# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2020

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

data_compound-2d
_database_code_depnum_ccdc_archive 'CCDC 1988260'
loop_
_audit_author_name
_audit_author_address
'Kyle G. Pearce'
;University of Sussex
United Kingdom
;
_audit_update_record             
;
2020-03-04 deposited with the CCDC.	2020-03-31 downloaded from the CCDC.
;
_audit_creation_date             2020-01-09
_audit_creation_method           
;
Olex2 1.3
(compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C11 H11 O2 P'
_chemical_formula_sum            'C11 H11 O2 P'
_chemical_formula_weight         206.17
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         C11H11O2P1
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'

_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           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'
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'

_cell_length_a                   14.2522(3)
_cell_length_b                   5.97640(10)
_cell_length_c                   12.0658(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1027.73(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9098
_cell_measurement_temperature    100
_cell_measurement_theta_max      68.1820
_cell_measurement_theta_min      6.1890
_shelx_estimated_absorpt_T_max   0.959
_shelx_estimated_absorpt_T_min   0.919
_exptl_absorpt_coefficient_mu    2.134
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61927
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.28e (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       rod
_exptl_crystal_F_000             432
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0362
_diffrn_reflns_av_unetI/netI     0.0225
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            15250
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.176
_diffrn_reflns_theta_min         6.211
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -77.00 -50.00   1.00   25.00    --    5.00  35.00  74.00   27
  2  ω    -25.00   0.00   1.00   25.00    --  -89.00  35.00  74.00   25
  3  ω    -25.00  45.00   1.00   25.00    --    5.00  35.00  74.00   70
  4  ω   -170.00   0.00   1.00   25.00    --  -89.00  57.00 120.00  170
  5  ω   -150.00 -71.00   1.00   25.00    --  -89.00  60.00-180.00   79
  6  ω    -42.00  -6.00   1.00   25.00    --  -89.00  60.00-180.00   36
  7  ω   -126.00  -1.00   1.00   25.00    --  -89.00  60.00 150.00  125
  8  ω    -51.00 -25.00   1.00    1.00    --    0.00  60.00 150.00   26
  9  ω    -37.00 -11.00   1.00   25.00    --  -89.00  60.00-150.00   26
 10  ω   -155.00-129.00   1.00   25.00    --  -89.00  60.00 -30.00   26
 11  ω   -113.00 -87.00   1.00   25.00    --  -89.00  60.00 -30.00   26
 12  ω   -115.00 -89.00   1.00   25.00    --  -89.00  60.00-150.00   26
 13  ω   -113.00 -88.00   1.00   25.00    --  -89.00  35.00  74.00   25
 14  ω     15.00  53.00   1.00    1.00    --    0.00  60.00-180.00   38
 15  ω    -41.00   9.00   1.00    1.00    --    0.00  60.00-180.00   50
 16  ω    -80.00 -54.00   1.00    1.00    --    0.00  60.00-180.00   26
 17  ω    -89.00 -63.00   1.00   25.00    --  -89.00  60.00  30.00   26
 18  ω   -103.00 -77.00   1.00   25.00    --  -89.00  29.00 -90.00   26
 19  ω   -178.00-124.00   1.00   25.00    --  -89.00  60.00   0.00   54
 20  ω   -177.00-151.00   1.00   25.00    --  -89.00  57.00  90.00   26
 21  ω    -71.00 -41.00   1.00   25.00    --  -89.00  60.00-180.00   30
 22  ω   -155.00-129.00   1.00   25.00    --  -89.00  60.00 -90.00   26
 23  ω    -74.00 -18.00   1.00   25.00    --  -89.00  57.00  90.00   56
 24  ω    -38.00 -12.00   1.00   25.00    --  -89.00  60.00  30.00   26
 25  ω    -52.00 -26.00   1.00   25.00    --  -89.00  29.00 -90.00   26
 26  ω   -159.00 -33.00   1.00   25.00    --  -89.00  60.00-120.00  126
 27  ω   -167.00-141.00   1.00   25.00    --  -89.00  60.00 150.00   26
 28  ω   -161.00-135.00   1.00   25.00    --  -89.00  60.00-150.00   26
 29  ω    -90.00 -61.00   1.00   25.00    --  -89.00  60.00-150.00   29
 30  ω   -151.00-126.00   1.00   25.00    --  -89.00  29.00 -30.00   25
 31  ω    -42.00 -14.00   1.00   25.00    --    5.00  29.00 -60.00   28
 32  ω    -83.00 -38.00   1.00   25.00    --    5.00  43.00 -60.00   45
 33  ω    -82.00   7.00   1.00   25.00    --    5.00  43.00 120.00   89
 34  ω    -74.00 -48.00   1.00   25.00    --    5.00  29.00 -60.00   26
 35  ω    -83.00 -52.00   1.00   25.00    --    5.00  29.00 150.00   31
 36  ω    -18.00   8.00   1.00   25.00    --    5.00  43.00 -60.00   26
 37  ω     69.00  94.00   1.00   25.00    --    5.00  29.00 150.00   25
 38  ω    -11.00  16.00   1.00   25.00    --    5.00  29.00 150.00   27
 39  ω    -10.00  17.00   1.00   25.00    --  -72.00  58.00  43.46   27
 40  ω   -152.00-127.00   1.00   25.00    --  -72.00  58.00  43.46   25
 41  ω   -123.00 -76.00   1.00   25.00    --  -72.00  58.00  43.46   47
 42  ω    -26.00   0.00   1.00   25.00    --  -89.00  57.00  30.00   26
 43  ω   -115.00 -89.00   1.00   25.00    --  -89.00  43.00   0.00   26
 44  ω    -26.00   0.00   1.00   25.00    --  -89.00  60.00 -30.00   26
 45  ω    -64.00 -39.00   1.00   25.00    --  -89.00  57.00  30.00   25
 46  ω    -28.00  -2.00   1.00   25.00    --  -89.00  43.00-150.00   26
 47  ω   -126.00 -88.00   1.00   25.00    --  -89.00  57.00  30.00   38
 48  ω    -26.00   0.00   1.00   25.00    --  -89.00  60.00 -60.00   26
 49  ω    -30.00  -5.00   1.00   25.00    --  -89.00  43.00 -90.00   25
 50  ω   -155.00-129.00   1.00   25.00    --  -89.00  57.00  30.00   26
 51  ω    -77.00 -51.00   1.00   25.00    --  -89.00  43.00 -90.00   26
 52  ω    -28.00   0.00   1.00   25.00    --  -89.00  60.00  60.00   28
 53  ω    -26.00   0.00   1.00   25.00    --  -89.00  57.00-150.00   26
 54  ω    -87.00   0.00   1.00   25.00    --  -89.00  43.00 -30.00   87
 55  ω   -152.00-126.00   1.00   25.00    --  -89.00  43.00  90.00   26
 56  ω   -102.00 -76.00   1.00   25.00    --  -89.00  43.00  90.00   26
 57  ω    -26.00   0.00   1.00   25.00    --  -89.00  43.00  90.00   26
 58  ω    -41.00  -5.00   1.00   25.00    --  -89.00  43.00-180.00   36
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RCD3): quarter-chi single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0389295000
_diffrn_orient_matrix_UB_12      0.1934728000
_diffrn_orient_matrix_UB_13      -0.0707464000
_diffrn_orient_matrix_UB_21      -0.0907490000
_diffrn_orient_matrix_UB_22      0.1338692000
_diffrn_orient_matrix_UB_23      0.0201810000
_diffrn_orient_matrix_UB_31      0.0439661000
_diffrn_orient_matrix_UB_32      0.1053162000
_diffrn_orient_matrix_UB_33      0.1043591000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\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         0.881
_reflns_Friedel_fraction_full    0.979
_reflns_Friedel_fraction_max     0.975
_reflns_number_gt                1772
_reflns_number_total             1857
_reflns_odcompleteness_completeness 100.00
_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 1.171.39.28e (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28e (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28e (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         1.239
_refine_diff_density_min         -0.440
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details 
;
 Flack x determined using 788 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.05(6)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     127
_refine_ls_number_reflns         1857
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0611
_refine_ls_R_factor_gt           0.0593
_refine_ls_restrained_S_all      1.098
_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)+(0.1069P)²+1.0138P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1632
_refine_ls_wR_factor_ref         0.1647
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C00C(H00C,H00D), C00D(H00E,H00F), C00E(H00G,H00H)
2.b Aromatic/amide H refined with riding coordinates:
 C005(H005), C006(H006), C009(H009), C00A(H00A), C00B(H00B)
;
_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
P001 P 0.70421(9) 0.1676(2) 0.54030(12) 0.0313(4) Uani 1 1 d . . . . .
O002 O 0.5933(3) 0.0325(8) 0.3725(4) 0.0412(10) Uani 1 1 d . . . . .
O003 O 0.7957(3) 0.5612(8) 0.5383(6) 0.0513(12) Uani 1 1 d . . . . .
C004 C 0.7938(4) 0.3817(11) 0.4952(5) 0.0333(13) Uani 1 1 d . . . . .
C005 C 0.4472(4) 0.5826(11) 0.6426(5) 0.0384(13) Uani 1 1 d . . . . .
H005 H 0.394906 0.669876 0.665495 0.046 Uiso 1 1 calc R U . . .
C006 C 0.4661(4) 0.3822(11) 0.6950(5) 0.0396(14) Uani 1 1 d . . . . .
H006 H 0.426322 0.329551 0.752600 0.048 Uiso 1 1 calc R U . . .
C007 C 0.6022(4) 0.3364(9) 0.5773(4) 0.0299(12) Uani 1 1 d . . . . .
C008 C 0.6736(4) 0.0630(10) 0.3993(5) 0.0341(12) Uani 1 1 d . . . . .
C009 C 0.5799(4) 0.5355(9) 0.5253(5) 0.0333(12) Uani 1 1 d . . . . .
H009 H 0.618260 0.588639 0.466520 0.040 Uiso 1 1 calc R U . . .
C00A C 0.5443(4) 0.2576(9) 0.6624(5) 0.0327(12) Uani 1 1 d . . . . .
H00A H 0.558222 0.119666 0.697941 0.039 Uiso 1 1 calc R U . . .
C00B C 0.5034(4) 0.6569(9) 0.5577(5) 0.0347(13) Uani 1 1 d . . . . .
H00B H 0.488897 0.793502 0.521181 0.042 Uiso 1 1 calc R U . . .
C00C C 0.8182(4) 0.2131(12) 0.3057(5) 0.0405(14) Uani 1 1 d . . . . .
H00C H 0.779827 0.333992 0.272544 0.049 Uiso 1 1 calc R U . . .
H00D H 0.867715 0.173012 0.251702 0.049 Uiso 1 1 calc R U . . .
C00D C 0.8645(4) 0.3010(12) 0.4118(5) 0.0391(14) Uani 1 1 d . . . . .
H00E H 0.902627 0.180217 0.445382 0.047 Uiso 1 1 calc R U . . .
H00F H 0.907282 0.425706 0.392662 0.047 Uiso 1 1 calc R U . . .
C00E C 0.7562(5) 0.0104(11) 0.3253(6) 0.0433(15) Uani 1 1 d . . . . .
H00G H 0.732862 -0.045547 0.253144 0.052 Uiso 1 1 calc R U . . .
H00H H 0.794063 -0.109860 0.359701 0.052 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P001 C004 1.887(6) . ?
P001 C007 1.825(5) . ?
P001 C008 1.864(6) . ?
O002 C008 1.202(7) . ?
O003 C004 1.193(8) . ?
C004 C00D 1.504(9) . ?
C005 H005 0.9500 . ?
C005 C006 1.381(9) . ?
C005 C00B 1.375(9) . ?
C006 H006 0.9500 . ?
C006 C00A 1.398(9) . ?
C007 C009 1.382(8) . ?
C007 C00A 1.398(8) . ?
C008 C00E 1.511(8) . ?
C009 H009 0.9500 . ?
C009 C00B 1.368(8) . ?
C00A H00A 0.9500 . ?
C00B H00B 0.9500 . ?
C00C H00C 0.9900 . ?
C00C H00D 0.9900 . ?
C00C C00D 1.534(9) . ?
C00C C00E 1.518(9) . ?
C00D H00E 0.9900 . ?
C00D H00F 0.9900 . ?
C00E H00G 0.9900 . ?
C00E H00H 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
C007 P001 C004 103.6(3) . . ?
C007 P001 C008 102.8(3) . . ?
C008 P001 C004 97.0(3) . . ?
O003 C004 P001 120.0(5) . . ?
O003 C004 C00D 124.4(6) . . ?
C00D C004 P001 115.4(5) . . ?
C006 C005 H005 119.7 . . ?
C00B C005 H005 119.7 . . ?
C00B C005 C006 120.5(5) . . ?
C005 C006 H006 120.4 . . ?
C005 C006 C00A 119.3(5) . . ?
C00A C006 H006 120.4 . . ?
C009 C007 P001 123.2(4) . . ?
C009 C007 C00A 119.2(5) . . ?
C00A C007 P001 117.6(4) . . ?
O002 C008 P001 121.3(4) . . ?
O002 C008 C00E 123.4(6) . . ?
C00E C008 P001 115.2(4) . . ?
C007 C009 H009 119.6 . . ?
C00B C009 C007 120.7(5) . . ?
C00B C009 H009 119.6 . . ?
C006 C00A H00A 120.1 . . ?
C007 C00A C006 119.9(5) . . ?
C007 C00A H00A 120.1 . . ?
C005 C00B H00B 119.8 . . ?
C009 C00B C005 120.4(5) . . ?
C009 C00B H00B 119.8 . . ?
H00C C00C H00D 107.8 . . ?
C00D C00C H00C 108.9 . . ?
C00D C00C H00D 108.9 . . ?
C00E C00C H00C 108.9 . . ?
C00E C00C H00D 108.9 . . ?
C00E C00C C00D 113.2(5) . . ?
C004 C00D C00C 112.3(5) . . ?
C004 C00D H00E 109.1 . . ?
C004 C00D H00F 109.1 . . ?
C00C C00D H00E 109.1 . . ?
C00C C00D H00F 109.1 . . ?
H00E C00D H00F 107.9 . . ?
C008 C00E C00C 112.3(5) . . ?
C008 C00E H00G 109.1 . . ?
C008 C00E H00H 109.1 . . ?
C00C C00E H00G 109.1 . . ?
C00C C00E H00H 109.1 . . ?
H00G C00E H00H 107.9 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
P001 C004 C00D C00C 57.8(7) . . . . ?
P001 C007 C009 C00B -179.0(4) . . . . ?
P001 C007 C00A C006 179.1(4) . . . . ?
P001 C008 C00E C00C -59.6(7) . . . . ?
O002 C008 C00E C00C 123.3(7) . . . . ?
O003 C004 C00D C00C -127.8(7) . . . . ?
C004 P001 C007 C009 32.2(5) . . . . ?
C004 P001 C007 C00A -147.9(4) . . . . ?
C004 P001 C008 O002 -135.5(5) . . . . ?
C004 P001 C008 C00E 47.3(5) . . . . ?
C005 C006 C00A C007 -0.2(9) . . . . ?
C006 C005 C00B C009 -1.3(9) . . . . ?
C007 P001 C004 O003 33.4(6) . . . . ?
C007 P001 C004 C00D -151.9(4) . . . . ?
C007 P001 C008 O002 -29.8(6) . . . . ?
C007 P001 C008 C00E 153.0(5) . . . . ?
C007 C009 C00B C005 0.0(8) . . . . ?
C008 P001 C004 O003 138.5(6) . . . . ?
C008 P001 C004 C00D -46.8(5) . . . . ?
C008 P001 C007 C009 -68.4(5) . . . . ?
C008 P001 C007 C00A 111.5(4) . . . . ?
C009 C007 C00A C006 -1.1(8) . . . . ?
C00A C007 C009 C00B 1.2(8) . . . . ?
C00B C005 C006 C00A 1.4(10) . . . . ?
C00D C00C C00E C008 63.6(7) . . . . ?
C00E C00C C00D C004 -62.8(7) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.595
_oxdiff_exptl_absorpt_empirical_full_min 0.387
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_compound-5a
_database_code_depnum_ccdc_archive 'CCDC 1988263'
loop_
_audit_author_name
_audit_author_address
'Kyle G. Pearce'
;University of Sussex
United Kingdom
;
_audit_update_record             
;
2020-03-04 deposited with the CCDC.	2020-03-31 downloaded from the CCDC.
;
_audit_creation_date             2020-01-09
_audit_creation_method           
;
Olex2 1.3
(compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C11 H9 O7 P W'
_chemical_formula_sum            'C11 H9 O7 P W'
_chemical_formula_weight         468.00
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C11 H9 P1 O7 W1'
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'
W W -5.4734 5.5774 '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                   6.89715(9)
_cell_length_b                   12.94011(18)
_cell_length_c                   15.83074(20)
_cell_angle_alpha                90
_cell_angle_beta                 101.0523(13)
_cell_angle_gamma                90
_cell_volume                     1386.69(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6470
_cell_measurement_temperature    100
_cell_measurement_theta_max      71.3890
_cell_measurement_theta_min      4.4410
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    16.818
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.44867
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear pale yellow'
_exptl_crystal_density_diffrn    2.242
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0242
_diffrn_reflns_av_unetI/netI     0.0199
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8789
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.630
_diffrn_reflns_theta_min         4.447
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1033
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     35.00 110.00   1.00    1.34    --   37.91 178.00  30.00   75
  2  ω     19.00 107.00   1.00    1.34    --   37.91  38.00  60.00   88
  3  ω     35.00 110.00   1.00    1.34    --   37.91 178.00-150.00   75
  4  ω    -33.00  67.00   1.00    1.34    --   37.91 -19.00-150.00  100
  5  ω     40.00 125.00   1.00    5.34    --  107.00 -61.00-120.00   85
  6  ω     39.00 134.00   1.00    5.34    --  107.00 -77.00 -90.00   95
  7  ω     79.00 177.00   1.00    5.34    --  107.00 111.00 -60.00   98
  8  ω     37.00  87.00   1.00    5.34    --  107.00-111.00 -90.00   50
  9  ω     89.00 174.00   1.00    5.34    --  107.00  61.00-150.00   85
 10  ω     38.00  84.00   1.00    5.34    --  107.00 -95.00 -60.00   46
 11  ω     79.00 177.00   1.00    5.34    --  107.00 111.00 -30.00   98
 12  ω     80.00 175.00   1.00    5.34    --  107.00  77.00  90.00   95
 13  ω     11.00 105.00   1.00    1.34    --   37.91  77.00 120.00   94
 14  ω     21.00 105.00   1.00    1.34    --   37.91  57.00 -60.00   84
 15  ω     21.00 105.00   1.00    1.34    --   37.91  57.00-150.00   84
 16  ω     89.00 174.00   1.00    5.34    --  107.00  61.00 150.00   85
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1938335000
_diffrn_orient_matrix_UB_12      0.0618498000
_diffrn_orient_matrix_UB_13      -0.0229038000
_diffrn_orient_matrix_UB_21      -0.1002119000
_diffrn_orient_matrix_UB_22      -0.0928943000
_diffrn_orient_matrix_UB_23      -0.0516069000
_diffrn_orient_matrix_UB_31      -0.0648334000
_diffrn_orient_matrix_UB_32      -0.0414003000
_diffrn_orient_matrix_UB_33      0.0815026000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2620
_reflns_number_total             2671
_reflns_odcompleteness_completeness 99.96
_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 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT n/a (Sheldrick, 2015)'
_refine_diff_density_max         0.643
_refine_diff_density_min         -1.230
_refine_diff_density_rms         0.138
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.201
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         2671
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0212
_refine_ls_R_factor_gt           0.0204
_refine_ls_restrained_S_all      1.201
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0261P)²+1.2348P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0503
_refine_ls_wR_factor_ref         0.0507
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C3(H3A,H3B), C2(H2A,H2B)
2.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C)
;
_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
W1 W 0.76256(2) 0.69597(2) 0.45758(2) 0.00492(7) Uani 1 1 d . . . . .
P1 P 0.63863(11) 0.78566(6) 0.31728(5) 0.00538(14) Uani 1 1 d . . . . .
O2 O 0.8114(3) 0.96554(19) 0.28798(15) 0.0135(5) Uani 1 1 d . . . . .
O5 O 0.5393(4) 0.4880(2) 0.38566(17) 0.0206(5) Uani 1 1 d . . . . .
O1 O 0.2888(3) 0.7291(2) 0.22254(16) 0.0162(5) Uani 1 1 d . . . . .
O6 O 0.9476(4) 0.5764(2) 0.62665(15) 0.0180(5) Uani 1 1 d . . . . .
O4 O 1.1501(3) 0.63819(19) 0.38630(17) 0.0167(5) Uani 1 1 d . . . . .
O7 O 0.3970(4) 0.7605(2) 0.54250(16) 0.0197(5) Uani 1 1 d . . . . .
O3 O 0.9854(4) 0.8976(2) 0.54014(17) 0.0218(5) Uani 1 1 d . . . . .
C8 C 1.0085(5) 0.6573(2) 0.4101(2) 0.0106(6) Uani 1 1 d . . . . .
C11 C 0.5255(5) 0.7368(3) 0.5105(2) 0.0128(6) Uani 1 1 d . . . . .
C5 C 0.6826(4) 0.9291(2) 0.32017(19) 0.0082(6) Uani 1 1 d . . . . .
C10 C 0.8778(5) 0.6196(3) 0.5652(2) 0.0121(6) Uani 1 1 d . . . . .
C7 C 0.9056(5) 0.8262(3) 0.5101(2) 0.0104(6) Uani 1 1 d . . . . .
C9 C 0.6180(5) 0.5628(3) 0.4090(2) 0.0105(6) Uani 1 1 d . . . . .
C1 C 0.3635(5) 0.7886(3) 0.2779(2) 0.0101(6) Uani 1 1 d . . . . .
C4 C 0.5447(5) 0.9905(3) 0.3644(2) 0.0121(6) Uani 1 1 d . . . . .
H4A H 0.581658 1.064470 0.365428 0.015 Uiso 1 1 calc R U . . .
H4B H 0.557704 0.966632 0.424625 0.015 Uiso 1 1 calc R U . . .
C6 C 0.7323(5) 0.7393(3) 0.2246(2) 0.0116(6) Uani 1 1 d . . . . .
H6A H 0.876781 0.735216 0.239014 0.017 Uiso 1 1 calc R U . . .
H6B H 0.692960 0.787146 0.176340 0.017 Uiso 1 1 calc R U . . .
H6C H 0.677840 0.670642 0.208372 0.017 Uiso 1 1 calc R U . . .
C3 C 0.3291(5) 0.9778(3) 0.3174(2) 0.0135(6) Uani 1 1 d . . . . .
H3A H 0.244559 1.024806 0.343899 0.016 Uiso 1 1 calc R U . . .
H3B H 0.318882 0.998961 0.256604 0.016 Uiso 1 1 calc R U . . .
C2 C 0.2508(5) 0.8676(3) 0.3198(2) 0.0146(7) Uani 1 1 d . . . . .
H2A H 0.256287 0.847478 0.380582 0.018 Uiso 1 1 calc R U . . .
H2B H 0.110498 0.866336 0.290495 0.018 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 P1 2.5065(7) . ?
W1 C8 2.045(3) . ?
W1 C11 2.045(3) . ?
W1 C10 1.998(3) . ?
W1 C7 2.047(3) . ?
W1 C9 2.064(3) . ?
P1 C5 1.880(3) . ?
P1 C1 1.881(3) . ?
P1 C6 1.815(3) . ?
O2 C5 1.202(4) . ?
O5 C9 1.136(4) . ?
O1 C1 1.206(4) . ?
O6 C10 1.144(4) . ?
O4 C8 1.140(4) . ?
O7 C11 1.144(4) . ?
O3 C7 1.132(4) . ?
C5 C4 1.511(4) . ?
C1 C2 1.512(5) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C4 C3 1.538(5) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C2 1.528(5) . ?
C2 H2A 0.9900 . ?
C2 H2B 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
C8 W1 P1 87.36(9) . . ?
C8 W1 C7 88.95(13) . . ?
C8 W1 C9 91.96(12) . . ?
C11 W1 P1 94.57(9) . . ?
C11 W1 C8 177.18(12) . . ?
C11 W1 C7 88.93(13) . . ?
C11 W1 C9 90.10(13) . . ?
C10 W1 P1 175.54(10) . . ?
C10 W1 C8 88.27(13) . . ?
C10 W1 C11 89.83(13) . . ?
C10 W1 C7 88.78(13) . . ?
C10 W1 C9 89.40(13) . . ?
C7 W1 P1 91.98(9) . . ?
C7 W1 C9 177.94(12) . . ?
C9 W1 P1 89.91(9) . . ?
C5 P1 W1 114.18(10) . . ?
C5 P1 C1 97.81(14) . . ?
C1 P1 W1 117.00(10) . . ?
C6 P1 W1 116.72(11) . . ?
C6 P1 C5 105.36(15) . . ?
C6 P1 C1 103.41(15) . . ?
O4 C8 W1 177.2(3) . . ?
O7 C11 W1 177.8(3) . . ?
O2 C5 P1 120.4(2) . . ?
O2 C5 C4 124.9(3) . . ?
C4 C5 P1 114.7(2) . . ?
O6 C10 W1 178.6(3) . . ?
O3 C7 W1 179.1(3) . . ?
O5 C9 W1 177.2(3) . . ?
O1 C1 P1 119.4(3) . . ?
O1 C1 C2 124.5(3) . . ?
C2 C1 P1 116.1(2) . . ?
C5 C4 H4A 109.5 . . ?
C5 C4 H4B 109.5 . . ?
C5 C4 C3 110.8(3) . . ?
H4A C4 H4B 108.1 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
P1 C6 H6A 109.5 . . ?
P1 C6 H6B 109.5 . . ?
P1 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C4 C3 H3A 108.8 . . ?
C4 C3 H3B 108.8 . . ?
H3A C3 H3B 107.7 . . ?
C2 C3 C4 113.6(3) . . ?
C2 C3 H3A 108.8 . . ?
C2 C3 H3B 108.8 . . ?
C1 C2 C3 113.9(3) . . ?
C1 C2 H2A 108.8 . . ?
C1 C2 H2B 108.8 . . ?
C3 C2 H2A 108.8 . . ?
C3 C2 H2B 108.8 . . ?
H2A C2 H2B 107.7 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
W1 P1 C5 O2 104.4(2) . . . . ?
W1 P1 C5 C4 -76.0(2) . . . . ?
W1 P1 C1 O1 -101.2(3) . . . . ?
W1 P1 C1 C2 78.6(3) . . . . ?
P1 C5 C4 C3 -61.7(3) . . . . ?
P1 C1 C2 C3 53.4(4) . . . . ?
O2 C5 C4 C3 117.8(3) . . . . ?
O1 C1 C2 C3 -126.8(4) . . . . ?
C5 P1 C1 O1 136.5(3) . . . . ?
C5 P1 C1 C2 -43.7(3) . . . . ?
C5 C4 C3 C2 64.8(4) . . . . ?
C1 P1 C5 O2 -131.3(3) . . . . ?
C1 P1 C5 C4 48.3(2) . . . . ?
C4 C3 C2 C1 -60.8(4) . . . . ?
C6 P1 C5 O2 -25.0(3) . . . . ?
C6 P1 C5 C4 154.6(2) . . . . ?
C6 P1 C1 O1 28.6(3) . . . . ?
C6 P1 C1 C2 -151.6(3) . . . . ?

_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 2.035
_oxdiff_exptl_absorpt_empirical_full_min 0.778
_chemical_properties_physical    Moisture-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_compound-2e
_database_code_depnum_ccdc_archive 'CCDC 1988261'
loop_
_audit_author_name
_audit_author_address
'Kyle G. Pearce'
;University of Sussex
United Kingdom
;
_audit_update_record             
;
2020-03-04 deposited with the CCDC.	2020-03-31 downloaded from the CCDC.
;
_audit_creation_date             2020-01-09
_audit_creation_method           
;
Olex2 1.3
(compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C14 H17 O2 P'
_chemical_formula_sum            'C14 H17 O2 P'
_chemical_formula_weight         248.24
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C14 H17 O2 P1 '
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'

_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                   10.8705(3)
_cell_length_b                   9.7423(2)
_cell_length_c                   11.9176(2)
_cell_angle_alpha                90
_cell_angle_beta                 93.452(2)
_cell_angle_gamma                90
_cell_volume                     1259.83(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2898
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      71.4210
_cell_measurement_theta_min      4.0620
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.828
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85176
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.309
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             528
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0194
_diffrn_reflns_av_unetI/netI     0.0271
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4524
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.722
_diffrn_reflns_theta_min         4.074
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1033
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     40.00  92.00   1.00    4.60    --   37.91 178.00 150.00   52
  2  ω     -6.00  64.00   1.00    4.60    --   37.91 -99.00-180.00   70
  3  ω     57.00 105.00   1.00    4.60    --   37.91 178.00  90.00   48
  4  ω     21.00  96.00   1.00    4.60    --   37.91  57.00 -90.00   75
  5  ω     93.00 167.00   1.00   18.40    --  107.00  61.00  60.00   74
  6  ω     42.00  69.00   1.00   18.40    --  107.00-111.00-150.00   27
  7  ω     84.00 120.00   1.00   18.40    --  107.00  77.00 150.00   36
  8  ω     38.00  79.00   1.00   18.40    --  107.00 -95.00 -60.00   41
  9  ω     55.00 123.00   1.00   18.40    --  107.00 -61.00 -60.00   68
 10  ω     51.00  78.00   1.00   18.40    --  107.00 -95.00-120.00   27
 11  ω     39.00  64.00   1.00   18.40    --  107.00 -95.00  90.00   25
 12  ω     92.00 171.00   1.00   18.40    --  107.00  45.00   0.00   79
 13  ω    150.00 175.00   1.00   18.40    --  107.00  77.00 150.00   25
 14  ω     89.00 170.00   1.00   18.40    --  107.00  77.00  30.00   81
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0663558000
_diffrn_orient_matrix_UB_12      -0.1392881000
_diffrn_orient_matrix_UB_13      0.0132216000
_diffrn_orient_matrix_UB_21      -0.0016084000
_diffrn_orient_matrix_UB_22      -0.0140546000
_diffrn_orient_matrix_UB_23      -0.1288788000
_diffrn_orient_matrix_UB_31      0.1255287000
_diffrn_orient_matrix_UB_32      0.0733385000
_diffrn_orient_matrix_UB_33      0.0001229000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2237
_reflns_number_total             2407
_reflns_odcompleteness_completeness 99.96
_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 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.372
_refine_diff_density_min         -0.296
_refine_diff_density_rms         0.054
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     157
_refine_ls_number_reflns         2407
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0379
_refine_ls_R_factor_gt           0.0344
_refine_ls_restrained_S_all      1.082
_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)+(0.0400P)²+0.8441P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0894
_refine_ls_wR_factor_ref         0.0915
_refine_special_details          ?
_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.a Secondary CH2 refined with riding coordinates:
 C2(H2a,H2b), C4(H4a,H4b), C3(H3a,H3b)
2.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C10(H10)
2.c Idealised Me refined as rotating group:
 C12(H12a,H12b,H12c), C14(H14a,H14b,H14c), C13(H13a,H13b,H13c)
;
_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
P1 P 0.30834(3) 0.39894(4) 0.69063(3) 0.01355(13) Uani 1 1 d . . . . .
O1 O 0.34667(10) 0.66697(12) 0.73565(10) 0.0204(3) Uani 1 1 d . . . . .
O2 O 0.09505(11) 0.26342(13) 0.64969(11) 0.0249(3) Uani 1 1 d . . . . .
C6 C 0.29690(14) 0.44146(16) 0.54205(12) 0.0130(3) Uani 1 1 d . . . . .
C11 C 0.20688(13) 0.53093(16) 0.49242(13) 0.0138(3) Uani 1 1 d . . . . .
C7 C 0.38291(13) 0.37823(16) 0.47444(13) 0.0135(3) Uani 1 1 d . . . . .
C8 C 0.37729(14) 0.40556(16) 0.35956(13) 0.0153(3) Uani 1 1 d . . . . .
H8 H 0.434732 0.364865 0.315301 0.018 Uiso 1 1 calc R . . . .
C9 C 0.28853(15) 0.49172(16) 0.30910(13) 0.0161(3) Uani 1 1 d . . . . .
C10 C 0.20397(14) 0.55352(16) 0.37670(13) 0.0152(3) Uani 1 1 d . . . . .
H10 H 0.144054 0.611335 0.343749 0.018 Uiso 1 1 calc R . . . .
C12 C 0.48160(14) 0.28075(17) 0.52096(13) 0.0169(3) Uani 1 1 d . . . . .
H12A H 0.527905 0.323774 0.582451 0.025 Uiso 1 1 calc GR . . . .
H12B H 0.535790 0.258050 0.463028 0.025 Uiso 1 1 calc GR . . . .
H12C H 0.443733 0.198569 0.546933 0.025 Uiso 1 1 calc GR . . . .
C1 C 0.30517(14) 0.56158(17) 0.77108(13) 0.0161(3) Uani 1 1 d . . . . .
C14 C 0.11481(14) 0.60746(17) 0.55883(13) 0.0169(3) Uani 1 1 d . . . . .
H14A H 0.076317 0.544778 0.608054 0.025 Uiso 1 1 calc GR . . . .
H14B H 0.053173 0.648077 0.508149 0.025 Uiso 1 1 calc GR . . . .
H14C H 0.156383 0.678170 0.602519 0.025 Uiso 1 1 calc GR . . . .
C5 C 0.15548(14) 0.32739(17) 0.72094(14) 0.0184(3) Uani 1 1 d . . . . .
C13 C 0.28454(17) 0.51818(18) 0.18458(14) 0.0226(4) Uani 1 1 d . . . . .
H13A H 0.361161 0.558083 0.165156 0.034 Uiso 1 1 calc GR . . . .
H13B H 0.218255 0.580168 0.164250 0.034 Uiso 1 1 calc GR . . . .
H13C H 0.271665 0.433170 0.144852 0.034 Uiso 1 1 calc GR . . . .
C2 C 0.25797(16) 0.5487(2) 0.88738(14) 0.0240(4) Uani 1 1 d . . . . .
H2A H 0.258482 0.638525 0.922475 0.029 Uiso 1 1 calc R . . . .
H2B H 0.313131 0.489815 0.932677 0.029 Uiso 1 1 calc R . . . .
C4 C 0.11739(16) 0.34298(19) 0.84043(15) 0.0242(4) Uani 1 1 d . . . . .
H4A H 0.168589 0.283546 0.888971 0.029 Uiso 1 1 calc R . . . .
H4B H 0.032789 0.312336 0.843778 0.029 Uiso 1 1 calc R . . . .
C3 C 0.12749(16) 0.4896(2) 0.88560(15) 0.0258(4) Uani 1 1 d . . . . .
H3A H 0.099678 0.491070 0.961411 0.031 Uiso 1 1 calc R . . . .
H3B H 0.072832 0.548185 0.839544 0.031 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
P1 C6 1.8154(15) . ?
P1 C1 1.8534(17) . ?
P1 C5 1.8574(16) . ?
O1 C1 1.208(2) . ?
O2 C5 1.214(2) . ?
C6 C11 1.413(2) . ?
C6 C7 1.412(2) . ?
C11 C10 1.395(2) . ?
C11 C14 1.510(2) . ?
C7 C8 1.392(2) . ?
C7 C12 1.513(2) . ?
C8 H8 0.9300 . ?
C8 C9 1.388(2) . ?
C9 C10 1.395(2) . ?
C9 C13 1.504(2) . ?
C10 H10 0.9300 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C1 C2 1.512(2) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C5 C4 1.514(2) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C3 1.530(2) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 C3 1.528(3) . ?
C3 H3A 0.9700 . ?
C3 H3B 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
C6 P1 C1 107.89(7) . . ?
C6 P1 C5 105.41(7) . . ?
C1 P1 C5 100.11(7) . . ?
C11 C6 P1 123.64(11) . . ?
C7 C6 P1 116.63(11) . . ?
C7 C6 C11 119.73(14) . . ?
C6 C11 C14 123.32(14) . . ?
C10 C11 C6 119.01(14) . . ?
C10 C11 C14 117.65(14) . . ?
C6 C7 C12 122.96(14) . . ?
C8 C7 C6 119.10(14) . . ?
C8 C7 C12 117.94(14) . . ?
C7 C8 H8 119.0 . . ?
C9 C8 C7 121.99(14) . . ?
C9 C8 H8 119.0 . . ?
C8 C9 C10 118.41(14) . . ?
C8 C9 C13 120.59(15) . . ?
C10 C9 C13 121.00(15) . . ?
C11 C10 H10 119.1 . . ?
C9 C10 C11 121.76(14) . . ?
C9 C10 H10 119.1 . . ?
C7 C12 H12A 109.5 . . ?
C7 C12 H12B 109.5 . . ?
C7 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O1 C1 P1 121.80(12) . . ?
O1 C1 C2 123.07(15) . . ?
C2 C1 P1 114.90(12) . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O2 C5 P1 120.62(13) . . ?
O2 C5 C4 122.83(15) . . ?
C4 C5 P1 116.34(12) . . ?
C9 C13 H13A 109.5 . . ?
C9 C13 H13B 109.5 . . ?
C9 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C1 C2 H2A 109.1 . . ?
C1 C2 H2B 109.1 . . ?
C1 C2 C3 112.59(14) . . ?
H2A C2 H2B 107.8 . . ?
C3 C2 H2A 109.1 . . ?
C3 C2 H2B 109.1 . . ?
C5 C4 H4A 108.7 . . ?
C5 C4 H4B 108.7 . . ?
C5 C4 C3 114.02(14) . . ?
H4A C4 H4B 107.6 . . ?
C3 C4 H4A 108.7 . . ?
C3 C4 H4B 108.7 . . ?
C2 C3 H3A 108.8 . . ?
C2 C3 H3B 108.8 . . ?
C4 C3 C2 113.80(15) . . ?
C4 C3 H3A 108.8 . . ?
C4 C3 H3B 108.8 . . ?
H3A C3 H3B 107.7 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.160
_oxdiff_exptl_absorpt_empirical_full_min 0.690
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_compound-4
_database_code_depnum_ccdc_archive 'CCDC 1988262'
loop_
_audit_author_name
_audit_author_address
'Kyle G. Pearce'
;University of Sussex
United Kingdom
;
_audit_update_record             
;
2020-03-04 deposited with the CCDC.	2020-03-31 downloaded from the CCDC.
;
_audit_creation_date             2020-01-09
_audit_creation_method           
;
Olex2 1.3
(compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C17 H26 Cl2 O2 P2 Pt'
_chemical_formula_sum            'C17 H26 Cl2 O2 P2 Pt'
_chemical_formula_weight         590.31
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C17 H10 Cl2 O2 P2 Pt1 '
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'
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'
Pt Pt -4.5932 6.9264 '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           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   7.4569(9)
_cell_length_b                   10.591(2)
_cell_length_c                   26.251(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2073.2(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1197
_cell_measurement_temperature    100
_cell_measurement_theta_max      56.9010
_cell_measurement_theta_min      3.3560
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    16.553
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.21583
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.29c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.891
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1144
_exptl_crystal_preparation       ?
_exptl_crystal_recrystallization_method ?
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1356
_diffrn_reflns_av_unetI/netI     0.1724
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            8810
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.247
_diffrn_reflns_theta_min         3.367
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -36.00  31.00   1.00   47.50    --    5.00  18.00  58.00   67
  2  ω   -125.00 -97.00   1.00   47.50    --  -89.00  18.00  58.00   28
  3  ω     48.00  91.00   1.00   47.50    --    5.00  18.00  58.00   43
  4  ω   -175.00  -2.00   1.00   47.50    --  -89.00  60.00-180.00  173
  5  ω   -161.00  -4.00   1.00   47.50    --  -89.00  60.00 120.00  157
  6  ω   -108.00  -1.00   1.00   47.50    --  -89.00  57.00 150.00  107
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RCD3): quarter-chi single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0551756000
_diffrn_orient_matrix_UB_12      0.0537849000
_diffrn_orient_matrix_UB_13      -0.0522670000
_diffrn_orient_matrix_UB_21      -0.0315175000
_diffrn_orient_matrix_UB_22      -0.1303474000
_diffrn_orient_matrix_UB_23      -0.0244795000
_diffrn_orient_matrix_UB_31      -0.1964664000
_diffrn_orient_matrix_UB_32      0.0358806000
_diffrn_orient_matrix_UB_33      -0.0107005000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\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         0.712
_reflns_Friedel_fraction_full    0.977
_reflns_Friedel_fraction_max     0.969
_reflns_number_gt                1793
_reflns_number_total             3724
_reflns_odcompleteness_completeness 99.54
_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 1.171.39.29c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT n/a (Sheldrick, 2015)'
_refine_diff_density_max         2.261
_refine_diff_density_min         -3.047
_refine_diff_density_rms         0.247
_refine_ls_abs_structure_details 
;
 Flack x determined using 359 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.06(2)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         3724
_refine_ls_number_restraints     54
_refine_ls_R_factor_all          0.1763
_refine_ls_R_factor_gt           0.1055
_refine_ls_restrained_S_all      1.003
_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)+(0.1272P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2316
_refine_ls_wR_factor_ref         0.3003
_refine_special_details          ?
_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
C1 \\sim O1 \\sim C5 \\sim O2: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
C2 \\sim C4: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
C12 \\sim C16 \\sim C14: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
C17 \\sim C13 \\sim C15: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
Uanis(C2) = Uanis(C4)
Uanis(C16) = Uanis(C17) = Uanis(C14) = Uanis(C15) = Uanis(C12) = Uanis(C13)
3. Rigid body (RIGU) restrains
 C6, C11, C10, C9, C8, C7
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C5, O2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1, O1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C16(H16A,H16B), C3(H3A,H3B), C12(H12A,H12B), C14(H14A,H14B),
 C2(H2A,H2B)
4.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C10(H10), C11(H11)
4.c Fitted hexagon refined as free rotating group:
 C6(C7,C8,C9,C10,C11)
4.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C15(H15A,H15B,H15C), C13(H13A,H13B,H13C)
;
_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
Pt1 Pt 0.3199(2) 0.3824(2) 0.65575(6) 0.0748(6) Uani 1 1 d . . . . .
Cl2 Cl 0.1519(13) 0.3588(11) 0.7291(4) 0.085(3) Uani 1 1 d . . . . .
P1 P 0.4799(13) 0.3888(13) 0.5838(4) 0.074(3) Uani 1 1 d . . . . .
P2 P 0.3783(13) 0.5814(11) 0.6838(4) 0.072(3) Uani 1 1 d . . . . .
Cl1 Cl 0.2491(15) 0.1690(12) 0.6365(4) 0.085(3) Uani 1 1 d . . . . .
O1 O 0.797(5) 0.516(4) 0.5819(13) 0.101(11) Uani 1 1 d . U . . .
O2 O 0.408(5) 0.209(3) 0.5136(13) 0.108(12) Uani 1 1 d . U . . .
C1 C 0.730(6) 0.417(5) 0.5926(17) 0.087(13) Uani 1 1 d . U . . .
C4 C 0.631(6) 0.140(6) 0.5743(17) 0.108(13) Uani 1 1 d . . . . .
H4A H 0.724580 0.122583 0.548436 0.129 Uiso 1 1 calc R U . . .
H4B H 0.569435 0.059452 0.581820 0.129 Uiso 1 1 calc R U . . .
C16 C 0.178(5) 0.665(4) 0.7034(14) 0.087(6) Uani 1 1 d . . . . .
H16A H 0.112556 0.612252 0.728447 0.105 Uiso 1 1 calc R U . . .
H16B H 0.213503 0.744063 0.720513 0.105 Uiso 1 1 calc R U . . .
C17 C 0.053(6) 0.696(4) 0.6589(15) 0.087(6) Uani 1 1 d . . . . .
H17A H 0.119139 0.743815 0.633097 0.131 Uiso 1 1 calc R U . . .
H17B H -0.048174 0.745799 0.671267 0.131 Uiso 1 1 calc R U . . .
H17C H 0.008633 0.617008 0.643767 0.131 Uiso 1 1 calc R U . . .
C15 C 0.523(6) 0.822(4) 0.6591(15) 0.087(6) Uani 1 1 d . . . . .
H15A H 0.543702 0.877201 0.629595 0.131 Uiso 1 1 calc R U . . .
H15B H 0.628520 0.823815 0.681287 0.131 Uiso 1 1 calc R U . . .
H15C H 0.418113 0.852447 0.678010 0.131 Uiso 1 1 calc R U . . .
C5 C 0.505(6) 0.226(5) 0.5534(19) 0.090(14) Uani 1 1 d . U . . .
C3 C 0.721(7) 0.187(5) 0.6225(12) 0.098(18) Uani 1 1 d . . . . .
H3A H 0.800018 0.119586 0.636396 0.117 Uiso 1 1 calc R U . . .
H3B H 0.629636 0.207133 0.648406 0.117 Uiso 1 1 calc R U . . .
C12 C 0.519(6) 0.576(4) 0.7417(15) 0.087(6) Uani 1 1 d . . . . .
H12A H 0.550479 0.663007 0.752119 0.105 Uiso 1 1 calc R U . . .
H12B H 0.450622 0.536492 0.769788 0.105 Uiso 1 1 calc R U . . .
C6 C 0.426(4) 0.492(3) 0.5318(10) 0.086(11) Uani 1 1 d G . . . .
C7 C 0.539(4) 0.501(3) 0.4898(12) 0.098(14) Uani 1 1 d G . . . .
H7 H 0.646031 0.453020 0.488534 0.117 Uiso 1 1 calc R U . . .
C8 C 0.495(4) 0.581(3) 0.4498(10) 0.102(15) Uani 1 1 d G . . . .
H8 H 0.571746 0.587646 0.421077 0.122 Uiso 1 1 calc R U . . .
C9 C 0.338(4) 0.652(3) 0.4517(10) 0.091(12) Uani 1 1 d G . . . .
H9 H 0.307514 0.706564 0.424290 0.109 Uiso 1 1 calc R U . . .
C10 C 0.225(4) 0.643(3) 0.4937(11) 0.105(15) Uani 1 1 d G . . . .
H10 H 0.117566 0.690858 0.494959 0.126 Uiso 1 1 calc R U . . .
C11 C 0.269(4) 0.563(3) 0.5337(9) 0.092(13) Uani 1 1 d G . . . .
H11 H 0.191849 0.556233 0.562416 0.110 Uiso 1 1 calc R U . . .
C13 C 0.690(6) 0.501(4) 0.7328(15) 0.087(6) Uani 1 1 d . . . . .
H13A H 0.769655 0.549437 0.710287 0.131 Uiso 1 1 calc R U . . .
H13B H 0.660392 0.420406 0.716866 0.131 Uiso 1 1 calc R U . . .
H13C H 0.750014 0.486476 0.765423 0.131 Uiso 1 1 calc R U . . .
C14 C 0.489(6) 0.685(4) 0.6405(15) 0.087(6) Uani 1 1 d . . . . .
H14A H 0.605992 0.647210 0.631502 0.105 Uiso 1 1 calc R U . . .
H14B H 0.416715 0.689289 0.608906 0.105 Uiso 1 1 calc R U . . .
C2 C 0.834(7) 0.305(5) 0.6104(19) 0.108(13) Uani 1 1 d . . . . .
H2A H 0.900841 0.328839 0.641444 0.129 Uiso 1 1 calc R U . . .
H2B H 0.922441 0.282663 0.583887 0.129 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pt1 Cl2 2.311(11) . ?
Pt1 P1 2.234(11) . ?
Pt1 P2 2.274(12) . ?
Pt1 Cl1 2.376(12) . ?
P1 C1 1.90(5) . ?
P1 C5 1.91(5) . ?
P1 C6 1.79(2) . ?
P2 C16 1.81(4) . ?
P2 C12 1.85(4) . ?
P2 C14 1.78(4) . ?
O1 C1 1.20(6) . ?
O2 C5 1.28(5) . ?
C1 C2 1.49(6) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C4 C5 1.41(6) . ?
C4 C3 1.51(6) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C16 C17 1.53(5) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C15 C14 1.55(5) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C2 1.54(7) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C12 C13 1.51(6) . ?
C6 C7 1.3900 . ?
C6 C11 1.3900 . ?
C7 H7 0.9500 . ?
C7 C8 1.3900 . ?
C8 H8 0.9500 . ?
C8 C9 1.3900 . ?
C9 H9 0.9500 . ?
C9 C10 1.3900 . ?
C10 H10 0.9500 . ?
C10 C11 1.3900 . ?
C11 H11 0.9500 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 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
Cl2 Pt1 Cl1 87.4(4) . . ?
P1 Pt1 Cl2 175.4(5) . . ?
P1 Pt1 P2 98.3(4) . . ?
P1 Pt1 Cl1 88.1(4) . . ?
P2 Pt1 Cl2 86.2(4) . . ?
P2 Pt1 Cl1 173.3(4) . . ?
C1 P1 Pt1 115.2(15) . . ?
C1 P1 C5 95(2) . . ?
C5 P1 Pt1 112.2(15) . . ?
C6 P1 Pt1 122.8(12) . . ?
C6 P1 C1 102.5(19) . . ?
C6 P1 C5 105(2) . . ?
C16 P2 Pt1 112.7(16) . . ?
C16 P2 C12 104.5(18) . . ?
C12 P2 Pt1 110.2(16) . . ?
C14 P2 Pt1 117.0(16) . . ?
C14 P2 C16 105(2) . . ?
C14 P2 C12 106(2) . . ?
O1 C1 P1 121(4) . . ?
O1 C1 C2 124(4) . . ?
C2 C1 P1 115(4) . . ?
H4A C4 H4B 107.6 . . ?
C5 C4 H4A 108.7 . . ?
C5 C4 H4B 108.7 . . ?
C5 C4 C3 114(5) . . ?
C3 C4 H4A 108.7 . . ?
C3 C4 H4B 108.7 . . ?
P2 C16 H16A 109.0 . . ?
P2 C16 H16B 109.0 . . ?
H16A C16 H16B 107.8 . . ?
C17 C16 P2 113(3) . . ?
C17 C16 H16A 109.0 . . ?
C17 C16 H16B 109.0 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
O2 C5 P1 114(4) . . ?
O2 C5 C4 127(5) . . ?
C4 C5 P1 119(4) . . ?
C4 C3 H3A 109.8 . . ?
C4 C3 H3B 109.8 . . ?
C4 C3 C2 110(4) . . ?
H3A C3 H3B 108.2 . . ?
C2 C3 H3A 109.8 . . ?
C2 C3 H3B 109.8 . . ?
P2 C12 H12A 109.3 . . ?
P2 C12 H12B 109.3 . . ?
H12A C12 H12B 108.0 . . ?
C13 C12 P2 112(3) . . ?
C13 C12 H12A 109.3 . . ?
C13 C12 H12B 109.3 . . ?
C7 C6 P1 120.7(19) . . ?
C7 C6 C11 120.0 . . ?
C11 C6 P1 119.3(19) . . ?
C6 C7 H7 120.0 . . ?
C8 C7 C6 120.0 . . ?
C8 C7 H7 120.0 . . ?
C7 C8 H8 120.0 . . ?
C7 C8 C9 120.0 . . ?
C9 C8 H8 120.0 . . ?
C8 C9 H9 120.0 . . ?
C8 C9 C10 120.0 . . ?
C10 C9 H9 120.0 . . ?
C9 C10 H10 120.0 . . ?
C11 C10 C9 120.0 . . ?
C11 C10 H10 120.0 . . ?
C6 C11 H11 120.0 . . ?
C10 C11 C6 120.0 . . ?
C10 C11 H11 120.0 . . ?
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 . . ?
P2 C14 H14A 108.1 . . ?
P2 C14 H14B 108.1 . . ?
C15 C14 P2 117(3) . . ?
C15 C14 H14A 108.1 . . ?
C15 C14 H14B 108.1 . . ?
H14A C14 H14B 107.3 . . ?
C1 C2 C3 116(4) . . ?
C1 C2 H2A 108.4 . . ?
C1 C2 H2B 108.4 . . ?
C3 C2 H2A 108.4 . . ?
C3 C2 H2B 108.4 . . ?
H2A C2 H2B 107.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Pt1 P1 C6 C7 173.9(12) . . . . ?
Pt1 P1 C6 C11 -6(2) . . . . ?
Pt1 P2 C16 C17 -68(3) . . . . ?
Pt1 P2 C12 C13 55(3) . . . . ?
Pt1 P2 C14 C15 178(3) . . . . ?
P1 C1 C2 C3 -4(6) . . . . ?
P1 C6 C7 C8 180(2) . . . . ?
P1 C6 C11 C10 -180(2) . . . . ?
O1 C1 C2 C3 180(5) . . . . ?
C1 P1 C6 C7 43(2) . . . . ?
C1 P1 C6 C11 -138(2) . . . . ?
C4 C3 C2 C1 64(6) . . . . ?
C16 P2 C12 C13 177(3) . . . . ?
C16 P2 C14 C15 52(4) . . . . ?
C5 P1 C6 C7 -57(2) . . . . ?
C5 P1 C6 C11 123(2) . . . . ?
C5 C4 C3 C2 -64(5) . . . . ?
C3 C4 C5 P1 5(6) . . . . ?
C3 C4 C5 O2 -179(4) . . . . ?
C12 P2 C16 C17 172(3) . . . . ?
C12 P2 C14 C15 -58(4) . . . . ?
C6 C7 C8 C9 0.0 . . . . ?
C7 C6 C11 C10 0.0 . . . . ?
C7 C8 C9 C10 0.0 . . . . ?
C8 C9 C10 C11 0.0 . . . . ?
C9 C10 C11 C6 0.0 . . . . ?
C11 C6 C7 C8 0.0 . . . . ?
C14 P2 C16 C17 60(4) . . . . ?
C14 P2 C12 C13 -72(4) . . . . ?

_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 2.350
_oxdiff_exptl_absorpt_empirical_full_min 0.272
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_compound-5c
_database_code_depnum_ccdc_archive 'CCDC 1988264'
loop_
_audit_author_name
_audit_author_address
'Kyle G. Pearce'
;University of Sussex
United Kingdom
;
_audit_update_record             
;
2020-03-04 deposited with the CCDC.	2020-03-31 downloaded from the CCDC.
;
_audit_creation_date             2020-01-09
_audit_creation_method           
;
Olex2 1.3
(compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C14 H15 O7 P W'
_chemical_formula_sum            'C14 H15 O7 P W'
_chemical_formula_weight         510.08
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C14 H15 P W O7 '
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'
W W -5.4734 5.5774 '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, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   12.3442(2)
_cell_length_b                   12.5495(2)
_cell_length_c                   21.9424(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3399.17(10)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    3379
_cell_measurement_temperature    100
_cell_measurement_theta_max      71.5830
_cell_measurement_theta_min      5.4160
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    13.786
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53756
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear pale yellow'
_exptl_crystal_density_diffrn    1.993
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1952
_exptl_crystal_size_max          0.1
_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  0.0279
_diffrn_reflns_av_unetI/netI     0.0333
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            6770
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.718
_diffrn_reflns_theta_min         4.029
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1033
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -20.00  12.00   1.00   27.63    --   37.66   0.00-180.00   32
  2  ω     -2.00  54.00   1.00   27.63    --   37.66 -57.00 -30.00   56
  3  ω     24.00 105.00   1.00   27.63    --   37.66   0.00-180.00   81
  4  ω     90.00 172.00   1.00  110.53    --  107.00  61.00-120.00   82
  5  ω    126.00 158.00   1.00  110.53    --  107.00  61.00 -60.00   32
  6  ω     55.00  82.00   1.00  110.53    --  107.00 -95.00  30.00   27
  7  ω     93.00 177.00   1.00  110.53    --  107.00 111.00  90.00   84
  8  ω     57.00 102.00   1.00  110.53    --  107.00 -61.00-180.00   45
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0537620000
_diffrn_orient_matrix_UB_12      -0.0361715000
_diffrn_orient_matrix_UB_13      -0.0598303000
_diffrn_orient_matrix_UB_21      0.1114892000
_diffrn_orient_matrix_UB_22      0.0009412000
_diffrn_orient_matrix_UB_23      0.0316320000
_diffrn_orient_matrix_UB_31      -0.0159638000
_diffrn_orient_matrix_UB_32      -0.1173102000
_diffrn_orient_matrix_UB_33      0.0186760000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2866
_reflns_number_total             3219
_reflns_odcompleteness_completeness 99.04
_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 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT n/a (Sheldrick, 2015)'
_refine_diff_density_max         1.717
_refine_diff_density_min         -1.456
_refine_diff_density_rms         0.154
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         3219
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0360
_refine_ls_R_factor_gt           0.0302
_refine_ls_restrained_S_all      1.064
_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)+(0.0495P)²+3.2855P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0821
_refine_ls_wR_factor_ref         0.0851
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C3(H3A,H3B), C2(H2A,H2B)
2.b Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C)
;
_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
W1 W 0.62662(2) 0.66130(2) 0.65910(2) 0.01244(10) Uani 1 1 d . . . . .
P1 P 0.48663(8) 0.76989(8) 0.60363(5) 0.0142(2) Uani 1 1 d . . . . .
O3 O 0.4647(3) 0.4629(3) 0.65971(15) 0.0265(8) Uani 1 1 d . . . . .
O7 O 0.8098(3) 0.5332(3) 0.72735(17) 0.0298(8) Uani 1 1 d . . . . .
O6 O 0.5436(3) 0.7242(3) 0.79182(15) 0.0305(8) Uani 1 1 d . . . . .
O5 O 0.7942(3) 0.8527(3) 0.64664(19) 0.0299(8) Uani 1 1 d . . . . .
O4 O 0.7147(3) 0.5645(3) 0.53534(17) 0.0360(9) Uani 1 1 d . . . . .
O2 O 0.5686(4) 0.9562(3) 0.56328(19) 0.0411(10) Uani 1 1 d . . . . .
O1 O 0.3259(3) 0.6385(3) 0.57121(19) 0.0380(9) Uani 1 1 d . . . . .
C14 C 0.7419(4) 0.5779(4) 0.7025(2) 0.0213(9) Uani 1 1 d . . . . .
C11 C 0.6838(4) 0.6015(4) 0.5797(2) 0.0216(9) Uani 1 1 d . . . . .
C12 C 0.7323(4) 0.7864(4) 0.6521(2) 0.0221(10) Uani 1 1 d . . . . .
C10 C 0.5210(4) 0.5342(4) 0.66080(18) 0.0175(9) Uani 1 1 d . . . . .
C13 C 0.5714(4) 0.7061(4) 0.7436(2) 0.0201(9) Uani 1 1 d . . . . .
C1 C 0.4061(5) 0.6816(4) 0.5514(2) 0.0266(10) Uani 1 1 d . . . . .
C5 C 0.5507(4) 0.8657(4) 0.5483(2) 0.0268(10) Uani 1 1 d . . . . .
C9 C 0.3178(4) 0.7795(5) 0.6883(2) 0.0306(11) Uani 1 1 d . . . . .
H9A H 0.284620 0.721454 0.664961 0.046 Uiso 1 1 calc R U . . .
H9B H 0.261087 0.821261 0.708385 0.046 Uiso 1 1 calc R U . . .
H9C H 0.366602 0.749586 0.719121 0.046 Uiso 1 1 calc R U . . .
C4 C 0.5803(5) 0.8200(4) 0.4868(2) 0.0315(12) Uani 1 1 d . . . . .
H4A H 0.639150 0.767127 0.492016 0.038 Uiso 1 1 calc R U . . .
H4B H 0.607841 0.877833 0.460328 0.038 Uiso 1 1 calc R U . . .
C7 C 0.3047(4) 0.9040(4) 0.5999(3) 0.0306(11) Uani 1 1 d . . . . .
H7A H 0.346509 0.943489 0.569417 0.046 Uiso 1 1 calc R U . . .
H7B H 0.256677 0.953150 0.621712 0.046 Uiso 1 1 calc R U . . .
H7C H 0.261320 0.849049 0.579669 0.046 Uiso 1 1 calc R U . . .
C8 C 0.4421(4) 0.9365(4) 0.6827(3) 0.0311(11) Uani 1 1 d . . . . .
H8A H 0.495799 0.901933 0.708982 0.047 Uiso 1 1 calc R U . . .
H8B H 0.389997 0.975601 0.707835 0.047 Uiso 1 1 calc R U . . .
H8C H 0.478785 0.986095 0.655031 0.047 Uiso 1 1 calc R U . . .
C6 C 0.3822(4) 0.8514(4) 0.6452(3) 0.0214(10) Uani 1 1 d . . . . .
C3 C 0.4834(6) 0.7663(5) 0.4558(2) 0.0395(13) Uani 1 1 d . . . . .
H3A H 0.421667 0.816658 0.455310 0.047 Uiso 1 1 calc R U . . .
H3B H 0.502581 0.750003 0.413003 0.047 Uiso 1 1 calc R U . . .
C2 C 0.4483(6) 0.6633(4) 0.4877(2) 0.0341(13) Uani 1 1 d . . . . .
H2A H 0.391109 0.628539 0.463091 0.041 Uiso 1 1 calc R U . . .
H2B H 0.510929 0.614103 0.489583 0.041 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 P1 2.5149(10) . ?
W1 C14 2.007(5) . ?
W1 C11 2.023(5) . ?
W1 C12 2.046(5) . ?
W1 C10 2.061(5) . ?
W1 C13 2.054(5) . ?
P1 C1 1.878(5) . ?
P1 C5 1.882(5) . ?
P1 C6 1.882(5) . ?
O3 C10 1.132(6) . ?
O7 C14 1.147(6) . ?
O6 C13 1.136(6) . ?
O5 C12 1.137(6) . ?
O4 C11 1.145(6) . ?
O2 C5 1.202(7) . ?
O1 C1 1.209(7) . ?
C1 C2 1.511(8) . ?
C5 C4 1.512(7) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C9 C6 1.529(7) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C4 C3 1.532(9) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C7 C6 1.529(7) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C8 C6 1.536(7) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C2 1.532(8) . ?
C2 H2A 0.9900 . ?
C2 H2B 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
C14 W1 P1 178.19(14) . . ?
C14 W1 C11 88.16(19) . . ?
C14 W1 C12 89.04(19) . . ?
C14 W1 C10 92.10(18) . . ?
C14 W1 C13 87.12(18) . . ?
C11 W1 P1 91.37(14) . . ?
C11 W1 C12 89.89(18) . . ?
C11 W1 C10 87.09(17) . . ?
C11 W1 C13 173.86(18) . . ?
C12 W1 P1 89.21(13) . . ?
C12 W1 C10 176.73(16) . . ?
C12 W1 C13 93.94(18) . . ?
C10 W1 P1 89.62(12) . . ?
C13 W1 P1 93.47(12) . . ?
C13 W1 C10 89.18(17) . . ?
C1 P1 W1 109.84(16) . . ?
C1 P1 C5 101.9(2) . . ?
C1 P1 C6 104.7(3) . . ?
C5 P1 W1 111.69(17) . . ?
C6 P1 W1 122.03(17) . . ?
C6 P1 C5 104.7(2) . . ?
O7 C14 W1 177.8(4) . . ?
O4 C11 W1 177.7(4) . . ?
O5 C12 W1 176.6(4) . . ?
O3 C10 W1 177.3(4) . . ?
O6 C13 W1 175.2(4) . . ?
O1 C1 P1 118.6(4) . . ?
O1 C1 C2 123.1(5) . . ?
C2 C1 P1 118.1(4) . . ?
O2 C5 P1 120.3(4) . . ?
O2 C5 C4 123.9(5) . . ?
C4 C5 P1 115.8(4) . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C6 C9 H9A 109.5 . . ?
C6 C9 H9B 109.5 . . ?
C6 C9 H9C 109.5 . . ?
C5 C4 H4A 109.2 . . ?
C5 C4 H4B 109.2 . . ?
C5 C4 C3 112.0(4) . . ?
H4A C4 H4B 107.9 . . ?
C3 C4 H4A 109.2 . . ?
C3 C4 H4B 109.2 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C6 C8 H8A 109.5 . . ?
C6 C8 H8B 109.5 . . ?
C6 C8 H8C 109.5 . . ?
C9 C6 P1 109.5(3) . . ?
C9 C6 C8 109.3(5) . . ?
C7 C6 P1 110.3(4) . . ?
C7 C6 C9 109.4(4) . . ?
C7 C6 C8 110.4(4) . . ?
C8 C6 P1 107.9(3) . . ?
C4 C3 H3A 109.0 . . ?
C4 C3 H3B 109.0 . . ?
H3A C3 H3B 107.8 . . ?
C2 C3 C4 112.9(5) . . ?
C2 C3 H3A 109.0 . . ?
C2 C3 H3B 109.0 . . ?
C1 C2 C3 113.1(4) . . ?
C1 C2 H2A 109.0 . . ?
C1 C2 H2B 109.0 . . ?
C3 C2 H2A 109.0 . . ?
C3 C2 H2B 109.0 . . ?
H2A C2 H2B 107.8 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
W1 P1 C1 O1 88.8(5) . . . . ?
W1 P1 C1 C2 -87.8(4) . . . . ?
W1 P1 C5 O2 -94.8(5) . . . . ?
W1 P1 C5 C4 83.1(4) . . . . ?
W1 P1 C6 C9 -56.6(4) . . . . ?
W1 P1 C6 C7 -177.1(3) . . . . ?
W1 P1 C6 C8 62.2(4) . . . . ?
P1 C1 C2 C3 -47.0(7) . . . . ?
P1 C5 C4 C3 54.5(6) . . . . ?
O2 C5 C4 C3 -127.8(6) . . . . ?
O1 C1 C2 C3 136.5(6) . . . . ?
C1 P1 C5 O2 148.0(5) . . . . ?
C1 P1 C5 C4 -34.1(5) . . . . ?
C1 P1 C6 C9 68.7(4) . . . . ?
C1 P1 C6 C7 -51.8(4) . . . . ?
C1 P1 C6 C8 -172.5(4) . . . . ?
C5 P1 C1 O1 -152.6(5) . . . . ?
C5 P1 C1 C2 30.7(5) . . . . ?
C5 P1 C6 C9 175.5(4) . . . . ?
C5 P1 C6 C7 55.0(4) . . . . ?
C5 P1 C6 C8 -65.7(4) . . . . ?
C5 C4 C3 C2 -69.4(6) . . . . ?
C4 C3 C2 C1 64.8(7) . . . . ?
C6 P1 C1 O1 -43.8(5) . . . . ?
C6 P1 C1 C2 139.5(4) . . . . ?
C6 P1 C5 O2 39.2(5) . . . . ?
C6 P1 C5 C4 -143.0(4) . . . . ?

_olex2_date_sample_data_collection 2019-02-18
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.737
_oxdiff_exptl_absorpt_empirical_full_min 0.733
_chemical_properties_physical    Moisture-sensitive
####################################################################### 
# 
# 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_MesP(SiMe3)2
_database_code_depnum_ccdc_archive 'CCDC 1988266'
loop_
_audit_author_name
_audit_author_address
'Kyle G. Pearce'
;University of Sussex
United Kingdom
;
_audit_update_record             
;
2020-03-04 deposited with the CCDC.	2020-03-31 downloaded from the CCDC.
;
_audit_creation_date             2020-01-09
_audit_creation_method           
;
Olex2 1.3
(compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C15 H29 P Si2)'
_chemical_formula_sum            'C30 H58 P2 Si4'
_chemical_formula_weight         593.06
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C15 H29 P1 Si2'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 '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                   12.2774(2)
_cell_length_b                   24.2123(3)
_cell_length_c                   13.4741(2)
_cell_angle_alpha                90
_cell_angle_beta                 113.140(2)
_cell_angle_gamma                90
_cell_volume                     3683.12(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    8781
_cell_measurement_temperature    100
_cell_measurement_theta_max      71.6330
_cell_measurement_theta_min      3.9950
_shelx_estimated_absorpt_T_max   0.529
_shelx_estimated_absorpt_T_min   0.376
_exptl_absorpt_coefficient_mu    2.430
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72754
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.070
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1296
_exptl_crystal_preparation       ?
_exptl_crystal_recrystallization_method ?
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0212
_diffrn_reflns_av_unetI/netI     0.0238
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            16420
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.627
_diffrn_reflns_theta_min         3.651
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1033
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     31.00 104.00   1.00    1.41    --   37.66  57.00-120.00   73
  2  ω     72.00 108.00   1.00    1.41    --   37.66 178.00-180.00   36
  3  ω     80.00 107.00   1.00    1.41    --   37.66  38.00 150.00   27
  4  ω     19.00  46.00   1.00    1.41    --   37.66  38.00 150.00   27
  5  ω    -25.00  73.00   1.00    1.41    --   37.66 -99.00-180.00   98
  6  ω    -30.00  10.00   1.00    1.41    --   37.66 -77.00 120.00   40
  7  ω     86.00 161.00   1.00    5.62    --  107.00  30.00  30.00   75
  8  ω     44.00 118.00   1.00    5.62    --  107.00 -45.00 -30.00   74
  9  ω     43.00  93.00   1.00    5.62    --  107.00 -91.00   1.56   50
 10  ω     93.00 166.00   1.00    5.62    --  107.00  61.00-120.00   73
 11  ω     45.00 115.00   1.00    5.62    --  107.00 -61.00-120.00   70
 12  ω     58.00 114.00   1.00    5.62    --  107.00 -91.00  73.67   56
 13  ω     40.00 128.00   1.00    5.62    --  107.00 -30.00-150.00   88
 14  ω     86.00 142.00   1.00    5.62    --  107.00 -91.00 125.41   56
 15  ω     56.00  83.00   1.00    5.62    --  107.00 -95.00-180.00   27
 16  ω     54.00  81.00   1.00    5.62    --  107.00 -91.00 125.41   27
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0470171000
_diffrn_orient_matrix_UB_12      -0.0595575000
_diffrn_orient_matrix_UB_13      0.0086957000
_diffrn_orient_matrix_UB_21      0.1278353000
_diffrn_orient_matrix_UB_22      0.0215281000
_diffrn_orient_matrix_UB_23      0.0561615000
_diffrn_orient_matrix_UB_31      -0.0082456000
_diffrn_orient_matrix_UB_32      -0.0062427000
_diffrn_orient_matrix_UB_33      0.1106037000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6594
_reflns_number_total             7100
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.95
_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 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT n/a (Sheldrick, 2015)'
_refine_diff_density_max         0.289
_refine_diff_density_min         -0.398
_refine_diff_density_rms         0.077
_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     343
_refine_ls_number_reflns         7100
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0356
_refine_ls_R_factor_gt           0.0331
_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)+(0.0516P)²+1.1425P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0873
_refine_ls_wR_factor_ref         0.0895
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C24(H24), C11(H11), C26(H26)
2.b Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C17(H17A,H17B,H17C), C13(H13A,H13B,H13C), C5(H5A,H5B,
 H5C), C15(H15A,H15B,H15C), C28(H28A,H28B,H28C), C4(H4A,H4B,H4C), C16(H16A,H16B,
 H16C), C19(H19A,H19B,H19C), C18(H18A,H18B,H18C), C6(H6A,H6B,H6C), C2(H2A,H2B,
 H2C), C20(H20A,H20B,H20C), C3(H3A,H3B,H3C), C21(H21A,H21B,H21C), C1(H1A,H1B,
 H1C), C14(H14A,H14B,H14C), C29(H29A,H29B,H29C)
;
_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
P2 P 1.02525(3) 0.67679(2) 0.73287(2) 0.01366(9) Uani 1 1 d . . . . .
P1 P 0.47268(3) 0.42426(2) 0.25997(2) 0.01332(9) Uani 1 1 d . . . . .
Si3 Si 0.90444(3) 0.62717(2) 0.59104(3) 0.01418(9) Uani 1 1 d . . . . .
Si2 Si 0.59876(3) 0.38532(2) 0.41421(3) 0.01484(9) Uani 1 1 d . . . . .
Si4 Si 0.99707(3) 0.65496(2) 0.88320(3) 0.01741(10) Uani 1 1 d . . . . .
Si1 Si 0.50844(3) 0.39451(2) 0.11772(3) 0.01736(9) Uani 1 1 d . . . . .
C8 C 0.37878(12) 0.52977(6) 0.20803(10) 0.0167(3) Uani 1 1 d . . . . .
C23 C 0.88592(12) 0.77797(6) 0.68356(10) 0.0171(3) Uani 1 1 d . . . . .
C22 C 0.99774(12) 0.75220(5) 0.72177(10) 0.0148(2) Uani 1 1 d . . . . .
C12 C 0.59371(12) 0.52999(6) 0.28714(10) 0.0166(3) Uani 1 1 d . . . . .
C7 C 0.48659(11) 0.50015(5) 0.25359(10) 0.0139(2) Uani 1 1 d . . . . .
C9 C 0.38049(13) 0.58682(6) 0.19518(11) 0.0202(3) Uani 1 1 d . . . . .
H9 H 0.307525 0.606084 0.163127 0.024 Uiso 1 1 calc R U . . .
C27 C 1.10010(12) 0.78602(6) 0.75869(10) 0.0187(3) Uani 1 1 d . . . . .
C24 C 0.87813(13) 0.83533(6) 0.68419(11) 0.0219(3) Uani 1 1 d . . . . .
H24 H 0.802067 0.852084 0.658430 0.026 Uiso 1 1 calc R U . . .
C11 C 0.59092(13) 0.58706(6) 0.27424(11) 0.0206(3) Uani 1 1 d . . . . .
H11 H 0.663679 0.606727 0.298053 0.025 Uiso 1 1 calc R U . . .
C10 C 0.48566(14) 0.61630(6) 0.22785(11) 0.0224(3) Uani 1 1 d . . . . .
C30 C 0.77154(12) 0.74606(6) 0.63924(12) 0.0238(3) Uani 1 1 d . . . . .
H30A H 0.751603 0.737557 0.562983 0.036 Uiso 1 1 calc R U . . .
H30B H 0.708079 0.768246 0.646067 0.036 Uiso 1 1 calc R U . . .
H30C H 0.780473 0.711588 0.679828 0.036 Uiso 1 1 calc R U . . .
C17 C 0.74923(12) 0.60971(6) 0.57367(12) 0.0229(3) Uani 1 1 d . . . . .
H17A H 0.746928 0.602916 0.644525 0.034 Uiso 1 1 calc R U . . .
H17B H 0.723056 0.576510 0.528948 0.034 Uiso 1 1 calc R U . . .
H17C H 0.696569 0.640574 0.538476 0.034 Uiso 1 1 calc R U . . .
C13 C 0.71299(12) 0.50239(6) 0.33780(12) 0.0223(3) Uani 1 1 d . . . . .
H13A H 0.732121 0.496197 0.414718 0.033 Uiso 1 1 calc R U . . .
H13B H 0.773488 0.526141 0.329480 0.033 Uiso 1 1 calc R U . . .
H13C H 0.710914 0.466897 0.302155 0.033 Uiso 1 1 calc R U . . .
C25 C 0.97775(15) 0.86877(6) 0.72118(12) 0.0264(3) Uani 1 1 d . . . . .
C5 C 0.75586(12) 0.36930(6) 0.43589(12) 0.0243(3) Uani 1 1 d . . . . .
H5A H 0.758955 0.356958 0.367780 0.036 Uiso 1 1 calc R U . . .
H5B H 0.786271 0.340019 0.490061 0.036 Uiso 1 1 calc R U . . .
H5C H 0.804496 0.402534 0.461180 0.036 Uiso 1 1 calc R U . . .
C15 C 0.25933(12) 0.50204(6) 0.17387(12) 0.0241(3) Uani 1 1 d . . . . .
H15A H 0.249309 0.475801 0.115543 0.036 Uiso 1 1 calc R U . . .
H15B H 0.196717 0.530019 0.148409 0.036 Uiso 1 1 calc R U . . .
H15C H 0.254499 0.482305 0.235517 0.036 Uiso 1 1 calc R U . . .
C28 C 1.22383(12) 0.76243(7) 0.79687(12) 0.0264(3) Uani 1 1 d . . . . .
H28A H 1.238698 0.739012 0.860193 0.040 Uiso 1 1 calc R U . . .
H28B H 1.281544 0.792651 0.816145 0.040 Uiso 1 1 calc R U . . .
H28C H 1.231480 0.740323 0.739014 0.040 Uiso 1 1 calc R U . . .
C26 C 1.08769(14) 0.84324(6) 0.75768(12) 0.0245(3) Uani 1 1 d . . . . .
H26 H 1.156916 0.865543 0.782866 0.029 Uiso 1 1 calc R U . . .
C4 C 0.52718(14) 0.31683(6) 0.41258(13) 0.0266(3) Uani 1 1 d . . . . .
H4A H 0.443907 0.322460 0.400636 0.040 Uiso 1 1 calc R U . . .
H4B H 0.568252 0.298190 0.481903 0.040 Uiso 1 1 calc R U . . .
H4C H 0.531922 0.294014 0.354336 0.040 Uiso 1 1 calc R U . . .
C16 C 0.90383(13) 0.66253(7) 0.46772(11) 0.0252(3) Uani 1 1 d . . . . .
H16A H 0.856506 0.696382 0.455054 0.038 Uiso 1 1 calc R U . . .
H16B H 0.869430 0.637903 0.405396 0.038 Uiso 1 1 calc R U . . .
H16C H 0.985217 0.671878 0.477960 0.038 Uiso 1 1 calc R U . . .
C19 C 1.02571(14) 0.57921(6) 0.90739(13) 0.0275(3) Uani 1 1 d . . . . .
H19A H 0.964510 0.558391 0.849977 0.041 Uiso 1 1 calc R U . . .
H19B H 1.023981 0.569320 0.977281 0.041 Uiso 1 1 calc R U . . .
H19C H 1.103644 0.570271 0.907580 0.041 Uiso 1 1 calc R U . . .
C18 C 0.98502(14) 0.55966(6) 0.61162(13) 0.0261(3) Uani 1 1 d . . . . .
H18A H 1.068355 0.566432 0.625155 0.039 Uiso 1 1 calc R U . . .
H18B H 0.948963 0.536802 0.546841 0.039 Uiso 1 1 calc R U . . .
H18C H 0.979867 0.540433 0.673637 0.039 Uiso 1 1 calc R U . . .
C6 C 0.59559(14) 0.42904(6) 0.52693(11) 0.0253(3) Uani 1 1 d . . . . .
H6A H 0.630563 0.465179 0.524779 0.038 Uiso 1 1 calc R U . . .
H6B H 0.641110 0.410985 0.595972 0.038 Uiso 1 1 calc R U . . .
H6C H 0.513439 0.433954 0.519277 0.038 Uiso 1 1 calc R U . . .
C2 C 0.65679(13) 0.40885(7) 0.11461(12) 0.0271(3) Uani 1 1 d . . . . .
H2A H 0.673400 0.448531 0.124153 0.041 Uiso 1 1 calc R U . . .
H2B H 0.656799 0.397043 0.045045 0.041 Uiso 1 1 calc R U . . .
H2C H 0.717876 0.388506 0.172992 0.041 Uiso 1 1 calc R U . . .
C20 C 0.84904(14) 0.67110(7) 0.88556(12) 0.0279(3) Uani 1 1 d . . . . .
H20A H 0.829992 0.710054 0.867148 0.042 Uiso 1 1 calc R U . . .
H20B H 0.851154 0.663896 0.957867 0.042 Uiso 1 1 calc R U . . .
H20C H 0.788459 0.647785 0.832904 0.042 Uiso 1 1 calc R U . . .
C3 C 0.39366(15) 0.42987(7) -0.00071(11) 0.0295(3) Uani 1 1 d . . . . .
H3A H 0.314652 0.417997 -0.007720 0.044 Uiso 1 1 calc R U . . .
H3B H 0.405306 0.420189 -0.066482 0.044 Uiso 1 1 calc R U . . .
H3C H 0.400875 0.469948 0.010021 0.044 Uiso 1 1 calc R U . . .
C21 C 1.11284(15) 0.69507(7) 0.99299(11) 0.0294(3) Uani 1 1 d . . . . .
H21A H 1.191572 0.683577 0.998572 0.044 Uiso 1 1 calc R U . . .
H21B H 1.105417 0.688053 1.061694 0.044 Uiso 1 1 calc R U . . .
H21C H 1.102166 0.734585 0.976224 0.044 Uiso 1 1 calc R U . . .
C1 C 0.48371(15) 0.31802(6) 0.10989(13) 0.0291(3) Uani 1 1 d . . . . .
H1A H 0.545161 0.300219 0.172096 0.044 Uiso 1 1 calc R U . . .
H1B H 0.487364 0.303834 0.043145 0.044 Uiso 1 1 calc R U . . .
H1C H 0.405672 0.309974 0.110328 0.044 Uiso 1 1 calc R U . . .
C14 C 0.48580(17) 0.67795(6) 0.21263(16) 0.0362(4) Uani 1 1 d . . . . .
H14A H 0.511877 0.686363 0.154261 0.054 Uiso 1 1 calc R U . . .
H14B H 0.539999 0.695194 0.279655 0.054 Uiso 1 1 calc R U . . .
H14C H 0.405617 0.692387 0.194074 0.054 Uiso 1 1 calc R U . . .
C29 C 0.9666(2) 0.93067(7) 0.72227(19) 0.0463(5) Uani 1 1 d . . . . .
H29A H 0.980009 0.946437 0.661043 0.069 Uiso 1 1 calc R U . . .
H29B H 1.025506 0.945355 0.789804 0.069 Uiso 1 1 calc R U . . .
H29C H 0.886947 0.940517 0.716676 0.069 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P2 Si3 2.2511(5) . ?
P2 Si4 2.2477(5) . ?
P2 C22 1.8522(13) . ?
P1 Si2 2.2529(4) . ?
P1 Si1 2.2465(5) . ?
P1 C7 1.8505(13) . ?
Si3 C17 1.8747(14) . ?
Si3 C16 1.8665(14) . ?
Si3 C18 1.8741(15) . ?
Si2 C5 1.8743(14) . ?
Si2 C4 1.8727(15) . ?
Si2 C6 1.8642(14) . ?
Si4 C19 1.8718(15) . ?
Si4 C20 1.8714(15) . ?
Si4 C21 1.8705(15) . ?
Si1 C2 1.8708(15) . ?
Si1 C3 1.8703(15) . ?
Si1 C1 1.8729(16) . ?
C8 C7 1.4158(18) . ?
C8 C9 1.3933(19) . ?
C8 C15 1.5109(19) . ?
C23 C22 1.4084(19) . ?
C23 C24 1.392(2) . ?
C23 C30 1.5056(19) . ?
C22 C27 1.4163(19) . ?
C12 C7 1.4102(18) . ?
C12 C11 1.3915(19) . ?
C12 C13 1.5071(18) . ?
C9 H9 0.9500 . ?
C9 C10 1.387(2) . ?
C27 C28 1.511(2) . ?
C27 C26 1.393(2) . ?
C24 H24 0.9500 . ?
C24 C25 1.386(2) . ?
C11 H11 0.9500 . ?
C11 C10 1.388(2) . ?
C10 C14 1.507(2) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C25 C26 1.387(2) . ?
C25 C29 1.506(2) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C26 H26 0.9500 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 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
Si4 P2 Si3 110.865(18) . . ?
C22 P2 Si3 114.78(4) . . ?
C22 P2 Si4 102.52(4) . . ?
Si1 P1 Si2 111.039(18) . . ?
C7 P1 Si2 114.58(4) . . ?
C7 P1 Si1 103.08(4) . . ?
C17 Si3 P2 121.64(5) . . ?
C16 Si3 P2 106.37(5) . . ?
C16 Si3 C17 110.12(7) . . ?
C16 Si3 C18 110.43(7) . . ?
C18 Si3 P2 101.92(5) . . ?
C18 Si3 C17 105.86(7) . . ?
C5 Si2 P1 121.49(5) . . ?
C4 Si2 P1 102.16(5) . . ?
C4 Si2 C5 105.55(7) . . ?
C6 Si2 P1 106.68(5) . . ?
C6 Si2 C5 109.89(7) . . ?
C6 Si2 C4 110.64(7) . . ?
C19 Si4 P2 107.60(5) . . ?
C20 Si4 P2 117.43(5) . . ?
C20 Si4 C19 108.59(7) . . ?
C21 Si4 P2 104.62(5) . . ?
C21 Si4 C19 109.79(7) . . ?
C21 Si4 C20 108.62(7) . . ?
C2 Si1 P1 118.55(5) . . ?
C2 Si1 C1 108.66(7) . . ?
C3 Si1 P1 104.29(5) . . ?
C3 Si1 C2 108.03(7) . . ?
C3 Si1 C1 110.70(8) . . ?
C1 Si1 P1 106.47(5) . . ?
C7 C8 C15 122.48(12) . . ?
C9 C8 C7 119.92(12) . . ?
C9 C8 C15 117.58(12) . . ?
C22 C23 C30 122.74(12) . . ?
C24 C23 C22 119.94(13) . . ?
C24 C23 C30 117.31(13) . . ?
C23 C22 P2 125.93(10) . . ?
C23 C22 C27 118.38(12) . . ?
C27 C22 P2 115.66(10) . . ?
C7 C12 C13 122.41(12) . . ?
C11 C12 C7 119.64(12) . . ?
C11 C12 C13 117.95(12) . . ?
C8 C7 P1 115.82(10) . . ?
C12 C7 P1 125.82(10) . . ?
C12 C7 C8 118.34(12) . . ?
C8 C9 H9 119.1 . . ?
C10 C9 C8 121.90(13) . . ?
C10 C9 H9 119.1 . . ?
C22 C27 C28 122.38(13) . . ?
C26 C27 C22 119.52(13) . . ?
C26 C27 C28 118.07(13) . . ?
C23 C24 H24 118.9 . . ?
C25 C24 C23 122.14(14) . . ?
C25 C24 H24 118.9 . . ?
C12 C11 H11 118.8 . . ?
C10 C11 C12 122.38(13) . . ?
C10 C11 H11 118.8 . . ?
C9 C10 C11 117.79(13) . . ?
C9 C10 C14 121.15(14) . . ?
C11 C10 C14 121.06(14) . . ?
C23 C30 H30A 109.5 . . ?
C23 C30 H30B 109.5 . . ?
C23 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
Si3 C17 H17A 109.5 . . ?
Si3 C17 H17B 109.5 . . ?
Si3 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
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 . . ?
C24 C25 C26 117.73(13) . . ?
C24 C25 C29 120.94(16) . . ?
C26 C25 C29 121.32(16) . . ?
Si2 C5 H5A 109.5 . . ?
Si2 C5 H5B 109.5 . . ?
Si2 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C8 C15 H15A 109.5 . . ?
C8 C15 H15B 109.5 . . ?
C8 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C26 H26 118.9 . . ?
C25 C26 C27 122.28(14) . . ?
C25 C26 H26 118.9 . . ?
Si2 C4 H4A 109.5 . . ?
Si2 C4 H4B 109.5 . . ?
Si2 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
Si3 C16 H16A 109.5 . . ?
Si3 C16 H16B 109.5 . . ?
Si3 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
Si4 C19 H19A 109.5 . . ?
Si4 C19 H19B 109.5 . . ?
Si4 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
Si3 C18 H18A 109.5 . . ?
Si3 C18 H18B 109.5 . . ?
Si3 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
Si2 C6 H6A 109.5 . . ?
Si2 C6 H6B 109.5 . . ?
Si2 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
Si1 C2 H2A 109.5 . . ?
Si1 C2 H2B 109.5 . . ?
Si1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
Si4 C20 H20A 109.5 . . ?
Si4 C20 H20B 109.5 . . ?
Si4 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
Si1 C3 H3A 109.5 . . ?
Si1 C3 H3B 109.5 . . ?
Si1 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
Si4 C21 H21A 109.5 . . ?
Si4 C21 H21B 109.5 . . ?
Si4 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
Si1 C1 H1A 109.5 . . ?
Si1 C1 H1B 109.5 . . ?
Si1 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 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 . . ?
C25 C29 H29A 109.5 . . ?
C25 C29 H29B 109.5 . . ?
C25 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
P2 C22 C27 C28 4.45(17) . . . . ?
P2 C22 C27 C26 -177.25(10) . . . . ?
Si3 P2 C22 C23 42.47(12) . . . . ?
Si3 P2 C22 C27 -139.56(8) . . . . ?
Si2 P1 C7 C8 -138.93(8) . . . . ?
Si2 P1 C7 C12 42.82(12) . . . . ?
Si4 P2 C22 C23 -77.82(11) . . . . ?
Si4 P2 C22 C27 100.15(9) . . . . ?
Si1 P1 C7 C8 100.31(9) . . . . ?
Si1 P1 C7 C12 -77.95(11) . . . . ?
C8 C9 C10 C11 0.1(2) . . . . ?
C8 C9 C10 C14 179.59(14) . . . . ?
C23 C22 C27 C28 -177.42(12) . . . . ?
C23 C22 C27 C26 0.88(18) . . . . ?
C23 C24 C25 C26 0.4(2) . . . . ?
C23 C24 C25 C29 -179.17(15) . . . . ?
C22 C23 C24 C25 0.3(2) . . . . ?
C22 C27 C26 C25 -0.2(2) . . . . ?
C12 C11 C10 C9 1.0(2) . . . . ?
C12 C11 C10 C14 -178.52(14) . . . . ?
C7 C8 C9 C10 -1.30(19) . . . . ?
C7 C12 C11 C10 -0.8(2) . . . . ?
C9 C8 C7 P1 -176.99(10) . . . . ?
C9 C8 C7 C12 1.40(18) . . . . ?
C24 C23 C22 P2 177.02(10) . . . . ?
C24 C23 C22 C27 -0.90(18) . . . . ?
C24 C25 C26 C27 -0.4(2) . . . . ?
C11 C12 C7 P1 177.84(10) . . . . ?
C11 C12 C7 C8 -0.37(18) . . . . ?
C30 C23 C22 P2 -4.07(18) . . . . ?
C30 C23 C22 C27 178.01(12) . . . . ?
C30 C23 C24 C25 -178.71(13) . . . . ?
C13 C12 C7 P1 -2.56(18) . . . . ?
C13 C12 C7 C8 179.22(11) . . . . ?
C13 C12 C11 C10 179.56(12) . . . . ?
C15 C8 C7 P1 4.23(16) . . . . ?
C15 C8 C7 C12 -177.38(12) . . . . ?
C15 C8 C9 C10 177.54(12) . . . . ?
C28 C27 C26 C25 178.15(13) . . . . ?
C29 C25 C26 C27 179.16(15) . . . . ?

_olex2_submission_original_sample_id VS004
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.288
_oxdiff_exptl_absorpt_empirical_full_min 0.656

# start Validation Reply Form
_vrf_PLAT973_compound-4          
;
PROBLEM: Check Calcd Positive Resid. Density on Pt1 2.86 eA-3
RESPONSE: weakly diffracting crystal used for connectivity only
;
_vrf_PLAT342_compound-4          
;
PROBLEM: Low Bond Precision on C-C Bonds ............... 0.05308 Ang.
RESPONSE: weakly diffracting crystal used for connectivity only
;
_vrf_PLAT972_compound-4          
;
PROBLEM: Check Calcd Resid. Dens. 0.87A From Pt1 -2.72 eA-3
RESPONSE: weakly diffracting crystal used for connectivity only
;
_vrf_PLAT430_compound-5d         
;
PROBLEM: Short Inter D...A Contact O3 ..O1AA . 2.71 Ang.
RESPONSE: result of disorder in the second molecule of asymm unit
;
# end Validation Reply Form
_chemical_properties_physical    Air-sensitive,Moisture-sensitive,Pyrophoric
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_compound-5d
_database_code_depnum_ccdc_archive 'CCDC 1988265'
loop_
_audit_author_name
_audit_author_address
'Kyle G. Pearce'
;University of Sussex
United Kingdom
;
_audit_update_record             
;
2020-03-04 deposited with the CCDC.	2020-03-31 downloaded from the CCDC.
;
_audit_creation_date             2020-01-09
_audit_creation_method           
;
Olex2 1.3
(compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C16 H11 O7 P W)'
_chemical_formula_sum            'C32 H22 O14 P2 W2'
_chemical_formula_weight         1060.13
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C32 H24 O14 P2 W2'
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'
W W -5.4734 5.5774 '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                   11.0044(3)
_cell_length_b                   9.7434(3)
_cell_length_c                   32.7494(10)
_cell_angle_alpha                90
_cell_angle_beta                 91.882(3)
_cell_angle_gamma                90
_cell_volume                     3509.51(18)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4509
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      71.2370
_cell_measurement_theta_min      5.6150
_shelx_estimated_absorpt_T_max   0.348
_shelx_estimated_absorpt_T_min   0.175
_exptl_absorpt_coefficient_mu    13.393
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.46354
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear pale yellow'
_exptl_crystal_density_diffrn    2.006
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2016
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0440
_diffrn_reflns_av_unetI/netI     0.0577
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            11703
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.754
_diffrn_reflns_theta_min         5.283
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      '100 (10)'
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1033
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -24.00  42.00   1.00    5.00    --    0.00 -99.00-180.00   66
  2  ω   -112.00 -18.00   1.00   30.00    --  -54.75 125.00 120.00   94
  3  ω     87.00 114.00   1.00   30.00    --   54.75 104.00 -16.00   27
  4  ω     73.00 126.00   1.00   30.00    --   54.75 125.00-120.00   53
  5  ω     35.00 110.00   1.00   30.00    --   54.75  57.00  60.00   75
  6  ω     52.00 131.00   1.00   60.00    --  109.50 -50.00  90.00   79
  7  ω     46.00 132.00   1.00   60.00    --  109.50 -64.00 -90.00   86
  8  ω     40.00  93.00   1.00   60.00    --  109.50 -50.00-150.00   53
  9  ω     95.00 172.00   1.00   60.00    --  109.50  50.00 -90.00   77
 10  ω    106.00 131.00   1.00   60.00    --  109.50 -50.00-150.00   25
 11  ω     90.00 131.00   1.00   60.00    --  109.50 -77.00   0.00   41
 12  ω     75.00 175.00   1.00   60.00    --  109.50  25.00  30.00  100
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1130521000
_diffrn_orient_matrix_UB_12      -0.0677978000
_diffrn_orient_matrix_UB_13      -0.0178676000
_diffrn_orient_matrix_UB_21      0.0681192000
_diffrn_orient_matrix_UB_22      0.0147360000
_diffrn_orient_matrix_UB_23      0.0415902000
_diffrn_orient_matrix_UB_31      -0.0469225000
_diffrn_orient_matrix_UB_32      -0.1420937000
_diffrn_orient_matrix_UB_33      0.0128603000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5673
_reflns_number_total             6635
_reflns_odcompleteness_completeness 98.94
_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 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT n/a (Sheldrick, 2015)'
_refine_diff_density_max         2.094
_refine_diff_density_min         -1.812
_refine_diff_density_rms         0.186
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.150
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     463
_refine_ls_number_reflns         6635
_refine_ls_number_restraints     78
_refine_ls_R_factor_all          0.0798
_refine_ls_R_factor_gt           0.0672
_refine_ls_restrained_S_all      1.144
_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)+(0.0461P)²+46.8306P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1603
_refine_ls_wR_factor_ref         0.1672
_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
 W2-C2AA \\sim W2-C2AB
 with sigma of 0.02
 C2AA-O5AA \\sim C2AB-O4A
 with sigma of 0.02
 W2-O5AA \\sim W2-O4A
 with sigma of 0.04
 W2-C2AA \\sim W2-C1AA
 with sigma of 0.02
 C2AA-O5AA \\sim C1AA-O0AA
 with sigma of 0.02
 W2-O5AA \\sim W2-O0AA
 with sigma of 0.04
 W2-O0AA \\sim W2-O0AB
 with sigma of 0.04
 W2-C1AA \\sim W2-C1AB
 with sigma of 0.02
 C1AA-O0AA \\sim C1AB-O0AB
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O5AA \\sim O2AA \\sim O4A \\sim O4B \\sim O0AB \\sim O0AC \\sim O0AA: within 2A
with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
O0AC \\sim O0AB \\sim O4B \\sim O4A \\sim O2AA \\sim O5AA \\sim O0AA: within 2A
with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
O2AA \\sim O4A \\sim O4B \\sim O0AB \\sim O0AC \\sim O0AA \\sim O1AA \\sim
O5AA: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within
2A
O4B \\sim O4A \\sim O2AA \\sim O1AA \\sim O5AA \\sim O0AA \\sim O0AC \\sim
O0AB: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within
2A
C0 \\sim C0AA: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
O1B \\sim O1A: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
C0AA \\sim C0: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
O1A \\sim O1B: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
Uanis(C0) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C1A) = Uanis(O1AA) = Uanis(C1AA) = Uanis(C1AC) = Uanis(O0AC) =
Uanis(O0AA) = Uanis(C1AB) = Uanis(O0AB) = Uanis(C2AC) = Uanis(O4B) = Uanis(O4A)
= Uanis(C2AB) = Uanis(C2AA) = Uanis(O5AA) = Uanis(C4AA) = Uanis(O2AA)
Uanis(O1A) = Uanis(C0) = Uanis(C0AA) = Uanis(O1B)
4. Rigid body (RIGU) restrains
 C0AA, C0, C4AA, C2AB, O4A, O2AA, C2AA, O1AA, O5AA, C1A, C1AB, C2AC, O4B, O0AB,
  C1AC, O0AC, C1AA, O0AA, O1B, O1A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(W2)=Sof(C2AA)=Sof(O5AA)=Sof(W2A)=Sof(O2AA)=Sof(C4AA)=1-FVAR(1)
 Sof(C2AB)=Sof(O4A)=Sof(C1AB)=Sof(O0AB)=Sof(C2AC)=Sof(O4B)=Sof(C1AC)=Sof(O0AC)=
 FVAR(1)
 Sof(O4AA)=1-FVAR(2)
 Sof(O3AA)=FVAR(2)
 Sof(C1A)=Sof(O1AA)=1-FVAR(3)
 Sof(C1AA)=Sof(O0AA)=FVAR(3)
 Fixed Sof: O1B(0.55) C0(0.45) C6AA(0.5) H6AA(0.5) H6AB(0.5) C5AA(0.5)
 H5AA(0.5) H5AB(0.5) C0AA(0.55) O1A(0.45)
6.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C25(H25A,H25B), C4(H4A,H4B), C3(H3A,H3B), C7AA(H7AA,H7AB),
 C6AA(H6AA,H6AB), C5AA(H5AA,H5AB)
6.b Aromatic/amide H refined with riding coordinates:
 C18(H18), C8(H8), C7(H7), C9(H9), C11(H11), C19(H19), C20(H20), C10(H10),
 C22(H22), C21(H21)
;
_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
W1 W 0.51792(4) 0.20873(5) 0.43926(2) 0.03323(17) Uani 1 1 d . . . . .
W2 W 0.17619(13) 0.70076(16) 0.33196(4) 0.0288(3) Uani 0.4994(16) 1 d D . P A 1
P1 P 0.7036(2) 0.3459(3) 0.42624(8) 0.0307(5) Uani 1 1 d . . . . .
P23 P 0.0213(3) 0.8831(3) 0.32468(11) 0.0460(7) Uani 1 1 d . . . . .
O7 O 0.2897(8) 0.0348(9) 0.4634(3) 0.054(2) Uani 1 1 d . . . . .
O2 O 0.8082(7) 0.2422(8) 0.3604(2) 0.0396(17) Uani 1 1 d . . . . .
O1 O 0.6897(7) 0.5797(9) 0.4683(3) 0.048(2) Uani 1 1 d . . . . .
O5 O 0.4708(9) 0.1598(12) 0.3442(3) 0.067(3) Uani 1 1 d . . . . .
O6 O 0.6735(8) -0.0675(8) 0.4399(3) 0.064(3) Uani 1 1 d . . . . .
C15 C 0.6195(10) 0.0361(13) 0.4412(4) 0.046(3) Uani 1 1 d . . . . .
C5 C 0.7462(9) 0.3378(11) 0.3711(3) 0.036(2) Uani 1 1 d . . . . .
O3 O 0.5638(9) 0.2624(11) 0.5342(3) 0.062(3) Uani 1 1 d . . . . .
O4 O 0.3418(8) 0.4668(9) 0.4299(4) 0.067(3) Uani 1 1 d . . . . .
C16 C 0.3733(10) 0.0952(12) 0.4540(4) 0.041(2) Uani 1 1 d . . . . .
O29 O 0.0518(9) 1.0663(10) 0.2654(4) 0.069(3) Uani 1 1 d . . . . .
C6 C 0.8466(9) 0.3159(10) 0.4542(3) 0.031(2) Uani 1 1 d . . . . .
C18 C -0.2289(10) 0.9312(11) 0.3148(4) 0.044(3) Uani 1 1 d . . . . .
H18 H -0.217432 0.996588 0.336125 0.053 Uiso 1 1 calc R U . . .
C17 C -0.1300(9) 0.8539(12) 0.3018(3) 0.038(2) Uani 1 1 d . . . . .
C14 C 0.4884(11) 0.1771(14) 0.3783(4) 0.048(3) Uani 1 1 d . . . . .
C28 C 0.0636(11) 1.0526(13) 0.3017(5) 0.054(3) Uani 1 1 d . . . . .
C8 C 1.0561(9) 0.3711(14) 0.4681(4) 0.048(3) Uani 1 1 d . . . . .
H8 H 1.124669 0.427231 0.463208 0.058 Uiso 1 1 calc R U . . .
C7 C 0.9470(10) 0.3955(14) 0.4470(4) 0.046(3) Uani 1 1 d . . . . .
H7 H 0.941448 0.467501 0.427459 0.056 Uiso 1 1 calc R U . . .
C9 C 1.0656(12) 0.2668(13) 0.4960(4) 0.053(3) Uani 1 1 d . . . . .
H9 H 1.140579 0.249778 0.510302 0.064 Uiso 1 1 calc R U . . .
C1 C 0.6764(9) 0.5354(12) 0.4341(4) 0.039(2) Uani 1 1 d . . . . .
C12 C 0.5480(10) 0.2450(13) 0.5005(3) 0.043(3) Uani 1 1 d . . . . .
C2 C 0.6289(12) 0.6134(13) 0.3977(4) 0.052(3) Uani 1 1 d . . . . .
H2A H 0.630537 0.712741 0.404039 0.062 Uiso 1 1 calc R U . . .
H2B H 0.543229 0.586899 0.391923 0.062 Uiso 1 1 calc R U . . .
C13 C 0.4038(10) 0.3729(14) 0.4344(4) 0.048(3) Uani 1 1 d . . . . .
O3AA O -0.070(5) 0.844(11) 0.3945(14) 0.08(2) Uani 0.68(17) 1 d . . P B 2
C11 C 0.8581(11) 0.2090(13) 0.4821(4) 0.047(3) Uani 1 1 d . . . . .
H11 H 0.791109 0.150340 0.486948 0.056 Uiso 1 1 calc R U . . .
C19 C -0.3428(11) 0.9127(12) 0.2968(4) 0.049(3) Uani 1 1 d . . . . .
H19 H -0.409255 0.966663 0.305332 0.058 Uiso 1 1 calc R U . . .
C20 C -0.3602(11) 0.8157(13) 0.2665(4) 0.049(3) Uani 1 1 d . . . . .
H20 H -0.438878 0.801199 0.254484 0.059 Uiso 1 1 calc R U . . .
C10 C 0.9683(13) 0.1890(15) 0.5028(4) 0.063(4) Uani 1 1 d . . . . .
H10 H 0.975021 0.117524 0.522464 0.076 Uiso 1 1 calc R U . . .
C22 C -0.1492(12) 0.7580(16) 0.2720(4) 0.059(4) Uani 1 1 d . . . . .
H22 H -0.083317 0.702590 0.263711 0.070 Uiso 1 1 calc R U . . .
C24 C -0.0106(11) 0.9330(15) 0.3786(4) 0.057(4) Uani 1 1 d . . . . .
C25 C 0.0576(15) 1.0512(16) 0.3957(5) 0.067(4) Uani 1 1 d . . . . .
H25A H -0.001436 1.109832 0.409771 0.081 Uiso 1 1 calc R U . . .
H25B H 0.114928 1.015157 0.416987 0.081 Uiso 1 1 calc R U . . .
C4 C 0.6933(11) 0.4441(14) 0.3430(4) 0.049(3) Uani 1 1 d . . . . .
H4A H 0.606767 0.421642 0.336987 0.059 Uiso 1 1 calc R U . . .
H4B H 0.736135 0.440837 0.316900 0.059 Uiso 1 1 calc R U . . .
C21 C -0.2625(15) 0.740(2) 0.2537(5) 0.078(5) Uani 1 1 d . . . . .
H21 H -0.273471 0.675329 0.232208 0.094 Uiso 1 1 calc R U . . .
C3 C 0.7013(14) 0.5880(15) 0.3599(5) 0.064(4) Uani 1 1 d . . . . .
H3A H 0.672995 0.652794 0.338352 0.076 Uiso 1 1 calc R U . . .
H3B H 0.787796 0.609074 0.366479 0.076 Uiso 1 1 calc R U . . .
O1B O 0.3601(16) 0.455(2) 0.3314(6) 0.051(3) Uani 0.55 1 d . U P A 1
C0 C 0.320(3) 0.569(4) 0.3191(11) 0.051(3) Uani 0.45 1 d . U P A 2
C2AA C 0.153(3) 0.676(3) 0.3926(6) 0.0607(14) Uani 0.4994(16) 1 d D . P A 1
O5AA O 0.1329(17) 0.6631(19) 0.4267(5) 0.0607(14) Uani 0.4994(16) 1 d D . P A 1
C2AB C 0.044(2) 0.559(2) 0.3212(10) 0.0607(14) Uani 0.5006(16) 1 d D . P A 1
O4A O -0.0221(15) 0.4693(17) 0.3161(6) 0.0607(14) Uani 0.5006(16) 1 d D U P A 1
C1AA C 0.3197(18) 0.820(2) 0.3491(8) 0.0607(14) Uani 0.597(12) 1 d D . P A 1
O0AA O 0.4041(13) 0.8790(16) 0.3608(5) 0.0607(14) Uani 0.597(12) 1 d D U P A 1
C1AB C 0.196(3) 0.736(3) 0.2719(6) 0.0607(14) Uani 0.5006(16) 1 d D . P A 1
O0AB O 0.2076(17) 0.7657(19) 0.2381(5) 0.0607(14) Uani 0.5006(16) 1 d D . P A 1
W2A W 0.19075(15) 0.70718(18) 0.31494(4) 0.0358(4) Uani 0.4994(16) 1 d . . P A
2
C2AC C 0.143(3) 0.615(3) 0.2618(9) 0.0607(14) Uani 0.5006(16) 1 d . . P A 2
O4B O 0.1233(17) 0.549(2) 0.2315(6) 0.0607(14) Uani 0.5006(16) 1 d . . P A 2
C1AC C 0.295(3) 0.844(3) 0.2841(10) 0.0607(14) Uani 0.5006(16) 1 d . . P A 2
O0AC O 0.3475(17) 0.914(2) 0.2628(6) 0.0607(14) Uani 0.5006(16) 1 d . . P A 2
C1A C 0.258(3) 0.779(4) 0.3685(12) 0.0607(14) Uani 0.403(12) 1 d . . P A 2
O2AA O 0.0177(17) 0.495(2) 0.3582(6) 0.0607(14) Uani 0.4994(16) 1 d . U P A 2
C4AA C 0.087(3) 0.576(3) 0.3426(10) 0.0607(14) Uani 0.4994(16) 1 d . . P A 2
O4AA O -0.089(4) 0.901(7) 0.404(2) 0.041(14) Uani 0.32(17) 1 d . . P B 1
C7AA C 0.1257(19) 1.139(3) 0.3699(7) 0.109(8) Uani 1 1 d . . . . .
H7AA H 0.208780 1.100639 0.368839 0.131 Uiso 1 1 calc R U . C 2
H7AB H 0.133094 1.229173 0.383781 0.131 Uiso 1 1 calc R U . C 2
C6AA C 0.081(3) 1.167(3) 0.3250(11) 0.059(8) Uani 0.5 1 d . . P D 2
H6AA H 0.003664 1.218852 0.325473 0.071 Uiso 0.5 1 calc R U P D 2
H6AB H 0.141528 1.226571 0.311824 0.071 Uiso 0.5 1 calc R U P D 2
C5AA C 0.152(3) 1.141(3) 0.3321(9) 0.056(7) Uani 0.5 1 d . . P D 1
H5AA H 0.235898 1.107374 0.329558 0.068 Uiso 0.5 1 calc R U P D 1
H5AB H 0.150136 1.237966 0.322686 0.068 Uiso 0.5 1 calc R U P D 1
C0AA C 0.292(3) 0.543(3) 0.3301(9) 0.051(3) Uani 0.55 1 d . U P A 1
O1A O 0.4027(19) 0.490(2) 0.3214(7) 0.051(3) Uani 0.45 1 d . U P A 2
O1AA O 0.315(2) 0.824(2) 0.3971(8) 0.0607(14) Uani 0.403(12) 1 d . U P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 P1 2.490(3) . ?
W1 C15 2.019(12) . ?
W1 C16 2.010(11) . ?
W1 C14 2.034(11) . ?
W1 C12 2.053(11) . ?
W1 C13 2.037(13) . ?
W2 P23 2.468(3) . ?
W2 C2AA 2.025(19) . ?
W2 C2AB 2.026(18) . ?
W2 C1AA 2.024(17) . ?
W2 C1AB 2.016(19) . ?
W2 C0AA 2.00(3) . ?
P1 C5 1.882(11) . ?
P1 C6 1.818(10) . ?
P1 C1 1.890(11) . ?
P23 C17 1.826(11) . ?
P23 C28 1.880(13) . ?
P23 C24 1.876(16) . ?
P23 W2A 2.561(3) . ?
O7 C16 1.142(13) . ?
O2 C5 1.214(13) . ?
O1 C1 1.204(13) . ?
O5 C14 1.142(14) . ?
O6 C15 1.173(15) . ?
C5 C4 1.491(15) . ?
O3 C12 1.123(14) . ?
O4 C13 1.148(15) . ?
O29 C28 1.200(17) . ?
C6 C7 1.376(15) . ?
C6 C11 1.389(15) . ?
C18 H18 0.9500 . ?
C18 C17 1.401(15) . ?
C18 C19 1.379(15) . ?
C17 C22 1.363(18) . ?
C28 C6AA 1.36(3) . ?
C28 C5AA 1.62(3) . ?
C8 H8 0.9500 . ?
C8 C7 1.386(16) . ?
C8 C9 1.367(19) . ?
C7 H7 0.9500 . ?
C9 H9 0.9500 . ?
C9 C10 1.34(2) . ?
C1 C2 1.495(17) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C3 1.513(19) . ?
O3AA C24 1.21(3) . ?
C11 H11 0.9500 . ?
C11 C10 1.383(17) . ?
C19 H19 0.9500 . ?
C19 C20 1.380(17) . ?
C20 H20 0.9500 . ?
C20 C21 1.38(2) . ?
C10 H10 0.9500 . ?
C22 H22 0.9500 . ?
C22 C21 1.38(2) . ?
C24 C25 1.47(2) . ?
C24 O4AA 1.25(5) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C7AA 1.43(2) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C4 C3 1.509(19) . ?
C21 H21 0.9500 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
O1B C0AA 1.15(3) . ?
C0 W2A 1.96(4) . ?
C0 O1A 1.19(4) . ?
C2AA O5AA 1.151(19) . ?
C2AB O4A 1.148(19) . ?
C1AA O0AA 1.149(19) . ?
C1AB O0AB 1.154(19) . ?
W2A C2AC 2.01(3) . ?
W2A C1AC 2.05(3) . ?
W2A C1A 2.01(4) . ?
W2A C4AA 1.96(3) . ?
C2AC O4B 1.19(3) . ?
O4B O0AC 1.36(3) 2_545 ?
C1AC O0AC 1.14(3) . ?
C1A O1AA 1.19(4) . ?
O2AA C4AA 1.22(3) . ?
C7AA H7AA 0.9900 . ?
C7AA H7AB 0.9900 . ?
C7AA C6AA 1.56(4) . ?
C7AA C5AA 1.28(3) . ?
C6AA H6AA 0.9900 . ?
C6AA H6AB 0.9900 . ?
C5AA H5AA 0.9900 . ?
C5AA H5AB 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
C15 W1 P1 89.8(3) . . ?
C15 W1 C14 88.6(5) . . ?
C15 W1 C12 92.3(5) . . ?
C15 W1 C13 174.8(5) . . ?
C16 W1 P1 175.7(3) . . ?
C16 W1 C15 88.6(5) . . ?
C16 W1 C14 92.9(5) . . ?
C16 W1 C12 87.9(5) . . ?
C16 W1 C13 87.7(5) . . ?
C14 W1 P1 91.1(4) . . ?
C14 W1 C12 178.8(5) . . ?
C14 W1 C13 87.9(5) . . ?
C12 W1 P1 88.2(3) . . ?
C13 W1 P1 94.2(3) . . ?
C13 W1 C12 91.2(5) . . ?
C2AA W2 P23 93.9(8) . . ?
C2AA W2 C2AB 88.6(12) . . ?
C2AB W2 P23 89.0(8) . . ?
C1AA W2 P23 98.3(7) . . ?
C1AA W2 C2AA 85.4(11) . . ?
C1AA W2 C2AB 170.8(11) . . ?
C1AB W2 P23 83.0(8) . . ?
C1AB W2 C2AA 176.6(11) . . ?
C1AB W2 C2AB 92.8(13) . . ?
C1AB W2 C1AA 93.6(12) . . ?
C0AA W2 P23 171.7(9) . . ?
C0AA W2 C2AA 92.5(11) . . ?
C0AA W2 C2AB 85.8(12) . . ?
C0AA W2 C1AA 87.5(11) . . ?
C0AA W2 C1AB 90.7(11) . . ?
C5 P1 W1 111.9(3) . . ?
C5 P1 C1 102.6(5) . . ?
C6 P1 W1 121.9(3) . . ?
C6 P1 C5 103.8(5) . . ?
C6 P1 C1 103.1(5) . . ?
C1 P1 W1 111.5(3) . . ?
C17 P23 W2 123.1(4) . . ?
C17 P23 C28 101.9(6) . . ?
C17 P23 C24 103.4(5) . . ?
C17 P23 W2A 120.2(4) . . ?
C28 P23 W2 119.4(4) . . ?
C28 P23 W2A 110.3(4) . . ?
C24 P23 W2 104.2(4) . . ?
C24 P23 C28 101.8(7) . . ?
C24 P23 W2A 116.7(4) . . ?
O6 C15 W1 175.1(10) . . ?
O2 C5 P1 118.0(8) . . ?
O2 C5 C4 124.5(10) . . ?
C4 C5 P1 117.3(8) . . ?
O7 C16 W1 177.3(11) . . ?
C7 C6 P1 120.6(8) . . ?
C7 C6 C11 118.7(10) . . ?
C11 C6 P1 120.7(8) . . ?
C17 C18 H18 119.9 . . ?
C19 C18 H18 119.9 . . ?
C19 C18 C17 120.2(11) . . ?
C18 C17 P23 119.8(9) . . ?
C22 C17 P23 121.2(9) . . ?
C22 C17 C18 118.9(11) . . ?
O5 C14 W1 179.4(11) . . ?
O29 C28 P23 118.3(11) . . ?
O29 C28 C6AA 118.2(18) . . ?
O29 C28 C5AA 126.4(15) . . ?
C6AA C28 P23 121.9(17) . . ?
C5AA C28 P23 112.1(14) . . ?
C7 C8 H8 119.8 . . ?
C9 C8 H8 119.8 . . ?
C9 C8 C7 120.4(11) . . ?
C6 C7 C8 120.3(11) . . ?
C6 C7 H7 119.9 . . ?
C8 C7 H7 119.9 . . ?
C8 C9 H9 120.4 . . ?
C10 C9 C8 119.2(11) . . ?
C10 C9 H9 120.4 . . ?
O1 C1 P1 117.5(9) . . ?
O1 C1 C2 126.1(11) . . ?
C2 C1 P1 116.1(8) . . ?
O3 C12 W1 178.7(12) . . ?
C1 C2 H2A 109.0 . . ?
C1 C2 H2B 109.0 . . ?
C1 C2 C3 112.9(11) . . ?
H2A C2 H2B 107.8 . . ?
C3 C2 H2A 109.0 . . ?
C3 C2 H2B 109.0 . . ?
O4 C13 W1 176.8(12) . . ?
C6 C11 H11 120.4 . . ?
C10 C11 C6 119.2(12) . . ?
C10 C11 H11 120.4 . . ?
C18 C19 H19 120.0 . . ?
C18 C19 C20 120.0(12) . . ?
C20 C19 H19 120.0 . . ?
C19 C20 H20 120.2 . . ?
C19 C20 C21 119.6(12) . . ?
C21 C20 H20 120.2 . . ?
C9 C10 C11 122.2(13) . . ?
C9 C10 H10 118.9 . . ?
C11 C10 H10 118.9 . . ?
C17 C22 H22 119.5 . . ?
C17 C22 C21 121.0(12) . . ?
C21 C22 H22 119.5 . . ?
O3AA C24 P23 110(5) . . ?
O3AA C24 C25 132(4) . . ?
C25 C24 P23 116.8(10) . . ?
O4AA C24 P23 135(4) . . ?
O4AA C24 C25 108(4) . . ?
C24 C25 H25A 107.1 . . ?
C24 C25 H25B 107.1 . . ?
H25A C25 H25B 106.8 . . ?
C7AA C25 C24 120.9(15) . . ?
C7AA C25 H25A 107.1 . . ?
C7AA C25 H25B 107.1 . . ?
C5 C4 H4A 108.8 . . ?
C5 C4 H4B 108.8 . . ?
C5 C4 C3 113.7(11) . . ?
H4A C4 H4B 107.7 . . ?
C3 C4 H4A 108.8 . . ?
C3 C4 H4B 108.8 . . ?
C20 C21 H21 119.9 . . ?
C22 C21 C20 120.3(13) . . ?
C22 C21 H21 119.9 . . ?
C2 C3 H3A 108.5 . . ?
C2 C3 H3B 108.5 . . ?
C4 C3 C2 115.2(11) . . ?
C4 C3 H3A 108.5 . . ?
C4 C3 H3B 108.5 . . ?
H3A C3 H3B 107.5 . . ?
O1A C0 W2A 177(3) . . ?
O5AA C2AA W2 176(2) . . ?
O4A C2AB W2 173(2) . . ?
O0AA C1AA W2 175(2) . . ?
O0AB C1AB W2 176(2) . . ?
C0 W2A P23 168.8(10) . . ?
C0 W2A C2AC 85.6(14) . . ?
C0 W2A C1AC 93.7(13) . . ?
C0 W2A C1A 86.1(15) . . ?
C2AC W2A P23 103.6(8) . . ?
C2AC W2A C1AC 90.0(12) . . ?
C1AC W2A P23 92.8(8) . . ?
C1A W2A P23 84.6(10) . . ?
C1A W2A C2AC 171.7(13) . . ?
C1A W2A C1AC 90.2(14) . . ?
C4AA W2A P23 86.7(8) . . ?
C4AA W2A C0 87.2(13) . . ?
C4AA W2A C2AC 88.3(13) . . ?
C4AA W2A C1AC 178.0(13) . . ?
C4AA W2A C1A 91.7(15) . . ?
O4B C2AC W2A 173(2) . . ?
C2AC O4B O0AC 112(2) . 2_545 ?
O0AC C1AC W2A 172(3) . . ?
O1AA C1A W2A 170(3) . . ?
O2AA C4AA W2A 176(3) . . ?
C25 C7AA H7AA 107.2 . . ?
C25 C7AA H7AB 107.2 . . ?
C25 C7AA C6AA 120.5(17) . . ?
H7AA C7AA H7AB 106.8 . . ?
C6AA C7AA H7AA 107.2 . . ?
C6AA C7AA H7AB 107.2 . . ?
C5AA C7AA C25 136(2) . . ?
C28 C6AA C7AA 115(2) . . ?
C28 C6AA H6AA 108.6 . . ?
C28 C6AA H6AB 108.6 . . ?
C7AA C6AA H6AA 108.6 . . ?
C7AA C6AA H6AB 108.6 . . ?
H6AA C6AA H6AB 107.6 . . ?
C28 C5AA H5AA 108.3 . . ?
C28 C5AA H5AB 108.3 . . ?
C7AA C5AA C28 116(2) . . ?
C7AA C5AA H5AA 108.3 . . ?
C7AA C5AA H5AB 108.3 . . ?
H5AA C5AA H5AB 107.4 . . ?
O1B C0AA W2 176(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
W1 P1 C5 O2 -85.4(8) . . . . ?
W1 P1 C5 C4 90.1(9) . . . . ?
W1 P1 C6 C7 -178.5(8) . . . . ?
W1 P1 C6 C11 4.1(10) . . . . ?
W1 P1 C1 O1 85.7(8) . . . . ?
W1 P1 C1 C2 -88.7(8) . . . . ?
W2 P23 C17 C18 149.5(8) . . . . ?
W2 P23 C17 C22 -30.5(12) . . . . ?
W2 P23 C28 O29 89.6(11) . . . . ?
W2 P23 C28 C5AA -71.4(16) . . . . ?
W2 P23 C24 C25 94.9(10) . . . . ?
W2 P23 C24 O4AA -97(3) . . . . ?
P1 C5 C4 C3 46.4(14) . . . . ?
P1 C6 C7 C8 -179.3(9) . . . . ?
P1 C6 C11 C10 179.8(10) . . . . ?
P1 C1 C2 C3 -49.9(13) . . . . ?
P23 C17 C22 C21 -177.5(13) . . . . ?
P23 C28 C6AA C7AA 28(3) . . . . ?
P23 C28 C5AA C7AA -41(3) . . . . ?
P23 C24 C25 C7AA 12(2) . . . . ?
O2 C5 C4 C3 -138.5(12) . . . . ?
O1 C1 C2 C3 136.3(12) . . . . ?
C5 P1 C6 C7 54.2(10) . . . . ?
C5 P1 C6 C11 -123.2(9) . . . . ?
C5 P1 C1 O1 -154.3(8) . . . . ?
C5 P1 C1 C2 31.3(9) . . . . ?
C5 C4 C3 C2 -64.5(16) . . . . ?
O29 C28 C6AA C7AA -166.3(16) . . . . ?
O29 C28 C5AA C7AA 160(2) . . . . ?
C6 P1 C5 O2 47.9(9) . . . . ?
C6 P1 C5 C4 -136.6(9) . . . . ?
C6 P1 C1 O1 -46.7(9) . . . . ?
C6 P1 C1 C2 138.9(8) . . . . ?
C6 C11 C10 C9 -2(2) . . . . ?
C18 C17 C22 C21 2(2) . . . . ?
C18 C19 C20 C21 -1(2) . . . . ?
C17 P23 C28 O29 -49.8(12) . . . . ?
C17 P23 C28 C6AA 115.5(19) . . . . ?
C17 P23 C28 C5AA 149.2(15) . . . . ?
C17 P23 C24 O3AA 56(4) . . . . ?
C17 P23 C24 C25 -135.4(10) . . . . ?
C17 P23 C24 O4AA 33(3) . . . . ?
C17 C18 C19 C20 1.4(19) . . . . ?
C17 C22 C21 C20 -3(3) . . . . ?
C28 P23 C17 C18 -73.0(10) . . . . ?
C28 P23 C17 C22 106.9(11) . . . . ?
C28 P23 C24 O3AA 162(4) . . . . ?
C28 P23 C24 C25 -29.9(12) . . . . ?
C28 P23 C24 O4AA 139(3) . . . . ?
C8 C9 C10 C11 1(2) . . . . ?
C7 C6 C11 C10 2.3(18) . . . . ?
C7 C8 C9 C10 0(2) . . . . ?
C9 C8 C7 C6 0.8(19) . . . . ?
C1 P1 C5 O2 154.9(8) . . . . ?
C1 P1 C5 C4 -29.6(10) . . . . ?
C1 P1 C6 C7 -52.5(10) . . . . ?
C1 P1 C6 C11 130.1(9) . . . . ?
C1 C2 C3 C4 66.7(16) . . . . ?
O3AA C24 C25 C7AA 177(7) . . . . ?
C11 C6 C7 C8 -1.8(17) . . . . ?
C19 C18 C17 P23 178.1(9) . . . . ?
C19 C18 C17 C22 -1.9(18) . . . . ?
C19 C20 C21 C22 2(3) . . . . ?
C24 P23 C17 C18 32.4(11) . . . . ?
C24 P23 C17 C22 -147.6(11) . . . . ?
C24 P23 C28 O29 -156.4(11) . . . . ?
C24 P23 C28 C6AA 8.9(19) . . . . ?
C24 P23 C28 C5AA 42.5(16) . . . . ?
C24 C25 C7AA C6AA 33(3) . . . . ?
C24 C25 C7AA C5AA -4(5) . . . . ?
C25 C7AA C6AA C28 -56(3) . . . . ?
C25 C7AA C5AA C28 20(5) . . . . ?
W2A P23 C17 C18 164.7(8) . . . . ?
W2A P23 C17 C22 -15.3(12) . . . . ?
W2A P23 C28 O29 79.0(11) . . . . ?
W2A P23 C28 C6AA -115.7(18) . . . . ?
W2A P23 C24 O3AA -78(4) . . . . ?
W2A P23 C24 C25 90.3(11) . . . . ?
O4AA C24 C25 C7AA -160(3) . . . . ?

_olex2_date_sample_data_collection 2019-07-09
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.851
_oxdiff_exptl_absorpt_empirical_full_min 0.697
_chemical_properties_physical    Moisture-sensitive
