  60.00   42
 10  ω     95.00 156.00   1.00    1.50    --  107.98  45.00 120.00   61
;
_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      0.1557678000
_diffrn_orient_matrix_UB_12      0.0186375000
_diffrn_orient_matrix_UB_13      0.0164539000
_diffrn_orient_matrix_UB_21      0.0182335000
_diffrn_orient_matrix_UB_22      -0.0626051000
_diffrn_orient_matrix_UB_23      -0.0604669000
_diffrn_orient_matrix_UB_31      -0.0338452000
_diffrn_orient_matrix_UB_32      0.0520542000
_diffrn_orient_matrix_UB_33      -0.0785526000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\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                5242
_reflns_number_total             5500
_reflns_odcompleteness_completeness 99.67
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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 1.171.39.44a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.44a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.44a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.676
_refine_diff_density_min         -0.706
_refine_diff_density_rms         0.095
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         5500
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0314
_refine_ls_R_factor_gt           0.0301
_refine_ls_restrained_S_all      1.050
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0550P)²+0.5750P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0788
_refine_ls_wR_factor_ref         0.0802
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C24(H24), C23(H23), C28(H28), C13(H13), C35(H35), C31(H31),
 C16(H16), C34(H34), C33(H33), C14(H14), C17(H17), C7(H7), C19(H19), C11(H11),
 C15(H15), C32(H32), C25(H25), C27(H27), C22(H22), C26(H26), C10(H10), C8(H8),
 C21(H21), C20(H20), C9(H9)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Sn1 Sn 0.85148(2) 0.20497(2) 0.31248(2) 0.01469(7) Uani 1 1 d . . . . .
P1 P 0.57377(5) 0.33986(3) 0.26419(4) 0.01797(12) Uani 1 1 d . . . . .
O1 O 0.84926(15) 0.31471(10) 0.32004(11) 0.0234(4) Uani 1 1 d . . . . .
C30 C 0.7543(2) 0.16814(12) 0.18455(13) 0.0170(4) Uani 1 1 d . . . . .
C6 C 0.3362(2) 0.42588(12) 0.23501(15) 0.0188(4) Uani 1 1 d . . . . .
C18 C 1.0726(2) 0.19829(11) 0.34941(15) 0.0164(4) Uani 1 1 d . . . . .
C2 C 0.7929(2) 0.43450(12) 0.33567(14) 0.0176(4) Uani 1 1 d . . . . .
H2 H 0.8877 0.4421 0.3588 0.021 Uiso 1 1 calc R . . . .
C4 C 0.5598(2) 0.48793(12) 0.29510(14) 0.0171(4) Uani 1 1 d . . . . .
H4 H 0.5065 0.5297 0.2919 0.021 Uiso 1 1 calc R . . . .
C1 C 0.7489(2) 0.36422(12) 0.30888(14) 0.0177(4) Uani 1 1 d . . . . .
C24 C 0.7775(3) 0.19345(13) 0.49052(16) 0.0219(5) Uani 1 1 d . . . . .
H24 H 0.8208 0.2384 0.5011 0.026 Uiso 1 1 calc R . . . .
C12 C 0.7604(2) 0.56544(12) 0.36542(14) 0.0175(4) Uani 1 1 d . . . . .
C3 C 0.7042(2) 0.49399(12) 0.33005(13) 0.0166(4) Uani 1 1 d . . . . .
C23 C 1.1529(2) 0.25804(13) 0.33842(15) 0.0210(4) Uani 1 1 d . . . . .
H23 H 1.1096 0.2990 0.3095 0.025 Uiso 1 1 calc R . . . .
C28 C 0.6975(3) 0.09281(13) 0.39544(16) 0.0247(5) Uani 1 1 d . . . . .
H28 H 0.6865 0.0699 0.3418 0.030 Uiso 1 1 calc R . . . .
C5 C 0.4913(2) 0.42370(12) 0.26501(13) 0.0163(4) Uani 1 1 d . . . . .
C13 C 0.8440(2) 0.57105(13) 0.45114(15) 0.0218(5) Uani 1 1 d . . . . .
H13 H 0.8719 0.5293 0.4839 0.026 Uiso 1 1 calc R . . . .
C35 C 0.8375(2) 0.14270(12) 0.13184(15) 0.0206(4) Uani 1 1 d . . . . .
H35 H 0.9340 0.1440 0.1520 0.025 Uiso 1 1 calc R . . . .
C31 C 0.6093(2) 0.16560(13) 0.15280(15) 0.0219(4) Uani 1 1 d . . . . .
H31 H 0.5531 0.1823 0.1875 0.026 Uiso 1 1 calc R . . . .
C16 C 0.7669(3) 0.69558(13) 0.35311(17) 0.0228(5) Uani 1 1 d . . . . .
H16 H 0.7429 0.7373 0.3197 0.027 Uiso 1 1 calc R . . . .
C34 C 0.7758(3) 0.11551(14) 0.04944(15) 0.0259(5) Uani 1 1 d . . . . .
H34 H 0.8315 0.0988 0.0145 0.031 Uiso 1 1 calc R . . . .
C33 C 0.6321(3) 0.11307(14) 0.01872(16) 0.0277(5) Uani 1 1 d . . . . .
H33 H 0.5917 0.0944 -0.0365 0.033 Uiso 1 1 calc R . . . .
C29 C 0.7625(2) 0.16041(12) 0.40971(14) 0.0165(4) Uani 1 1 d . . . . .
C14 C 0.8853(2) 0.63866(14) 0.48738(16) 0.0261(5) Uani 1 1 d . . . . .
H14 H 0.9398 0.6420 0.5444 0.031 Uiso 1 1 calc R . . . .
C17 C 0.7240(2) 0.62848(12) 0.31701(15) 0.0195(4) Uani 1 1 d . . . . .
H17 H 0.6702 0.6256 0.2597 0.023 Uiso 1 1 calc R . . . .
C7 C 0.2638(3) 0.39290(13) 0.15732(16) 0.0242(5) Uani 1 1 d . . . . .
H7 H 0.3121 0.3672 0.1239 0.029 Uiso 1 1 calc R . . . .
C19 C 1.1394(3) 0.13645(13) 0.39099(16) 0.0250(5) Uani 1 1 d . . . . .
H19 H 1.0875 0.0960 0.3982 0.030 Uiso 1 1 calc R . . . .
C11 C 0.2604(2) 0.46371(13) 0.28422(17) 0.0245(5) Uani 1 1 d . . . . .
H11 H 0.3072 0.4856 0.3363 0.029 Uiso 1 1 calc R . . . .
C15 C 0.8454(3) 0.70108(12) 0.43874(18) 0.0246(5) Uani 1 1 d . . . . .
H15 H 0.8711 0.7464 0.4634 0.030 Uiso 1 1 calc R . . . .
C32 C 0.5484(2) 0.13852(14) 0.07052(16) 0.0260(5) Uani 1 1 d . . . . .
H32 H 0.4520 0.1373 0.0499 0.031 Uiso 1 1 calc R . . . .
C25 C 0.7287(3) 0.16009(14) 0.55554(16) 0.0267(5) Uani 1 1 d . . . . .
H25 H 0.7390 0.1828 0.6092 0.032 Uiso 1 1 calc R . . . .
C27 C 0.6493(3) 0.05942(14) 0.46043(18) 0.0299(5) Uani 1 1 d . . . . .
H27 H 0.6064 0.0143 0.4501 0.036 Uiso 1 1 calc R . . . .
C22 C 1.2964(2) 0.25672(15) 0.37026(16) 0.0271(5) Uani 1 1 d . . . . .
H22 H 1.3490 0.2971 0.3639 0.033 Uiso 1 1 calc R . . . .
C26 C 0.6647(3) 0.09273(14) 0.54033(16) 0.0272(5) Uani 1 1 d . . . . .
H26 H 0.6323 0.0702 0.5838 0.033 Uiso 1 1 calc R . . . .
C10 C 0.1165(3) 0.46903(14) 0.25649(19) 0.0303(5) Uani 1 1 d . . . . .
H10 H 0.0676 0.4945 0.2897 0.036 Uiso 1 1 calc R . . . .
C8 C 0.1194(3) 0.39847(14) 0.12987(19) 0.0333(6) Uani 1 1 d . . . . .
H8 H 0.0720 0.3766 0.0779 0.040 Uiso 1 1 calc R . . . .
C21 C 1.3616(3) 0.19532(16) 0.41152(19) 0.0315(6) Uani 1 1 d . . . . .
H21 H 1.4580 0.1944 0.4325 0.038 Uiso 1 1 calc R . . . .
C20 C 1.2838(3) 0.13541(15) 0.42162(18) 0.0319(6) Uani 1 1 d . . . . .
H20 H 1.3282 0.0941 0.4490 0.038 Uiso 1 1 calc R . . . .
C9 C 0.0454(3) 0.43606(15) 0.1788(2) 0.0371(7) Uani 1 1 d . . . . .
H9 H -0.0511 0.4393 0.1600 0.045 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sn1 O1 2.0284(19) . ?
Sn1 C30 2.123(2) . ?
Sn1 C18 2.127(2) . ?
Sn1 C29 2.128(2) . ?
P1 C1 1.760(2) . ?
P1 C5 1.752(2) . ?
O1 C1 1.330(3) . ?
C30 C35 1.398(3) . ?
C30 C31 1.400(3) . ?
C6 C5 1.492(3) . ?
C6 C7 1.397(3) . ?
C6 C11 1.401(3) . ?
C18 C23 1.397(3) . ?
C18 C19 1.397(3) . ?
C2 H2 0.9300 . ?
C2 C1 1.399(3) . ?
C2 C3 1.396(3) . ?
C4 H4 0.9300 . ?
C4 C3 1.404(3) . ?
C4 C5 1.389(3) . ?
C24 H24 0.9300 . ?
C24 C29 1.392(3) . ?
C24 C25 1.390(3) . ?
C12 C3 1.484(3) . ?
C12 C13 1.404(3) . ?
C12 C17 1.389(3) . ?
C23 H23 0.9300 . ?
C23 C22 1.386(3) . ?
C28 H28 0.9300 . ?
C28 C29 1.396(3) . ?
C28 C27 1.387(4) . ?
C13 H13 0.9300 . ?
C13 C14 1.390(3) . ?
C35 H35 0.9300 . ?
C35 C34 1.387(3) . ?
C31 H31 0.9300 . ?
C31 C32 1.383(3) . ?
C16 H16 0.9300 . ?
C16 C17 1.385(3) . ?
C16 C15 1.386(4) . ?
C34 H34 0.9300 . ?
C34 C33 1.386(4) . ?
C33 H33 0.9300 . ?
C33 C32 1.391(4) . ?
C14 H14 0.9300 . ?
C14 C15 1.386(4) . ?
C17 H17 0.9300 . ?
C7 H7 0.9300 . ?
C7 C8 1.392(4) . ?
C19 H19 0.9300 . ?
C19 C20 1.392(3) . ?
C11 H11 0.9300 . ?
C11 C10 1.387(3) . ?
C15 H15 0.9300 . ?
C32 H32 0.9300 . ?
C25 H25 0.9300 . ?
C25 C26 1.389(4) . ?
C27 H27 0.9300 . ?
C27 C26 1.381(4) . ?
C22 H22 0.9300 . ?
C22 C21 1.383(4) . ?
C26 H26 0.9300 . ?
C10 H10 0.9300 . ?
C10 C9 1.393(4) . ?
C8 H8 0.9300 . ?
C8 C9 1.384(4) . ?
C21 H21 0.9300 . ?
C21 C20 1.381(4) . ?
C20 H20 0.9300 . ?
C9 H9 0.9300 . ?

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
O1 Sn1 C30 111.51(7) . . ?
O1 Sn1 C18 93.88(7) . . ?
O1 Sn1 C29 109.27(7) . . ?
C30 Sn1 C18 115.47(9) . . ?
C30 Sn1 C29 113.37(8) . . ?
C18 Sn1 C29 111.64(8) . . ?
C5 P1 C1 100.81(10) . . ?
C1 O1 Sn1 134.14(14) . . ?
C35 C30 Sn1 118.97(16) . . ?
C35 C30 C31 119.0(2) . . ?
C31 C30 Sn1 121.97(16) . . ?
C7 C6 C5 121.7(2) . . ?
C7 C6 C11 118.6(2) . . ?
C11 C6 C5 119.6(2) . . ?
C23 C18 Sn1 120.12(16) . . ?
C23 C18 C19 119.1(2) . . ?
C19 C18 Sn1 120.64(17) . . ?
C1 C2 H2 117.8 . . ?
C3 C2 H2 117.8 . . ?
C3 C2 C1 124.5(2) . . ?
C3 C4 H4 117.8 . . ?
C5 C4 H4 117.8 . . ?
C5 C4 C3 124.4(2) . . ?
O1 C1 P1 120.54(17) . . ?
O1 C1 C2 115.49(19) . . ?
C2 C1 P1 123.97(17) . . ?
C29 C24 H24 119.6 . . ?
C25 C24 H24 119.6 . . ?
C25 C24 C29 120.9(2) . . ?
C13 C12 C3 120.2(2) . . ?
C17 C12 C3 120.99(19) . . ?
C17 C12 C13 118.6(2) . . ?
C2 C3 C4 121.8(2) . . ?
C2 C3 C12 120.27(19) . . ?
C4 C3 C12 117.86(19) . . ?
C18 C23 H23 119.8 . . ?
C22 C23 C18 120.5(2) . . ?
C22 C23 H23 119.8 . . ?
C29 C28 H28 119.7 . . ?
C27 C28 H28 119.7 . . ?
C27 C28 C29 120.6(2) . . ?
C6 C5 P1 117.91(15) . . ?
C4 C5 P1 124.50(16) . . ?
C4 C5 C6 117.53(19) . . ?
C12 C13 H13 119.8 . . ?
C14 C13 C12 120.4(2) . . ?
C14 C13 H13 119.8 . . ?
C30 C35 H35 120.1 . . ?
C34 C35 C30 119.9(2) . . ?
C34 C35 H35 120.1 . . ?
C30 C31 H31 119.6 . . ?
C32 C31 C30 120.8(2) . . ?
C32 C31 H31 119.6 . . ?
C17 C16 H16 119.8 . . ?
C17 C16 C15 120.5(2) . . ?
C15 C16 H16 119.8 . . ?
C35 C34 H34 119.7 . . ?
C33 C34 C35 120.6(2) . . ?
C33 C34 H34 119.7 . . ?
C34 C33 H33 120.0 . . ?
C34 C33 C32 119.9(2) . . ?
C32 C33 H33 120.0 . . ?
C24 C29 Sn1 122.07(16) . . ?
C24 C29 C28 118.5(2) . . ?
C28 C29 Sn1 119.22(16) . . ?
C13 C14 H14 119.9 . . ?
C15 C14 C13 120.2(2) . . ?
C15 C14 H14 119.9 . . ?
C12 C17 H17 119.6 . . ?
C16 C17 C12 120.7(2) . . ?
C16 C17 H17 119.6 . . ?
C6 C7 H7 120.0 . . ?
C8 C7 C6 120.0(2) . . ?
C8 C7 H7 120.0 . . ?
C18 C19 H19 120.0 . . ?
C20 C19 C18 119.9(2) . . ?
C20 C19 H19 120.0 . . ?
C6 C11 H11 119.5 . . ?
C10 C11 C6 121.0(2) . . ?
C10 C11 H11 119.5 . . ?
C16 C15 C14 119.6(2) . . ?
C16 C15 H15 120.2 . . ?
C14 C15 H15 120.2 . . ?
C31 C32 C33 119.7(2) . . ?
C31 C32 H32 120.1 . . ?
C33 C32 H32 120.1 . . ?
C24 C25 H25 120.0 . . ?
C26 C25 C24 119.9(2) . . ?
C26 C25 H25 120.0 . . ?
C28 C27 H27 119.8 . . ?
C26 C27 C28 120.4(2) . . ?
C26 C27 H27 119.8 . . ?
C23 C22 H22 120.0 . . ?
C21 C22 C23 120.0(2) . . ?
C21 C22 H22 120.0 . . ?
C25 C26 H26 120.1 . . ?
C27 C26 C25 119.7(2) . . ?
C27 C26 H26 120.1 . . ?
C11 C10 H10 120.1 . . ?
C11 C10 C9 119.8(2) . . ?
C9 C10 H10 120.1 . . ?
C7 C8 H8 119.5 . . ?
C9 C8 C7 121.0(2) . . ?
C9 C8 H8 119.5 . . ?
C22 C21 H21 119.9 . . ?
C20 C21 C22 120.2(2) . . ?
C20 C21 H21 119.9 . . ?
C19 C20 H20 119.8 . . ?
C21 C20 C19 120.4(2) . . ?
C21 C20 H20 119.8 . . ?
C10 C9 H9 120.2 . . ?
C8 C9 C10 119.5(2) . . ?
C8 C9 H9 120.2 . . ?

_olex2_date_sample_data_collection 2018-03-20
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.886
_oxdiff_exptl_absorpt_empirical_full_min 0.759
####################################################################### 
# 
# 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_exp_1747
_database_code_depnum_ccdc_archive 'CCDC 1872116'
_audit_update_record             
;
2018-10-09 deposited with the CCDC.
2019-01-17 downloaded from the CCDC.
;
_audit_creation_date             2018-04-18
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.04.03 svn.r3497 for OlexSys, GUI svn.r5486)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C17 H13 Au Cl O P, C2 H3 N'
_chemical_formula_sum            'C19 H16 Au Cl N O P'
_chemical_formula_weight         537.71
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 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'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Au Au -4.4197 7.2980 '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'

_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      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y-1/2, z-1/2'

_cell_length_a                   12.7694(3)
_cell_length_b                   7.3282(3)
_cell_length_c                   38.4557(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3598.57(18)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    1298
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      41.7090
_cell_measurement_theta_min      4.5800
_shelx_estimated_absorpt_T_max   0.208
_shelx_estimated_absorpt_T_min   0.113
_exptl_absorpt_coefficient_mu    17.610
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56875
_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.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.985
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2048
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.13
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0416
_diffrn_reflns_av_unetI/netI     0.0430
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            7089
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        66.007
_diffrn_reflns_theta_max         66.007
_diffrn_reflns_theta_min         4.156
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6525
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -66.00  17.00   1.00    2.00    --  -41.14  38.00   0.00   83
  2  ω   -103.00 -45.00   1.00    2.00    --  -41.14 -38.00-180.00   58
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1202138000
_diffrn_orient_matrix_UB_12      -0.0149161000
_diffrn_orient_matrix_UB_13      -0.0006776000
_diffrn_orient_matrix_UB_21      0.0026049000
_diffrn_orient_matrix_UB_22      0.0117227000
_diffrn_orient_matrix_UB_23      0.0399615000
_diffrn_orient_matrix_UB_31      -0.0083783000
_diffrn_orient_matrix_UB_32      -0.2094114000
_diffrn_orient_matrix_UB_33      0.0022769000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\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                2563
_reflns_number_total             3130
_reflns_odcompleteness_completeness 35.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_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 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         2.607
_refine_diff_density_min         -2.439
_refine_diff_density_rms         0.227
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     219
_refine_ls_number_reflns         3130
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0589
_refine_ls_R_factor_gt           0.0491
_refine_ls_restrained_S_all      1.041
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0866P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1287
_refine_ls_wR_factor_ref         0.1388
_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, All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C11(H11), C2(H2), C16(H16), C15(H15), C9(H9), C17(H17), C4(H4), C13(H13),
 C10(H10), C14(H14), C7(H7), C8(H8)
2.b Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C)
2.c Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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
Au1 Au 0.23416(3) 0.03804(5) 0.43588(2) 0.02771(18) Uani 1 1 d . . . . .
P1 P 0.19614(16) 0.0433(3) 0.37984(5) 0.0259(4) Uani 1 1 d . . . . .
Cl1 Cl 0.27422(18) 0.0230(3) 0.49342(6) 0.0397(6) Uani 1 1 d . . . . .
C11 C -0.1131(7) -0.0045(13) 0.3695(2) 0.039(2) Uani 1 1 d . . . . .
H11 H -0.1139 -0.0769 0.3490 0.046 Uiso 1 1 calc R . . . .
C3 C 0.1561(6) 0.0215(9) 0.3006(2) 0.0207(16) Uani 1 1 d . . . . .
O1 O 0.3919(4) 0.0183(8) 0.35462(15) 0.0317(13) Uani 1 1 d . . . . .
H1 H 0.4013 0.0388 0.3759 0.048 Uiso 1 1 calc GR . . . .
C5 C 0.0757(6) 0.0611(9) 0.3588(2) 0.0234(17) Uani 1 1 d . . . . .
C2 C 0.2601(6) 0.0092(10) 0.3124(2) 0.0230(17) Uani 1 1 d . . . . .
H2 H 0.3139 -0.0102 0.2958 0.028 Uiso 1 1 calc R . . . .
C12 C 0.1363(6) 0.0045(10) 0.2625(2) 0.0223(16) Uani 1 1 d . . . . .
C6 C -0.0204(6) 0.0824(11) 0.3799(2) 0.0274(17) Uani 1 1 d . . . . .
C16 C 0.0430(6) 0.0953(11) 0.2107(2) 0.0299(17) Uani 1 1 d . . . . .
H16 H -0.0079 0.1701 0.1997 0.036 Uiso 1 1 calc R . . . .
C18 C -0.0175(7) -0.2139(13) 0.4754(3) 0.048(2) Uani 1 1 d . . . . .
H18A H -0.0790 -0.1346 0.4732 0.072 Uiso 1 1 calc GR . . . .
H18B H 0.0426 -0.1418 0.4832 0.072 Uiso 1 1 calc GR . . . .
H18C H -0.0320 -0.3106 0.4923 0.072 Uiso 1 1 calc GR . . . .
C19 C 0.0059(6) -0.2950(12) 0.4418(2) 0.0326(19) Uani 1 1 d . . . . .
C15 C 0.1000(6) -0.0289(11) 0.1913(2) 0.0312(18) Uani 1 1 d . . . . .
H15 H 0.0866 -0.0420 0.1671 0.037 Uiso 1 1 calc R . . . .
C9 C -0.2027(7) 0.1154(16) 0.4192(3) 0.050(3) Uani 1 1 d . . . . .
H9 H -0.2644 0.1221 0.4330 0.060 Uiso 1 1 calc R . . . .
C1 C 0.2883(6) 0.0240(11) 0.3474(2) 0.0243(16) Uani 1 1 d . . . . .
C17 C 0.0602(6) 0.1107(10) 0.24619(19) 0.0246(16) Uani 1 1 d . . . . .
H17 H 0.0199 0.1943 0.2595 0.030 Uiso 1 1 calc R . . . .
C4 C 0.0716(6) 0.0488(10) 0.3230(2) 0.0243(16) Uani 1 1 d . . . . .
H4 H 0.0045 0.0600 0.3126 0.029 Uiso 1 1 calc R . . . .
C13 C 0.1949(6) -0.1172(10) 0.2422(2) 0.0251(16) Uani 1 1 d . . . . .
H13 H 0.2480 -0.1889 0.2529 0.030 Uiso 1 1 calc R . . . .
C10 C -0.2028(8) 0.0153(14) 0.3890(3) 0.048(3) Uani 1 1 d . . . . .
H10 H -0.2658 -0.0412 0.3814 0.057 Uiso 1 1 calc R . . . .
C14 C 0.1765(6) -0.1341(11) 0.2071(2) 0.0313(18) Uani 1 1 d . . . . .
H14 H 0.2164 -0.2179 0.1937 0.038 Uiso 1 1 calc R . . . .
C7 C -0.0218(6) 0.1893(12) 0.4103(2) 0.0332(19) Uani 1 1 d . . . . .
H7 H 0.0403 0.2500 0.4175 0.040 Uiso 1 1 calc R . . . .
N1 N 0.0249(6) -0.3542(11) 0.4154(2) 0.0424(19) Uani 1 1 d . . . . .
C8 C -0.1125(7) 0.2072(14) 0.4299(2) 0.045(3) Uani 1 1 d . . . . .
H8 H -0.1131 0.2809 0.4502 0.054 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Au1 P1 2.210(2) . ?
Au1 Cl1 2.273(2) . ?
P1 C5 1.743(8) . ?
P1 C1 1.720(8) . ?
C11 C6 1.403(12) . ?
C11 C10 1.377(13) . ?
C3 C2 1.407(10) . ?
C3 C12 1.492(10) . ?
C3 C4 1.395(11) . ?
O1 C1 1.353(10) . ?
C5 C6 1.480(10) . ?
C5 C4 1.378(11) . ?
C2 C1 1.396(11) . ?
C12 C17 1.394(10) . ?
C12 C13 1.402(10) . ?
C6 C7 1.405(11) . ?
C16 C15 1.384(11) . ?
C16 C17 1.387(10) . ?
C18 C19 1.452(12) . ?
C19 N1 1.131(10) . ?
C15 C14 1.386(11) . ?
C9 C10 1.375(15) . ?
C9 C8 1.395(15) . ?
C13 C14 1.378(10) . ?
C7 C8 1.388(11) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
P1 Au1 Cl1 178.20(8) . . ?
C5 P1 Au1 130.4(3) . . ?
C1 P1 Au1 123.7(3) . . ?
C1 P1 C5 105.8(4) . . ?
C10 C11 C6 119.9(9) . . ?
C2 C3 C12 118.1(7) . . ?
C4 C3 C2 122.7(7) . . ?
C4 C3 C12 119.2(7) . . ?
C6 C5 P1 118.9(6) . . ?
C4 C5 P1 119.4(6) . . ?
C4 C5 C6 121.6(7) . . ?
C1 C2 C3 123.3(7) . . ?
C17 C12 C3 120.9(7) . . ?
C17 C12 C13 118.4(7) . . ?
C13 C12 C3 120.6(7) . . ?
C11 C6 C5 119.6(8) . . ?
C11 C6 C7 118.7(8) . . ?
C7 C6 C5 121.7(7) . . ?
C15 C16 C17 120.1(7) . . ?
N1 C19 C18 178.4(10) . . ?
C16 C15 C14 119.9(8) . . ?
C10 C9 C8 120.4(9) . . ?
O1 C1 P1 121.6(6) . . ?
O1 C1 C2 116.5(7) . . ?
C2 C1 P1 121.9(6) . . ?
C16 C17 C12 120.6(7) . . ?
C5 C4 C3 126.6(7) . . ?
C14 C13 C12 120.8(7) . . ?
C9 C10 C11 121.1(10) . . ?
C13 C14 C15 120.1(8) . . ?
C8 C7 C6 120.9(9) . . ?
C7 C8 C9 119.0(9) . . ?

_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.532
_oxdiff_exptl_absorpt_empirical_full_min 0.724
####################################################################### 
# 
# 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_exp_97
_database_code_depnum_ccdc_archive 'CCDC 1872117'
_audit_update_record             
;
2018-10-09 deposited with the CCDC.
2019-01-17 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT602_exp_97              
;
PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure        ! Info
RESPONSE: There are some disordered solvents and thus the comment "solvent mask" is used here.
;
_vrf_PLAT342_exp_97              
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.02316 Ang.
RESPONSE: There are some disordered solvents
;
# Added during the CSD deposition process: Tuesday 09 October 2018 02:13 AM
# end Validation Reply Form

_audit_creation_date             2018-03-14
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C87 H66 Au6 Cl O5 P5 S, 2(C H2 Cl2), C3 H7'
_chemical_formula_sum            'C92 H77 Au6 Cl5 O5 P5 S'
_chemical_formula_weight         2808.49
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 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'
Au Au -4.4197 7.2980 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
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                   15.31190(10)
_cell_length_b                   21.8107(2)
_cell_length_c                   28.8693(2)
_cell_angle_alpha                90
_cell_angle_beta                 99.0770(10)
_cell_angle_gamma                90
_cell_volume                     9520.55(13)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    108189
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.8940
_cell_measurement_theta_min      3.5660
_shelx_estimated_absorpt_T_max   0.145
_shelx_estimated_absorpt_T_min   0.111
_exptl_absorpt_coefficient_mu    19.613
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.33546
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.28b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.959
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             5276
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0620
_diffrn_reflns_av_unetI/netI     0.0242
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            170600
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.451
_diffrn_reflns_theta_min         2.551
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -89.00  17.00   0.50    2.00    --    0.00 -38.00   0.00  212
  2  ω    -17.00  89.00   0.50    2.00    --    0.00  38.00 -30.00  212
  3  ω    -89.00  17.00   0.50    2.00    --    0.00 -38.00-180.00  212
  4  ω    -89.00  17.00   0.50    2.00    --    0.00 -38.00  90.00  212
  5  ω    -17.00  89.00   0.50    2.00    --    0.00  38.00-180.00  212
  6  ω    -29.00  89.00   0.50    2.00    --    0.00  77.00  60.00  236
  7  ω    -17.00  89.00   0.50    2.00    --    0.00  38.00-120.00  212
  8  ω     71.00 185.00   0.50   10.00    --   95.20  65.00-150.21  228
  9  ω      6.00 119.00   0.50   10.00    --   95.20 -15.00 -90.00  226
 10  ω      6.00 119.00   0.50   10.00    --   95.20 -61.00  60.00  226
 11  ω      6.00 127.00   0.50   10.00    --   95.20 -82.00 -90.00  242
 12  ω      6.00 127.00   0.50   10.00    --   95.20 -82.00  60.00  242
 13  ω      6.00 127.00   0.50   10.00    --   95.20 -82.00 120.00  242
 14  ω     79.00 185.00   0.50   10.00    --   95.20  30.00 -90.00  212
 15  ω      6.00 127.00   0.50   10.00    --   95.20 -82.00   0.00  242
 16  ω      6.00 119.00   0.50   10.00    --   95.20 -61.00-180.00  226
 17  ω     79.00 185.00   0.50   10.00    --   95.20  30.00 -60.00  212
 18  ω      6.00 115.00   0.50   10.00    --   95.20 -45.00 120.00  218
 19  ω      6.00 127.00   0.50   10.00    --   95.20 -82.00-150.00  242
 20  ω      6.00 127.00   0.50   10.00    --   95.20 -82.00-180.00  242
 21  ω      6.00 119.00   0.50   10.00    --   95.20 -61.00 -60.00  226
 22  ω      6.00 112.00   0.50   10.00    --   95.20 -30.00 -90.00  212
 23  ω    -31.00  89.00   0.50    2.00    --    0.00  82.00  90.00  240
 24  ω    -31.00  48.00   0.50    2.00    --    0.00  82.00 150.00  158
 25  ω    -89.00  22.00   0.50    2.00    --    0.00 -57.00-120.00  222
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa dual home/near'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0729985000
_diffrn_orient_matrix_UB_12      0.0350615000
_diffrn_orient_matrix_UB_13      0.0322736000
_diffrn_orient_matrix_UB_21      0.0660152000
_diffrn_orient_matrix_UB_22      -0.0519120000
_diffrn_orient_matrix_UB_23      -0.0053579000
_diffrn_orient_matrix_UB_31      0.0263437000
_diffrn_orient_matrix_UB_32      0.0327194000
_diffrn_orient_matrix_UB_33      -0.0429783000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                17794
_reflns_number_total             19015
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_refine_diff_density_max         3.334
_refine_diff_density_min         -1.701
_refine_diff_density_rms         0.282
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1000
_refine_ls_number_reflns         19015
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0700
_refine_ls_R_factor_gt           0.0666
_refine_ls_restrained_S_all      1.119
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0564P)²+341.5175P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1710
_refine_ls_wR_factor_ref         0.1722
_refine_special_details          SQUEEZE
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C34) = Uanis(C33) = Uanis(C32) = Uanis(C31) = Uanis(C30) = Uanis(C29)
3.a Secondary CH2 refined with riding coordinates:
 C7BA(H7BA,H7BB), C3AA(H3AA,H3AB), C7AA(H7AA,H7AB), C1BA(H1BA,H1BB)
3.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C11(H11), C75(H75), C2(H2), C72(H72), C17(H17), C7(H7), C51(H51),
 C9(H9), C42(H42), C16(H16), C70(H70), C50(H50), C82(H82), C19(H19), C83(H83),
 C53(H53), C79(H79), C78(H78), C47(H47), C55(H55), C81(H81), C8(H8), C48(H48),
 C10(H10), C13(H13), C49(H49), C64(H64), C85(H85), C84(H84), C67(H67), C21(H21),
  C76(H76), C28(H28), C27(H27), C43(H43), C77(H77), C15(H15), C66(H66),
 C57(H57), C68(H68), C24(H24), C58(H58), C25(H25), C26(H26), C45(H45), C61(H61),
  C14(H14), C33(H33), C44(H44), C65(H65), C59(H59), C34(H34), C30(H30),
 C32(H32), C38(H38), C41(H41), C36(H36), C60(H60), C31(H31)
3.c Idealised Me refined as rotating group:
 C8AA(H8AA,H8AB,H8AC), C0AA(H0AA,H0AB,H0AC), C6AA(H6AA,H6AB,H6AC)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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
Au6 Au 0.68237(3) 0.62036(2) 0.62706(2) 0.02821(12) Uani 1 1 d . . . . .
Au4 Au 0.82956(3) 0.82740(2) 0.75427(2) 0.03059(12) Uani 1 1 d . . . . .
Au2 Au 0.54747(3) 0.63957(2) 0.72823(2) 0.03000(12) Uani 1 1 d . . . . .
Au3 Au 0.63184(4) 0.76714(3) 0.80453(2) 0.03335(13) Uani 1 1 d . . . . .
Au5 Au 0.86090(3) 0.74074(2) 0.64404(2) 0.03068(12) Uani 1 1 d . . . . .
Au1 Au 0.72061(4) 0.71137(3) 0.71658(2) 0.03465(13) Uani 1 1 d . . . . .
Cl1 Cl 0.6230(2) 0.78100(15) 0.67756(11) 0.0393(7) Uani 1 1 d . . . . .
P1 P 0.57034(19) 0.58193(14) 0.66385(10) 0.0254(6) Uani 1 1 d . . . . .
P5 P 0.7972(2) 0.66338(14) 0.59483(10) 0.0261(6) Uani 1 1 d . . . . .
P4 P 0.9177(2) 0.81694(15) 0.69626(11) 0.0293(6) Uani 1 1 d . . . . .
P3 P 0.7443(2) 0.83910(15) 0.81343(11) 0.0317(7) Uani 1 1 d . . . . .
P2 P 0.5218(2) 0.69278(16) 0.79374(11) 0.0351(7) Uani 1 1 d . . . . .
S1 S 0.8163(3) 0.6374(2) 0.75019(14) 0.0493(9) Uani 1 1 d . . . . .
O3 O 0.8590(7) 0.7762(5) 0.8736(4) 0.047(2) Uani 1 1 d . . . . .
O4 O 1.0497(7) 0.7446(5) 0.7392(4) 0.047(2) Uani 1 1 d . . . . .
O5 O 0.9116(7) 0.5724(5) 0.6205(3) 0.043(2) Uani 1 1 d . . . . .
O1 O 0.6670(7) 0.4995(5) 0.7168(4) 0.043(2) Uani 1 1 d . . . . .
C4 C 0.4240(8) 0.5166(6) 0.6247(4) 0.030(3) Uani 1 1 d . . . . .
H4 H 0.3693 0.5136 0.6056 0.036 Uiso 1 1 calc R . . . .
C12 C 0.3963(9) 0.4064(6) 0.6441(4) 0.033(3) Uani 1 1 d . . . . .
C73 C 0.7657(8) 0.6931(6) 0.5359(5) 0.030(2) Uani 1 1 d . . . . .
C11 C 0.3697(9) 0.6127(7) 0.5548(5) 0.037(3) Uani 1 1 d . . . . .
H11 H 0.3641 0.5733 0.5425 0.044 Uiso 1 1 calc R . . . .
C1 C 0.5987(8) 0.5071(6) 0.6905(4) 0.031(3) Uani 1 1 d . . . . .
C46 C 0.8066(9) 0.9729(6) 0.9392(4) 0.034(3) Uani 1 1 d . . . . .
C75 C 0.6485(10) 0.7605(8) 0.5589(5) 0.047(4) Uani 1 1 d . . . . .
H75 H 0.6822 0.7642 0.5886 0.056 Uiso 1 1 calc R . . . .
C2 C 0.5340(8) 0.4566(6) 0.6790(4) 0.030(3) Uani 1 1 d . . . . .
H2 H 0.5480 0.4188 0.6931 0.036 Uiso 1 1 calc R . . . .
C71 C 0.8938(8) 0.6448(6) 0.5068(4) 0.031(3) Uani 1 1 d . . . . .
C72 C 0.8158(8) 0.6817(5) 0.5024(4) 0.028(2) Uani 1 1 d . . . . .
H72 H 0.7975 0.6997 0.4733 0.034 Uiso 1 1 calc R . . . .
O2 O 0.6046(9) 0.6173(7) 0.8575(4) 0.067(3) Uani 1 1 d . . . . .
C3 C 0.4572(8) 0.4613(6) 0.6501(4) 0.029(2) Uani 1 1 d . . . . .
C40 C 0.6371(8) 0.9417(6) 0.7798(4) 0.031(3) Uani 1 1 d . . . . .
C17 C 0.4293(11) 0.3472(6) 0.6427(5) 0.039(3) Uani 1 1 d . . . . .
H17 H 0.4901 0.3409 0.6461 0.046 Uiso 1 1 calc R . . . .
C7 C 0.4317(10) 0.6831(6) 0.6153(5) 0.041(3) Uani 1 1 d . . . . .
H7 H 0.4686 0.6909 0.6435 0.049 Uiso 1 1 calc R . . . .
C51 C 0.8884(9) 0.9999(6) 0.9498(5) 0.035(3) Uani 1 1 d . . . . .
H51 H 0.9331 0.9889 0.9329 0.043 Uiso 1 1 calc R . . . .
C37 C 0.7884(9) 0.9277(6) 0.8991(4) 0.033(3) Uani 1 1 d . . . . .
C54 C 1.0749(9) 0.9087(6) 0.7245(4) 0.033(3) Uani 1 1 d . . . . .
C9 C 0.3326(12) 0.7201(8) 0.5485(5) 0.049(4) Uani 1 1 d . . . . .
H9 H 0.3013 0.7520 0.5321 0.059 Uiso 1 1 calc R . . . .
C18 C 0.4077(10) 0.7171(6) 0.7857(5) 0.040(3) Uani 1 1 d . . . . .
C80 C 0.9380(8) 0.6367(6) 0.4649(4) 0.031(3) Uani 1 1 d . . . . .
C42 C 0.5233(9) 1.0139(6) 0.7501(5) 0.038(3) Uani 1 1 d . . . . .
H42 H 0.4845 1.0446 0.7563 0.046 Uiso 1 1 calc R . . . .
C62 C 0.8566(9) 0.9191(7) 0.6389(5) 0.038(3) Uani 1 1 d . . . . .
C74 C 0.6791(9) 0.7268(7) 0.5248(5) 0.039(3) Uani 1 1 d . . . . .
C5 C 0.4649(8) 0.5716(6) 0.6263(4) 0.030(2) Uani 1 1 d . . . . .
C16 C 0.3724(13) 0.2975(7) 0.6361(5) 0.049(4) Uani 1 1 d . . . . .
H16 H 0.3947 0.2581 0.6342 0.059 Uiso 1 1 calc R . . . .
C56 C 0.9281(8) 0.8945(7) 0.6744(5) 0.036(3) Uani 1 1 d . . . . .
C70 C 0.9278(8) 0.6127(6) 0.5462(4) 0.028(2) Uani 1 1 d . . . . .
H70 H 0.9805 0.5916 0.5460 0.034 Uiso 1 1 calc R . . . .
C63 C 1.1450(9) 0.9549(6) 0.7402(5) 0.036(3) Uani 1 1 d . . . . .
C50 C 0.9055(12) 1.0433(7) 0.9852(5) 0.049(4) Uani 1 1 d . . . . .
H50 H 0.9601 1.0629 0.9911 0.059 Uiso 1 1 calc R . . . .
C52 C 1.0284(9) 0.7994(6) 0.7279(4) 0.034(3) Uani 1 1 d . . . . .
C82 C 1.0011(11) 0.5750(8) 0.4100(5) 0.047(4) Uani 1 1 d . . . . .
H82 H 1.0173 0.5366 0.4003 0.056 Uiso 1 1 calc R . . . .
C19 C 0.3539(12) 0.6978(7) 0.8153(6) 0.049(4) Uani 1 1 d . . . . .
H19 H 0.2950 0.7100 0.8089 0.058 Uiso 1 1 calc R . . . .
C83 C 1.0141(10) 0.6268(8) 0.3838(6) 0.049(4) Uani 1 1 d . . . . .
H83 H 1.0414 0.6234 0.3573 0.059 Uiso 1 1 calc R . . . .
C53 C 1.0879(9) 0.8512(7) 0.7409(5) 0.036(3) Uani 1 1 d . . . . .
H53 H 1.1388 0.8437 0.7623 0.043 Uiso 1 1 calc R . . . .
C6 C 0.4228(8) 0.6238(5) 0.5983(4) 0.028(2) Uani 1 1 d . . . . .
C79 C 0.6275(9) 0.7208(6) 0.4815(5) 0.037(3) Uani 1 1 d . . . . .
H79 H 0.6475 0.6965 0.4588 0.044 Uiso 1 1 calc R . . . .
C69 C 0.8871(8) 0.6090(6) 0.5890(4) 0.032(3) Uani 1 1 d . . . . .
C78 C 0.5472(10) 0.7497(8) 0.4710(6) 0.048(4) Uani 1 1 d . . . . .
H78 H 0.5138 0.7461 0.4413 0.057 Uiso 1 1 calc R . . . .
C47 C 0.7401(10) 0.9875(7) 0.9650(4) 0.038(3) Uani 1 1 d . . . . .
H47 H 0.6840 0.9704 0.9578 0.045 Uiso 1 1 calc R . . . .
C55 C 1.0001(9) 0.9273(6) 0.6912(5) 0.036(3) Uani 1 1 d . . . . .
H55 H 1.0017 0.9672 0.6798 0.044 Uiso 1 1 calc R . . . .
C81 C 0.9638(9) 0.5808(7) 0.4508(5) 0.042(3) Uani 1 1 d . . . . .
H81 H 0.9564 0.5462 0.4687 0.050 Uiso 1 1 calc R . . . .
C8 C 0.3864(11) 0.7310(7) 0.5908(6) 0.051(4) Uani 1 1 d . . . . .
H8 H 0.3922 0.7706 0.6029 0.061 Uiso 1 1 calc R . . . .
C48 C 0.7599(11) 1.0281(7) 1.0016(5) 0.045(4) Uani 1 1 d . . . . .
H48 H 0.7172 1.0362 1.0203 0.054 Uiso 1 1 calc R . . . .
C10 C 0.3260(11) 0.6613(7) 0.5308(5) 0.046(4) Uani 1 1 d . . . . .
H10 H 0.2911 0.6541 0.5018 0.055 Uiso 1 1 calc R . . . .
C13 C 0.3051(9) 0.4160(7) 0.6406(5) 0.037(3) Uani 1 1 d . . . . .
H13 H 0.2823 0.4554 0.6418 0.044 Uiso 1 1 calc R . . . .
C49 C 0.8401(12) 1.0572(7) 1.0116(5) 0.050(4) Uani 1 1 d . . . . .
H49 H 0.8503 1.0858 1.0357 0.060 Uiso 1 1 calc R . . . .
C64 C 1.2336(10) 0.9402(8) 0.7480(6) 0.051(4) Uani 1 1 d . . . . .
H64 H 1.2506 0.9001 0.7431 0.061 Uiso 1 1 calc R . . . .
C85 C 0.9496(8) 0.6885(7) 0.4378(5) 0.035(3) Uani 1 1 d . . . . .
H85 H 0.9326 0.7270 0.4470 0.042 Uiso 1 1 calc R . . . .
C23 C 0.3741(10) 0.7574(8) 0.7465(6) 0.048(4) Uani 1 1 d . . . . .
C84 C 0.9869(10) 0.6818(7) 0.3970(5) 0.042(3) Uani 1 1 d . . . . .
H84 H 0.9931 0.7161 0.3786 0.050 Uiso 1 1 calc R . . . .
C67 C 1.1814(12) 1.0600(8) 0.7630(6) 0.056(4) Uani 1 1 d . . . . .
H67 H 1.1640 1.0996 0.7692 0.068 Uiso 1 1 calc R . . . .
C21 C 0.4595(12) 0.6344(8) 0.8684(6) 0.054(4) Uani 1 1 d . . . . .
H21 H 0.4672 0.6087 0.8944 0.065 Uiso 1 1 calc R . . . .
C22 C 0.5349(12) 0.6437(8) 0.8449(5) 0.049(4) Uani 1 1 d . . . . .
C76 C 0.5660(11) 0.7894(9) 0.5489(6) 0.058(5) Uani 1 1 d . . . . .
H76 H 0.5452 0.8121 0.5721 0.069 Uiso 1 1 calc R . . . .
C28 C 0.4266(11) 0.8048(7) 0.7312(6) 0.046(3) Uani 1 1 d . . . . .
H28 H 0.4841 0.8108 0.7465 0.055 Uiso 1 1 calc R . . . .
C27 C 0.3924(13) 0.8433(10) 0.6929(7) 0.065(5) Uani 1 1 d . . . . .
H27 H 0.4271 0.8748 0.6840 0.078 Uiso 1 1 calc R . . . .
C43 C 0.5242(11) 0.9965(9) 0.7048(6) 0.058(4) Uani 1 1 d . . . . .
H43 H 0.4854 1.0138 0.6802 0.070 Uiso 1 1 calc R . . . .
C77 C 0.5161(11) 0.7850(9) 0.5063(6) 0.058(5) Uani 1 1 d . . . . .
H77 H 0.4618 0.8049 0.5000 0.070 Uiso 1 1 calc R . . . .
C15 C 0.2846(12) 0.3068(8) 0.6326(5) 0.054(5) Uani 1 1 d . . . . .
H15 H 0.2469 0.2731 0.6283 0.065 Uiso 1 1 calc R . . . .
C66 C 1.2717(12) 1.0435(8) 0.7706(7) 0.059(4) Uani 1 1 d . . . . .
H66 H 1.3145 1.0729 0.7807 0.070 Uiso 1 1 calc R . . . .
C57 C 0.7742(12) 0.8956(9) 0.6315(8) 0.068(6) Uani 1 1 d . . . . .
H57 H 0.7571 0.8651 0.6507 0.082 Uiso 1 1 calc R . . . .
C68 C 1.1199(10) 1.0165(7) 0.7466(6) 0.044(3) Uani 1 1 d . . . . .
H68 H 1.0607 1.0276 0.7395 0.052 Uiso 1 1 calc R . . . .
C24 C 0.2880(12) 0.7505(9) 0.7212(6) 0.057(4) Uani 1 1 d . . . . .
H24 H 0.2514 0.7201 0.7302 0.069 Uiso 1 1 calc R . . . .
C29 C 0.3101(19) 0.6469(10) 0.8854(10) 0.093(4) Uani 1 1 d . . . . .
C20 C 0.3794(13) 0.6596(7) 0.8562(6) 0.055(5) Uani 1 1 d . . . . .
C58 C 0.7142(14) 0.9197(12) 0.5927(9) 0.090(8) Uani 1 1 d . . . . .
H58 H 0.6633 0.8972 0.5825 0.109 Uiso 1 1 calc R . . . .
C25 C 0.2567(12) 0.7874(10) 0.6836(7) 0.065(5) Uani 1 1 d . . . . .
H25 H 0.1999 0.7814 0.6673 0.078 Uiso 1 1 calc R . . . .
C26 C 0.3104(13) 0.8344(10) 0.6696(7) 0.066(5) Uani 1 1 d . . . . .
H26 H 0.2888 0.8593 0.6441 0.079 Uiso 1 1 calc R . . . .
C45 C 0.6414(13) 0.9254(9) 0.7333(5) 0.060(5) Uani 1 1 d . . . . .
H45 H 0.6824 0.8965 0.7267 0.071 Uiso 1 1 calc R . . . .
C61 C 0.8785(15) 0.9646(11) 0.6065(8) 0.088(8) Uani 1 1 d . . . . .
H61 H 0.9359 0.9791 0.6074 0.105 Uiso 1 1 calc R . . . .
C14 C 0.2487(11) 0.3648(8) 0.6352(5) 0.050(4) Uani 1 1 d . . . . .
H14 H 0.1880 0.3698 0.6333 0.060 Uiso 1 1 calc R . . . .
C33 C 0.2667(19) 0.6407(9) 0.9641(11) 0.093(4) Uani 1 1 d . . . . .
H33 H 0.2813 0.6400 0.9966 0.112 Uiso 1 1 calc R . . . .
C44 C 0.5837(14) 0.9530(10) 0.6968(6) 0.068(6) Uani 1 1 d . . . . .
H44 H 0.5861 0.9412 0.6660 0.082 Uiso 1 1 calc R . . . .
C65 C 1.2972(12) 0.9829(10) 0.7628(7) 0.063(5) Uani 1 1 d . . . . .
H65 H 1.3567 0.9720 0.7677 0.076 Uiso 1 1 calc R . . . .
C59 C 0.7247(15) 0.9689(10) 0.5713(9) 0.087(8) Uani 1 1 d . . . . .
H59 H 0.6780 0.9914 0.5551 0.104 Uiso 1 1 calc R . . . .
C34 C 0.3313(19) 0.6505(9) 0.9359(10) 0.093(4) Uani 1 1 d . . . . .
H34 H 0.3889 0.6594 0.9497 0.112 Uiso 1 1 calc R . . . .
C30 C 0.2224(18) 0.6380(9) 0.8669(10) 0.093(4) Uani 1 1 d . . . . .
H30 H 0.2064 0.6391 0.8345 0.112 Uiso 1 1 calc R . . . .
C32 C 0.1826(19) 0.6324(9) 0.9431(10) 0.093(4) Uani 1 1 d . . . . .
H32 H 0.1391 0.6299 0.9622 0.112 Uiso 1 1 calc R . . . .
C38 C 0.8343(9) 0.8741(6) 0.9028(4) 0.032(3) Uani 1 1 d . . . . .
H38 H 0.8771 0.8683 0.9291 0.039 Uiso 1 1 calc R . . . .
C41 C 0.5783(10) 0.9874(8) 0.7868(5) 0.045(3) Uani 1 1 d . . . . .
H41 H 0.5758 1.0005 0.8172 0.054 Uiso 1 1 calc R . . . .
C35 C 0.7001(8) 0.9152(6) 0.8196(4) 0.032(3) Uani 1 1 d . . . . .
C36 C 0.7237(8) 0.9469(5) 0.8593(4) 0.027(2) Uani 1 1 d . . . . .
H36 H 0.6963 0.9846 0.8616 0.032 Uiso 1 1 calc R . . . .
C39 C 0.8209(9) 0.8258(6) 0.8686(5) 0.037(3) Uani 1 1 d . . . . .
Cl2 Cl 0.1622(3) 0.5606(2) 0.5968(2) 0.0751(14) Uani 1 1 d . . . . .
Cl0A Cl 0.1003(3) 0.6625(3) 0.6498(2) 0.0768(14) Uani 1 1 d . . . . .
Cl1A Cl 0.7768(5) 0.6353(3) 0.9750(2) 0.0941(19) Uani 1 1 d . . . . .
C7BA C 0.179(2) 0.6366(12) 0.6142(13) 0.117(12) Uani 1 1 d . . . . .
H7BA H 0.1755 0.6624 0.5866 0.141 Uiso 1 1 calc R . . . .
H7BB H 0.2385 0.6408 0.6318 0.141 Uiso 1 1 calc R . . . .
Cl2A Cl 0.6730(5) 0.7393(4) 0.9369(2) 0.109(2) Uani 1 1 d . . . . .
C8AA C 0.9034(10) 0.6735(9) 0.7887(6) 0.058(4) Uani 1 1 d . . . . .
H8AA H 0.9567 0.6723 0.7751 0.087 Uiso 1 1 calc GR . . . .
H8AB H 0.9127 0.6524 0.8182 0.087 Uiso 1 1 calc GR . . . .
H8AC H 0.8878 0.7154 0.7935 0.087 Uiso 1 1 calc GR . . . .
C0AA C 0.7634(14) 0.5942(9) 0.7903(6) 0.067(5) Uani 1 1 d . . . . .
H0AA H 0.8028 0.5628 0.8044 0.101 Uiso 1 1 calc GR . . . .
H0AB H 0.7107 0.5756 0.7737 0.101 Uiso 1 1 calc GR . . . .
H0AC H 0.7481 0.6209 0.8142 0.101 Uiso 1 1 calc GR . . . .
C6AA C 0.4206(15) 0.9320(11) 0.5822(6) 0.072(6) Uani 1 1 d . . . . .
H6AA H 0.3967 0.9013 0.5600 0.108 Uiso 1 1 calc GR . . . .
H6AB H 0.3760 0.9445 0.6002 0.108 Uiso 1 1 calc GR . . . .
H6AC H 0.4703 0.9155 0.6028 0.108 Uiso 1 1 calc GR . . . .
C3AA C 0.4493(15) 0.9857(11) 0.5570(8) 0.080(6) Uani 1 1 d . . . . .
H3AA H 0.4932 1.0076 0.5787 0.096 Uiso 1 1 calc R . . . .
H3AB H 0.3987 1.0127 0.5494 0.096 Uiso 1 1 calc R . . . .
C7AA C 0.4885(14) 0.9750(10) 0.5113(8) 0.078(6) Uani 1 1 d . . . . .
H7AA H 0.5404 0.9493 0.5188 0.093 Uiso 1 1 calc R . . . .
H7AB H 0.4455 0.9521 0.4897 0.093 Uiso 1 1 calc R . . . .
C60 C 0.8090(18) 0.9855(10) 0.5741(10) 0.097(9) Uani 1 1 d . . . . .
H60 H 0.8223 1.0137 0.5521 0.117 Uiso 1 1 calc R . . . .
C31 C 0.1559(19) 0.6273(9) 0.8942(10) 0.093(4) Uani 1 1 d . . . . .
H31 H 0.0982 0.6175 0.8810 0.112 Uiso 1 1 calc R . . . .
C1BA C 0.756(2) 0.6850(19) 0.9294(13) 0.139(14) Uani 1 1 d . . . . .
H1BA H 0.7367 0.6621 0.9008 0.167 Uiso 1 1 calc R . . . .
H1BB H 0.8096 0.7065 0.9260 0.167 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Au6 Au1 3.2381(7) . ?
Au6 P1 2.313(3) . ?
Au6 P5 2.314(3) . ?
Au4 Au1 3.1301(7) . ?
Au4 P4 2.322(3) . ?
Au4 P3 2.321(3) . ?
Au2 Au1 3.1424(7) . ?
Au2 P1 2.316(3) . ?
Au2 P2 2.305(3) . ?
Au3 Au1 3.2960(7) . ?
Au3 P3 2.314(3) . ?
Au3 P2 2.324(4) . ?
Au5 Au1 3.2908(7) . ?
Au5 P5 2.319(3) . ?
Au5 P4 2.319(3) . ?
Au1 Cl1 2.298(3) . ?
Au1 S1 2.290(4) . ?
P1 C1 1.827(14) . ?
P1 C5 1.810(13) . ?
P5 C73 1.814(13) . ?
P5 C69 1.845(14) . ?
P4 C56 1.820(15) . ?
P4 C52 1.835(14) . ?
P3 C35 1.811(14) . ?
P3 C39 1.845(14) . ?
P2 C18 1.806(16) . ?
P2 C22 1.811(17) . ?
S1 C8AA 1.780(17) . ?
S1 C0AA 1.783(19) . ?
O3 C39 1.227(16) . ?
O4 C52 1.268(17) . ?
O5 C69 1.224(16) . ?
O1 C1 1.204(16) . ?
C4 H4 0.9300 . ?
C4 C3 1.459(17) . ?
C4 C5 1.353(17) . ?
C12 C3 1.512(17) . ?
C12 C17 1.39(2) . ?
C12 C13 1.400(19) . ?
C73 C72 1.349(17) . ?
C73 C74 1.505(18) . ?
C11 H11 0.9300 . ?
C11 C6 1.405(17) . ?
C11 C10 1.38(2) . ?
C1 C2 1.483(18) . ?
C46 C51 1.374(19) . ?
C46 C37 1.512(17) . ?
C46 C47 1.392(19) . ?
C75 H75 0.9300 . ?
C75 C74 1.370(19) . ?
C75 C76 1.40(2) . ?
C2 H2 0.9300 . ?
C2 C3 1.336(18) . ?
C71 C72 1.429(18) . ?
C71 C80 1.486(16) . ?
C71 C70 1.368(17) . ?
C72 H72 0.9300 . ?
O2 C22 1.22(2) . ?
C40 C45 1.40(2) . ?
C40 C41 1.38(2) . ?
C40 C35 1.497(17) . ?
C17 H17 0.9300 . ?
C17 C16 1.38(2) . ?
C7 H7 0.9300 . ?
C7 C6 1.382(17) . ?
C7 C8 1.38(2) . ?
C51 H51 0.9300 . ?
C51 C50 1.39(2) . ?
C37 C38 1.360(19) . ?
C37 C36 1.455(17) . ?
C54 C63 1.490(17) . ?
C54 C53 1.34(2) . ?
C54 C55 1.435(19) . ?
C9 H9 0.9300 . ?
C9 C8 1.38(2) . ?
C9 C10 1.38(2) . ?
C18 C19 1.34(2) . ?
C18 C23 1.46(2) . ?
C80 C81 1.36(2) . ?
C80 C85 1.400(18) . ?
C42 H42 0.9300 . ?
C42 C43 1.37(2) . ?
C42 C41 1.37(2) . ?
C62 C56 1.478(18) . ?
C62 C57 1.35(2) . ?
C62 C61 1.44(2) . ?
C74 C79 1.375(19) . ?
C5 C6 1.483(16) . ?
C16 H16 0.9300 . ?
C16 C15 1.35(3) . ?
C56 C55 1.339(19) . ?
C70 H70 0.9300 . ?
C70 C69 1.470(17) . ?
C63 C64 1.38(2) . ?
C63 C68 1.42(2) . ?
C50 H50 0.9300 . ?
C50 C49 1.38(2) . ?
C52 C53 1.462(19) . ?
C82 H82 0.9300 . ?
C82 C83 1.39(2) . ?
C82 C81 1.395(18) . ?
C19 H19 0.9300 . ?
C19 C20 1.45(2) . ?
C83 H83 0.9300 . ?
C83 C84 1.34(2) . ?
C53 H53 0.9300 . ?
C79 H79 0.9300 . ?
C79 C78 1.37(2) . ?
C78 H78 0.9300 . ?
C78 C77 1.42(2) . ?
C47 H47 0.9300 . ?
C47 C48 1.37(2) . ?
C55 H55 0.9300 . ?
C81 H81 0.9300 . ?
C8 H8 0.9300 . ?
C48 H48 0.9300 . ?
C48 C49 1.37(2) . ?
C10 H10 0.9300 . ?
C13 H13 0.9300 . ?
C13 C14 1.40(2) . ?
C49 H49 0.9300 . ?
C64 H64 0.9300 . ?
C64 C65 1.37(2) . ?
C85 H85 0.9300 . ?
C85 C84 1.397(19) . ?
C23 C28 1.42(2) . ?
C23 C24 1.41(2) . ?
C84 H84 0.9300 . ?
C67 H67 0.9300 . ?
C67 C66 1.41(3) . ?
C67 C68 1.37(2) . ?
C21 H21 0.9300 . ?
C21 C22 1.44(2) . ?
C21 C20 1.34(3) . ?
C76 H76 0.9300 . ?
C76 C77 1.34(2) . ?
C28 H28 0.9300 . ?
C28 C27 1.42(2) . ?
C27 H27 0.9300 . ?
C27 C26 1.34(3) . ?
C43 H43 0.9300 . ?
C43 C44 1.36(3) . ?
C77 H77 0.9300 . ?
C15 H15 0.9300 . ?
C15 C14 1.39(3) . ?
C66 H66 0.9300 . ?
C66 C65 1.41(3) . ?
C57 H57 0.9300 . ?
C57 C58 1.43(3) . ?
C68 H68 0.9300 . ?
C24 H24 0.9300 . ?
C24 C25 1.38(3) . ?
C29 C20 1.48(2) . ?
C29 C34 1.44(4) . ?
C29 C30 1.38(4) . ?
C58 H58 0.9300 . ?
C58 C59 1.26(3) . ?
C25 H25 0.9300 . ?
C25 C26 1.41(3) . ?
C26 H26 0.9300 . ?
C45 H45 0.9300 . ?
C45 C44 1.40(2) . ?
C61 H61 0.9300 . ?
C61 C60 1.38(3) . ?
C14 H14 0.9300 . ?
C33 H33 0.9300 . ?
C33 C34 1.39(3) . ?
C33 C32 1.35(4) . ?
C44 H44 0.9300 . ?
C65 H65 0.9300 . ?
C59 H59 0.9300 . ?
C59 C60 1.33(3) . ?
C34 H34 0.9300 . ?
C30 H30 0.9300 . ?
C30 C31 1.40(3) . ?
C32 H32 0.9300 . ?
C32 C31 1.41(4) . ?
C38 H38 0.9300 . ?
C38 C39 1.436(18) . ?
C41 H41 0.9300 . ?
C35 C36 1.338(17) . ?
C36 H36 0.9300 . ?
Cl2 C7BA 1.74(3) . ?
Cl0A C7BA 1.80(2) . ?
Cl1A C1BA 1.70(3) . ?
C7BA H7BA 0.9700 . ?
C7BA H7BB 0.9700 . ?
Cl2A C1BA 1.77(3) . ?
C8AA H8AA 0.9600 . ?
C8AA H8AB 0.9600 . ?
C8AA H8AC 0.9600 . ?
C0AA H0AA 0.9600 . ?
C0AA H0AB 0.9600 . ?
C0AA H0AC 0.9600 . ?
C6AA H6AA 0.9600 . ?
C6AA H6AB 0.9600 . ?
C6AA H6AC 0.9600 . ?
C6AA C3AA 1.48(3) . ?
C3AA H3AA 0.9700 . ?
C3AA H3AB 0.9700 . ?
C3AA C7AA 1.55(3) . ?
C7AA C7AA 1.35(4) 3_676 ?
C7AA H7AA 0.9700 . ?
C7AA H7AB 0.9700 . ?
C60 H60 0.9300 . ?
C31 H31 0.9300 . ?
C1BA H1BA 0.9700 . ?
C1BA H1BB 0.9700 . ?

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
P1 Au6 Au1 84.80(7) . . ?
P1 Au6 P5 175.90(10) . . ?
P5 Au6 Au1 91.10(7) . . ?
P4 Au4 Au1 90.48(8) . . ?
P3 Au4 Au1 90.80(8) . . ?
P3 Au4 P4 178.58(12) . . ?
P1 Au2 Au1 87.01(7) . . ?
P2 Au2 Au1 95.33(9) . . ?
P2 Au2 P1 177.21(12) . . ?
P3 Au3 Au1 86.88(8) . . ?
P3 Au3 P2 177.84(12) . . ?
P2 Au3 Au1 91.01(8) . . ?
P5 Au5 Au1 89.69(7) . . ?
P4 Au5 Au1 86.64(8) . . ?
P4 Au5 P5 176.32(11) . . ?
Au6 Au1 Au3 142.80(2) . . ?
Au6 Au1 Au5 70.451(16) . . ?
Au4 Au1 Au6 142.41(2) . . ?
Au4 Au1 Au2 141.08(2) . . ?
Au4 Au1 Au3 72.290(17) . . ?
Au4 Au1 Au5 72.438(17) . . ?
Au2 Au1 Au6 74.366(17) . . ?
Au2 Au1 Au3 69.151(17) . . ?
Au2 Au1 Au5 144.24(2) . . ?
Au5 Au1 Au3 143.93(2) . . ?
Cl1 Au1 Au6 89.55(8) . . ?
Cl1 Au1 Au4 84.61(9) . . ?
Cl1 Au1 Au2 83.52(9) . . ?
Cl1 Au1 Au3 79.52(8) . . ?
Cl1 Au1 Au5 89.94(9) . . ?
S1 Au1 Au6 85.94(10) . . ?
S1 Au1 Au4 98.76(11) . . ?
S1 Au1 Au2 95.60(11) . . ?
S1 Au1 Au3 104.35(10) . . ?
S1 Au1 Au5 88.20(11) . . ?
S1 Au1 Cl1 175.47(13) . . ?
Au6 P1 Au2 112.89(12) . . ?
C1 P1 Au6 111.9(4) . . ?
C1 P1 Au2 101.8(4) . . ?
C5 P1 Au6 115.2(4) . . ?
C5 P1 Au2 108.3(4) . . ?
C5 P1 C1 105.7(6) . . ?
Au6 P5 Au5 108.75(11) . . ?
C73 P5 Au6 114.6(4) . . ?
C73 P5 Au5 109.8(4) . . ?
C73 P5 C69 103.7(6) . . ?
C69 P5 Au6 113.7(4) . . ?
C69 P5 Au5 106.1(4) . . ?
Au5 P4 Au4 109.76(13) . . ?
C56 P4 Au4 104.6(4) . . ?
C56 P4 Au5 119.0(4) . . ?
C56 P4 C52 104.0(6) . . ?
C52 P4 Au4 105.0(4) . . ?
C52 P4 Au5 113.4(4) . . ?
Au3 P3 Au4 109.80(13) . . ?
C35 P3 Au4 115.8(5) . . ?
C35 P3 Au3 110.4(4) . . ?
C35 P3 C39 104.8(6) . . ?
C39 P3 Au4 105.2(5) . . ?
C39 P3 Au3 110.5(5) . . ?
Au2 P2 Au3 104.32(13) . . ?
C18 P2 Au2 109.3(5) . . ?
C18 P2 Au3 118.6(5) . . ?
C18 P2 C22 105.0(8) . . ?
C22 P2 Au2 111.2(5) . . ?
C22 P2 Au3 108.6(6) . . ?
C8AA S1 Au1 108.6(7) . . ?
C8AA S1 C0AA 101.7(9) . . ?
C0AA S1 Au1 108.7(7) . . ?
C3 C4 H4 116.8 . . ?
C5 C4 H4 116.8 . . ?
C5 C4 C3 126.4(11) . . ?
C17 C12 C3 121.3(12) . . ?
C17 C12 C13 120.1(13) . . ?
C13 C12 C3 118.6(12) . . ?
C72 C73 P5 120.6(10) . . ?
C72 C73 C74 121.3(12) . . ?
C74 C73 P5 118.0(9) . . ?
C6 C11 H11 120.5 . . ?
C10 C11 H11 120.5 . . ?
C10 C11 C6 119.0(13) . . ?
O1 C1 P1 120.9(10) . . ?
O1 C1 C2 121.4(13) . . ?
C2 C1 P1 117.6(9) . . ?
C51 C46 C37 120.1(12) . . ?
C51 C46 C47 120.1(12) . . ?
C47 C46 C37 119.9(13) . . ?
C74 C75 H75 120.3 . . ?
C74 C75 C76 119.4(14) . . ?
C76 C75 H75 120.3 . . ?
C1 C2 H2 117.5 . . ?
C3 C2 C1 125.0(12) . . ?
C3 C2 H2 117.5 . . ?
C72 C71 C80 118.5(11) . . ?
C70 C71 C72 124.3(11) . . ?
C70 C71 C80 117.0(11) . . ?
C73 C72 C71 127.1(12) . . ?
C73 C72 H72 116.4 . . ?
C71 C72 H72 116.4 . . ?
C4 C3 C12 116.0(11) . . ?
C2 C3 C4 125.5(12) . . ?
C2 C3 C12 118.5(11) . . ?
C45 C40 C35 121.1(12) . . ?
C41 C40 C45 117.1(13) . . ?
C41 C40 C35 121.6(12) . . ?
C12 C17 H17 119.8 . . ?
C16 C17 C12 120.5(15) . . ?
C16 C17 H17 119.8 . . ?
C6 C7 H7 119.6 . . ?
C6 C7 C8 120.8(13) . . ?
C8 C7 H7 119.6 . . ?
C46 C51 H51 119.5 . . ?
C46 C51 C50 121.0(14) . . ?
C50 C51 H51 119.5 . . ?
C38 C37 C46 118.0(11) . . ?
C38 C37 C36 126.0(11) . . ?
C36 C37 C46 115.9(11) . . ?
C53 C54 C63 117.7(13) . . ?
C53 C54 C55 124.0(12) . . ?
C55 C54 C63 118.2(12) . . ?
C8 C9 H9 120.4 . . ?
C10 C9 H9 120.4 . . ?
C10 C9 C8 119.1(14) . . ?
C19 C18 P2 120.2(13) . . ?
C19 C18 C23 120.3(15) . . ?
C23 C18 P2 119.5(10) . . ?
C81 C80 C71 122.6(12) . . ?
C81 C80 C85 119.2(12) . . ?
C85 C80 C71 118.1(12) . . ?
C43 C42 H42 119.2 . . ?
C43 C42 C41 121.6(14) . . ?
C41 C42 H42 119.2 . . ?
C57 C62 C56 122.9(15) . . ?
C57 C62 C61 118.0(16) . . ?
C61 C62 C56 118.6(14) . . ?
C75 C74 C73 119.9(13) . . ?
C75 C74 C79 119.5(13) . . ?
C79 C74 C73 120.5(12) . . ?
C4 C5 P1 119.7(10) . . ?
C4 C5 C6 120.2(11) . . ?
C6 C5 P1 120.1(9) . . ?
C17 C16 H16 120.2 . . ?
C15 C16 C17 119.5(15) . . ?
C15 C16 H16 120.2 . . ?
C62 C56 P4 118.9(10) . . ?
C55 C56 P4 119.0(11) . . ?
C55 C56 C62 122.2(14) . . ?
C71 C70 H70 117.6 . . ?
C71 C70 C69 124.8(12) . . ?
C69 C70 H70 117.6 . . ?
C64 C63 C54 122.4(13) . . ?
C64 C63 C68 118.6(13) . . ?
C68 C63 C54 118.9(13) . . ?
C51 C50 H50 120.5 . . ?
C49 C50 C51 119.1(15) . . ?
C49 C50 H50 120.5 . . ?
O4 C52 P4 120.2(11) . . ?
O4 C52 C53 122.5(13) . . ?
C53 C52 P4 117.2(10) . . ?
C83 C82 H82 120.0 . . ?
C83 C82 C81 119.9(15) . . ?
C81 C82 H82 120.0 . . ?
C18 C19 H19 117.1 . . ?
C18 C19 C20 125.8(17) . . ?
C20 C19 H19 117.1 . . ?
C82 C83 H83 120.2 . . ?
C84 C83 C82 119.6(13) . . ?
C84 C83 H83 120.2 . . ?
C54 C53 C52 125.3(12) . . ?
C54 C53 H53 117.3 . . ?
C52 C53 H53 117.3 . . ?
C11 C6 C5 119.7(11) . . ?
C7 C6 C11 119.3(12) . . ?
C7 C6 C5 121.0(11) . . ?
C74 C79 H79 119.2 . . ?
C78 C79 C74 121.6(14) . . ?
C78 C79 H79 119.2 . . ?
O5 C69 P5 119.8(10) . . ?
O5 C69 C70 122.6(12) . . ?
C70 C69 P5 117.6(9) . . ?
C79 C78 H78 120.6 . . ?
C79 C78 C77 118.8(15) . . ?
C77 C78 H78 120.6 . . ?
C46 C47 H47 121.1 . . ?
C48 C47 C46 117.9(14) . . ?
C48 C47 H47 121.1 . . ?
C54 C55 H55 116.0 . . ?
C56 C55 C54 128.0(13) . . ?
C56 C55 H55 116.0 . . ?
C80 C81 C82 120.6(14) . . ?
C80 C81 H81 119.7 . . ?
C82 C81 H81 119.7 . . ?
C7 C8 H8 120.0 . . ?
C9 C8 C7 120.1(15) . . ?
C9 C8 H8 120.0 . . ?
C47 C48 H48 118.6 . . ?
C49 C48 C47 122.8(15) . . ?
C49 C48 H48 118.6 . . ?
C11 C10 H10 119.2 . . ?
C9 C10 C11 121.7(14) . . ?
C9 C10 H10 119.2 . . ?
C12 C13 H13 120.8 . . ?
C12 C13 C14 118.5(14) . . ?
C14 C13 H13 120.8 . . ?
C50 C49 H49 120.5 . . ?
C48 C49 C50 119.0(14) . . ?
C48 C49 H49 120.5 . . ?
C63 C64 H64 119.1 . . ?
C65 C64 C63 121.8(17) . . ?
C65 C64 H64 119.1 . . ?
C80 C85 H85 120.3 . . ?
C84 C85 C80 119.5(13) . . ?
C84 C85 H85 120.3 . . ?
C28 C23 C18 122.0(14) . . ?
C24 C23 C18 121.5(16) . . ?
C24 C23 C28 116.5(16) . . ?
C83 C84 C85 121.1(13) . . ?
C83 C84 H84 119.4 . . ?
C85 C84 H84 119.4 . . ?
C66 C67 H67 120.6 . . ?
C68 C67 H67 120.6 . . ?
C68 C67 C66 118.8(16) . . ?
C22 C21 H21 117.1 . . ?
C20 C21 H21 117.1 . . ?
C20 C21 C22 125.9(16) . . ?
O2 C22 P2 120.1(13) . . ?
O2 C22 C21 121.6(16) . . ?
C21 C22 P2 118.2(14) . . ?
C75 C76 H76 119.3 . . ?
C77 C76 C75 121.4(15) . . ?
C77 C76 H76 119.3 . . ?
C23 C28 H28 119.5 . . ?
C27 C28 C23 120.9(17) . . ?
C27 C28 H28 119.5 . . ?
C28 C27 H27 119.8 . . ?
C26 C27 C28 120(2) . . ?
C26 C27 H27 119.8 . . ?
C42 C43 H43 121.1 . . ?
C44 C43 C42 117.8(15) . . ?
C44 C43 H43 121.1 . . ?
C78 C77 H77 120.4 . . ?
C76 C77 C78 119.2(15) . . ?
C76 C77 H77 120.4 . . ?
C16 C15 H15 119.0 . . ?
C16 C15 C14 122.1(15) . . ?
C14 C15 H15 119.0 . . ?
C67 C66 H66 119.9 . . ?
C65 C66 C67 120.3(16) . . ?
C65 C66 H66 119.9 . . ?
C62 C57 H57 121.6 . . ?
C62 C57 C58 116.9(19) . . ?
C58 C57 H57 121.6 . . ?
C63 C68 H68 119.4 . . ?
C67 C68 C63 121.1(15) . . ?
C67 C68 H68 119.4 . . ?
C23 C24 H24 119.1 . . ?
C25 C24 C23 121.7(19) . . ?
C25 C24 H24 119.1 . . ?
C34 C29 C20 120(3) . . ?
C30 C29 C20 123(3) . . ?
C30 C29 C34 117(2) . . ?
C19 C20 C29 116.5(19) . . ?
C21 C20 C19 124.7(15) . . ?
C21 C20 C29 118.8(18) . . ?
C57 C58 H58 117.2 . . ?
C59 C58 C57 126(2) . . ?
C59 C58 H58 117.2 . . ?
C24 C25 H25 119.8 . . ?
C24 C25 C26 120.4(18) . . ?
C26 C25 H25 119.8 . . ?
C27 C26 C25 120.1(19) . . ?
C27 C26 H26 120.0 . . ?
C25 C26 H26 120.0 . . ?
C40 C45 H45 120.2 . . ?
C40 C45 C44 119.5(16) . . ?
C44 C45 H45 120.2 . . ?
C62 C61 H61 122.1 . . ?
C60 C61 C62 116(2) . . ?
C60 C61 H61 122.1 . . ?
C13 C14 H14 120.3 . . ?
C15 C14 C13 119.4(15) . . ?
C15 C14 H14 120.3 . . ?
C34 C33 H33 120.9 . . ?
C32 C33 H33 120.9 . . ?
C32 C33 C34 118(3) . . ?
C43 C44 C45 122.1(16) . . ?
C43 C44 H44 118.9 . . ?
C45 C44 H44 118.9 . . ?
C64 C65 C66 119.3(17) . . ?
C64 C65 H65 120.4 . . ?
C66 C65 H65 120.4 . . ?
C58 C59 H59 123.3 . . ?
C58 C59 C60 113.5(19) . . ?
C60 C59 H59 123.3 . . ?
C29 C34 H34 119.5 . . ?
C33 C34 C29 121(3) . . ?
C33 C34 H34 119.5 . . ?
C29 C30 H30 118.1 . . ?
C29 C30 C31 124(3) . . ?
C31 C30 H30 118.1 . . ?
C33 C32 H32 117.7 . . ?
C33 C32 C31 125(2) . . ?
C31 C32 H32 117.7 . . ?
C37 C38 H38 118.0 . . ?
C37 C38 C39 124.1(12) . . ?
C39 C38 H38 118.0 . . ?
C40 C41 H41 119.1 . . ?
C42 C41 C40 121.8(14) . . ?
C42 C41 H41 119.1 . . ?
C40 C35 P3 118.9(9) . . ?
C36 C35 P3 120.2(9) . . ?
C36 C35 C40 120.8(12) . . ?
C37 C36 H36 117.1 . . ?
C35 C36 C37 125.8(11) . . ?
C35 C36 H36 117.1 . . ?
O3 C39 P3 117.7(11) . . ?
O3 C39 C38 123.5(13) . . ?
C38 C39 P3 118.8(10) . . ?
Cl2 C7BA Cl0A 112.3(14) . . ?
Cl2 C7BA H7BA 109.1 . . ?
Cl2 C7BA H7BB 109.1 . . ?
Cl0A C7BA H7BA 109.1 . . ?
Cl0A C7BA H7BB 109.1 . . ?
H7BA C7BA H7BB 107.9 . . ?
S1 C8AA H8AA 109.5 . . ?
S1 C8AA H8AB 109.5 . . ?
S1 C8AA H8AC 109.5 . . ?
H8AA C8AA H8AB 109.5 . . ?
H8AA C8AA H8AC 109.5 . . ?
H8AB C8AA H8AC 109.5 . . ?
S1 C0AA H0AA 109.5 . . ?
S1 C0AA H0AB 109.5 . . ?
S1 C0AA H0AC 109.5 . . ?
H0AA C0AA H0AB 109.5 . . ?
H0AA C0AA H0AC 109.5 . . ?
H0AB C0AA H0AC 109.5 . . ?
H6AA C6AA H6AB 109.5 . . ?
H6AA C6AA H6AC 109.5 . . ?
H6AB C6AA H6AC 109.5 . . ?
C3AA C6AA H6AA 109.5 . . ?
C3AA C6AA H6AB 109.5 . . ?
C3AA C6AA H6AC 109.5 . . ?
C6AA C3AA H3AA 107.6 . . ?
C6AA C3AA H3AB 107.6 . . ?
C6AA C3AA C7AA 119(2) . . ?
H3AA C3AA H3AB 107.0 . . ?
C7AA C3AA H3AA 107.6 . . ?
C7AA C3AA H3AB 107.6 . . ?
C3AA C7AA H7AA 108.0 . . ?
C3AA C7AA H7AB 108.0 . . ?
C7AA C7AA C3AA 117(3) 3_676 . ?
C7AA C7AA H7AA 108.0 3_676 . ?
C7AA C7AA H7AB 108.0 3_676 . ?
H7AA C7AA H7AB 107.2 . . ?
C61 C60 H60 117.0 . . ?
C59 C60 C61 126(2) . . ?
C59 C60 H60 117.0 . . ?
C30 C31 C32 115(3) . . ?
C30 C31 H31 122.3 . . ?
C32 C31 H31 122.3 . . ?
Cl1A C1BA Cl2A 112.8(18) . . ?
Cl1A C1BA H1BA 109.0 . . ?
Cl1A C1BA H1BB 109.0 . . ?
Cl2A C1BA H1BA 109.0 . . ?
Cl2A C1BA H1BB 109.0 . . ?
H1BA C1BA H1BB 107.8 . . ?

_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 3.734
_oxdiff_exptl_absorpt_empirical_full_min 0.638
####################################################################### 
# 
# 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_exp_1727_a
_database_code_depnum_ccdc_archive 'CCDC 1872118'
_audit_update_record             
;
2018-10-09 deposited with the CCDC.
2019-01-17 downloaded from the CCDC.
;
_audit_creation_date             2018-03-14
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C18 H20 Cl2 Cu2 N2 O6 P2'
_chemical_formula_sum            'C18 H20 Cl2 Cu2 N2 O6 P2'
_chemical_formula_weight         620.28
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 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'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 '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'

_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                   7.3741(6)
_cell_length_b                   7.5275(7)
_cell_length_c                   11.8201(10)
_cell_angle_alpha                78.770(7)
_cell_angle_beta                 87.887(7)
_cell_angle_gamma                67.556(8)
_cell_volume                     594.30(10)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    1975
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      74.0300
_cell_measurement_theta_min      6.4630
_shelx_estimated_absorpt_T_max   0.757
_shelx_estimated_absorpt_T_min   0.619
_exptl_absorpt_coefficient_mu    5.886
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55518
_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.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.733
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             312
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0556
_diffrn_reflns_av_unetI/netI     0.0549
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.939
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            3417
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.939
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.352
_diffrn_reflns_theta_min         3.816
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6525
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.939
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -64.00  18.00   1.00    2.00    --  -41.14  38.00-120.00   82
  2  ω    -73.00  25.00   1.00    2.00    --  -41.14  77.00 -30.00   98
  3  ω    100.00 130.00   1.00    2.00    --   41.14 178.00-150.00   30
  4  ω    153.00 178.00   1.00    3.00    --  107.98  77.00 -90.00   25
  5  ω     95.00 120.00   1.00    3.00    --  107.98  77.00 -90.00   25
  6  ω     56.00 168.00   1.00    3.00    --  107.98  15.00-120.00  112
  7  ω     53.00  99.00   1.00    3.00    --  107.98 -95.00  30.00   46
  8  ω     44.00 105.00   1.00    3.00    --  107.98 -95.00 120.00   61
  9  ω     36.00 121.00   1.00    3.00    --  107.98-125.00   0.00   85
 10  ω     36.00 132.00   1.00    3.00    --  107.98 -45.00 -30.00   96
 11  ω     89.00 178.00   1.00    3.00    --  107.98  61.00 120.00   89
 12  ω     36.00 137.00   1.00    3.00    --  107.98 -61.00 150.00  101
 13  ω   -115.00 -17.00   1.00    2.00    --  -41.14 -38.00  60.00   98
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1478243000
_diffrn_orient_matrix_UB_12      0.0531982000
_diffrn_orient_matrix_UB_13      -0.1018394000
_diffrn_orient_matrix_UB_21      -0.0010758000
_diffrn_orient_matrix_UB_22      0.2090343000
_diffrn_orient_matrix_UB_23      -0.0279932000
_diffrn_orient_matrix_UB_31      0.1712515000
_diffrn_orient_matrix_UB_32      -0.0667594000
_diffrn_orient_matrix_UB_33      -0.0808197000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\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                2002
_reflns_number_total             2282
_reflns_odcompleteness_completeness 99.29
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_refine_diff_density_max         1.265
_refine_diff_density_min         -1.605
_refine_diff_density_rms         0.190
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     148
_refine_ls_number_reflns         2282
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0689
_refine_ls_R_factor_gt           0.0636
_refine_ls_restrained_S_all      1.068
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1496P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1843
_refine_ls_wR_factor_ref         0.1994
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5)
2.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C9(H9A,H9B,H9C)
2.c Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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
Cu1 Cu 0.68065(8) 0.44126(9) 0.91285(4) 0.0218(3) Uani 1 1 d . . . . .
Cl1 Cl 0.56676(14) 0.69409(14) 1.02570(7) 0.0212(3) Uani 1 1 d . . . . .
P1 P 0.60690(14) 0.55328(16) 0.72901(7) 0.0189(3) Uani 1 1 d . . . . .
O1 O 0.2306(4) 0.5766(5) 0.7443(2) 0.0262(7) Uani 1 1 d . . . . .
H1 H 0.2836 0.5088 0.8084 0.031 Uiso 1 1 calc GR . . . .
O2 O 0.9099(4) 0.7687(6) 0.4236(2) 0.0298(8) Uani 1 1 d . . . . .
O3 O 0.6392(4) 0.8728(5) 0.3100(2) 0.0228(7) Uani 1 1 d . . . . .
N1 N 0.9215(5) 0.2624(6) 1.0049(3) 0.0244(8) Uani 1 1 d . . . . .
C1 C 0.3670(6) 0.6183(6) 0.6767(3) 0.0176(8) Uani 1 1 d . . . . .
C2 C 0.3031(6) 0.7175(6) 0.5639(3) 0.0213(8) Uani 1 1 d . . . . .
H2 H 0.1703 0.7493 0.5414 0.026 Uiso 1 1 calc R . . . .
C3 C 0.4221(6) 0.7721(6) 0.4829(3) 0.0200(8) Uani 1 1 d . . . . .
H3 H 0.3660 0.8393 0.4080 0.024 Uiso 1 1 calc R . . . .
C4 C 0.6205(6) 0.7344(6) 0.5045(3) 0.0183(8) Uani 1 1 d . . . . .
C5 C 0.7157(6) 0.6395(6) 0.6115(3) 0.0188(8) Uani 1 1 d . . . . .
H5 H 0.8496 0.6211 0.6203 0.023 Uiso 1 1 calc R . . . .
C6 C 0.7412(6) 0.7919(6) 0.4109(3) 0.0192(8) Uani 1 1 d . . . . .
C7 C 0.7504(7) 0.9256(8) 0.2150(3) 0.0276(10) Uani 1 1 d . . . . .
H7A H 0.8035 1.0176 0.2344 0.041 Uiso 1 1 calc GR . . . .
H7B H 0.6643 0.9874 0.1454 0.041 Uiso 1 1 calc GR . . . .
H7C H 0.8587 0.8075 0.2011 0.041 Uiso 1 1 calc GR . . . .
C8 C 1.0395(6) 0.1755(6) 1.0750(3) 0.0208(8) Uani 1 1 d . . . . .
C9 C 1.1886(6) 0.0630(7) 1.1665(3) 0.0267(9) Uani 1 1 d . . . . .
H9A H 1.2224 0.1527 1.2035 0.040 Uiso 1 1 calc GR . . . .
H9B H 1.3061 -0.0224 1.1338 0.040 Uiso 1 1 calc GR . . . .
H9C H 1.1378 -0.0172 1.2240 0.040 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 Cl1 2.4347(11) 2_667 ?
Cu1 Cl1 2.4067(11) . ?
Cu1 P1 2.1799(10) . ?
Cu1 N1 1.974(4) . ?
Cl1 Cu1 2.4347(11) 2_667 ?
P1 C1 1.747(4) . ?
P1 C5 1.720(4) . ?
O1 H1 0.8400 . ?
O1 C1 1.354(5) . ?
O2 C6 1.199(5) . ?
O3 C6 1.340(4) . ?
O3 C7 1.448(5) . ?
N1 C8 1.131(6) . ?
C1 C2 1.396(5) . ?
C2 H2 0.9500 . ?
C2 C3 1.384(6) . ?
C3 H3 0.9500 . ?
C3 C4 1.403(5) . ?
C4 C5 1.390(5) . ?
C4 C6 1.496(5) . ?
C5 H5 0.9500 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C9 1.455(5) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl1 Cu1 Cl1 95.33(4) . 2_667 ?
P1 Cu1 Cl1 112.98(4) . . ?
P1 Cu1 Cl1 102.39(4) . 2_667 ?
N1 Cu1 Cl1 105.24(11) . 2_667 ?
N1 Cu1 Cl1 99.36(11) . . ?
N1 Cu1 P1 134.76(10) . . ?
Cu1 Cl1 Cu1 84.67(4) . 2_667 ?
C1 P1 Cu1 119.79(12) . . ?
C5 P1 Cu1 136.37(13) . . ?
C5 P1 C1 102.87(17) . . ?
C1 O1 H1 109.5 . . ?
C6 O3 C7 114.7(3) . . ?
C8 N1 Cu1 166.4(3) . . ?
O1 C1 P1 121.6(3) . . ?
O1 C1 C2 115.8(3) . . ?
C2 C1 P1 122.5(3) . . ?
C1 C2 H2 118.1 . . ?
C3 C2 C1 123.8(4) . . ?
C3 C2 H2 118.1 . . ?
C2 C3 H3 118.0 . . ?
C2 C3 C4 124.0(3) . . ?
C4 C3 H3 118.0 . . ?
C3 C4 C6 120.8(3) . . ?
C5 C4 C3 122.5(4) . . ?
C5 C4 C6 116.8(3) . . ?
P1 C5 H5 117.8 . . ?
C4 C5 P1 124.3(3) . . ?
C4 C5 H5 117.8 . . ?
O2 C6 O3 123.3(3) . . ?
O2 C6 C4 124.5(3) . . ?
O3 C6 C4 112.2(3) . . ?
O3 C7 H7A 109.5 . . ?
O3 C7 H7B 109.5 . . ?
O3 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N1 C8 C9 178.9(4) . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?

_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 4.102
_oxdiff_exptl_absorpt_empirical_full_min 0.385
####################################################################### 
# 
# 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_fp090115
_database_code_depnum_ccdc_archive 'CCDC 1872115'
_audit_update_record             
;
2018-10-09 deposited with the CCDC.
2019-01-17 downloaded from the CCDC.
;
_audit_creation_date             2018-06-05
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C92 H76 Cu4 O4 P8), 3(C H2 Cl2)'
_chemical_formula_sum            'C187 H158 Cl6 Cu8 O8 P16'
_chemical_formula_weight         3749.66
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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'

_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                   14.7461(6)
_cell_length_b                   15.0636(7)
_cell_length_c                   22.9640(7)
_cell_angle_alpha                87.081(3)
_cell_angle_beta                 75.816(3)
_cell_angle_gamma                63.403(4)
_cell_volume                     4412.0(3)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    37364
_cell_measurement_temperature    200.15
_cell_measurement_theta_max      24.71
_cell_measurement_theta_min      2.63
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.237
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1918
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0844
_diffrn_reflns_av_unetI/netI     0.1760
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            37269
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        24.713
_diffrn_reflns_theta_max         24.713
_diffrn_reflns_theta_min         2.634
_diffrn_ambient_temperature      200.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7359
_reflns_number_total             15005
_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       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         1.530
_refine_diff_density_min         -0.944
_refine_diff_density_rms         0.084
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.826
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     994
_refine_ls_number_reflns         15005
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.1296
_refine_ls_R_factor_gt           0.0579
_refine_ls_restrained_S_all      0.847
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0488P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1109
_refine_ls_wR_factor_ref         0.1258
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C1A-Cl4
 1.74 with sigma of 0.001
 C1A-Cl3
 1.74 with sigma of 0.001
3. Others
 Fixed Sof: Cl3(0.5) Cl4(0.5) C1A(0.5) H1AA(0.5) H1AB(0.5)
4.a Free rotating group:
 Cl3(Cl4,C1A)
4.b Secondary CH2 refined with riding coordinates:
 C93(H93A,H93B), C1A(H1AA,H1AB)
4.c Aromatic/amide H refined with riding coordinates:
 C64(H64), C28(H28), C13(H13), C35(H35), C16(H16), C11(H11), C9(H9), C17(H17),
 C6(H6), C67(H67), C68(H68), C18(H18), C34(H34), C8(H8), C44(H44), C32(H32),
 C7(H7), C40(H40), C86(H86), C2(H2), C22(H22), C12(H12), C1(H1), C70(H70),
 C29(H29), C65(H65), C23(H23), C72(H72), C49(H49), C52(H52), C19(H19), C66(H66),
  C14(H14), C78(H78), C58(H58), C82(H82), C30(H30), C71(H71), C77(H77),
 C48(H48), C4(H4), C47(H47), C31(H31), C46(H46), C50(H50), C41(H41), C55(H55),
 C59(H59), C74(H74), C62(H62), C92(H92), C38(H38), C36(H36), C26(H26), C53(H53),
  C37(H37), C76(H76), C56(H56), C90(H90), C89(H89), C91(H91), C88(H88),
 C80(H80), C61(H61), C3(H3), C73(H73), C42(H42), C25(H25), C85(H85), C43(H43),
 C24(H24), C54(H54), C79(H79), C83(H83), C60(H60), C84(H84)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.74054(6) 1.01947(6) 0.18313(3) 0.0295(2) Uani 1 1 d . . . . .
Cu2 Cu 0.77262(6) 0.93544(6) 0.32794(3) 0.0296(2) Uani 1 1 d . . . . .
Cu3 Cu 0.65235(6) 0.82984(6) 0.22295(3) 0.0314(2) Uani 1 1 d . . . . .
Cu4 Cu 0.93264(6) 0.73667(6) 0.20678(3) 0.0311(2) Uani 1 1 d . . . . .
P8 P 1.08246(14) 0.59074(13) 0.19874(7) 0.0349(4) Uani 1 1 d . . . . .
P6 P 0.78777(13) 1.00680(13) 0.40850(7) 0.0305(4) Uani 1 1 d . . . . .
P5 P 0.68174(13) 1.16079(12) 0.13277(7) 0.0301(4) Uani 1 1 d . . . . .
P1 P 0.64800(13) 1.04674(13) 0.28342(7) 0.0298(4) Uani 1 1 d . . . . .
P3 P 0.78753(13) 0.71776(12) 0.26086(7) 0.0297(4) Uani 1 1 d . . . . .
P2 P 0.72664(13) 0.89378(12) 0.14093(7) 0.0288(4) Uani 1 1 d . . . . .
P7 P 0.55145(13) 0.76600(13) 0.19707(7) 0.0305(4) Uani 1 1 d . . . . .
P4 P 0.93218(13) 0.86492(12) 0.25625(7) 0.0282(4) Uani 1 1 d . . . . .
O2 O 0.9276(3) 0.7556(3) 0.12007(16) 0.0304(10) Uani 1 1 d . . . . .
O1 O 0.5420(3) 0.9413(3) 0.28258(16) 0.0334(11) Uani 1 1 d . . . . .
O4 O 0.8874(3) 1.0001(3) 0.17356(16) 0.0341(11) Uani 1 1 d . . . . .
O3 O 0.7445(3) 0.8225(3) 0.36380(16) 0.0307(10) Uani 1 1 d . . . . .
C10 C 0.8502(5) 0.8030(4) 0.0967(3) 0.0292(15) Uani 1 1 d . . . . .
C15 C 0.7620(4) 0.7393(5) 0.3408(3) 0.0281(15) Uani 1 1 d . . . . .
C81 C 1.1225(6) 0.5459(5) 0.2683(3) 0.0434(19) Uani 1 1 d . . . . .
C63 C 0.4458(5) 0.8605(5) 0.1680(3) 0.0293(15) Uani 1 1 d . . . . .
C64 C 0.4239(6) 0.8498(5) 0.1140(3) 0.0440(19) Uani 1 1 d . . . . .
H64 H 0.4643 0.7888 0.0900 0.053 Uiso 1 1 calc R . . . .
C39 C 0.8131(5) 1.1154(5) 0.3948(3) 0.0362(17) Uani 1 1 d . . . . .
C57 C 0.4830(5) 0.7208(4) 0.2595(3) 0.0311(16) Uani 1 1 d . . . . .
C20 C 0.9527(5) 0.9519(4) 0.2053(2) 0.0242(14) Uani 1 1 d . . . . .
C5 C 0.5348(5) 1.0256(5) 0.2975(2) 0.0298(16) Uani 1 1 d . . . . .
C28 C 0.8216(5) 1.0672(5) 0.0254(3) 0.0407(18) Uani 1 1 d . . . . .
H28 H 0.8047 1.0140 0.0374 0.049 Uiso 1 1 calc R . . . .
C13 C 0.7757(6) 0.5708(5) 0.3596(3) 0.047(2) Uani 1 1 d . . . . .
H13 H 0.7703 0.5266 0.3898 0.057 Uiso 1 1 calc R . . . .
C35 C 0.3798(6) 1.2209(5) 0.1520(4) 0.057(2) Uani 1 1 d . . . . .
H35 H 0.3254 1.2208 0.1843 0.069 Uiso 1 1 calc R . . . .
C16 C 1.0369(5) 0.8267(5) 0.2906(3) 0.0362(17) Uani 1 1 d . . . . .
H16 H 1.0416 0.7797 0.3203 0.043 Uiso 1 1 calc R . . . .
C11 C 0.8059(5) 0.5953(5) 0.2541(3) 0.0419(18) Uani 1 1 d . . . . .
H11 H 0.8212 0.5674 0.2146 0.050 Uiso 1 1 calc R . . . .
C27 C 0.7730(5) 1.1545(5) 0.0612(3) 0.0292(16) Uani 1 1 d . . . . .
C9 C 0.8616(5) 0.7848(5) 0.0343(3) 0.0386(17) Uani 1 1 d . . . . .
H9 H 0.9288 0.7392 0.0115 0.046 Uiso 1 1 calc R . . . .
C17 C 1.1115(5) 0.8591(5) 0.2779(3) 0.0416(18) Uani 1 1 d . . . . .
H17 H 1.1635 0.8365 0.3001 0.050 Uiso 1 1 calc R . . . .
C6 C 0.6476(5) 0.9325(5) 0.0892(3) 0.0345(17) Uani 1 1 d . . . . .
H6 H 0.5767 0.9806 0.1031 0.041 Uiso 1 1 calc R . . . .
C45 C 0.6782(5) 1.0493(5) 0.4747(3) 0.0353(17) Uani 1 1 d . . . . .
C67 C 0.3041(5) 1.0269(5) 0.1829(3) 0.0391(17) Uani 1 1 d . . . . .
H67 H 0.2615 1.0873 0.2073 0.047 Uiso 1 1 calc R . . . .
C87 C 1.0701(5) 0.4879(5) 0.1697(3) 0.0372(17) Uani 1 1 d . . . . .
C21 C 0.6646(5) 1.2668(5) 0.1767(3) 0.0349(17) Uani 1 1 d . . . . .
C51 C 0.8970(5) 0.9149(5) 0.4363(3) 0.0339(16) Uani 1 1 d . . . . .
C68 C 0.3837(5) 0.9511(5) 0.2014(3) 0.0387(18) Uani 1 1 d . . . . .
H68 H 0.3972 0.9605 0.2384 0.046 Uiso 1 1 calc R . . . .
C18 C 1.1135(5) 0.9246(5) 0.2333(3) 0.0449(19) Uani 1 1 d . . . . .
H18 H 1.1698 0.9417 0.2259 0.054 Uiso 1 1 calc R . . . .
C34 C 0.4745(6) 1.1968(5) 0.1618(3) 0.049(2) Uani 1 1 d . . . . .
H34 H 0.4861 1.1786 0.2005 0.058 Uiso 1 1 calc R . . . .
C8 C 0.7851(6) 0.8267(5) 0.0049(3) 0.0422(19) Uani 1 1 d . . . . .
H8 H 0.8023 0.8066 -0.0365 0.051 Uiso 1 1 calc R . . . .
C33 C 0.5552(5) 1.1982(4) 0.1161(3) 0.0354(17) Uani 1 1 d . . . . .
C44 C 0.7606(6) 1.2031(5) 0.4296(3) 0.052(2) Uani 1 1 d . . . . .
H44 H 0.7076 1.2097 0.4647 0.063 Uiso 1 1 calc R . . . .
C32 C 0.7983(6) 1.2307(6) 0.0428(3) 0.052(2) Uani 1 1 d . . . . .
H32 H 0.7646 1.2918 0.0667 0.062 Uiso 1 1 calc R . . . .
C7 C 0.6820(6) 0.8976(5) 0.0306(3) 0.0430(19) Uani 1 1 d . . . . .
H7 H 0.6341 0.9224 0.0058 0.052 Uiso 1 1 calc R . . . .
C40 C 0.8916(6) 1.1085(6) 0.3440(3) 0.049(2) Uani 1 1 d . . . . .
H40 H 0.9303 1.0485 0.3190 0.059 Uiso 1 1 calc R . . . .
C86 C 1.0467(6) 0.5466(5) 0.3171(3) 0.053(2) Uani 1 1 d . . . . .
H86 H 0.9769 0.5704 0.3135 0.063 Uiso 1 1 calc R . . . .
C69 C 0.6183(5) 0.6641(5) 0.1386(3) 0.0302(15) Uani 1 1 d . . . . .
C2 C 0.4941(6) 1.2295(5) 0.3358(3) 0.052(2) Uani 1 1 d . . . . .
H2 H 0.4735 1.2959 0.3493 0.063 Uiso 1 1 calc R . . . .
C22 C 0.5686(6) 1.3498(5) 0.1976(3) 0.0460(19) Uani 1 1 d . . . . .
H22 H 0.5093 1.3567 0.1847 0.055 Uiso 1 1 calc R . . . .
C12 C 0.8001(6) 0.5367(5) 0.3003(3) 0.053(2) Uani 1 1 d . . . . .
H12 H 0.8132 0.4704 0.2917 0.063 Uiso 1 1 calc R . . . .
C1 C 0.5962(6) 1.1701(5) 0.3115(3) 0.0389(18) Uani 1 1 d . . . . .
H1 H 0.6439 1.1972 0.3094 0.047 Uiso 1 1 calc R . . . .
C70 C 0.6994(6) 0.6637(5) 0.0940(3) 0.0479(19) Uani 1 1 d . . . . .
H70 H 0.7197 0.7151 0.0950 0.057 Uiso 1 1 calc R . . . .
C75 C 1.1987(5) 0.5917(5) 0.1493(3) 0.0370(17) Uani 1 1 d . . . . .
C29 C 0.8938(5) 1.0567(5) -0.0274(3) 0.0448(19) Uani 1 1 d . . . . .
H29 H 0.9260 0.9964 -0.0519 0.054 Uiso 1 1 calc R . . . .
C65 C 0.3447(6) 0.9261(6) 0.0951(3) 0.060(2) Uani 1 1 d . . . . .
H65 H 0.3302 0.9172 0.0583 0.071 Uiso 1 1 calc R . . . .
C23 C 0.5585(7) 1.4221(6) 0.2367(3) 0.063(2) Uani 1 1 d . . . . .
H23 H 0.4921 1.4770 0.2521 0.076 Uiso 1 1 calc R . . . .
C72 C 0.7255(6) 0.5172(6) 0.0452(3) 0.055(2) Uani 1 1 d . . . . .
H72 H 0.7634 0.4660 0.0137 0.066 Uiso 1 1 calc R . . . .
C49 C 0.6049(6) 1.0871(6) 0.5813(3) 0.057(2) Uani 1 1 d . . . . .
H49 H 0.6145 1.0878 0.6207 0.068 Uiso 1 1 calc R . . . .
C52 C 0.9816(5) 0.9288(6) 0.4421(3) 0.0475(19) Uani 1 1 d . . . . .
H52 H 0.9812 0.9918 0.4354 0.057 Uiso 1 1 calc R . . . .
C19 C 1.0434(5) 0.9668(5) 0.1990(3) 0.0402(18) Uani 1 1 d . . . . .
H19 H 1.0557 1.0087 0.1690 0.048 Uiso 1 1 calc R . . . .
C66 C 0.2862(6) 1.0147(6) 0.1284(3) 0.053(2) Uani 1 1 d . . . . .
H66 H 0.2332 1.0680 0.1140 0.063 Uiso 1 1 calc R . . . .
C14 C 0.7588(5) 0.6623(5) 0.3783(3) 0.0416(18) Uani 1 1 d . . . . .
H14 H 0.7433 0.6760 0.4205 0.050 Uiso 1 1 calc R . . . .
C78 C 1.3745(6) 0.6018(7) 0.0781(3) 0.065(2) Uani 1 1 d . . . . .
H78 H 1.4346 0.6059 0.0540 0.078 Uiso 1 1 calc R . . . .
C58 C 0.3933(5) 0.7122(5) 0.2595(3) 0.0438(18) Uani 1 1 d . . . . .
H58 H 0.3634 0.7325 0.2260 0.053 Uiso 1 1 calc R . . . .
C82 C 1.2219(6) 0.5121(6) 0.2755(4) 0.068(2) Uani 1 1 d . . . . .
H82 H 1.2764 0.5103 0.2427 0.081 Uiso 1 1 calc R . . . .
C30 C 0.9211(5) 1.1319(6) -0.0459(3) 0.047(2) Uani 1 1 d . . . . .
H30 H 0.9721 1.1237 -0.0824 0.056 Uiso 1 1 calc R . . . .
C71 C 0.7525(6) 0.5903(6) 0.0474(3) 0.057(2) Uani 1 1 d . . . . .
H71 H 0.8084 0.5920 0.0169 0.069 Uiso 1 1 calc R . . . .
C77 C 1.2902(7) 0.6861(7) 0.1082(3) 0.066(2) Uani 1 1 d . . . . .
H77 H 1.2924 0.7483 0.1046 0.079 Uiso 1 1 calc R . . . .
C48 C 0.5070(6) 1.1178(6) 0.5741(3) 0.060(2) Uani 1 1 d . . . . .
H48 H 0.4481 1.1427 0.6078 0.072 Uiso 1 1 calc R . . . .
C4 C 0.4349(5) 1.1036(6) 0.3246(3) 0.050(2) Uani 1 1 d . . . . .
H4 H 0.3762 1.0902 0.3313 0.060 Uiso 1 1 calc R . . . .
C47 C 0.4940(6) 1.1123(6) 0.5172(3) 0.056(2) Uani 1 1 d . . . . .
H47 H 0.4257 1.1324 0.5121 0.068 Uiso 1 1 calc R . . . .
C31 C 0.8725(6) 1.2189(6) -0.0102(3) 0.055(2) Uani 1 1 d . . . . .
H31 H 0.8902 1.2717 -0.0221 0.066 Uiso 1 1 calc R . . . .
C46 C 0.5780(6) 1.0784(5) 0.4677(3) 0.048(2) Uani 1 1 d . . . . .
H46 H 0.5675 1.0748 0.4289 0.057 Uiso 1 1 calc R . . . .
C50 C 0.6912(5) 1.0547(5) 0.5325(3) 0.0445(19) Uani 1 1 d . . . . .
H50 H 0.7589 1.0363 0.5383 0.053 Uiso 1 1 calc R . . . .
C41 C 0.9129(6) 1.1876(7) 0.3300(4) 0.062(2) Uani 1 1 d . . . . .
H41 H 0.9653 1.1821 0.2948 0.074 Uiso 1 1 calc R . . . .
C55 C 0.9843(7) 0.7464(6) 0.4613(3) 0.062(2) Uani 1 1 d . . . . .
H55 H 0.9837 0.6840 0.4688 0.074 Uiso 1 1 calc R . . . .
C59 C 0.3464(6) 0.6750(5) 0.3070(4) 0.053(2) Uani 1 1 d . . . . .
H59 H 0.2867 0.6668 0.3056 0.064 Uiso 1 1 calc R . . . .
C74 C 0.5910(6) 0.5887(6) 0.1350(3) 0.061(2) Uani 1 1 d . . . . .
H74 H 0.5351 0.5866 0.1652 0.073 Uiso 1 1 calc R . . . .
C62 C 0.5210(5) 0.6946(5) 0.3097(3) 0.0470(19) Uani 1 1 d . . . . .
H62 H 0.5823 0.7000 0.3109 0.056 Uiso 1 1 calc R . . . .
C92 C 1.0878(5) 0.4009(5) 0.1967(3) 0.0484(19) Uani 1 1 d . . . . .
H92 H 1.1167 0.3888 0.2307 0.058 Uiso 1 1 calc R . . . .
C38 C 0.5362(6) 1.2234(6) 0.0603(3) 0.055(2) Uani 1 1 d . . . . .
H38 H 0.5901 1.2249 0.0282 0.066 Uiso 1 1 calc R . . . .
C36 C 0.3612(6) 1.2451(6) 0.0973(4) 0.065(3) Uani 1 1 d . . . . .
H36 H 0.2944 1.2611 0.0911 0.078 Uiso 1 1 calc R . . . .
C26 C 0.7500(6) 1.2610(6) 0.1945(3) 0.055(2) Uani 1 1 d . . . . .
H26 H 0.8165 1.2056 0.1804 0.066 Uiso 1 1 calc R . . . .
C53 C 1.0660(6) 0.8518(7) 0.4575(3) 0.066(2) Uani 1 1 d . . . . .
H53 H 1.1227 0.8624 0.4624 0.079 Uiso 1 1 calc R . . . .
C37 C 0.4394(7) 1.2464(6) 0.0505(4) 0.074(3) Uani 1 1 d . . . . .
H37 H 0.4270 1.2631 0.0118 0.088 Uiso 1 1 calc R . . . .
C76 C 1.2033(6) 0.6814(6) 0.1434(3) 0.0486(19) Uani 1 1 d . . . . .
H76 H 1.1456 0.7403 0.1639 0.058 Uiso 1 1 calc R . . . .
C56 C 0.8998(6) 0.8246(6) 0.4457(3) 0.051(2) Uani 1 1 d . . . . .
H56 H 0.8426 0.8143 0.4416 0.062 Uiso 1 1 calc R . . . .
C90 C 1.0246(6) 0.3462(7) 0.1278(4) 0.067(2) Uani 1 1 d . . . . .
H90 H 1.0083 0.2982 0.1137 0.080 Uiso 1 1 calc R . . . .
C89 C 1.0071(6) 0.4317(7) 0.0993(3) 0.066(2) Uani 1 1 d . . . . .
H89 H 0.9794 0.4428 0.0649 0.079 Uiso 1 1 calc R . . . .
C91 C 1.0658(6) 0.3297(6) 0.1767(4) 0.061(2) Uani 1 1 d . . . . .
H91 H 1.0790 0.2700 0.1967 0.073 Uiso 1 1 calc R . . . .
C88 C 1.0289(6) 0.5015(5) 0.1197(3) 0.054(2) Uani 1 1 d . . . . .
H88 H 1.0157 0.5609 0.0994 0.065 Uiso 1 1 calc R . . . .
C80 C 1.2850(7) 0.5061(6) 0.1176(4) 0.067(2) Uani 1 1 d . . . . .
H80 H 1.2830 0.4438 0.1205 0.080 Uiso 1 1 calc R . . . .
C61 C 0.4734(7) 0.6609(6) 0.3582(3) 0.061(2) Uani 1 1 d . . . . .
H61 H 0.5002 0.6455 0.3930 0.073 Uiso 1 1 calc R . . . .
C3 C 0.4174(6) 1.1968(6) 0.3418(3) 0.060(2) Uani 1 1 d . . . . .
H3 H 0.3471 1.2433 0.3594 0.072 Uiso 1 1 calc R . . . .
C73 C 0.6437(7) 0.5156(6) 0.0879(4) 0.075(3) Uani 1 1 d . . . . .
H73 H 0.6229 0.4649 0.0854 0.090 Uiso 1 1 calc R . . . .
C42 C 0.8602(8) 1.2747(7) 0.3658(4) 0.068(3) Uani 1 1 d . . . . .
H42 H 0.8775 1.3283 0.3566 0.082 Uiso 1 1 calc R . . . .
C25 C 0.7399(8) 1.3334(6) 0.2317(4) 0.072(3) Uani 1 1 d . . . . .
H25 H 0.7994 1.3286 0.2433 0.087 Uiso 1 1 calc R . . . .
C85 C 1.0696(8) 0.5137(6) 0.3710(4) 0.075(3) Uani 1 1 d . . . . .
H85 H 1.0158 0.5146 0.4041 0.090 Uiso 1 1 calc R . . . .
C43 C 0.7833(8) 1.2826(6) 0.4145(4) 0.073(3) Uani 1 1 d . . . . .
H43 H 0.7441 1.3433 0.4388 0.087 Uiso 1 1 calc R . . . .
C24 C 0.6435(9) 1.4143(7) 0.2530(4) 0.075(3) Uani 1 1 d . . . . .
H24 H 0.6372 1.4646 0.2792 0.090 Uiso 1 1 calc R . . . .
C54 C 1.0684(7) 0.7597(6) 0.4658(3) 0.067(3) Uani 1 1 d . . . . .
H54 H 1.1279 0.7058 0.4746 0.080 Uiso 1 1 calc R . . . .
C79 C 1.3719(7) 0.5118(7) 0.0828(4) 0.082(3) Uani 1 1 d . . . . .
H79 H 1.4302 0.4536 0.0620 0.099 Uiso 1 1 calc R . . . .
C83 C 1.2429(8) 0.4811(7) 0.3299(4) 0.082(3) Uani 1 1 d . . . . .
H83 H 1.3117 0.4598 0.3344 0.098 Uiso 1 1 calc R . . . .
C60 C 0.3881(7) 0.6497(6) 0.3565(4) 0.065(2) Uani 1 1 d . . . . .
H60 H 0.3566 0.6241 0.3897 0.079 Uiso 1 1 calc R . . . .
C84 C 1.1682(9) 0.4799(7) 0.3772(4) 0.083(3) Uani 1 1 d . . . . .
H84 H 1.1846 0.4559 0.4142 0.100 Uiso 1 1 calc R . . . .
Cl2 Cl 0.17796(19) 0.04040(18) 0.34386(10) 0.0861(7) Uiso 1 1 d . . . . .
Cl1 Cl 0.1295(3) 0.2486(3) 0.35219(14) 0.1378(11) Uiso 1 1 d . . . . .
C93 C 0.1316(7) 0.1465(6) 0.3913(4) 0.084(3) Uiso 1 1 d . . . . .
H93A H 0.0599 0.1626 0.4153 0.100 Uiso 1 1 calc R . . . .
H93B H 0.1767 0.1325 0.4196 0.100 Uiso 1 1 calc R . . . .
Cl3 Cl 1.3428(4) 0.4318(4) 0.4726(2) 0.1088(18) Uiso 0.5 1 d D . P A -1
Cl4 Cl 1.5168(5) 0.4622(6) 0.4915(4) 0.172(3) Uiso 0.5 1 d DG . P A -1
C1A C 1.4790(4) 0.3806(6) 0.4638(8) 0.125(8) Uiso 0.5 1 d DG . P A -1
H1AA H 1.5023 0.3186 0.4851 0.149 Uiso 0.5 1 calc R . P A -1
H1AB H 1.5146 0.3630 0.4205 0.149 Uiso 0.5 1 calc R . P A -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 P5 2.2822(18) . ?
Cu1 P1 2.3214(17) . ?
Cu1 P2 2.2797(18) . ?
Cu1 O4 2.008(4) . ?
Cu2 P6 2.2909(16) . ?
Cu2 P1 2.2849(17) . ?
Cu2 P4 2.3274(18) . ?
Cu2 O3 2.016(4) . ?
Cu3 P3 2.2954(17) . ?
Cu3 P2 2.3289(18) . ?
Cu3 P7 2.2945(18) . ?
Cu3 O1 2.009(4) . ?
Cu4 P8 2.2891(18) . ?
Cu4 P3 2.3258(19) . ?
Cu4 P4 2.2871(18) . ?
Cu4 O2 2.012(4) . ?
P8 C81 1.831(6) . ?
P8 C87 1.816(7) . ?
P8 C75 1.815(7) . ?
P6 C39 1.832(7) . ?
P6 C45 1.817(6) . ?
P6 C51 1.827(6) . ?
P5 C27 1.828(6) . ?
P5 C21 1.818(6) . ?
P5 C33 1.825(6) . ?
P1 C5 1.787(7) . ?
P1 C1 1.750(7) . ?
P3 C15 1.798(6) . ?
P3 C11 1.750(7) . ?
P2 C10 1.796(6) . ?
P2 C6 1.764(6) . ?
P7 C63 1.824(6) . ?
P7 C57 1.828(6) . ?
P7 C69 1.827(6) . ?
P4 C20 1.790(6) . ?
P4 C16 1.759(6) . ?
O2 C10 1.277(6) . ?
O1 C5 1.283(7) . ?
O4 C20 1.284(6) . ?
O3 C15 1.276(7) . ?
C10 C9 1.429(8) . ?
C15 C14 1.421(8) . ?
C81 C86 1.371(9) . ?
C81 C82 1.370(9) . ?
C63 C64 1.389(7) . ?
C63 C68 1.391(8) . ?
C64 H64 0.9500 . ?
C64 C65 1.367(9) . ?
C39 C44 1.367(9) . ?
C39 C40 1.398(9) . ?
C57 C58 1.386(8) . ?
C57 C62 1.369(8) . ?
C20 C19 1.425(8) . ?
C5 C4 1.418(9) . ?
C28 H28 0.9500 . ?
C28 C27 1.377(8) . ?
C28 C29 1.367(8) . ?
C13 H13 0.9500 . ?
C13 C12 1.383(9) . ?
C13 C14 1.358(9) . ?
C35 H35 0.9500 . ?
C35 C34 1.350(9) . ?
C35 C36 1.349(10) . ?
C16 H16 0.9500 . ?
C16 C17 1.358(8) . ?
C11 H11 0.9500 . ?
C11 C12 1.357(8) . ?
C27 C32 1.377(9) . ?
C9 H9 0.9500 . ?
C9 C8 1.348(8) . ?
C17 H17 0.9500 . ?
C17 C18 1.391(9) . ?
C6 H6 0.9500 . ?
C6 C7 1.358(8) . ?
C45 C46 1.390(8) . ?
C45 C50 1.399(8) . ?
C67 H67 0.9500 . ?
C67 C68 1.362(8) . ?
C67 C66 1.377(8) . ?
C87 C92 1.363(9) . ?
C87 C88 1.390(8) . ?
C21 C22 1.394(9) . ?
C21 C26 1.382(9) . ?
C51 C52 1.392(9) . ?
C51 C56 1.349(9) . ?
C68 H68 0.9500 . ?
C18 H18 0.9500 . ?
C18 C19 1.361(8) . ?
C34 H34 0.9500 . ?
C34 C33 1.387(9) . ?
C8 H8 0.9500 . ?
C8 C7 1.403(9) . ?
C33 C38 1.377(8) . ?
C44 H44 0.9500 . ?
C44 C43 1.387(10) . ?
C32 H32 0.9500 . ?
C32 C31 1.380(9) . ?
C7 H7 0.9500 . ?
C40 H40 0.9500 . ?
C40 C41 1.366(10) . ?
C86 H86 0.9500 . ?
C86 C85 1.372(9) . ?
C69 C70 1.369(8) . ?
C69 C74 1.376(9) . ?
C2 H2 0.9500 . ?
C2 C1 1.346(9) . ?
C2 C3 1.398(10) . ?
C22 H22 0.9500 . ?
C22 C23 1.380(9) . ?
C12 H12 0.9500 . ?
C1 H1 0.9500 . ?
C70 H70 0.9500 . ?
C70 C71 1.383(9) . ?
C75 C76 1.381(9) . ?
C75 C80 1.409(9) . ?
C29 H29 0.9500 . ?
C29 C30 1.378(9) . ?
C65 H65 0.9500 . ?
C65 C66 1.365(9) . ?
C23 H23 0.9500 . ?
C23 C24 1.349(10) . ?
C72 H72 0.9500 . ?
C72 C71 1.336(10) . ?
C72 C73 1.364(10) . ?
C49 H49 0.9500 . ?
C49 C48 1.355(9) . ?
C49 C50 1.383(9) . ?
C52 H52 0.9500 . ?
C52 C53 1.379(9) . ?
C19 H19 0.9500 . ?
C66 H66 0.9500 . ?
C14 H14 0.9500 . ?
C78 H78 0.9500 . ?
C78 C77 1.375(10) . ?
C78 C79 1.371(11) . ?
C58 H58 0.9500 . ?
C58 C59 1.377(9) . ?
C82 H82 0.9500 . ?
C82 C83 1.369(10) . ?
C30 H30 0.9500 . ?
C30 C31 1.373(9) . ?
C71 H71 0.9500 . ?
C77 H77 0.9500 . ?
C77 C76 1.366(10) . ?
C48 H48 0.9500 . ?
C48 C47 1.378(9) . ?
C4 H4 0.9500 . ?
C4 C3 1.371(9) . ?
C47 H47 0.9500 . ?
C47 C46 1.374(9) . ?
C31 H31 0.9500 . ?
C46 H46 0.9500 . ?
C50 H50 0.9500 . ?
C41 H41 0.9500 . ?
C41 C42 1.374(10) . ?
C55 H55 0.9500 . ?
C55 C56 1.389(9) . ?
C55 C54 1.370(10) . ?
C59 H59 0.9500 . ?
C59 C60 1.381(10) . ?
C74 H74 0.9500 . ?
C74 C73 1.388(9) . ?
C62 H62 0.9500 . ?
C62 C61 1.367(9) . ?
C92 H92 0.9500 . ?
C92 C91 1.379(9) . ?
C38 H38 0.9500 . ?
C38 C37 1.384(10) . ?
C36 H36 0.9500 . ?
C36 C37 1.378(11) . ?
C26 H26 0.9500 . ?
C26 C25 1.353(9) . ?
C53 H53 0.9500 . ?
C53 C54 1.377(10) . ?
C37 H37 0.9500 . ?
C76 H76 0.9500 . ?
C56 H56 0.9500 . ?
C90 H90 0.9500 . ?
C90 C89 1.361(10) . ?
C90 C91 1.364(10) . ?
C89 H89 0.9500 . ?
C89 C88 1.363(10) . ?
C91 H91 0.9500 . ?
C88 H88 0.9500 . ?
C80 H80 0.9500 . ?
C80 C79 1.370(10) . ?
C61 H61 0.9500 . ?
C61 C60 1.352(10) . ?
C3 H3 0.9500 . ?
C73 H73 0.9500 . ?
C42 H42 0.9500 . ?
C42 C43 1.350(11) . ?
C25 H25 0.9500 . ?
C25 C24 1.383(11) . ?
C85 H85 0.9500 . ?
C85 C84 1.351(12) . ?
C43 H43 0.9500 . ?
C24 H24 0.9500 . ?
C54 H54 0.9500 . ?
C79 H79 0.9500 . ?
C83 H83 0.9500 . ?
C83 C84 1.350(12) . ?
C60 H60 0.9500 . ?
C84 H84 0.9500 . ?
Cl2 C93 1.744(8) . ?
Cl1 C93 1.732(9) . ?
C93 H93A 0.9900 . ?
C93 H93B 0.9900 . ?
Cl3 C1A 1.7603 . ?
Cl4 C1A 1.7596 . ?
C1A H1AA 0.9900 . ?
C1A H1AB 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
P5 Cu1 P1 111.51(7) . . ?
P2 Cu1 P5 111.68(6) . . ?
P2 Cu1 P1 108.10(7) . . ?
O4 Cu1 P5 98.03(12) . . ?
O4 Cu1 P1 112.02(12) . . ?
O4 Cu1 P2 115.30(13) . . ?
P6 Cu2 P4 110.30(6) . . ?
P1 Cu2 P6 112.51(7) . . ?
P1 Cu2 P4 108.81(6) . . ?
O3 Cu2 P6 102.82(11) . . ?
O3 Cu2 P1 115.08(12) . . ?
O3 Cu2 P4 107.08(13) . . ?
P3 Cu3 P2 106.65(7) . . ?
P7 Cu3 P3 114.60(7) . . ?
P7 Cu3 P2 111.52(6) . . ?
O1 Cu3 P3 114.03(11) . . ?
O1 Cu3 P2 109.97(13) . . ?
O1 Cu3 P7 100.07(13) . . ?
P8 Cu4 P3 110.60(7) . . ?
P4 Cu4 P8 113.46(7) . . ?
P4 Cu4 P3 106.01(6) . . ?
O2 Cu4 P8 101.56(12) . . ?
O2 Cu4 P3 109.88(12) . . ?
O2 Cu4 P4 115.37(12) . . ?
C81 P8 Cu4 117.1(2) . . ?
C87 P8 Cu4 111.3(2) . . ?
C87 P8 C81 103.0(3) . . ?
C75 P8 Cu4 114.6(2) . . ?
C75 P8 C81 103.6(3) . . ?
C75 P8 C87 106.0(3) . . ?
C39 P6 Cu2 116.8(2) . . ?
C45 P6 Cu2 117.5(2) . . ?
C45 P6 C39 102.7(3) . . ?
C45 P6 C51 103.8(3) . . ?
C51 P6 Cu2 109.0(2) . . ?
C51 P6 C39 105.7(3) . . ?
C27 P5 Cu1 113.3(2) . . ?
C21 P5 Cu1 110.65(19) . . ?
C21 P5 C27 105.4(3) . . ?
C21 P5 C33 104.9(3) . . ?
C33 P5 Cu1 115.6(2) . . ?
C33 P5 C27 106.3(3) . . ?
Cu2 P1 Cu1 101.31(7) . . ?
C5 P1 Cu1 114.14(19) . . ?
C5 P1 Cu2 112.0(2) . . ?
C1 P1 Cu1 113.2(2) . . ?
C1 P1 Cu2 113.8(2) . . ?
C1 P1 C5 102.8(3) . . ?
Cu3 P3 Cu4 104.20(7) . . ?
C15 P3 Cu3 112.0(2) . . ?
C15 P3 Cu4 113.2(2) . . ?
C11 P3 Cu3 113.2(2) . . ?
C11 P3 Cu4 112.2(2) . . ?
C11 P3 C15 102.4(3) . . ?
Cu1 P2 Cu3 103.86(6) . . ?
C10 P2 Cu1 112.4(2) . . ?
C10 P2 Cu3 113.6(2) . . ?
C6 P2 Cu1 114.1(2) . . ?
C6 P2 Cu3 110.1(2) . . ?
C6 P2 C10 103.0(3) . . ?
C63 P7 Cu3 111.4(2) . . ?
C63 P7 C57 103.5(3) . . ?
C63 P7 C69 104.2(3) . . ?
C57 P7 Cu3 114.9(2) . . ?
C69 P7 Cu3 116.4(2) . . ?
C69 P7 C57 105.1(3) . . ?
Cu4 P4 Cu2 105.99(7) . . ?
C20 P4 Cu2 113.2(2) . . ?
C20 P4 Cu4 111.56(18) . . ?
C16 P4 Cu2 110.6(2) . . ?
C16 P4 Cu4 113.2(2) . . ?
C16 P4 C20 102.5(3) . . ?
C10 O2 Cu4 130.6(4) . . ?
C5 O1 Cu3 131.7(4) . . ?
C20 O4 Cu1 129.5(4) . . ?
C15 O3 Cu2 132.2(4) . . ?
O2 C10 P2 121.2(4) . . ?
O2 C10 C9 119.9(6) . . ?
C9 C10 P2 118.9(5) . . ?
O3 C15 P3 121.1(4) . . ?
O3 C15 C14 120.4(5) . . ?
C14 C15 P3 118.4(5) . . ?
C86 C81 P8 117.3(6) . . ?
C82 C81 P8 125.2(6) . . ?
C82 C81 C86 117.5(6) . . ?
C64 C63 P7 124.9(5) . . ?
C64 C63 C68 117.1(6) . . ?
C68 C63 P7 117.9(4) . . ?
C63 C64 H64 119.7 . . ?
C65 C64 C63 120.7(7) . . ?
C65 C64 H64 119.7 . . ?
C44 C39 P6 125.4(6) . . ?
C44 C39 C40 117.4(7) . . ?
C40 C39 P6 117.1(5) . . ?
C58 C57 P7 123.9(5) . . ?
C62 C57 P7 118.9(5) . . ?
C62 C57 C58 117.3(6) . . ?
O4 C20 P4 120.8(4) . . ?
O4 C20 C19 119.5(6) . . ?
C19 C20 P4 119.7(4) . . ?
O1 C5 P1 121.0(5) . . ?
O1 C5 C4 119.3(6) . . ?
C4 C5 P1 119.7(5) . . ?
C27 C28 H28 119.8 . . ?
C29 C28 H28 119.8 . . ?
C29 C28 C27 120.3(7) . . ?
C12 C13 H13 117.3 . . ?
C14 C13 H13 117.3 . . ?
C14 C13 C12 125.5(7) . . ?
C34 C35 H35 119.4 . . ?
C36 C35 H35 119.4 . . ?
C36 C35 C34 121.1(8) . . ?
P4 C16 H16 117.5 . . ?
C17 C16 P4 125.1(5) . . ?
C17 C16 H16 117.5 . . ?
P3 C11 H11 117.2 . . ?
C12 C11 P3 125.6(5) . . ?
C12 C11 H11 117.2 . . ?
C28 C27 P5 117.8(5) . . ?
C28 C27 C32 118.9(6) . . ?
C32 C27 P5 123.3(5) . . ?
C10 C9 H9 117.2 . . ?
C8 C9 C10 125.7(6) . . ?
C8 C9 H9 117.2 . . ?
C16 C17 H17 119.2 . . ?
C16 C17 C18 121.5(6) . . ?
C18 C17 H17 119.2 . . ?
P2 C6 H6 118.0 . . ?
C7 C6 P2 124.0(5) . . ?
C7 C6 H6 118.0 . . ?
C46 C45 P6 119.1(5) . . ?
C46 C45 C50 118.8(6) . . ?
C50 C45 P6 122.1(5) . . ?
C68 C67 H67 120.5 . . ?
C68 C67 C66 119.0(6) . . ?
C66 C67 H67 120.5 . . ?
C92 C87 P8 125.0(5) . . ?
C92 C87 C88 116.4(7) . . ?
C88 C87 P8 118.3(5) . . ?
C22 C21 P5 123.7(5) . . ?
C26 C21 P5 118.0(5) . . ?
C26 C21 C22 118.1(6) . . ?
C52 C51 P6 124.1(5) . . ?
C56 C51 P6 116.8(5) . . ?
C56 C51 C52 118.7(6) . . ?
C63 C68 H68 118.8 . . ?
C67 C68 C63 122.3(6) . . ?
C67 C68 H68 118.8 . . ?
C17 C18 H18 116.6 . . ?
C19 C18 C17 126.9(7) . . ?
C19 C18 H18 116.6 . . ?
C35 C34 H34 119.5 . . ?
C35 C34 C33 121.0(7) . . ?
C33 C34 H34 119.5 . . ?
C9 C8 H8 117.4 . . ?
C9 C8 C7 125.3(6) . . ?
C7 C8 H8 117.4 . . ?
C34 C33 P5 118.0(5) . . ?
C38 C33 P5 124.1(6) . . ?
C38 C33 C34 117.9(6) . . ?
C39 C44 H44 119.3 . . ?
C39 C44 C43 121.3(8) . . ?
C43 C44 H44 119.3 . . ?
C27 C32 H32 119.8 . . ?
C27 C32 C31 120.3(7) . . ?
C31 C32 H32 119.8 . . ?
C6 C7 C8 123.0(6) . . ?
C6 C7 H7 118.5 . . ?
C8 C7 H7 118.5 . . ?
C39 C40 H40 119.8 . . ?
C41 C40 C39 120.3(7) . . ?
C41 C40 H40 119.8 . . ?
C81 C86 H86 119.3 . . ?
C81 C86 C85 121.4(7) . . ?
C85 C86 H86 119.3 . . ?
C70 C69 P7 118.1(5) . . ?
C70 C69 C74 117.2(6) . . ?
C74 C69 P7 124.7(5) . . ?
C1 C2 H2 118.9 . . ?
C1 C2 C3 122.3(7) . . ?
C3 C2 H2 118.9 . . ?
C21 C22 H22 119.6 . . ?
C23 C22 C21 120.8(7) . . ?
C23 C22 H22 119.6 . . ?
C13 C12 H12 119.1 . . ?
C11 C12 C13 121.8(7) . . ?
C11 C12 H12 119.1 . . ?
P1 C1 H1 117.5 . . ?
C2 C1 P1 125.1(6) . . ?
C2 C1 H1 117.5 . . ?
C69 C70 H70 119.2 . . ?
C69 C70 C71 121.6(7) . . ?
C71 C70 H70 119.2 . . ?
C76 C75 P8 117.9(5) . . ?
C76 C75 C80 118.3(7) . . ?
C80 C75 P8 123.8(6) . . ?
C28 C29 H29 119.3 . . ?
C28 C29 C30 121.4(7) . . ?
C30 C29 H29 119.3 . . ?
C64 C65 H65 119.6 . . ?
C66 C65 C64 120.8(6) . . ?
C66 C65 H65 119.6 . . ?
C22 C23 H23 120.2 . . ?
C24 C23 C22 119.6(8) . . ?
C24 C23 H23 120.2 . . ?
C71 C72 H72 119.8 . . ?
C71 C72 C73 120.3(8) . . ?
C73 C72 H72 119.8 . . ?
C48 C49 H49 119.3 . . ?
C48 C49 C50 121.4(6) . . ?
C50 C49 H49 119.3 . . ?
C51 C52 H52 119.8 . . ?
C53 C52 C51 120.4(7) . . ?
C53 C52 H52 119.8 . . ?
C20 C19 H19 118.0 . . ?
C18 C19 C20 124.0(6) . . ?
C18 C19 H19 118.0 . . ?
C67 C66 H66 120.0 . . ?
C65 C66 C67 120.0(6) . . ?
C65 C66 H66 120.0 . . ?
C15 C14 H14 116.9 . . ?
C13 C14 C15 126.2(6) . . ?
C13 C14 H14 116.9 . . ?
C77 C78 H78 119.9 . . ?
C79 C78 H78 119.9 . . ?
C79 C78 C77 120.2(8) . . ?
C57 C58 H58 119.2 . . ?
C59 C58 C57 121.6(6) . . ?
C59 C58 H58 119.2 . . ?
C81 C82 H82 119.9 . . ?
C83 C82 C81 120.3(8) . . ?
C83 C82 H82 119.9 . . ?
C29 C30 H30 120.9 . . ?
C31 C30 C29 118.2(7) . . ?
C31 C30 H30 120.9 . . ?
C70 C71 H71 119.9 . . ?
C72 C71 C70 120.2(8) . . ?
C72 C71 H71 119.9 . . ?
C78 C77 H77 119.7 . . ?
C76 C77 C78 120.6(8) . . ?
C76 C77 H77 119.7 . . ?
C49 C48 H48 120.5 . . ?
C49 C48 C47 119.1(7) . . ?
C47 C48 H48 120.5 . . ?
C5 C4 H4 117.7 . . ?
C3 C4 C5 124.5(7) . . ?
C3 C4 H4 117.7 . . ?
C48 C47 H47 119.3 . . ?
C46 C47 C48 121.4(7) . . ?
C46 C47 H47 119.3 . . ?
C32 C31 H31 119.6 . . ?
C30 C31 C32 120.8(7) . . ?
C30 C31 H31 119.6 . . ?
C45 C46 H46 120.1 . . ?
C47 C46 C45 119.8(6) . . ?
C47 C46 H46 120.1 . . ?
C45 C50 H50 120.2 . . ?
C49 C50 C45 119.5(6) . . ?
C49 C50 H50 120.2 . . ?
C40 C41 H41 119.3 . . ?
C40 C41 C42 121.5(8) . . ?
C42 C41 H41 119.3 . . ?
C56 C55 H55 120.2 . . ?
C54 C55 H55 120.2 . . ?
C54 C55 C56 119.6(8) . . ?
C58 C59 H59 120.7 . . ?
C58 C59 C60 118.6(7) . . ?
C60 C59 H59 120.7 . . ?
C69 C74 H74 119.4 . . ?
C69 C74 C73 121.2(7) . . ?
C73 C74 H74 119.4 . . ?
C57 C62 H62 119.0 . . ?
C61 C62 C57 122.0(7) . . ?
C61 C62 H62 119.0 . . ?
C87 C92 H92 118.6 . . ?
C87 C92 C91 122.9(7) . . ?
C91 C92 H92 118.6 . . ?
C33 C38 H38 119.7 . . ?
C33 C38 C37 120.6(7) . . ?
C37 C38 H38 119.7 . . ?
C35 C36 H36 120.1 . . ?
C35 C36 C37 119.8(7) . . ?
C37 C36 H36 120.1 . . ?
C21 C26 H26 119.6 . . ?
C25 C26 C21 120.7(7) . . ?
C25 C26 H26 119.6 . . ?
C52 C53 H53 119.9 . . ?
C54 C53 C52 120.2(8) . . ?
C54 C53 H53 119.9 . . ?
C38 C37 H37 120.3 . . ?
C36 C37 C38 119.4(7) . . ?
C36 C37 H37 120.3 . . ?
C75 C76 H76 119.7 . . ?
C77 C76 C75 120.5(7) . . ?
C77 C76 H76 119.7 . . ?
C51 C56 C55 121.6(7) . . ?
C51 C56 H56 119.2 . . ?
C55 C56 H56 119.2 . . ?
C89 C90 H90 120.1 . . ?
C89 C90 C91 119.7(8) . . ?
C91 C90 H90 120.1 . . ?
C90 C89 H89 119.7 . . ?
C90 C89 C88 120.5(7) . . ?
C88 C89 H89 119.7 . . ?
C92 C91 H91 120.5 . . ?
C90 C91 C92 119.0(8) . . ?
C90 C91 H91 120.5 . . ?
C87 C88 H88 119.3 . . ?
C89 C88 C87 121.5(7) . . ?
C89 C88 H88 119.3 . . ?
C75 C80 H80 119.7 . . ?
C79 C80 C75 120.6(8) . . ?
C79 C80 H80 119.7 . . ?
C62 C61 H61 120.1 . . ?
C60 C61 C62 119.8(7) . . ?
C60 C61 H61 120.1 . . ?
C2 C3 H3 117.2 . . ?
C4 C3 C2 125.6(7) . . ?
C4 C3 H3 117.2 . . ?
C72 C73 C74 119.5(8) . . ?
C72 C73 H73 120.3 . . ?
C74 C73 H73 120.3 . . ?
C41 C42 H42 120.7 . . ?
C43 C42 C41 118.6(8) . . ?
C43 C42 H42 120.7 . . ?
C26 C25 H25 119.8 . . ?
C26 C25 C24 120.5(8) . . ?
C24 C25 H25 119.8 . . ?
C86 C85 H85 119.8 . . ?
C84 C85 C86 120.3(9) . . ?
C84 C85 H85 119.8 . . ?
C44 C43 H43 119.6 . . ?
C42 C43 C44 120.8(8) . . ?
C42 C43 H43 119.6 . . ?
C23 C24 C25 120.3(8) . . ?
C23 C24 H24 119.8 . . ?
C25 C24 H24 119.8 . . ?
C55 C54 C53 119.5(7) . . ?
C55 C54 H54 120.3 . . ?
C53 C54 H54 120.3 . . ?
C78 C79 H79 120.1 . . ?
C80 C79 C78 119.8(8) . . ?
C80 C79 H79 120.1 . . ?
C82 C83 H83 119.2 . . ?
C84 C83 C82 121.7(9) . . ?
C84 C83 H83 119.2 . . ?
C59 C60 H60 119.7 . . ?
C61 C60 C59 120.7(7) . . ?
C61 C60 H60 119.7 . . ?
C85 C84 H84 120.6 . . ?
C83 C84 C85 118.8(8) . . ?
C83 C84 H84 120.6 . . ?
Cl2 C93 H93A 109.1 . . ?
Cl2 C93 H93B 109.1 . . ?
Cl1 C93 Cl2 112.7(5) . . ?
Cl1 C93 H93A 109.1 . . ?
Cl1 C93 H93B 109.1 . . ?
H93A C93 H93B 107.8 . . ?
Cl3 C1A H1AA 109.0 . . ?
Cl3 C1A H1AB 109.0 . . ?
Cl4 C1A Cl3 112.9 . . ?
Cl4 C1A H1AA 109.0 . . ?
Cl4 C1A H1AB 109.0 . . ?
H1AA C1A H1AB 107.8 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_exp_1726_a
_database_code_depnum_ccdc_archive 'CCDC 1872120'
_audit_update_record             
;
2018-10-09 deposited with the CCDC.
2019-01-17 downloaded from the CCDC.
;
_audit_creation_date             2018-03-14
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C40 H60 Cl2 Cu2 O4 P4'
_chemical_formula_sum            'C40 H60 Cl2 Cu2 O4 P4'
_chemical_formula_weight         926.74
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 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'

_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                   9.1382(8)
_cell_length_b                   11.4943(8)
_cell_length_c                   12.1632(7)
_cell_angle_alpha                79.859(5)
_cell_angle_beta                 71.565(6)
_cell_angle_gamma                66.823(7)
_cell_volume                     1112.26(16)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    3370
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      73.1790
_cell_measurement_theta_min      5.4580
_shelx_estimated_absorpt_T_max   0.694
_shelx_estimated_absorpt_T_min   0.538
_exptl_absorpt_coefficient_mu    3.937
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66051
_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.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.384
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             484
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0482
_diffrn_reflns_av_unetI/netI     0.0557
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6787
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.772
_diffrn_reflns_theta_min         3.838
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6525
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -65.00  27.00   1.00    2.00    --  -41.14  38.00  30.00   92
  2  ω    -73.00  24.00   1.00    2.00    --  -41.14  77.00 120.00   97
  3  ω    100.00 128.00   1.00    2.00    --   41.14 178.00   0.00   28
  4  ω    101.00 176.00   1.00    7.00    --  106.40 125.00 -90.00   75
  5  ω    144.00 171.00   1.00    7.00    --  106.40  77.00-150.00   27
  6  ω     82.00 169.00   1.00    7.00    --  106.40  45.00 -30.00   87
  7  ω     82.00 135.00   1.00    7.00    --  106.40 -61.00-120.00   53
  8  ω     77.00 109.00   1.00    7.00    --  106.40 -95.00 -90.00   32
  9  ω     48.00 114.00   1.00    7.00    --  106.40 -77.00   0.00   66
 10  ω     47.00  78.00   1.00    7.00    --  106.40 -61.00-120.00   31
 11  ω     24.00  55.00   1.00    7.00    --  106.40 -95.00 -90.00   31
 12  ω     29.00  98.00   1.00    7.00    --  106.40 -95.00-150.00   69
 13  ω     76.00 112.00   1.00    7.00    --  106.40  77.00-150.00   36
 14  ω     56.00 173.00   1.00    7.00    --  106.40  15.00  90.00  117
 15  ω     93.00 120.00   1.00    7.00    --  106.40-125.00 150.00   27
 16  ω     38.00  64.00   1.00    7.00    --  106.40-125.00 150.00   26
 17  ω   -113.00 -17.00   1.00    2.00    --  -41.14 -38.00-150.00   96
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1628292000
_diffrn_orient_matrix_UB_12      -0.0161773000
_diffrn_orient_matrix_UB_13      0.0240958000
_diffrn_orient_matrix_UB_21      0.0895419000
_diffrn_orient_matrix_UB_22      -0.0145625000
_diffrn_orient_matrix_UB_23      -0.1302559000
_diffrn_orient_matrix_UB_31      -0.0424817000
_diffrn_orient_matrix_UB_32      0.1444193000
_diffrn_orient_matrix_UB_33      -0.0184386000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\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                3704
_reflns_number_total             4298
_reflns_odcompleteness_completeness 99.54
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_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 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.616
_refine_diff_density_min         -0.705
_refine_diff_density_rms         0.096
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     239
_refine_ls_number_reflns         4298
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0563
_refine_ls_R_factor_gt           0.0503
_refine_ls_restrained_S_all      1.035
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0850P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1304
_refine_ls_wR_factor_ref         0.1397
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C6(H6A,H6B),
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B)
2.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C14(H14), C2(H2A), C3(H3), C4(H4)
2.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C10(H10A,H10B,H10C)
2.d Idealised tetrahedral OH refined as rotating group:
 O2(H2), O1(H1)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.56588(5) 0.43008(4) 0.60260(4) 0.02675(15) Uani 1 1 d . . . . .
Cl1 Cl 0.66461(8) 0.37232(6) 0.40531(6) 0.02631(17) Uani 1 1 d . . . . .
P2 P 0.72708(8) 0.50227(6) 0.65321(6) 0.02552(18) Uani 1 1 d . . . . .
P1 P 0.48795(9) 0.27163(6) 0.70046(6) 0.02721(18) Uani 1 1 d . . . . .
O2 O 0.4979(2) 0.72364(19) 0.74089(19) 0.0310(4) Uani 1 1 d . . . . .
H2 H 0.4481 0.7013 0.7060 0.037 Uiso 1 1 calc GR . . . .
O1 O 0.5277(3) 0.1427(2) 0.5223(2) 0.0395(5) Uani 1 1 d . . . . .
H1 H 0.5772 0.1930 0.4903 0.047 Uiso 1 1 calc GR . . . .
C11 C 0.6596(3) 0.6448(2) 0.7174(2) 0.0244(5) Uani 1 1 d . . . . .
C12 C 0.7666(4) 0.6844(3) 0.7480(3) 0.0297(6) Uani 1 1 d . . . . .
H12 H 0.7230 0.7637 0.7820 0.036 Uiso 1 1 calc R . . . .
C13 C 0.9331(4) 0.6135(3) 0.7312(3) 0.0346(6) Uani 1 1 d . . . . .
H13 H 0.9974 0.6473 0.7547 0.041 Uiso 1 1 calc R . . . .
C14 C 1.0135(4) 0.4964(3) 0.6824(3) 0.0326(6) Uani 1 1 d . . . . .
H14 H 1.1283 0.4550 0.6759 0.039 Uiso 1 1 calc R . . . .
C15 C 0.9368(3) 0.4362(3) 0.6425(2) 0.0274(6) Uani 1 1 d . . . . .
C16 C 1.0291(4) 0.3095(3) 0.5877(3) 0.0326(6) Uani 1 1 d . . . . .
H16A H 1.1485 0.2958 0.5591 0.039 Uiso 1 1 calc R . . . .
H16B H 0.9897 0.3116 0.5201 0.039 Uiso 1 1 calc R . . . .
C17 C 1.0064(4) 0.1989(3) 0.6717(3) 0.0336(6) Uani 1 1 d . . . . .
H17A H 0.8870 0.2191 0.7107 0.040 Uiso 1 1 calc R . . . .
H17B H 1.0630 0.1874 0.7322 0.040 Uiso 1 1 calc R . . . .
C18 C 1.0746(5) 0.0753(3) 0.6114(3) 0.0468(8) Uani 1 1 d . . . . .
H18A H 1.1913 0.0593 0.5667 0.056 Uiso 1 1 calc R . . . .
H18B H 1.0113 0.0847 0.5556 0.056 Uiso 1 1 calc R . . . .
C19 C 1.0662(5) -0.0391(3) 0.6956(4) 0.0542(10) Uani 1 1 d . . . . .
H19A H 1.1228 -0.1165 0.6513 0.065 Uiso 1 1 calc R . . . .
H19B H 1.1279 -0.0471 0.7521 0.065 Uiso 1 1 calc R . . . .
C20 C 0.8933(5) -0.0330(3) 0.7617(4) 0.0536(10) Uani 1 1 d . . . . .
H20A H 0.8396 0.0386 0.8120 0.080 Uiso 1 1 calc GR . . . .
H20B H 0.8986 -0.1120 0.8094 0.080 Uiso 1 1 calc GR . . . .
H20C H 0.8294 -0.0217 0.7068 0.080 Uiso 1 1 calc GR . . . .
C1 C 0.4896(4) 0.1454(3) 0.6382(3) 0.0300(6) Uani 1 1 d . . . . .
C2 C 0.4498(4) 0.0453(3) 0.7056(3) 0.0365(7) Uani 1 1 d . . . . .
H2A H 0.4531 -0.0212 0.6671 0.044 Uiso 1 1 calc R . . . .
C3 C 0.4059(5) 0.0374(3) 0.8253(3) 0.0427(8) Uani 1 1 d . . . . .
H3 H 0.3806 -0.0344 0.8642 0.051 Uiso 1 1 calc R . . . .
C4 C 0.3960(5) 0.1280(3) 0.8936(3) 0.0408(7) Uani 1 1 d . . . . .
H4 H 0.3644 0.1140 0.9756 0.049 Uiso 1 1 calc R . . . .
C5 C 0.4299(4) 0.2372(3) 0.8480(3) 0.0319(6) Uani 1 1 d . . . . .
C6 C 0.4162(4) 0.3343(3) 0.9239(3) 0.0372(7) Uani 1 1 d . . . . .
H6A H 0.5168 0.3564 0.8950 0.045 Uiso 1 1 calc R . . . .
H6B H 0.4112 0.2964 1.0041 0.045 Uiso 1 1 calc R . . . .
C7 C 0.2646(4) 0.4549(3) 0.9263(3) 0.0384(7) Uani 1 1 d . . . . .
H7A H 0.1645 0.4362 0.9714 0.046 Uiso 1 1 calc R . . . .
H7B H 0.2559 0.4817 0.8459 0.046 Uiso 1 1 calc R . . . .
C8 C 0.2686(4) 0.5642(3) 0.9793(3) 0.0363(7) Uani 1 1 d . . . . .
H8A H 0.2672 0.5403 1.0618 0.044 Uiso 1 1 calc R . . . .
H8B H 0.3734 0.5780 0.9386 0.044 Uiso 1 1 calc R . . . .
C9 C 0.1258(5) 0.6863(4) 0.9722(5) 0.0592(11) Uani 1 1 d . . . . .
H9A H 0.0230 0.6770 1.0251 0.071 Uiso 1 1 calc R . . . .
H9B H 0.1140 0.7011 0.8922 0.071 Uiso 1 1 calc R . . . .
C10 C 0.1430(6) 0.8008(3) 1.0029(4) 0.0528(10) Uani 1 1 d . . . . .
H10A H 0.1591 0.7860 1.0809 0.079 Uiso 1 1 calc GR . . . .
H10B H 0.0426 0.8751 1.0013 0.079 Uiso 1 1 calc GR . . . .
H10C H 0.2386 0.8157 0.9466 0.079 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 Cu1 3.0378(8) 2_666 ?
Cu1 Cl1 2.4269(8) 2_666 ?
Cu1 Cl1 2.3946(8) . ?
Cu1 P2 2.2254(7) . ?
Cu1 P1 2.2276(7) . ?
Cl1 Cu1 2.4270(8) 2_666 ?
P2 C11 1.739(3) . ?
P2 C15 1.732(3) . ?
P1 C1 1.744(3) . ?
P1 C5 1.724(3) . ?
O2 H2 0.8400 . ?
O2 C11 1.363(3) . ?
O1 H1 0.8400 . ?
O1 C1 1.344(4) . ?
C11 C12 1.394(4) . ?
C12 H12 0.9500 . ?
C12 C13 1.381(4) . ?
C13 H13 0.9500 . ?
C13 C14 1.390(5) . ?
C14 H14 0.9500 . ?
C14 C15 1.385(4) . ?
C15 C16 1.515(4) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C16 C17 1.523(4) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C17 C18 1.525(4) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C18 C19 1.530(5) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19 C20 1.509(6) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C1 C2 1.392(4) . ?
C2 H2A 0.9500 . ?
C2 C3 1.379(5) . ?
C3 H3 0.9500 . ?
C3 C4 1.402(5) . ?
C4 H4 0.9500 . ?
C4 C5 1.389(4) . ?
C5 C6 1.514(5) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C6 C7 1.523(5) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C7 C8 1.527(4) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C8 C9 1.505(5) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C9 C10 1.506(5) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl1 Cu1 Cu1 51.42(2) . 2_666 ?
Cl1 Cu1 Cu1 50.47(2) 2_666 2_666 ?
Cl1 Cu1 Cl1 101.90(3) . 2_666 ?
P2 Cu1 Cu1 116.58(3) . 2_666 ?
P2 Cu1 Cl1 113.84(3) . . ?
P2 Cu1 Cl1 99.28(3) . 2_666 ?
P2 Cu1 P1 123.33(3) . . ?
P1 Cu1 Cu1 119.98(3) . 2_666 ?
P1 Cu1 Cl1 103.44(3) . . ?
P1 Cu1 Cl1 113.34(3) . 2_666 ?
Cu1 Cl1 Cu1 78.10(3) . 2_666 ?
C11 P2 Cu1 124.90(10) . . ?
C15 P2 Cu1 130.64(10) . . ?
C15 P2 C11 104.45(14) . . ?
C1 P1 Cu1 125.23(11) . . ?
C5 P1 Cu1 129.90(11) . . ?
C5 P1 C1 104.70(15) . . ?
C11 O2 H2 109.5 . . ?
C1 O1 H1 109.5 . . ?
O2 C11 P2 121.38(19) . . ?
O2 C11 C12 116.4(2) . . ?
C12 C11 P2 122.2(2) . . ?
C11 C12 H12 118.5 . . ?
C13 C12 C11 122.9(3) . . ?
C13 C12 H12 118.5 . . ?
C12 C13 H13 117.6 . . ?
C12 C13 C14 124.7(3) . . ?
C14 C13 H13 117.6 . . ?
C13 C14 H14 117.9 . . ?
C15 C14 C13 124.2(3) . . ?
C15 C14 H14 117.9 . . ?
C14 C15 P2 121.4(2) . . ?
C14 C15 C16 122.8(3) . . ?
C16 C15 P2 115.8(2) . . ?
C15 C16 H16A 109.0 . . ?
C15 C16 H16B 109.0 . . ?
C15 C16 C17 112.9(2) . . ?
H16A C16 H16B 107.8 . . ?
C17 C16 H16A 109.0 . . ?
C17 C16 H16B 109.0 . . ?
C16 C17 H17A 109.1 . . ?
C16 C17 H17B 109.1 . . ?
C16 C17 C18 112.5(3) . . ?
H17A C17 H17B 107.8 . . ?
C18 C17 H17A 109.1 . . ?
C18 C17 H17B 109.1 . . ?
C17 C18 H18A 108.9 . . ?
C17 C18 H18B 108.9 . . ?
C17 C18 C19 113.3(3) . . ?
H18A C18 H18B 107.7 . . ?
C19 C18 H18A 108.9 . . ?
C19 C18 H18B 108.9 . . ?
C18 C19 H19A 108.6 . . ?
C18 C19 H19B 108.6 . . ?
H19A C19 H19B 107.6 . . ?
C20 C19 C18 114.7(3) . . ?
C20 C19 H19A 108.6 . . ?
C20 C19 H19B 108.6 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O1 C1 P1 120.6(2) . . ?
O1 C1 C2 117.6(3) . . ?
C2 C1 P1 121.8(3) . . ?
C1 C2 H2A 118.3 . . ?
C3 C2 C1 123.4(3) . . ?
C3 C2 H2A 118.3 . . ?
C2 C3 H3 117.7 . . ?
C2 C3 C4 124.6(3) . . ?
C4 C3 H3 117.7 . . ?
C3 C4 H4 118.2 . . ?
C5 C4 C3 123.6(3) . . ?
C5 C4 H4 118.2 . . ?
C4 C5 P1 121.8(3) . . ?
C4 C5 C6 122.6(3) . . ?
C6 C5 P1 115.6(2) . . ?
C5 C6 H6A 109.0 . . ?
C5 C6 H6B 109.0 . . ?
C5 C6 C7 112.8(3) . . ?
H6A C6 H6B 107.8 . . ?
C7 C6 H6A 109.0 . . ?
C7 C6 H6B 109.0 . . ?
C6 C7 H7A 108.9 . . ?
C6 C7 H7B 108.9 . . ?
C6 C7 C8 113.5(3) . . ?
H7A C7 H7B 107.7 . . ?
C8 C7 H7A 108.9 . . ?
C8 C7 H7B 108.9 . . ?
C7 C8 H8A 108.9 . . ?
C7 C8 H8B 108.9 . . ?
H8A C8 H8B 107.7 . . ?
C9 C8 C7 113.3(3) . . ?
C9 C8 H8A 108.9 . . ?
C9 C8 H8B 108.9 . . ?
C8 C9 H9A 108.7 . . ?
C8 C9 H9B 108.7 . . ?
C8 C9 C10 114.3(3) . . ?
H9A C9 H9B 107.6 . . ?
C10 C9 H9A 108.7 . . ?
C10 C9 H9B 108.7 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?

_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.493
_oxdiff_exptl_absorpt_empirical_full_min 0.519
####################################################################### 
# 
# 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_exp_1748
_database_code_depnum_ccdc_archive 'CCDC 1872114'
_audit_update_record             
;
2018-10-09 deposited with the CCDC.
2019-01-17 downloaded from the CCDC.
;
_audit_creation_date             2018-03-14
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C28 H36 Cl2 Cu2 O4 P4'
_chemical_formula_sum            'C28 H36 Cl2 Cu2 O4 P4'
_chemical_formula_weight         758.43
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 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'
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'
P P 0.2955 0.4335 '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                   8.0889(4)
_cell_length_b                   9.7187(5)
_cell_length_c                   10.6284(5)
_cell_angle_alpha                78.259(4)
_cell_angle_beta                 87.754(4)
_cell_angle_gamma                80.431(4)
_cell_volume                     806.66(7)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    3088
_cell_measurement_temperature    290.85(10)
_cell_measurement_theta_max      72.8260
_cell_measurement_theta_min      5.5380
_shelx_estimated_absorpt_T_max   0.504
_shelx_estimated_absorpt_T_min   0.403
_exptl_absorpt_coefficient_mu    5.293
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.10003
_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.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.561
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             388
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0353
_diffrn_reflns_av_unetI/netI     0.0369
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.948
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4593
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.247
_diffrn_reflns_theta_min         4.249
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      290.85(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6525
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -66.00  27.00   1.00    1.00    --  -41.14  57.00  60.00   93
  2  ω   -106.00 -13.00   1.00    1.00    --  -41.14 -57.00 -90.00   93
  3  ω   -130.00 -37.00   1.00    1.00    --  -41.14-178.00  60.00   93
  4  ω     79.00 121.00   1.00    1.00    --  106.40-125.00 150.00   42
  5  ω     46.00  72.00   1.00    1.00    --  106.40-125.00 150.00   26
  6  ω     33.00 139.00   1.00    1.00    --  106.40 -77.00 -60.00  106
  7  ω     81.00 165.00   1.00    1.00    --  106.40  45.00  30.00   84
  8  ω     96.00 177.00   1.00    1.00    --  106.40 125.00 -90.00   81
  9  ω     96.00 148.00   1.00    1.00    --  106.40 125.00  30.00   52
 10  ω     86.00 178.00   1.00    1.00    --  106.40  61.00 -30.00   92
 11  ω     77.00 157.00   1.00    1.00    --  106.40  61.00  90.00   80
 12  ω     30.00 107.00   1.00    1.00    --  106.40 -95.00-120.00   77
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0305249000
_diffrn_orient_matrix_UB_12      0.1363478000
_diffrn_orient_matrix_UB_13      0.0560807000
_diffrn_orient_matrix_UB_21      -0.0175996000
_diffrn_orient_matrix_UB_22      0.0911829000
_diffrn_orient_matrix_UB_23      -0.1369395000
_diffrn_orient_matrix_UB_31      -0.1899021000
_diffrn_orient_matrix_UB_32      -0.0033749000
_diffrn_orient_matrix_UB_33      0.0045130000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\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                2904
_reflns_number_total             3062
_reflns_odcompleteness_completeness 98.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_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 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.898
_refine_diff_density_min         -0.843
_refine_diff_density_rms         0.133
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         3062
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0555
_refine_ls_restrained_S_all      1.121
_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)+(0.0941P)²+1.1527P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1528
_refine_ls_wR_factor_ref         0.1545
_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, All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C11(H11), C2(H2A), C9(H9), C4(H4)
2.b Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C6(H6A,H6B,H6C), C14(H14A,H14B,H14C), C7(H7A,H7B,H7C)
2.c Idealised tetrahedral OH refined as rotating group:
 O2(H2), O1(H1)
;
_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
Cu1 Cu 0.86334(6) 0.46080(5) 0.56516(5) 0.0199(2) Uani 1 1 d . . . . .
Cl1 Cl 0.91324(11) 0.26179(9) 0.73255(8) 0.0237(2) Uani 1 1 d . . . . .
P1 P 0.62434(11) 0.58658(9) 0.62540(8) 0.0197(2) Uani 1 1 d . . . . .
P2 P 0.94076(11) 0.37371(9) 0.38812(8) 0.0182(2) Uani 1 1 d . . . . .
O2 O 1.1167(3) 0.1315(3) 0.5238(3) 0.0273(6) Uani 1 1 d . . . . .
H2 H 1.0561 0.1627 0.5812 0.041 Uiso 1 1 calc GR . . . .
O1 O 0.6785(4) 0.4672(3) 0.8764(3) 0.0324(6) Uani 1 1 d . . . . .
H1 H 0.7278 0.4052 0.8372 0.049 Uiso 1 1 calc GR . . . .
C8 C 1.0613(4) 0.2036(4) 0.4077(3) 0.0199(7) Uani 1 1 d . . . . .
C12 C 0.8972(4) 0.4193(4) 0.2242(3) 0.0198(7) Uani 1 1 d . . . . .
C10 C 1.0677(5) 0.1997(4) 0.1767(4) 0.0235(7) Uani 1 1 d . . . . .
C13 C 0.7840(5) 0.5578(4) 0.1748(3) 0.0238(7) Uani 1 1 d . . . . .
H13A H 0.6796 0.5619 0.2248 0.036 Uiso 1 1 calc GR . . . .
H13B H 0.7587 0.5644 0.0841 0.036 Uiso 1 1 calc GR . . . .
H13C H 0.8402 0.6374 0.1832 0.036 Uiso 1 1 calc GR . . . .
C11 C 0.9640(5) 0.3314(4) 0.1409(3) 0.0232(7) Uani 1 1 d . . . . .
H11 H 0.9372 0.3632 0.0524 0.028 Uiso 1 1 calc R . . . .
C5 C 0.5052(4) 0.7487(4) 0.5581(4) 0.0222(7) Uani 1 1 d . . . . .
C1 C 0.6028(5) 0.5809(4) 0.7903(4) 0.0243(7) Uani 1 1 d . . . . .
C2 C 0.5044(5) 0.6883(4) 0.8413(4) 0.0263(8) Uani 1 1 d . . . . .
H2A H 0.4965 0.6767 0.9321 0.032 Uiso 1 1 calc R . . . .
C9 C 1.1093(5) 0.1382(4) 0.3039(4) 0.0232(7) Uani 1 1 d . . . . .
H9 H 1.1746 0.0458 0.3210 0.028 Uiso 1 1 calc R . . . .
C4 C 0.4184(5) 0.8371(4) 0.6329(4) 0.0253(8) Uani 1 1 d . . . . .
H4 H 0.3538 0.9232 0.5895 0.030 Uiso 1 1 calc R . . . .
C3 C 0.4171(5) 0.8113(4) 0.7673(4) 0.0275(8) Uani 1 1 d . . . . .
C6 C 0.4958(5) 0.7867(4) 0.4136(4) 0.0277(8) Uani 1 1 d . . . . .
H6A H 0.6040 0.7524 0.3768 0.041 Uiso 1 1 calc GR . . . .
H6B H 0.4687 0.8903 0.3859 0.041 Uiso 1 1 calc GR . . . .
H6C H 0.4084 0.7420 0.3842 0.041 Uiso 1 1 calc GR . . . .
C14 C 1.1365(6) 0.1178(4) 0.0747(4) 0.0332(9) Uani 1 1 d . . . . .
H14A H 1.0589 0.1413 0.0022 0.050 Uiso 1 1 calc GR . . . .
H14B H 1.1498 0.0154 0.1107 0.050 Uiso 1 1 calc GR . . . .
H14C H 1.2457 0.1434 0.0451 0.050 Uiso 1 1 calc GR . . . .
C7 C 0.3206(6) 0.9220(5) 0.8356(5) 0.0371(10) Uani 1 1 d . . . . .
H7A H 0.2806 0.8748 0.9189 0.056 Uiso 1 1 calc GR . . . .
H7B H 0.2245 0.9745 0.7832 0.056 Uiso 1 1 calc GR . . . .
H7C H 0.3940 0.9883 0.8490 0.056 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 Cu1 2.6976(10) 2_766 ?
Cu1 Cl1 2.3378(9) . ?
Cu1 P1 2.2534(10) . ?
Cu1 P2 2.2424(9) . ?
Cu1 P2 2.5648(10) 2_766 ?
P1 C5 1.736(4) . ?
P1 C1 1.745(4) . ?
P2 Cu1 2.5648(10) 2_766 ?
P2 C8 1.752(4) . ?
P2 C12 1.743(3) . ?
O2 H2 0.8400 . ?
O2 C8 1.343(4) . ?
O1 H1 0.8400 . ?
O1 C1 1.357(5) . ?
C8 C9 1.393(5) . ?
C12 C13 1.506(5) . ?
C12 C11 1.386(5) . ?
C10 C11 1.399(5) . ?
C10 C9 1.392(5) . ?
C10 C14 1.508(5) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C11 H11 0.9500 . ?
C5 C4 1.378(5) . ?
C5 C6 1.506(5) . ?
C1 C2 1.391(5) . ?
C2 H2A 0.9500 . ?
C2 C3 1.388(6) . ?
C9 H9 0.9500 . ?
C4 H4 0.9500 . ?
C4 C3 1.398(6) . ?
C3 C7 1.513(5) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl1 Cu1 Cu1 115.87(4) . 2_766 ?
Cl1 Cu1 P2 104.33(3) . 2_766 ?
P1 Cu1 Cu1 132.54(4) . 2_766 ?
P1 Cu1 Cl1 103.57(4) . . ?
P1 Cu1 P2 96.35(3) . 2_766 ?
P2 Cu1 Cu1 50.36(3) 2_766 2_766 ?
P2 Cu1 Cu1 61.74(3) . 2_766 ?
P2 Cu1 Cl1 104.00(3) . . ?
P2 Cu1 P1 133.39(4) . . ?
P2 Cu1 P2 112.11(3) . 2_766 ?
C5 P1 Cu1 133.37(13) . . ?
C5 P1 C1 103.38(18) . . ?
C1 P1 Cu1 115.06(13) . . ?
Cu1 P2 Cu1 67.89(3) . 2_766 ?
C8 P2 Cu1 106.20(12) . 2_766 ?
C8 P2 Cu1 117.94(12) . . ?
C12 P2 Cu1 137.73(13) . . ?
C12 P2 Cu1 107.31(12) . 2_766 ?
C12 P2 C8 103.90(17) . . ?
C8 O2 H2 109.5 . . ?
C1 O1 H1 109.5 . . ?
O2 C8 P2 121.3(3) . . ?
O2 C8 C9 116.6(3) . . ?
C9 C8 P2 122.1(3) . . ?
C13 C12 P2 118.0(3) . . ?
C11 C12 P2 121.5(3) . . ?
C11 C12 C13 120.5(3) . . ?
C11 C10 C14 119.5(3) . . ?
C9 C10 C11 122.9(3) . . ?
C9 C10 C14 117.6(3) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C11 C10 125.3(3) . . ?
C12 C11 H11 117.4 . . ?
C10 C11 H11 117.4 . . ?
C4 C5 P1 121.8(3) . . ?
C4 C5 C6 121.1(3) . . ?
C6 C5 P1 117.0(3) . . ?
O1 C1 P1 120.9(3) . . ?
O1 C1 C2 116.3(3) . . ?
C2 C1 P1 122.8(3) . . ?
C1 C2 H2A 118.0 . . ?
C3 C2 C1 123.9(4) . . ?
C3 C2 H2A 118.0 . . ?
C8 C9 H9 117.9 . . ?
C10 C9 C8 124.2(3) . . ?
C10 C9 H9 117.9 . . ?
C5 C4 H4 117.1 . . ?
C5 C4 C3 125.7(4) . . ?
C3 C4 H4 117.1 . . ?
C2 C3 C4 122.4(3) . . ?
C2 C3 C7 118.2(4) . . ?
C4 C3 C7 119.4(4) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C10 C14 H14A 109.5 . . ?
C10 C14 H14B 109.5 . . ?
C10 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C3 C7 H7A 109.5 . . ?
C3 C7 H7B 109.5 . . ?
C3 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?

_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 4.635
_oxdiff_exptl_absorpt_empirical_full_min 0.527
####################################################################### 
# 
# 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_exp_1709
_database_code_depnum_ccdc_archive 'CCDC 1872122'
_audit_update_record             
;
2018-10-09 deposited with the CCDC.
2019-01-17 downloaded from the CCDC.
;
_audit_creation_date             2018-03-14
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C58 H72 Na2 O14 P2, C4 H8 O'
_chemical_formula_sum            'C62 H80 Na2 O15 P2'
_chemical_formula_weight         1173.18
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H N O P Na'
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'
Na Na 0.1353 0.1239 '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'

_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      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   27.5839(10)
_cell_length_b                   9.1559(2)
_cell_length_c                   28.1190(11)
_cell_angle_alpha                90
_cell_angle_beta                 121.726(5)
_cell_angle_gamma                90
_cell_volume                     6040.4(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    7737
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      73.4410
_cell_measurement_theta_min      3.6240
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.339
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83177
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.290
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2496
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0244
_diffrn_reflns_av_unetI/netI     0.0240
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            17565
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.905
_diffrn_reflns_theta_min         3.635
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector_area_resol_mean 10.6525
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega -114.00  -14.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.7038  -57.0000   30.0000 100

#__ type_ start__ end____ width___ exp.time_
  2 omega  -71.00   35.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.7038   77.0000  150.0000 106

#__ type_ start__ end____ width___ exp.time_
  3 omega   -6.00   79.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       40.7038  -93.0000  -69.0000 85

#__ type_ start__ end____ width___ exp.time_
  4 omega   34.00   95.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7326  -45.0000   30.0000 61

#__ type_ start__ end____ width___ exp.time_
  5 omega   41.00   86.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7326  -30.0000  120.0000 45

#__ type_ start__ end____ width___ exp.time_
  6 omega   38.00  109.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7326  -95.0000  -90.0000 71

#__ type_ start__ end____ width___ exp.time_
  7 omega   92.00  177.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7326   30.0000 -180.0000 85

#__ type_ start__ end____ width___ exp.time_
  8 omega   60.00  170.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7326   15.0000  -60.0000 110

#__ type_ start__ end____ width___ exp.time_
  9 omega  110.00  170.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7326  125.0000  120.0000 60

#__ type_ start__ end____ width___ exp.time_
 10 omega   37.00  137.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7326  -77.0000  120.0000 100

#__ type_ start__ end____ width___ exp.time_
 11 omega   26.00  109.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7326  -95.0000   60.0000 83

#__ type_ start__ end____ width___ exp.time_
 12 omega   34.00   98.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7326  -45.0000 -120.0000 64
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0426422000
_diffrn_orient_matrix_UB_12      -0.0634375000
_diffrn_orient_matrix_UB_13      -0.0142397000
_diffrn_orient_matrix_UB_21      0.0478665000
_diffrn_orient_matrix_UB_22      0.0096717000
_diffrn_orient_matrix_UB_23      0.0620853000
_diffrn_orient_matrix_UB_31      -0.0143109000
_diffrn_orient_matrix_UB_32      -0.1554907000
_diffrn_orient_matrix_UB_33      0.0096466000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5196
_reflns_number_total             6005
_reflns_odcompleteness_completeness 99.70
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.681
_refine_diff_density_min         -0.551
_refine_diff_density_rms         0.047
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         6005
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0381
_refine_ls_restrained_S_all      1.061
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0496P)²+5.6347P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0970
_refine_ls_wR_factor_ref         0.1015
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Others
 Fixed Sof: O2(0.5) C31(0.5) H31A(0.5) H31B(0.5) C32(0.5) H32A(0.5) H32B(0.5)
 C33(0.5) H33A(0.5) H33B(0.5) C34(0.5) H34A(0.5) H34B(0.5)
3.a Free rotating group:
 O2(C31,C32,C33,C34)
3.b Secondary CH2 refined with riding coordinates:
 C24(H24A,H24B), C19(H19A,H19B), C22(H22A,H22B), C30(H30A,H30B), C20(H20A,
 H20B), C23(H23A,H23B), C29(H29A,H29B), C27(H27A,H27B), C25(H25A,H25B),
 C21(H21A,H21B), C26(H26A,H26B), C28(H28A,H28B), C31(H31A,H31B), C32(H32A,H32B),
  C33(H33A,H33B), C34(H34A,H34B)
3.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C17(H17), C13(H13), C14(H14), C15(H15), C16(H16), C7(H7),
 C11(H11), C8(H8), C10(H10), C9(H9)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.39685(2) 0.75423(4) 0.43210(2) 0.02139(10) Uani 1 1 d . . . . .
Na1 Na 0.31128(3) 0.39561(6) 0.48392(3) 0.02146(14) Uani 1 1 d . . . . .
O6 O 0.38671(4) 0.52553(11) 0.57916(5) 0.0221(2) Uani 1 1 d . . . . .
O5 O 0.26859(4) 0.54863(11) 0.52721(5) 0.0211(2) Uani 1 1 d . . . . .
O7 O 0.42098(4) 0.30260(12) 0.53352(5) 0.0229(2) Uani 1 1 d . . . . .
O4 O 0.18683(4) 0.32393(11) 0.45882(5) 0.0209(2) Uani 1 1 d . . . . .
O3 O 0.22321(5) 0.29025(13) 0.38240(5) 0.0245(2) Uani 1 1 d . . . . .
O8 O 0.33607(5) 0.28048(13) 0.42001(5) 0.0253(2) Uani 1 1 d . . . . .
O1 O 0.32653(5) 0.60779(12) 0.45272(5) 0.0270(3) Uani 1 1 d . . . . .
C2 C 0.27799(6) 0.72532(15) 0.36600(6) 0.0167(3) Uani 1 1 d . . . . .
H2 H 0.2432 0.6908 0.3611 0.020 Uiso 1 1 calc R . . . .
C4 C 0.32351(6) 0.86569(15) 0.32481(6) 0.0173(3) Uani 1 1 d . . . . .
H4 H 0.3183 0.9182 0.2933 0.021 Uiso 1 1 calc R . . . .
C3 C 0.27465(6) 0.80886(15) 0.32262(6) 0.0167(3) Uani 1 1 d . . . . .
C12 C 0.21738(6) 0.83884(16) 0.27244(6) 0.0169(3) Uani 1 1 d . . . . .
C5 C 0.37853(6) 0.84891(15) 0.37041(6) 0.0180(3) Uani 1 1 d . . . . .
C1 C 0.32922(7) 0.68759(15) 0.41698(6) 0.0201(3) Uani 1 1 d . . . . .
C6 C 0.42626(6) 0.90737(16) 0.36562(6) 0.0196(3) Uani 1 1 d . . . . .
C17 C 0.20608(6) 0.96963(16) 0.24264(6) 0.0194(3) Uani 1 1 d . . . . .
H17 H 0.2354 1.0405 0.2546 0.023 Uiso 1 1 calc R . . . .
C13 C 0.17295(6) 0.73673(16) 0.25334(6) 0.0193(3) Uani 1 1 d . . . . .
H13 H 0.1796 0.6469 0.2727 0.023 Uiso 1 1 calc R . . . .
C14 C 0.11940(7) 0.76474(17) 0.20660(7) 0.0237(3) Uani 1 1 d . . . . .
H14 H 0.0898 0.6945 0.1944 0.028 Uiso 1 1 calc R . . . .
C15 C 0.10916(6) 0.89521(18) 0.17782(7) 0.0245(3) Uani 1 1 d . . . . .
H15 H 0.0726 0.9146 0.1459 0.029 Uiso 1 1 calc R . . . .
C24 C 0.36005(7) 0.66289(16) 0.57363(7) 0.0224(3) Uani 1 1 d . . . . .
H24A H 0.3506 0.7103 0.5381 0.027 Uiso 1 1 calc R . . . .
H24B H 0.3860 0.7280 0.6049 0.027 Uiso 1 1 calc R . . . .
C19 C 0.17010(6) 0.35627(17) 0.36523(7) 0.0232(3) Uani 1 1 d . . . . .
H19A H 0.1425 0.3361 0.3252 0.028 Uiso 1 1 calc R . . . .
H19B H 0.1746 0.4634 0.3706 0.028 Uiso 1 1 calc R . . . .
C22 C 0.21955(7) 0.50957(17) 0.52940(7) 0.0224(3) Uani 1 1 d . . . . .
H22A H 0.2067 0.5948 0.5416 0.027 Uiso 1 1 calc R . . . .
H22B H 0.2295 0.4300 0.5569 0.027 Uiso 1 1 calc R . . . .
C30 C 0.24210(7) 0.31260(18) 0.34452(7) 0.0241(3) Uani 1 1 d . . . . .
H30A H 0.2497 0.4175 0.3427 0.029 Uiso 1 1 calc R . . . .
H30B H 0.2127 0.2794 0.3065 0.029 Uiso 1 1 calc R . . . .
C16 C 0.15256(7) 0.99760(17) 0.19573(7) 0.0234(3) Uani 1 1 d . . . . .
H16 H 0.1457 1.0868 0.1759 0.028 Uiso 1 1 calc R . . . .
C20 C 0.14945(6) 0.29174(17) 0.40073(7) 0.0229(3) Uani 1 1 d . . . . .
H20A H 0.1110 0.3306 0.3881 0.027 Uiso 1 1 calc R . . . .
H20B H 0.1462 0.1845 0.3955 0.027 Uiso 1 1 calc R . . . .
C7 C 0.47133(6) 0.98633(16) 0.40897(7) 0.0232(3) Uani 1 1 d . . . . .
H7 H 0.4726 1.0006 0.4431 0.028 Uiso 1 1 calc R . . . .
C11 C 0.42685(7) 0.88381(17) 0.31682(7) 0.0238(3) Uani 1 1 d . . . . .
H11 H 0.3971 0.8288 0.2872 0.029 Uiso 1 1 calc R . . . .
C23 C 0.30661(7) 0.63613(17) 0.57420(7) 0.0232(3) Uani 1 1 d . . . . .
H23A H 0.3161 0.5855 0.6092 0.028 Uiso 1 1 calc R . . . .
H23B H 0.2882 0.7304 0.5726 0.028 Uiso 1 1 calc R . . . .
C29 C 0.29560(7) 0.22567(18) 0.36596(7) 0.0238(3) Uani 1 1 d . . . . .
H29A H 0.2881 0.1209 0.3682 0.029 Uiso 1 1 calc R . . . .
H29B H 0.3102 0.2362 0.3406 0.029 Uiso 1 1 calc R . . . .
C27 C 0.43300(7) 0.31545(19) 0.49006(7) 0.0270(3) Uani 1 1 d . . . . .
H27A H 0.4725 0.2834 0.5039 0.032 Uiso 1 1 calc R . . . .
H27B H 0.4291 0.4184 0.4778 0.032 Uiso 1 1 calc R . . . .
C25 C 0.43847(6) 0.53772(17) 0.57962(7) 0.0241(3) Uani 1 1 d . . . . .
H25A H 0.4670 0.5945 0.6126 0.029 Uiso 1 1 calc R . . . .
H25B H 0.4316 0.5878 0.5454 0.029 Uiso 1 1 calc R . . . .
C8 C 0.51429(7) 1.04418(18) 0.40260(8) 0.0289(4) Uani 1 1 d . . . . .
H8 H 0.5442 1.0994 0.4321 0.035 Uiso 1 1 calc R . . . .
C21 C 0.17262(7) 0.46044(16) 0.47305(7) 0.0234(3) Uani 1 1 d . . . . .
H21A H 0.1369 0.4499 0.4731 0.028 Uiso 1 1 calc R . . . .
H21B H 0.1662 0.5347 0.4447 0.028 Uiso 1 1 calc R . . . .
C26 C 0.45971(6) 0.38428(17) 0.58209(7) 0.0252(3) Uani 1 1 d . . . . .
H26A H 0.4973 0.3883 0.5855 0.030 Uiso 1 1 calc R . . . .
H26B H 0.4648 0.3344 0.6157 0.030 Uiso 1 1 calc R . . . .
C28 C 0.39160(7) 0.22119(18) 0.44207(7) 0.0269(3) Uani 1 1 d . . . . .
H28A H 0.4014 0.2197 0.4129 0.032 Uiso 1 1 calc R . . . .
H28B H 0.3931 0.1198 0.4550 0.032 Uiso 1 1 calc R . . . .
C10 C 0.47042(7) 0.93984(19) 0.31095(8) 0.0290(4) Uani 1 1 d . . . . .
H10 H 0.4704 0.9219 0.2777 0.035 Uiso 1 1 calc R . . . .
C9 C 0.51374(7) 1.02176(18) 0.35366(8) 0.0313(4) Uani 1 1 d . . . . .
H9 H 0.5429 1.0623 0.3493 0.038 Uiso 1 1 calc R . . . .
O2 O 0.47429(12) 0.6484(3) 0.22604(13) 0.0549(8) Uani 0.5 1 d . . P A -1
C31 C 0.44138(13) 0.5358(4) 0.23220(16) 0.0572(13) Uani 0.5 1 d G . P A -1
H31A H 0.4028 0.5298 0.1982 0.069 Uiso 0.5 1 calc R . P A -1
H31B H 0.4376 0.5568 0.2647 0.069 Uiso 0.5 1 calc R . P A -1
C32 C 0.4739(2) 0.3922(3) 0.2412(2) 0.0505(15) Uani 0.5 1 d G . P A -1
H32A H 0.4629 0.3453 0.2051 0.061 Uiso 0.5 1 calc R . P A -1
H32B H 0.4674 0.3228 0.2643 0.061 Uiso 0.5 1 calc R . P A -1
C33 C 0.53597(16) 0.4460(4) 0.27205(19) 0.0521(15) Uani 0.5 1 d G . P A -1
H33A H 0.5513 0.4602 0.3124 0.063 Uiso 0.5 1 calc R . P A -1
H33B H 0.5609 0.3774 0.2673 0.063 Uiso 0.5 1 calc R . P A -1
C34 C 0.52980(13) 0.5918(4) 0.24246(17) 0.0728(17) Uani 0.5 1 d G . P A -1
H34A H 0.5600 0.6607 0.2681 0.087 Uiso 0.5 1 calc R . P A -1
H34B H 0.5328 0.5766 0.2092 0.087 Uiso 0.5 1 calc R . P A -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1 C5 1.7589(15) . ?
P1 C1 1.7887(16) . ?
Na1 O6 2.6564(13) . ?
Na1 O5 2.5176(12) . ?
Na1 O7 2.7181(12) . ?
Na1 O4 2.5588(12) 7_556 ?
Na1 O3 2.7727(13) . ?
Na1 O8 2.4701(12) . ?
Na1 O1 2.2603(13) . ?
O6 C24 1.4235(18) . ?
O6 C25 1.4253(18) . ?
O5 C22 1.4316(17) . ?
O5 C23 1.4248(19) . ?
O7 C27 1.430(2) . ?
O7 C26 1.4253(19) . ?
O4 Na1 2.5588(12) 7_556 ?
O4 C20 1.4308(19) . ?
O4 C21 1.4287(18) . ?
O3 C19 1.4146(18) . ?
O3 C30 1.4253(19) . ?
O8 C29 1.4225(19) . ?
O8 C28 1.4234(19) . ?
O1 C1 1.2757(19) . ?
C2 H2 0.9500 . ?
C2 C3 1.401(2) . ?
C2 C1 1.428(2) . ?
C4 H4 0.9500 . ?
C4 C3 1.416(2) . ?
C4 C5 1.387(2) . ?
C3 C12 1.489(2) . ?
C12 C17 1.400(2) . ?
C12 C13 1.404(2) . ?
C5 C6 1.492(2) . ?
C6 C7 1.400(2) . ?
C6 C11 1.398(2) . ?
C17 H17 0.9500 . ?
C17 C16 1.392(2) . ?
C13 H13 0.9500 . ?
C13 C14 1.390(2) . ?
C14 H14 0.9500 . ?
C14 C15 1.386(2) . ?
C15 H15 0.9500 . ?
C15 C16 1.390(2) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C24 C23 1.503(2) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19 C20 1.506(2) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C22 C21 1.494(2) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C30 C29 1.496(2) . ?
C16 H16 0.9500 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C7 H7 0.9500 . ?
C7 C8 1.393(2) . ?
C11 H11 0.9500 . ?
C11 C10 1.394(2) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C27 C28 1.500(2) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C26 1.510(2) . ?
C8 H8 0.9500 . ?
C8 C9 1.384(3) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C10 H10 0.9500 . ?
C10 C9 1.387(3) . ?
C9 H9 0.9500 . ?
O2 C31 1.4432 . ?
O2 C34 1.4433 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C32 1.5353 . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C32 C33 1.5388 . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C33 C34 1.5345 . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C5 P1 C1 102.17(7) . . ?
O6 Na1 O7 63.42(4) . . ?
O6 Na1 O3 172.53(4) . . ?
O5 Na1 O6 65.22(4) . . ?
O5 Na1 O7 127.14(4) . . ?
O5 Na1 O4 89.59(4) . 7_556 ?
O5 Na1 O3 108.19(4) . . ?
O7 Na1 O3 123.75(4) . . ?
O4 Na1 O6 88.36(4) 7_556 . ?
O4 Na1 O7 77.42(4) 7_556 . ?
O4 Na1 O3 95.25(4) 7_556 . ?
O8 Na1 O6 123.70(4) . . ?
O8 Na1 O5 165.48(5) . . ?
O8 Na1 O7 65.18(4) . . ?
O8 Na1 O4 101.58(4) . 7_556 ?
O8 Na1 O3 61.99(4) . . ?
O1 Na1 O6 78.43(4) . . ?
O1 Na1 O5 86.52(4) . . ?
O1 Na1 O7 94.83(4) . . ?
O1 Na1 O4 166.67(5) . 7_556 ?
O1 Na1 O3 98.08(4) . . ?
O1 Na1 O8 84.55(5) . . ?
C24 O6 Na1 101.52(8) . . ?
C24 O6 C25 112.91(11) . . ?
C25 O6 Na1 107.10(9) . . ?
C22 O5 Na1 125.07(9) . . ?
C23 O5 Na1 117.26(9) . . ?
C23 O5 C22 110.60(11) . . ?
C27 O7 Na1 103.39(9) . . ?
C26 O7 Na1 113.48(9) . . ?
C26 O7 C27 112.47(12) . . ?
C20 O4 Na1 108.70(8) . 7_556 ?
C21 O4 Na1 115.39(9) . 7_556 ?
C21 O4 C20 111.15(11) . . ?
C19 O3 Na1 113.09(9) . . ?
C19 O3 C30 113.80(12) . . ?
C30 O3 Na1 104.65(9) . . ?
C29 O8 Na1 124.45(9) . . ?
C29 O8 C28 113.03(12) . . ?
C28 O8 Na1 119.46(10) . . ?
C1 O1 Na1 153.87(11) . . ?
C3 C2 H2 117.2 . . ?
C3 C2 C1 125.67(13) . . ?
C1 C2 H2 117.2 . . ?
C3 C4 H4 118.2 . . ?
C5 C4 H4 118.2 . . ?
C5 C4 C3 123.60(14) . . ?
C2 C3 C4 122.51(13) . . ?
C2 C3 C12 118.49(13) . . ?
C4 C3 C12 119.01(13) . . ?
C17 C12 C3 121.08(13) . . ?
C17 C12 C13 117.77(13) . . ?
C13 C12 C3 121.14(13) . . ?
C4 C5 P1 125.00(12) . . ?
C4 C5 C6 117.73(13) . . ?
C6 C5 P1 117.16(11) . . ?
O1 C1 P1 119.57(12) . . ?
O1 C1 C2 119.50(14) . . ?
C2 C1 P1 120.91(11) . . ?
C7 C6 C5 121.90(14) . . ?
C11 C6 C5 120.00(14) . . ?
C11 C6 C7 118.10(14) . . ?
C12 C17 H17 119.5 . . ?
C16 C17 C12 121.07(14) . . ?
C16 C17 H17 119.5 . . ?
C12 C13 H13 119.4 . . ?
C14 C13 C12 121.21(14) . . ?
C14 C13 H13 119.4 . . ?
C13 C14 H14 120.0 . . ?
C15 C14 C13 120.00(14) . . ?
C15 C14 H14 120.0 . . ?
C14 C15 H15 120.1 . . ?
C14 C15 C16 119.83(15) . . ?
C16 C15 H15 120.1 . . ?
O6 C24 H24A 110.1 . . ?
O6 C24 H24B 110.1 . . ?
O6 C24 C23 107.94(12) . . ?
H24A C24 H24B 108.4 . . ?
C23 C24 H24A 110.1 . . ?
C23 C24 H24B 110.1 . . ?
O3 C19 H19A 110.3 . . ?
O3 C19 H19B 110.3 . . ?
O3 C19 C20 106.92(12) . . ?
H19A C19 H19B 108.6 . . ?
C20 C19 H19A 110.3 . . ?
C20 C19 H19B 110.3 . . ?
O5 C22 H22A 109.7 . . ?
O5 C22 H22B 109.7 . . ?
O5 C22 C21 109.93(13) . . ?
H22A C22 H22B 108.2 . . ?
C21 C22 H22A 109.7 . . ?
C21 C22 H22B 109.7 . . ?
O3 C30 H30A 110.3 . . ?
O3 C30 H30B 110.3 . . ?
O3 C30 C29 107.04(12) . . ?
H30A C30 H30B 108.6 . . ?
C29 C30 H30A 110.3 . . ?
C29 C30 H30B 110.3 . . ?
C17 C16 H16 119.9 . . ?
C15 C16 C17 120.11(14) . . ?
C15 C16 H16 119.9 . . ?
O4 C20 C19 112.29(12) . . ?
O4 C20 H20A 109.1 . . ?
O4 C20 H20B 109.1 . . ?
C19 C20 H20A 109.1 . . ?
C19 C20 H20B 109.1 . . ?
H20A C20 H20B 107.9 . . ?
C6 C7 H7 119.7 . . ?
C8 C7 C6 120.68(16) . . ?
C8 C7 H7 119.7 . . ?
C6 C11 H11 119.5 . . ?
C10 C11 C6 121.02(16) . . ?
C10 C11 H11 119.5 . . ?
O5 C23 C24 109.24(12) . . ?
O5 C23 H23A 109.8 . . ?
O5 C23 H23B 109.8 . . ?
C24 C23 H23A 109.8 . . ?
C24 C23 H23B 109.8 . . ?
H23A C23 H23B 108.3 . . ?
O8 C29 C30 107.26(12) . . ?
O8 C29 H29A 110.3 . . ?
O8 C29 H29B 110.3 . . ?
C30 C29 H29A 110.3 . . ?
C30 C29 H29B 110.3 . . ?
H29A C29 H29B 108.5 . . ?
O7 C27 H27A 110.1 . . ?
O7 C27 H27B 110.1 . . ?
O7 C27 C28 108.22(13) . . ?
H27A C27 H27B 108.4 . . ?
C28 C27 H27A 110.1 . . ?
C28 C27 H27B 110.1 . . ?
O6 C25 H25A 110.3 . . ?
O6 C25 H25B 110.3 . . ?
O6 C25 C26 106.87(12) . . ?
H25A C25 H25B 108.6 . . ?
C26 C25 H25A 110.3 . . ?
C26 C25 H25B 110.3 . . ?
C7 C8 H8 119.8 . . ?
C9 C8 C7 120.43(16) . . ?
C9 C8 H8 119.8 . . ?
O4 C21 C22 110.38(12) . . ?
O4 C21 H21A 109.6 . . ?
O4 C21 H21B 109.6 . . ?
C22 C21 H21A 109.6 . . ?
C22 C21 H21B 109.6 . . ?
H21A C21 H21B 108.1 . . ?
O7 C26 C25 111.53(13) . . ?
O7 C26 H26A 109.3 . . ?
O7 C26 H26B 109.3 . . ?
C25 C26 H26A 109.3 . . ?
C25 C26 H26B 109.3 . . ?
H26A C26 H26B 108.0 . . ?
O8 C28 C27 107.96(13) . . ?
O8 C28 H28A 110.1 . . ?
O8 C28 H28B 110.1 . . ?
C27 C28 H28A 110.1 . . ?
C27 C28 H28B 110.1 . . ?
H28A C28 H28B 108.4 . . ?
C11 C10 H10 120.0 . . ?
C9 C10 C11 120.02(17) . . ?
C9 C10 H10 120.0 . . ?
C8 C9 C10 119.69(15) . . ?
C8 C9 H9 120.2 . . ?
C10 C9 H9 120.2 . . ?
C31 O2 C34 109.5 . . ?
O2 C31 H31A 110.5 . . ?
O2 C31 H31B 110.5 . . ?
O2 C31 C32 106.4 . . ?
H31A C31 H31B 108.6 . . ?
C32 C31 H31A 110.5 . . ?
C32 C31 H31B 110.5 . . ?
C31 C32 H32A 111.5 . . ?
C31 C32 H32B 111.5 . . ?
C31 C32 C33 101.5 . . ?
H32A C32 H32B 109.3 . . ?
C33 C32 H32A 111.5 . . ?
C33 C32 H32B 111.5 . . ?
C32 C33 H33A 111.5 . . ?
C32 C33 H33B 111.5 . . ?
H33A C33 H33B 109.3 . . ?
C34 C33 C32 101.5 . . ?
C34 C33 H33A 111.5 . . ?
C34 C33 H33B 111.5 . . ?
O2 C34 C33 106.4 . . ?
O2 C34 H34A 110.4 . . ?
O2 C34 H34B 110.4 . . ?
C33 C34 H34A 110.4 . . ?
C33 C34 H34B 110.4 . . ?
H34A C34 H34B 108.6 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_exp_1839
_database_code_depnum_ccdc_archive 'CCDC 1872121'
_audit_update_record             
;
2018-10-09 deposited with the CCDC.
2019-01-17 downloaded from the CCDC.
;
_audit_creation_date             2018-03-14
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C17 H13 Cl Cu O P'
_chemical_formula_sum            'C17 H13 Cl Cu O P'
_chemical_formula_weight         363.23
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 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'

_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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   17.1019(13)
_cell_length_b                   3.8793(3)
_cell_length_c                   21.547(2)
_cell_angle_alpha                90
_cell_angle_beta                 97.229(9)
_cell_angle_gamma                90
_cell_volume                     1418.2(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1029
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      72.6880
_cell_measurement_theta_min      4.5900
_shelx_estimated_absorpt_T_max   0.639
_shelx_estimated_absorpt_T_min   0.590
_exptl_absorpt_coefficient_mu    4.916
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.41647
_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.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.701
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0638
_diffrn_reflns_av_unetI/netI     0.0785
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       3
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            4132
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.088
_diffrn_reflns_theta_min         4.604
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6525
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     81.00 178.00   1.00    5.48    --  106.40  61.00 120.00   97
  2  ω    102.00 129.00   1.00    5.48    --  106.40  80.00 -93.00   27
  3  ω     55.00 116.00   1.00    5.48    --  106.40 -15.00  90.00   61
  4  ω     35.00 132.00   1.00    5.48    --  106.40 -45.00 -30.00   97
  5  ω     28.00 105.00   1.00    5.48    --  106.40 -95.00-120.00   77
  6  ω    -72.00 -34.00   1.00    2.00    --  -41.14 178.00 -60.00   38
  7  ω   -117.00  -9.00   1.00    2.00    --  -41.14 -77.00 150.00  108
  8  ω   -124.00 -79.00   1.00    2.00    --  -41.14 178.00 -60.00   45
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0410596000
_diffrn_orient_matrix_UB_12      0.2063888000
_diffrn_orient_matrix_UB_13      -0.0559597000
_diffrn_orient_matrix_UB_21      0.0796983000
_diffrn_orient_matrix_UB_22      0.0441891000
_diffrn_orient_matrix_UB_23      -0.0254785000
_diffrn_orient_matrix_UB_31      -0.0147651000
_diffrn_orient_matrix_UB_32      -0.3362918000
_diffrn_orient_matrix_UB_33      -0.0375362000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\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                1952
_reflns_number_total             2694
_reflns_odcompleteness_completeness 98.23
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_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 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.853
_refine_diff_density_min         -1.429
_refine_diff_density_rms         0.213
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         2694
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1146
_refine_ls_R_factor_gt           0.0907
_refine_ls_restrained_S_all      1.036
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2423
_refine_ls_wR_factor_ref         0.2810
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C2(H2), C9(H9), C7(H7), C10(H10), C11(H11), C8(H8), C16(H16),
 C17(H17), C13(H13), C15(H15), C14(H14)
2.b Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;
_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
Cu1 Cu 0.94885(5) 0.5113(2) 0.69902(5) 0.0267(4) Uani 1 1 d . . . . .
P1 P 0.82320(8) 0.4240(4) 0.67182(8) 0.0211(4) Uani 1 1 d . . . . .
O1 O 0.7843(3) 0.3435(15) 0.7891(2) 0.0325(12) Uani 1 1 d . . . . .
H1 H 0.8330 0.3805 0.7954 0.049 Uiso 1 1 calc GR . . . .
C4 C 0.6877(3) 0.2363(16) 0.5977(3) 0.0223(13) Uani 1 1 d . . . . .
H4 H 0.6597 0.2048 0.5572 0.027 Uiso 1 1 calc R . . . .
C6 C 0.8016(3) 0.4032(15) 0.5424(3) 0.0199(12) Uani 1 1 d . . . . .
C3 C 0.6471(3) 0.1710(15) 0.6486(3) 0.0198(12) Uani 1 1 d . . . . .
C2 C 0.6836(3) 0.2081(16) 0.7099(3) 0.0216(12) Uani 1 1 d . . . . .
H2 H 0.6536 0.1557 0.7429 0.026 Uiso 1 1 calc R . . . .
C5 C 0.7663(3) 0.3444(16) 0.6011(3) 0.0214(13) Uani 1 1 d . . . . .
C9 C 0.8654(4) 0.4873(16) 0.4297(4) 0.0272(14) Uani 1 1 d . . . . .
H9 H 0.8873 0.5163 0.3916 0.033 Uiso 1 1 calc R . . . .
C12 C 0.5635(3) 0.0655(16) 0.6360(3) 0.0203(12) Uani 1 1 d . . . . .
C7 C 0.8778(3) 0.2828(17) 0.5358(3) 0.0260(14) Uani 1 1 d . . . . .
H7 H 0.9084 0.1721 0.5699 0.031 Uiso 1 1 calc R . . . .
C10 C 0.7900(4) 0.6085(17) 0.4346(3) 0.0254(14) Uani 1 1 d . . . . .
H10 H 0.7604 0.7199 0.4001 0.030 Uiso 1 1 calc R . . . .
C11 C 0.7582(3) 0.5662(16) 0.4903(3) 0.0203(12) Uani 1 1 d . . . . .
H11 H 0.7064 0.6479 0.4935 0.024 Uiso 1 1 calc R . . . .
C8 C 0.9083(4) 0.3253(17) 0.4796(3) 0.0278(14) Uani 1 1 d . . . . .
H8 H 0.9596 0.2414 0.4755 0.033 Uiso 1 1 calc R . . . .
C1 C 0.7609(4) 0.3163(17) 0.7260(3) 0.0252(13) Uani 1 1 d . . . . .
C16 C 0.4300(4) 0.0785(18) 0.6645(3) 0.0271(14) Uani 1 1 d . . . . .
H16 H 0.3946 0.1461 0.6928 0.033 Uiso 1 1 calc R . . . .
C17 C 0.5094(3) 0.1647(16) 0.6766(3) 0.0234(13) Uani 1 1 d . . . . .
H17 H 0.5274 0.2935 0.7131 0.028 Uiso 1 1 calc R . . . .
C13 C 0.5343(4) -0.1216(17) 0.5831(3) 0.0245(13) Uani 1 1 d . . . . .
H13 H 0.5695 -0.1889 0.5545 0.029 Uiso 1 1 calc R . . . .
C15 C 0.4025(4) -0.1063(18) 0.6109(4) 0.0298(15) Uani 1 1 d . . . . .
H15 H 0.3481 -0.1591 0.6019 0.036 Uiso 1 1 calc R . . . .
C14 C 0.4553(3) -0.2135(16) 0.5707(3) 0.0244(13) Uani 1 1 d . . . . .
H14 H 0.4374 -0.3487 0.5349 0.029 Uiso 1 1 calc R . . . .
Cl1 Cl 1.02620(8) 0.9915(3) 0.68410(7) 0.0206(4) 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
Cu1 P1 2.1815(16) . ?
Cu1 Cl1 2.5019(19) 2_746 ?
Cu1 Cl1 2.3301(16) . ?
Cu1 Cl1 2.4550(16) 1_545 ?
P1 C5 1.730(6) . ?
P1 C1 1.728(7) . ?
O1 H1 0.8400 . ?
O1 C1 1.373(8) . ?
C4 H4 0.9500 . ?
C4 C3 1.392(9) . ?
C4 C5 1.402(8) . ?
C6 C5 1.484(9) . ?
C6 C7 1.409(8) . ?
C6 C11 1.416(9) . ?
C3 C2 1.396(8) . ?
C3 C12 1.479(7) . ?
C2 H2 0.9500 . ?
C2 C1 1.388(8) . ?
C9 H9 0.9500 . ?
C9 C10 1.389(9) . ?
C9 C8 1.375(10) . ?
C12 C17 1.404(9) . ?
C12 C13 1.390(9) . ?
C7 H7 0.9500 . ?
C7 C8 1.387(10) . ?
C10 H10 0.9500 . ?
C10 C11 1.388(9) . ?
C11 H11 0.9500 . ?
C8 H8 0.9500 . ?
C16 H16 0.9500 . ?
C16 C17 1.390(9) . ?
C16 C15 1.389(11) . ?
C17 H17 0.9500 . ?
C13 H13 0.9500 . ?
C13 C14 1.392(8) . ?
C15 H15 0.9500 . ?
C15 C14 1.391(10) . ?
C14 H14 0.9500 . ?
Cl1 Cu1 2.5019(19) 2_756 ?
Cl1 Cu1 2.4550(16) 1_565 ?

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
P1 Cu1 Cl1 130.11(7) . . ?
P1 Cu1 Cl1 111.46(7) . 1_545 ?
P1 Cu1 Cl1 107.65(7) . 2_746 ?
Cl1 Cu1 Cl1 108.30(7) . 1_545 ?
Cl1 Cu1 Cl1 94.59(6) 1_545 2_746 ?
Cl1 Cu1 Cl1 97.79(6) . 2_746 ?
C5 P1 Cu1 133.6(2) . . ?
C1 P1 Cu1 121.8(2) . . ?
C1 P1 C5 103.0(3) . . ?
C1 O1 H1 109.5 . . ?
C3 C4 H4 117.1 . . ?
C3 C4 C5 125.8(6) . . ?
C5 C4 H4 117.1 . . ?
C7 C6 C5 121.1(6) . . ?
C7 C6 C11 117.8(6) . . ?
C11 C6 C5 121.0(5) . . ?
C4 C3 C2 121.2(5) . . ?
C4 C3 C12 118.2(6) . . ?
C2 C3 C12 120.6(5) . . ?
C3 C2 H2 117.8 . . ?
C1 C2 C3 124.4(6) . . ?
C1 C2 H2 117.8 . . ?
C4 C5 P1 121.9(5) . . ?
C4 C5 C6 119.5(5) . . ?
C6 C5 P1 118.6(4) . . ?
C10 C9 H9 119.9 . . ?
C8 C9 H9 119.9 . . ?
C8 C9 C10 120.2(7) . . ?
C17 C12 C3 120.5(6) . . ?
C13 C12 C3 122.2(6) . . ?
C13 C12 C17 117.2(5) . . ?
C6 C7 H7 119.9 . . ?
C8 C7 C6 120.3(6) . . ?
C8 C7 H7 119.9 . . ?
C9 C10 H10 120.1 . . ?
C11 C10 C9 119.7(6) . . ?
C11 C10 H10 120.1 . . ?
C6 C11 H11 119.5 . . ?
C10 C11 C6 121.0(6) . . ?
C10 C11 H11 119.5 . . ?
C9 C8 C7 121.0(6) . . ?
C9 C8 H8 119.5 . . ?
C7 C8 H8 119.5 . . ?
O1 C1 P1 121.5(4) . . ?
O1 C1 C2 114.9(6) . . ?
C2 C1 P1 123.6(5) . . ?
C17 C16 H16 120.0 . . ?
C15 C16 H16 120.0 . . ?
C15 C16 C17 120.0(7) . . ?
C12 C17 H17 119.3 . . ?
C16 C17 C12 121.4(6) . . ?
C16 C17 H17 119.3 . . ?
C12 C13 H13 119.0 . . ?
C12 C13 C14 122.1(6) . . ?
C14 C13 H13 119.0 . . ?
C16 C15 H15 120.2 . . ?
C16 C15 C14 119.6(6) . . ?
C14 C15 H15 120.2 . . ?
C13 C14 H14 120.2 . . ?
C15 C14 C13 119.6(6) . . ?
C15 C14 H14 120.2 . . ?
Cu1 Cl1 Cu1 85.04(6) . 2_756 ?
Cu1 Cl1 Cu1 82.49(5) 1_565 2_756 ?
Cu1 Cl1 Cu1 108.30(7) . 1_565 ?

_olex2_date_sample_data_collection 2017-09-04
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.467
_oxdiff_exptl_absorpt_empirical_full_min 0.417
####################################################################### 
# 
# 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_exp_2681
_database_code_depnum_ccdc_archive 'CCDC 1872119'
_audit_update_record             
;
2018-10-09 deposited with the CCDC.
2019-01-17 downloaded from the CCDC.
;
_audit_creation_date             2018-04-18
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.04.03 svn.r3497 for OlexSys, GUI svn.r5486)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C35 H27 Au O P2'
_chemical_formula_sum            'C35 H27 Au O P2'
_chemical_formula_weight         722.47
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 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'
Au Au -4.4197 7.2980 '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                   10.7949(4)
_cell_length_b                   11.5285(6)
_cell_length_c                   11.9802(5)
_cell_angle_alpha                87.576(4)
_cell_angle_beta                 84.280(4)
_cell_angle_gamma                71.512(4)
_cell_volume                     1406.85(11)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4096
_cell_measurement_temperature    149.98(10)
_cell_measurement_theta_max      73.2400
_cell_measurement_theta_min      4.0270
_shelx_estimated_absorpt_T_max   0.435
_shelx_estimated_absorpt_T_min   0.326
_exptl_absorpt_coefficient_mu    11.107
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60181
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.44a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.706
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             708
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0595
_diffrn_reflns_av_unetI/netI     0.0773
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8375
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.433
_diffrn_reflns_theta_min         3.708
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.98(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6525
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -113.00 -17.00   1.00    2.00    --  -41.14 -38.00 -60.00   96
  2  ω    -74.00  25.00   1.00    1.00    --  -41.14  77.00-150.00   99
  3  ω    -65.00  27.00   1.00    1.00    --  -41.14  38.00 120.00   92
  4  ω     31.00 133.00   1.00    1.87    --  106.40 -30.00  60.00  102
  5  ω     84.00 110.00   1.00    1.87    --  106.40  30.00-120.00   26
  6  ω    128.00 178.00   1.00    1.87    --  106.40  30.00-120.00   50
  7  ω     43.00 135.00   1.00    1.87    --  106.40 -30.00 -90.00   92
  8  ω     47.00 109.00   1.00    1.87    --  106.40 -95.00-180.00   62
  9  ω     34.00 118.00   1.00    1.87    --  106.40 -77.00-120.00   84
 10  ω     67.00 134.00   1.00    1.87    --  106.40 -30.00-180.00   67
 11  ω     25.00 105.00   1.00    1.87    --  106.40 -95.00  90.00   80
 12  ω     60.00 118.00   1.00    1.87    --  106.40-119.00  41.00   58
 13  ω     30.00  62.00   1.00    1.87    --  106.40 -30.00-180.00   32
 14  ω    106.00 131.00   1.00    1.00    --   42.53 178.00-150.00   25
;
_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      -0.0255649000
_diffrn_orient_matrix_UB_12      0.1382563000
_diffrn_orient_matrix_UB_13      0.0127829000
_diffrn_orient_matrix_UB_21      0.0079466000
_diffrn_orient_matrix_UB_22      -0.0181145000
_diffrn_orient_matrix_UB_23      0.1275381000
_diffrn_orient_matrix_UB_31      0.1487153000
_diffrn_orient_matrix_UB_32      -0.0203293000
_diffrn_orient_matrix_UB_33      -0.0165735000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\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                4812
_reflns_number_total             5385
_reflns_odcompleteness_completeness 99.10
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_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 1.171.39.44a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.44a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.44a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         2.309
_refine_diff_density_min         -1.533
_refine_diff_density_rms         0.189
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         5385
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0490
_refine_ls_restrained_S_all      1.028
_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)+(0.0680P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1211
_refine_ls_wR_factor_ref         0.1281
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C21(H21), C19(H19), C29(H29), C4(H4), C20(H20), C25(H25), C10(H10), C22(H22),
 C23(H23), C12(H12), C2(H2), C31(H31), C35(H35), C16(H16), C6(H6), C28(H28),
 C26(H26), C32(H32), C13(H13), C15(H15), C14(H14), C7(H7), C9(H9), C27(H27),
 C8(H8), C33(H33), C34(H34)
;
_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
Au1 Au 0.31389(3) 0.72125(2) 0.61341(2) 0.02454(11) Uani 1 1 d . . . . .
P2 P 0.29977(15) 0.88610(15) 0.72067(13) 0.0204(3) Uani 1 1 d . . . . .
P1 P 0.32641(18) 0.55117(16) 0.51444(14) 0.0261(4) Uani 1 1 d . . . . .
O1 O 0.4088(5) 0.6254(5) 0.3177(4) 0.0324(11) Uani 1 1 d . . . . .
C18 C 0.4111(6) 0.9719(6) 0.6754(5) 0.0213(12) Uani 1 1 d . . . . .
C21 C 0.5995(7) 1.0863(7) 0.6237(6) 0.0283(14) Uani 1 1 d . . . . .
H21 H 0.6630 1.1249 0.6075 0.034 Uiso 1 1 calc R . . . .
C5 C 0.2327(6) 0.4531(6) 0.5503(6) 0.0224(13) Uani 1 1 d . . . . .
C17 C 0.1995(7) 0.3178(6) 0.2757(6) 0.0261(13) Uani 1 1 d . . . . .
C19 C 0.5361(6) 0.9039(6) 0.6328(6) 0.0246(13) Uani 1 1 d . . . . .
H19 H 0.5570 0.8204 0.6206 0.030 Uiso 1 1 calc R . . . .
C24 C 0.1373(6) 0.9978(6) 0.7313(6) 0.0227(12) Uani 1 1 d . . . . .
C3 C 0.2379(6) 0.3966(6) 0.3509(5) 0.0237(13) Uani 1 1 d . . . . .
C29 C 0.0674(7) 1.0383(7) 0.8347(6) 0.0300(14) Uani 1 1 d . . . . .
H29 H 0.1035 1.0073 0.9012 0.036 Uiso 1 1 calc R . . . .
C4 C 0.2080(6) 0.3857(6) 0.4689(6) 0.0237(13) Uani 1 1 d . . . . .
H4 H 0.1679 0.3273 0.4926 0.028 Uiso 1 1 calc R . . . .
C20 C 0.6308(7) 0.9639(7) 0.6085(6) 0.0305(15) Uani 1 1 d . . . . .
H20 H 0.7158 0.9193 0.5817 0.037 Uiso 1 1 calc R . . . .
C25 C 0.0816(7) 1.0449(7) 0.6325(6) 0.0323(15) Uani 1 1 d . . . . .
H25 H 0.1283 1.0197 0.5636 0.039 Uiso 1 1 calc R . . . .
C10 C 0.0741(7) 0.4123(7) 0.7015(6) 0.0311(15) Uani 1 1 d . . . . .
H10 H 0.0221 0.4060 0.6460 0.037 Uiso 1 1 calc R . . . .
C22 C 0.4731(7) 1.1538(7) 0.6632(6) 0.0285(14) Uani 1 1 d . . . . .
H22 H 0.4517 1.2380 0.6710 0.034 Uiso 1 1 calc R . . . .
C23 C 0.3773(7) 1.0972(6) 0.6914(6) 0.0281(14) Uani 1 1 d . . . . .
H23 H 0.2932 1.1420 0.7201 0.034 Uiso 1 1 calc R . . . .
C11 C 0.1928(7) 0.4371(6) 0.6711(6) 0.0255(13) Uani 1 1 d . . . . .
C30 C 0.3377(6) 0.8355(6) 0.8628(6) 0.0246(13) Uani 1 1 d . . . . .
C12 C 0.2766(7) 0.2730(7) 0.1772(6) 0.0302(14) Uani 1 1 d . . . . .
H12 H 0.3526 0.2939 0.1586 0.036 Uiso 1 1 calc R . . . .
C2 C 0.3051(6) 0.4736(6) 0.3051(5) 0.0251(13) Uani 1 1 d . . . . .
H2 H 0.3220 0.4731 0.2274 0.030 Uiso 1 1 calc R . . . .
C1 C 0.3517(6) 0.5549(6) 0.3651(5) 0.0244(13) Uani 1 1 d . . . . .
C31 C 0.3730(7) 0.9084(7) 0.9357(6) 0.0313(15) Uani 1 1 d . . . . .
H31 H 0.3732 0.9865 0.9130 0.038 Uiso 1 1 calc R . . . .
C35 C 0.3393(8) 0.7177(7) 0.8975(7) 0.0347(16) Uani 1 1 d . . . . .
H35 H 0.3172 0.6673 0.8498 0.042 Uiso 1 1 calc R . . . .
C16 C 0.0834(8) 0.2896(7) 0.2993(7) 0.0327(15) Uani 1 1 d . . . . .
H16 H 0.0295 0.3195 0.3641 0.039 Uiso 1 1 calc R . . . .
C6 C 0.2688(7) 0.4442(6) 0.7561(6) 0.0308(15) Uani 1 1 d . . . . .
H6 H 0.3478 0.4599 0.7378 0.037 Uiso 1 1 calc R . . . .
C28 C -0.0587(6) 1.1268(8) 0.8373(6) 0.0345(17) Uani 1 1 d . . . . .
H28 H -0.1044 1.1568 0.9055 0.041 Uiso 1 1 calc R . . . .
C26 C -0.0420(8) 1.1283(8) 0.6365(7) 0.0390(18) Uani 1 1 d . . . . .
H26 H -0.0785 1.1585 0.5699 0.047 Uiso 1 1 calc R . . . .
C32 C 0.4072(7) 0.8660(8) 1.0402(6) 0.0351(16) Uani 1 1 d . . . . .
H32 H 0.4296 0.9157 1.0884 0.042 Uiso 1 1 calc R . . . .
C13 C 0.2438(8) 0.1984(7) 0.1062(7) 0.0373(17) Uani 1 1 d . . . . .
H13 H 0.2984 0.1667 0.0423 0.045 Uiso 1 1 calc R . . . .
C15 C 0.0473(9) 0.2175(8) 0.2275(8) 0.043(2) Uani 1 1 d . . . . .
H15 H -0.0311 0.2001 0.2437 0.052 Uiso 1 1 calc R . . . .
C14 C 0.1266(9) 0.1717(8) 0.1326(7) 0.043(2) Uani 1 1 d . . . . .
H14 H 0.1024 0.1223 0.0853 0.052 Uiso 1 1 calc R . . . .
C7 C 0.2283(8) 0.4281(8) 0.8686(6) 0.0374(17) Uani 1 1 d . . . . .
H7 H 0.2804 0.4327 0.9245 0.045 Uiso 1 1 calc R . . . .
C9 C 0.0340(8) 0.3972(7) 0.8130(7) 0.0373(17) Uani 1 1 d . . . . .
H9 H -0.0449 0.3816 0.8321 0.045 Uiso 1 1 calc R . . . .
C27 C -0.1132(7) 1.1682(7) 0.7377(7) 0.0360(16) Uani 1 1 d . . . . .
H27 H -0.1978 1.2229 0.7388 0.043 Uiso 1 1 calc R . . . .
C8 C 0.1116(8) 0.4054(7) 0.8966(7) 0.0400(18) Uani 1 1 d . . . . .
H8 H 0.0844 0.3956 0.9715 0.048 Uiso 1 1 calc R . . . .
C33 C 0.4086(8) 0.7491(8) 1.0748(7) 0.0404(18) Uani 1 1 d . . . . .
H33 H 0.4328 0.7205 1.1457 0.048 Uiso 1 1 calc R . . . .
C34 C 0.3746(9) 0.6767(8) 1.0049(7) 0.045(2) Uani 1 1 d . . . . .
H34 H 0.3748 0.5989 1.0289 0.054 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Au1 P2 2.2958(16) . ?
Au1 P1 2.2946(17) . ?
P2 C18 1.816(6) . ?
P2 C24 1.813(6) . ?
P2 C30 1.820(7) . ?
P1 C5 1.756(6) . ?
P1 C1 1.783(7) . ?
O1 C1 1.254(8) . ?
C18 C19 1.386(9) . ?
C18 C23 1.389(9) . ?
C21 H21 0.9300 . ?
C21 C20 1.359(10) . ?
C21 C22 1.386(10) . ?
C5 C4 1.369(9) . ?
C5 C11 1.489(9) . ?
C17 C3 1.480(9) . ?
C17 C12 1.392(10) . ?
C17 C16 1.392(10) . ?
C19 H19 0.9300 . ?
C19 C20 1.407(9) . ?
C24 C29 1.400(9) . ?
C24 C25 1.392(10) . ?
C3 C4 1.427(9) . ?
C3 C2 1.379(9) . ?
C29 H29 0.9300 . ?
C29 C28 1.417(10) . ?
C4 H4 0.9300 . ?
C20 H20 0.9300 . ?
C25 H25 0.9300 . ?
C25 C26 1.373(11) . ?
C10 H10 0.9300 . ?
C10 C11 1.410(9) . ?
C10 C9 1.383(10) . ?
C22 H22 0.9300 . ?
C22 C23 1.396(9) . ?
C23 H23 0.9300 . ?
C11 C6 1.390(11) . ?
C30 C31 1.395(10) . ?
C30 C35 1.398(10) . ?
C12 H12 0.9300 . ?
C12 C13 1.378(10) . ?
C2 H2 0.9300 . ?
C2 C1 1.441(9) . ?
C31 H31 0.9300 . ?
C31 C32 1.367(10) . ?
C35 H35 0.9300 . ?
C35 C34 1.399(11) . ?
C16 H16 0.9300 . ?
C16 C15 1.384(11) . ?
C6 H6 0.9300 . ?
C6 C7 1.398(10) . ?
C28 H28 0.9300 . ?
C28 C27 1.383(11) . ?
C26 H26 0.9300 . ?
C26 C27 1.382(12) . ?
C32 H32 0.9300 . ?
C32 C33 1.388(12) . ?
C13 H13 0.9300 . ?
C13 C14 1.398(12) . ?
C15 H15 0.9300 . ?
C15 C14 1.369(12) . ?
C14 H14 0.9300 . ?
C7 H7 0.9300 . ?
C7 C8 1.372(11) . ?
C9 H9 0.9300 . ?
C9 C8 1.393(13) . ?
C27 H27 0.9300 . ?
C8 H8 0.9300 . ?
C33 H33 0.9300 . ?
C33 C34 1.359(13) . ?
C34 H34 0.9300 . ?

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
P1 Au1 P2 177.09(5) . . ?
C18 P2 Au1 116.3(2) . . ?
C18 P2 C30 104.7(3) . . ?
C24 P2 Au1 112.8(2) . . ?
C24 P2 C18 105.5(3) . . ?
C24 P2 C30 107.0(3) . . ?
C30 P2 Au1 109.9(2) . . ?
C5 P1 Au1 124.8(2) . . ?
C5 P1 C1 107.2(3) . . ?
C1 P1 Au1 119.2(2) . . ?
C19 C18 P2 116.2(5) . . ?
C19 C18 C23 121.5(6) . . ?
C23 C18 P2 122.1(5) . . ?
C20 C21 H21 119.9 . . ?
C20 C21 C22 120.1(6) . . ?
C22 C21 H21 119.9 . . ?
C4 C5 P1 119.8(5) . . ?
C4 C5 C11 121.6(5) . . ?
C11 C5 P1 118.3(5) . . ?
C12 C17 C3 120.8(6) . . ?
C12 C17 C16 117.9(7) . . ?
C16 C17 C3 121.2(6) . . ?
C18 C19 H19 120.8 . . ?
C18 C19 C20 118.5(6) . . ?
C20 C19 H19 120.8 . . ?
C29 C24 P2 122.4(5) . . ?
C25 C24 P2 118.2(5) . . ?
C25 C24 C29 119.4(6) . . ?
C4 C3 C17 118.0(6) . . ?
C2 C3 C17 119.1(6) . . ?
C2 C3 C4 122.8(6) . . ?
C24 C29 H29 120.2 . . ?
C24 C29 C28 119.6(7) . . ?
C28 C29 H29 120.2 . . ?
C5 C4 C3 126.1(6) . . ?
C5 C4 H4 116.9 . . ?
C3 C4 H4 116.9 . . ?
C21 C20 C19 120.7(6) . . ?
C21 C20 H20 119.6 . . ?
C19 C20 H20 119.6 . . ?
C24 C25 H25 119.9 . . ?
C26 C25 C24 120.2(7) . . ?
C26 C25 H25 119.9 . . ?
C11 C10 H10 119.7 . . ?
C9 C10 H10 119.7 . . ?
C9 C10 C11 120.7(7) . . ?
C21 C22 H22 119.6 . . ?
C21 C22 C23 120.9(7) . . ?
C23 C22 H22 119.6 . . ?
C18 C23 C22 118.2(7) . . ?
C18 C23 H23 120.9 . . ?
C22 C23 H23 120.9 . . ?
C10 C11 C5 119.2(6) . . ?
C6 C11 C5 122.7(6) . . ?
C6 C11 C10 118.1(6) . . ?
C31 C30 P2 121.6(5) . . ?
C31 C30 C35 119.2(7) . . ?
C35 C30 P2 119.1(5) . . ?
C17 C12 H12 119.0 . . ?
C13 C12 C17 122.0(7) . . ?
C13 C12 H12 119.0 . . ?
C3 C2 H2 116.6 . . ?
C3 C2 C1 126.7(6) . . ?
C1 C2 H2 116.6 . . ?
O1 C1 P1 119.8(5) . . ?
O1 C1 C2 123.4(6) . . ?
C2 C1 P1 116.9(5) . . ?
C30 C31 H31 119.8 . . ?
C32 C31 C30 120.5(7) . . ?
C32 C31 H31 119.8 . . ?
C30 C35 H35 120.4 . . ?
C30 C35 C34 119.1(7) . . ?
C34 C35 H35 120.4 . . ?
C17 C16 H16 119.6 . . ?
C15 C16 C17 120.7(7) . . ?
C15 C16 H16 119.6 . . ?
C11 C6 H6 119.5 . . ?
C11 C6 C7 121.0(7) . . ?
C7 C6 H6 119.5 . . ?
C29 C28 H28 120.3 . . ?
C27 C28 C29 119.4(7) . . ?
C27 C28 H28 120.3 . . ?
C25 C26 H26 119.4 . . ?
C25 C26 C27 121.2(7) . . ?
C27 C26 H26 119.4 . . ?
C31 C32 H32 119.8 . . ?
C31 C32 C33 120.4(8) . . ?
C33 C32 H32 119.8 . . ?
C12 C13 H13 120.8 . . ?
C12 C13 C14 118.5(7) . . ?
C14 C13 H13 120.8 . . ?
C16 C15 H15 119.9 . . ?
C14 C15 C16 120.2(7) . . ?
C14 C15 H15 119.9 . . ?
C13 C14 H14 119.7 . . ?
C15 C14 C13 120.6(7) . . ?
C15 C14 H14 119.7 . . ?
C6 C7 H7 120.0 . . ?
C8 C7 C6 120.1(8) . . ?
C8 C7 H7 120.0 . . ?
C10 C9 H9 120.0 . . ?
C10 C9 C8 120.1(7) . . ?
C8 C9 H9 120.0 . . ?
C28 C27 H27 120.0 . . ?
C26 C27 C28 120.0(7) . . ?
C26 C27 H27 120.0 . . ?
C7 C8 C9 120.1(7) . . ?
C7 C8 H8 120.0 . . ?
C9 C8 H8 120.0 . . ?
C32 C33 H33 120.0 . . ?
C34 C33 C32 119.9(7) . . ?
C34 C33 H33 120.0 . . ?
C35 C34 H34 119.6 . . ?
C33 C34 C35 120.9(8) . . ?
C33 C34 H34 119.6 . . ?

_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.212
_oxdiff_exptl_absorpt_empirical_full_min 0.638
