# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_rk08_scaled
_database_code_depnum_ccdc_archive 'CCDC 1515752'
_audit_update_record             
;
2016-11-08 deposited with the CCDC.
2016-12-12 downloaded from the CCDC.
;
_audit_creation_date             2016-09-28
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_shelxl_version_number           2013-3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C35 H53 Br O2 P2 W'
_chemical_formula_sum            'C35 H53 Br O2 P2 W'
_chemical_formula_weight         831.47
_chemical_melting_point          ?
_chemical_oxdiff_formula         C35H53BrO2P2W
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'
Br Br -0.6763 1.2805 '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                   11.41025(11)
_cell_length_b                   13.66762(12)
_cell_length_c                   23.3661(3)
_cell_angle_alpha                90
_cell_angle_beta                 100.0542(10)
_cell_angle_gamma                90
_cell_volume                     3588.01(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    37403
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      73.7430
_cell_measurement_theta_min      3.7230
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    8.322
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.10723
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear orangish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.539
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1672
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-7 0 6 0.2057
7 0 -6 0.2057
4 8 -2 0.1141
-4 7 5 0.1558
6 -5 -6 0.2106
0 0 15 0.0176
0 0 -15 0.0247
-2 -9 0 0.1186
-6 -6 3 0.1762

_exptl_crystal_preparation       
'slow evaporation of pentane/chloroform solution'
_exptl_crystal_recrystallization_method 'achieved in air'
_exptl_crystal_size_max          0.454
_exptl_crystal_size_mid          0.262
_exptl_crystal_size_min          0.042
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-6.9930 -0.0038 6.0008 0.2200 0.9402 -0.1182
6.9930 0.0038 -6.0008 -0.2200 -0.9402 0.1182
4.0011 8.0010 -1.9745 -0.1475 -0.6223 -0.8352
-3.9917 6.9967 5.0228 0.1280 0.4629 -0.8602
5.9909 -4.9961 -6.0169 -0.1726 -0.7527 0.6651
-0.0037 -0.0077 14.9814 0.9943 0.0013 -0.1316
0.0037 0.0077 -14.9814 -0.9943 -0.0013 0.1316
-2.0037 -8.9998 -0.0288 0.0802 0.3643 0.9827
-5.9976 -6.0019 2.9825 0.1339 0.8696 0.5851

_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0486
_diffrn_reflns_av_unetI/netI     0.0212
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            55340
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.351
_diffrn_reflns_theta_min         3.762
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1297
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -108.00  -8.00   1.00    1.00    --  -36.95 -19.00 150.00  100
  2  ω      1.00  76.00   1.00    1.00    --   36.95 -99.00 -30.00   75
  3  ω     20.00 104.00   1.00    1.00    --   36.95  57.00 150.00   84
  4  ω     20.00 104.00   1.00    1.00    --   36.95  57.00-120.00   84
  5  ω     20.00 104.00   1.00    1.00    --   36.95  57.00-180.00   84
  6  ω     23.00  90.00   1.00    1.00    --   36.95-125.00  60.00   67
  7  ω    -32.00  56.00   1.00    1.00    --   36.95 -38.00 -90.00   88
  8  ω    -34.00  66.00   1.00    1.00    --   36.95 -19.00   0.00  100
  9  ω     23.00  90.00   1.00    1.00    --   36.95-125.00  90.00   67
 10  ω     24.00  51.00   1.00    1.00    --   36.95 -57.00   0.00   27
 11  ω    -29.00  14.00   1.00    1.00    --   36.95 -57.00   0.00   43
 12  ω    -31.00  55.00   1.00    1.00    --   36.95 -38.00  60.00   86
 13  ω     23.00  86.00   1.00    1.00    --   36.95-125.00-120.00   63
 14  ω     32.00  65.00   1.00    1.00    --   36.95-125.00 -30.00   33
 15  ω     39.00  65.00   1.00    1.00    --   36.95 -99.00 150.00   26
 16  ω     42.00  67.00   1.00    1.00    --  111.00-111.00  30.00   25
 17  ω     95.00 139.00   1.00    1.00    --  111.00  38.00-120.00   44
 18  ω     44.00  69.00   1.00    1.00    --  111.00 -50.00  90.00   25
 19  ω     80.00 113.00   1.00    1.00    --  111.00-111.00-120.00   33
 20  ω     57.00 113.00   1.00    1.00    --  111.00-111.00-180.00   56
 21  ω     73.00 106.00   1.00    1.00    --  111.00 -38.00  60.00   33
 22  ω    152.00 177.00   1.00    1.00    --  111.00  38.00   0.00   25
 23  ω     61.00 132.00   1.00    1.00    --  111.00 -25.00  60.00   71
 24  ω    100.00 126.00   1.00    1.00    --  111.00 -64.00   0.00   26
 25  ω     72.00 126.00   1.00    1.00    --  111.00 -50.00 150.00   54
 26  ω     42.00  68.00   1.00    1.00    --  111.00 -92.00 -90.00   26
 27  ω     91.00 150.00   1.00    1.00    --  111.00  25.00 120.00   59
 28  ω     53.00 101.00   1.00    1.00    --  111.00 -64.00  90.00   48
 29  ω     69.00 115.00   1.00    1.00    --  111.00 -25.00-150.00   46
 30  ω    153.00 178.00   1.00    1.00    --  111.00  12.00  90.00   25
 31  ω     65.00 127.00   1.00    1.00    --  111.00  12.00  90.00   62
 32  ω     43.00 103.00   1.00    1.00    --  111.00 -50.00-150.00   60
 33  ω     76.00 102.00   1.00    1.00    --  111.00 -64.00 -60.00   26
 34  ω     92.00 119.00   1.00    1.00    --  111.00  25.00 -30.00   27
 35  ω    105.00 130.00   1.00    1.00    --  111.00 -38.00 -30.00   25
 36  ω     95.00 132.00   1.00    1.00    --  111.00  38.00   0.00   37
 37  ω     45.00 104.00   1.00    1.00    --  111.00 -92.00   0.00   59
 38  ω     43.00 113.00   1.00    1.00    --  111.00-111.00-150.00   70
 39  ω    102.00 176.00   1.00    1.00    --  111.00  77.00-120.00   74
 40  ω     43.00  93.00   1.00    1.00    --  111.00-111.00  90.00   50
 41  ω    131.00 177.00   1.00    1.00    --  111.00  12.00-150.00   46
 42  ω    104.00 130.00   1.00    1.00    --  111.00 -64.00 -60.00   26
 43  ω     70.00 104.00   1.00    1.00    --  111.00 -38.00 120.00   34
 44  ω     73.00 120.00   1.00    1.00    --  111.00 -92.00 -30.00   47
 45  ω     52.00 114.00   1.00    1.00    --  111.00-111.00 120.00   62
 46  ω     47.00  72.00   1.00    1.00    --  111.00 -92.00  90.00   25
 47  ω     90.00 116.00   1.00    1.00    --  111.00 -92.00  90.00   26
 48  ω    104.00 177.00   1.00    1.00    --  111.00  50.00  60.00   73
 49  ω    101.00 149.00   1.00    1.00    --  111.00 178.00  60.00   48
 50  ω     68.00  93.00   1.00    1.00    --  111.00 -77.00   0.00   25
 51  ω    104.00 134.00   1.00    1.00    --  111.00 -77.00   0.00   30
 52  ω     91.00 117.00   1.00    1.00    --  111.00  12.00-150.00   26
 53  ω    129.00 155.00   1.00    1.00    --  111.00  50.00  30.00   26
 54  ω     42.00  86.00   1.00    1.00    --  111.00 -38.00 -30.00   44
 55  ω    106.00 132.00   1.00    1.00    --  111.00 -25.00   0.00   26
 56  ω     47.00 125.00   1.00    1.00    --  111.00 -64.00 150.00   78
 57  ω     98.00 130.00   1.00    1.00    --  111.00 -77.00-150.00   32
 58  ω     59.00  85.00   1.00    1.00    --  111.00 -25.00   0.00   26
 59  ω     43.00 131.00   1.00    1.00    --  111.00   5.00  31.63   88
 60  ω    135.00 161.00   1.00    1.00    --  111.00  38.00 150.00   26
 61  ω     75.00 116.00   1.00    1.00    --  111.00-111.00 -90.00   41
 62  ω    117.00 143.00   1.00    1.00    --  111.00  38.00  60.00   26
 63  ω     99.00 125.00   1.00    1.00    --  111.00 -77.00-180.00   26
 64  ω     54.00  84.00   1.00    1.00    --  111.00 -50.00 -30.00   30
 65  ω     94.00 139.00   1.00    1.00    --  111.00  50.00 120.00   45
 66  ω     43.00 108.00   1.00    1.00    --  111.00 -50.00 -90.00   65
 67  ω     92.00 133.00   1.00    1.00    --  111.00  64.00-125.03   41
 68  ω     58.00  83.00   1.00    1.00    --  111.00 -25.00  90.00   25
 69  ω     84.00 110.00   1.00    1.00    --  111.00 -77.00 150.00   26
 70  ω    104.00 130.00   1.00    1.00    --  111.00 -92.00 -90.00   26
 71  ω     53.00  78.00   1.00    1.00    --  111.00 -92.00  60.00   25
 72  ω     83.00 114.00   1.00    1.00    --  111.00 -81.00  83.87   31
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0254962000
_diffrn_orient_matrix_UB_12      -0.0148056000
_diffrn_orient_matrix_UB_13      0.0663694000
_diffrn_orient_matrix_UB_21      -0.1344013000
_diffrn_orient_matrix_UB_22      -0.0105577000
_diffrn_orient_matrix_UB_23      0.0000503000
_diffrn_orient_matrix_UB_31      0.0093691000
_diffrn_orient_matrix_UB_32      -0.1112479000
_diffrn_orient_matrix_UB_33      -0.0088422000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7100
_reflns_number_total             7242
_reflns_odcompleteness_completeness 98.59
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         1.321
_refine_diff_density_min         -2.190
_refine_diff_density_rms         0.156
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         7242
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0343
_refine_ls_R_factor_gt           0.0339
_refine_ls_restrained_S_all      1.085
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0652P)²+2.5986P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0908
_refine_ls_wR_factor_ref         0.0914
_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 Ternary CH refined with riding coordinates:
 C12(H12), C30(H30), C24(H24), C18(H18)
2.b Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C14(H14A,H14B), C15(H15A,H15B), C13(H13A,H13B), C16(H16A,
 H16B), C31(H31A,H31B), C35(H35A,H35B), C20(H20A,H20B), C19(H19A,H19B),
 C23(H23A,H23B), C25(H25A,H25B), C26(H26A,H26B), C32(H32A,H32B), C29(H29A,H29B),
  C22(H22A,H22B), C34(H34A,H34B), C21(H21A,H21B), C28(H28A,H28B), C33(H33A,
 H33B), C27(H27A,H27B), C10(H10A,H10B), C11(H11A,H11B)
2.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C4(H4), C5(H5), C3(H3)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_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 0.02530(2) 0.50522(2) 0.74479(2) 0.01172(7) Uani 1 1 d . . . . .
C6 C 0.5010(5) 0.5106(3) 0.7486(2) 0.0427(12) Uani 1 1 d . . . . .
H6 H 0.5514 0.5636 0.7468 0.051 Uiso 1 1 calc R . . . .
C7 C 0.3800(3) 0.5260(3) 0.74489(19) 0.0369(8) Uani 1 1 d . . . . .
H7 H 0.3499 0.5893 0.7410 0.044 Uiso 1 1 calc R . . . .
C4 C 0.4720(2) 0.3384(3) 0.75564(13) 0.0275(7) Uani 1 1 d . . . . .
H4 H 0.5028 0.2753 0.7587 0.033 Uiso 1 1 calc R . . . .
C12 C 0.0012(2) 0.3424(2) 0.60943(11) 0.0180(5) Uani 1 1 d . . . . .
H12 H -0.0645 0.3265 0.5778 0.022 Uiso 1 1 calc R . . . .
C5 C 0.5472(3) 0.4172(2) 0.75507(14) 0.0264(6) Uani 1 1 d . . . . .
H5 H 0.6289 0.4075 0.7590 0.032 Uiso 1 1 calc R . . . .
C2 C 0.3024(2) 0.4471(2) 0.74693(11) 0.0168(5) Uani 1 1 d . . . . .
C3 C 0.3511(3) 0.3530(2) 0.75171(14) 0.0248(6) Uani 1 1 d . . . . .
H3 H 0.3012 0.2993 0.7523 0.030 Uiso 1 1 calc R . . . .
C17 C 0.0673(3) 0.4289(2) 0.58916(13) 0.0302(7) Uani 1 1 d . . . . .
H17A H 0.1303 0.4490 0.6204 0.036 Uiso 1 1 calc R . . . .
H17B H 0.0128 0.4834 0.5802 0.036 Uiso 1 1 calc R . . . .
C14 C 0.1333(3) 0.2290(3) 0.56360(14) 0.0398(8) Uani 1 1 d . . . . .
H14A H 0.1855 0.1726 0.5705 0.048 Uiso 1 1 calc R . . . .
H14B H 0.0686 0.2127 0.5323 0.048 Uiso 1 1 calc R . . . .
C15 C 0.2013(3) 0.3144(4) 0.54573(16) 0.0490(11) Uani 1 1 d . . . . .
H15A H 0.2312 0.2983 0.5105 0.059 Uiso 1 1 calc R . . . .
H15B H 0.2688 0.3285 0.5760 0.059 Uiso 1 1 calc R . . . .
C13 C 0.0826(3) 0.2517(3) 0.61883(13) 0.0320(7) Uani 1 1 d . . . . .
H13A H 0.1474 0.2636 0.6509 0.038 Uiso 1 1 calc R . . . .
H13B H 0.0376 0.1959 0.6288 0.038 Uiso 1 1 calc R . . . .
C16 C 0.1217(3) 0.4041(3) 0.53519(15) 0.0410(9) Uani 1 1 d . . . . .
H16A H 0.0583 0.3921 0.5025 0.049 Uiso 1 1 calc R . . . .
H16B H 0.1678 0.4594 0.5256 0.049 Uiso 1 1 calc R . . . .
P1 P -0.06669(5) 0.37454(5) 0.67417(3) 0.01242(13) Uani 1 1 d . . . . .
P2 P -0.02692(5) 0.37934(5) 0.81631(3) 0.01310(13) Uani 1 1 d . . . . .
O1 O 0.1324(2) 0.65590(18) 0.84293(11) 0.0394(6) Uani 1 1 d . . . . .
O2 O 0.0383(3) 0.65808(18) 0.64449(11) 0.0420(6) Uani 1 1 d . . . . .
C31 C -0.0818(4) 0.4919(2) 0.90986(16) 0.0274(7) Uani 1 1 d . . . . .
H31A H -0.0428 0.5437 0.8918 0.033 Uiso 1 1 calc R . . . .
H31B H -0.0231 0.4615 0.9395 0.033 Uiso 1 1 calc R . . . .
C9 C 0.0345(3) 0.6032(2) 0.68053(13) 0.0241(6) Uani 1 1 d . . . . .
C35 C -0.1979(3) 0.3344(2) 0.89132(14) 0.0292(6) Uani 1 1 d . . . . .
H35A H -0.2304 0.2873 0.8617 0.035 Uiso 1 1 calc R . . . .
H35B H -0.1423 0.3004 0.9208 0.035 Uiso 1 1 calc R . . . .
C30 C -0.1324(3) 0.4157(2) 0.86395(11) 0.0200(5) Uani 1 1 d . . . . .
H30 H -0.1957 0.4505 0.8381 0.024 Uiso 1 1 calc R . . . .
C24 C 0.1064(3) 0.3169(2) 0.85680(12) 0.0213(6) Uani 1 1 d . . . . .
H24 H 0.1471 0.2891 0.8269 0.026 Uiso 1 1 calc R . . . .
C20 C -0.3796(4) 0.4985(3) 0.58512(19) 0.0380(10) Uani 1 1 d . . . . .
H20A H -0.4102 0.5195 0.6193 0.046 Uiso 1 1 calc R . . . .
H20B H -0.3910 0.5515 0.5571 0.046 Uiso 1 1 calc R . . . .
C18 C -0.2269(2) 0.3911(2) 0.64551(11) 0.0174(5) Uani 1 1 d . . . . .
H18 H -0.2637 0.4110 0.6786 0.021 Uiso 1 1 calc R . . . .
C8 C 0.0910(2) 0.6025(2) 0.80802(13) 0.0232(6) Uani 1 1 d . . . . .
C19 C -0.2462(3) 0.4760(3) 0.60190(14) 0.0257(6) Uani 1 1 d . . . . .
H19A H -0.2142 0.4587 0.5674 0.031 Uiso 1 1 calc R . . . .
H19B H -0.2044 0.5336 0.6190 0.031 Uiso 1 1 calc R . . . .
C23 C -0.2942(3) 0.2995(2) 0.61976(13) 0.0257(6) Uani 1 1 d . . . . .
H23A H -0.2846 0.2478 0.6486 0.031 Uiso 1 1 calc R . . . .
H23B H -0.2608 0.2769 0.5867 0.031 Uiso 1 1 calc R . . . .
C25 C 0.1965(3) 0.3876(3) 0.89145(13) 0.0311(7) Uani 1 1 d . . . . .
H25A H 0.2119 0.4412 0.8666 0.037 Uiso 1 1 calc R . . . .
H25B H 0.1636 0.4147 0.9236 0.037 Uiso 1 1 calc R . . . .
C26 C 0.3133(3) 0.3344(3) 0.91484(14) 0.0399(9) Uani 1 1 d . . . . .
H26A H 0.3508 0.3147 0.8825 0.048 Uiso 1 1 calc R . . . .
H26B H 0.3668 0.3790 0.9389 0.048 Uiso 1 1 calc R . . . .
C32 C -0.1831(3) 0.5356(3) 0.93795(15) 0.0362(7) Uani 1 1 d . . . . .
H32A H -0.1499 0.5811 0.9683 0.043 Uiso 1 1 calc R . . . .
H32B H -0.2376 0.5715 0.9088 0.043 Uiso 1 1 calc R . . . .
C29 C 0.0843(3) 0.2303(3) 0.89499(16) 0.0400(8) Uani 1 1 d . . . . .
H29A H 0.0279 0.1855 0.8727 0.048 Uiso 1 1 calc R . . . .
H29B H 0.0504 0.2535 0.9278 0.048 Uiso 1 1 calc R . . . .
C22 C -0.4276(3) 0.3216(3) 0.60037(14) 0.0358(8) Uani 1 1 d . . . . .
H22A H -0.4666 0.2645 0.5811 0.043 Uiso 1 1 calc R . . . .
H22B H -0.4631 0.3349 0.6344 0.043 Uiso 1 1 calc R . . . .
C34 C -0.2987(3) 0.3780(3) 0.91872(15) 0.0363(8) Uani 1 1 d . . . . .
H34A H -0.3576 0.4072 0.8886 0.044 Uiso 1 1 calc R . . . .
H34B H -0.3371 0.3264 0.9371 0.044 Uiso 1 1 calc R . . . .
C21 C -0.4484(3) 0.4091(3) 0.55912(15) 0.0404(9) Uani 1 1 d . . . . .
H21A H -0.4237 0.3924 0.5227 0.048 Uiso 1 1 calc R . . . .
H21B H -0.5327 0.4244 0.5510 0.048 Uiso 1 1 calc R . . . .
C28 C 0.2016(4) 0.1768(3) 0.91696(18) 0.0496(11) Uani 1 1 d . . . . .
H28A H 0.1870 0.1230 0.9419 0.060 Uiso 1 1 calc R . . . .
H28B H 0.2322 0.1496 0.8841 0.060 Uiso 1 1 calc R . . . .
C33 C -0.2511(3) 0.4556(3) 0.96374(15) 0.0399(8) Uani 1 1 d . . . . .
H33A H -0.1988 0.4248 0.9959 0.048 Uiso 1 1 calc R . . . .
H33B H -0.3171 0.4846 0.9788 0.048 Uiso 1 1 calc R . . . .
C27 C 0.2934(4) 0.2448(4) 0.95037(16) 0.0528(12) Uani 1 1 d . . . . .
H27A H 0.3680 0.2099 0.9612 0.063 Uiso 1 1 calc R . . . .
H27B H 0.2671 0.2653 0.9858 0.063 Uiso 1 1 calc R . . . .
Br1 Br -0.18539(2) 0.59182(2) 0.74812(2) 0.02121(9) Uani 1 1 d . . . . .
C1 C 0.1772(2) 0.46484(19) 0.74434(11) 0.0160(5) Uani 1 1 d . . . . .
C10 C -0.0603(2) 0.26151(19) 0.71709(10) 0.0169(5) Uani 1 1 d . . . . .
H10A H -0.1071 0.2109 0.6946 0.020 Uiso 1 1 calc R . . . .
H10B H 0.0214 0.2389 0.7266 0.020 Uiso 1 1 calc R . . . .
C11 C -0.1093(2) 0.28073(19) 0.77329(11) 0.0170(5) Uani 1 1 d . . . . .
H11A H -0.1034 0.2213 0.7963 0.020 Uiso 1 1 calc R . . . .
H11B H -0.1927 0.2985 0.7636 0.020 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
W1 P1 2.5318(6) . ?
W1 P2 2.5407(6) . ?
W1 C9 2.028(3) . ?
W1 C8 2.032(3) . ?
W1 Br1 2.6929(3) . ?
W1 C1 1.821(3) . ?
C6 C7 1.384(6) . ?
C6 C5 1.379(5) . ?
C7 C2 1.402(4) . ?
C4 C5 1.379(5) . ?
C4 C3 1.381(4) . ?
C12 C17 1.522(4) . ?
C12 C13 1.541(4) . ?
C12 P1 1.868(3) . ?
C2 C3 1.398(4) . ?
C2 C1 1.439(4) . ?
C17 C16 1.537(4) . ?
C14 C15 1.501(6) . ?
C14 C13 1.535(4) . ?
C15 C16 1.520(6) . ?
P1 C18 1.848(3) . ?
P1 C10 1.836(3) . ?
P2 C30 1.845(3) . ?
P2 C24 1.854(3) . ?
P2 C11 1.838(3) . ?
O1 C8 1.134(4) . ?
O2 C9 1.135(4) . ?
C31 C30 1.534(4) . ?
C31 C32 1.546(5) . ?
C35 C30 1.539(4) . ?
C35 C34 1.531(4) . ?
C24 C25 1.535(4) . ?
C24 C29 1.529(4) . ?
C20 C19 1.535(5) . ?
C20 C21 1.520(5) . ?
C18 C19 1.534(4) . ?
C18 C23 1.535(4) . ?
C23 C22 1.540(4) . ?
C25 C26 1.532(4) . ?
C26 C27 1.520(6) . ?
C32 C33 1.525(5) . ?
C29 C28 1.533(5) . ?
C22 C21 1.528(5) . ?
C34 C33 1.524(5) . ?
C28 C27 1.511(7) . ?
C10 C11 1.537(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
P1 W1 P2 80.38(2) . . ?
P1 W1 Br1 93.338(15) . . ?
P2 W1 Br1 88.030(16) . . ?
C9 W1 P1 92.99(8) . . ?
C9 W1 P2 169.22(8) . . ?
C9 W1 C8 92.64(12) . . ?
C9 W1 Br1 83.86(8) . . ?
C8 W1 P1 173.84(8) . . ?
C8 W1 P2 93.68(8) . . ?
C8 W1 Br1 84.79(8) . . ?
C1 W1 P1 93.97(8) . . ?
C1 W1 P2 97.55(8) . . ?
C1 W1 C9 91.34(12) . . ?
C1 W1 C8 88.39(11) . . ?
C1 W1 Br1 171.46(8) . . ?
C5 C6 C7 120.4(4) . . ?
C6 C7 C2 120.7(3) . . ?
C5 C4 C3 120.2(3) . . ?
C17 C12 C13 110.4(3) . . ?
C17 C12 P1 111.56(19) . . ?
C13 C12 P1 113.49(19) . . ?
C4 C5 C6 119.8(3) . . ?
C7 C2 C1 119.8(3) . . ?
C3 C2 C7 117.8(3) . . ?
C3 C2 C1 122.4(2) . . ?
C4 C3 C2 121.1(3) . . ?
C12 C17 C16 112.2(3) . . ?
C15 C14 C13 111.4(3) . . ?
C14 C15 C16 110.4(3) . . ?
C14 C13 C12 110.4(3) . . ?
C15 C16 C17 111.1(3) . . ?
C12 P1 W1 120.70(9) . . ?
C18 P1 W1 114.91(9) . . ?
C18 P1 C12 105.01(12) . . ?
C10 P1 W1 105.37(8) . . ?
C10 P1 C12 105.17(12) . . ?
C10 P1 C18 104.09(12) . . ?
C30 P2 W1 117.86(9) . . ?
C30 P2 C24 112.32(13) . . ?
C24 P2 W1 112.45(10) . . ?
C11 P2 W1 107.04(8) . . ?
C11 P2 C30 101.68(13) . . ?
C11 P2 C24 103.70(13) . . ?
C30 C31 C32 110.0(3) . . ?
O2 C9 W1 179.3(3) . . ?
C34 C35 C30 110.3(3) . . ?
C31 C30 P2 113.5(2) . . ?
C31 C30 C35 110.5(2) . . ?
C35 C30 P2 118.1(2) . . ?
C25 C24 P2 113.2(2) . . ?
C29 C24 P2 116.7(2) . . ?
C29 C24 C25 110.1(3) . . ?
C21 C20 C19 111.2(3) . . ?
C19 C18 P1 110.57(19) . . ?
C19 C18 C23 110.6(2) . . ?
C23 C18 P1 116.0(2) . . ?
O1 C8 W1 177.1(3) . . ?
C18 C19 C20 110.0(3) . . ?
C18 C23 C22 110.9(3) . . ?
C26 C25 C24 110.5(3) . . ?
C27 C26 C25 111.9(3) . . ?
C33 C32 C31 111.1(3) . . ?
C24 C29 C28 109.9(3) . . ?
C21 C22 C23 112.1(3) . . ?
C33 C34 C35 110.9(3) . . ?
C20 C21 C22 111.3(3) . . ?
C27 C28 C29 111.4(4) . . ?
C34 C33 C32 111.7(3) . . ?
C28 C27 C26 111.7(3) . . ?
C2 C1 W1 171.6(2) . . ?
C11 C10 P1 109.70(17) . . ?
C10 C11 P2 111.42(18) . . ?


_ins_header                      
;
TITL RK08_scaled in P2(1)/n 
REM P2(1)/n (#14 in standard setting)
CELL 1.54184  11.410255  13.667622  23.366128  90.0000 100.0542  90.0000
ZERR    5.00   0.000113   0.000120   0.000262   0.0000   0.0010   0.0000
LATT  1
SYMM -x+1/2, y+1/2,-z+1/2 
SFAC C H O P Br W
UNIT 175.00 265.00 10.00 10.00 5.00 5.00
TREF
HKLF 4
END
;
_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 5.434
_oxdiff_exptl_absorpt_empirical_full_min 0.595
####################################################################### 
# 
# 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_rk12_scaled
_database_code_depnum_ccdc_archive 'CCDC 1515753'
_audit_update_record             
;
2016-11-08 deposited with the CCDC.
2016-12-12 downloaded from the CCDC.
;
_audit_creation_date             2016-11-08
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_shelxl_version_number           2013-3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         '2(C33 H53 Br3 P2 W)'
_chemical_formula_sum            'C66 H106 Br6 P4 W2'
_chemical_formula_weight         1870.54
_chemical_melting_point          ?
_chemical_oxdiff_formula         C33H53Br3P2W
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'
Br Br -0.6763 1.2805 '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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.7140(4)
_cell_length_b                   15.8440(3)
_cell_length_c                   20.4006(4)
_cell_angle_alpha                81.8120(17)
_cell_angle_beta                 88.384(2)
_cell_angle_gamma                84.131(2)
_cell_volume                     3727.67(17)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    26714
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      73.4680
_cell_measurement_theta_min      3.3010
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    10.458
_exptl_absorpt_correction_T_max  0.43727
_exptl_absorpt_correction_T_min  0.37910
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Spherical absorption correction
 using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.667
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1840
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-4 0 -12 0.0213
4 0 12 0.0302
-1 -10 -1 0.1355
1 10 2 0.1126
-7 0 3 0.0123
7 0 -3 0.0123

_exptl_crystal_size_max          0.251
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.025
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-4.0020 0.0007 -12.0087 0.2498 0.9992 -0.2130
4.0020 -0.0007 12.0087 -0.2498 -0.9992 0.2130
-1.0107 -9.9956 -0.9850 0.0628 0.1477 0.9614
1.0108 9.9962 1.9847 -0.0412 -0.2193 -0.9467
-7.0000 0.0153 2.9782 0.9555 0.0288 -0.0197
7.0000 -0.0153 -2.9782 -0.9555 -0.0288 0.0197

_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0491
_diffrn_reflns_av_unetI/netI     0.0423
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            61566
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.082
_diffrn_reflns_theta_min         2.188
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1297
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -105.00 -10.00   1.00    4.00    --  -37.20 -77.00 120.00   95
  2  ω    -64.00  30.00   1.00    4.00    --  -37.20  77.00-120.00   94
  3  ω    -32.00 106.00   1.00    4.00    --   37.20   0.00 -90.00  138
  4  ω      8.00 109.00   1.00    4.00    --   37.20  19.00-120.00  101
  5  ω     23.00  91.00   1.00    4.00    --   37.20-125.00-150.00   68
  6  ω     23.00  91.00   1.00    4.00    --   37.20-125.00   0.00   68
  7  ω      1.00  76.00   1.00    4.00    --   37.20 -99.00 -60.00   75
  8  ω    -30.00  54.00   1.00    4.00    --   37.20 -57.00-150.00   84
  9  ω    -32.00  56.00   1.00    4.00    --   37.20 -38.00  90.00   88
 10  ω     10.00 105.00   1.00    4.00    --   37.20  77.00 -30.00   95
 11  ω     23.00  91.00   1.00    4.00    --   37.20-125.00  30.00   68
 12  ω    -32.00  56.00   1.00    4.00    --   37.20 -38.00   0.00   88
 13  ω     27.00  80.00   1.00    4.00    --   37.20-112.00  60.00   53
 14  ω     31.00  73.00   1.00    4.00    --   37.20-125.00 150.00   42
 15  ω     62.00 106.00   1.00    4.00    --   37.20  38.00  30.00   44
 16  ω    -30.00   3.00   1.00    4.00    --   37.20 -57.00  90.00   33
 17  ω     19.00  53.00   1.00    4.00    --   37.20  38.00  30.00   34
 18  ω     54.00  81.00   1.00    4.00    --   37.20-125.00 120.00   27
 19  ω      2.00  27.00   1.00    4.00    --   37.20 -99.00 120.00   25
 20  ω     44.00 128.00   1.00   16.00    --  111.00 -50.00 -60.00   84
 21  ω     86.00 120.00   1.00   16.00    --  111.00 -50.00 -30.00   34
 22  ω     50.00  77.00   1.00   16.00    --  111.00 -50.00 -30.00   27
 23  ω     42.00  69.00   1.00   16.00    --  111.00-111.00-180.00   27
 24  ω     98.00 132.00   1.00   16.00    --  111.00  38.00-180.00   34
 25  ω    104.00 147.00   1.00   16.00    --  111.00 178.00-150.00   43
 26  ω     73.00 100.00   1.00   16.00    --  111.00 -77.00 150.00   27
 27  ω     86.00 136.00   1.00   16.00    --  111.00 -25.00  90.00   50
 28  ω    129.00 156.00   1.00   16.00    --  111.00  64.00-120.00   27
 29  ω     85.00 112.00   1.00   16.00    --  111.00-111.00   0.00   27
 30  ω    148.00 175.00   1.00   16.00    --  111.00 111.00  60.00   27
 31  ω     77.00 135.00   1.00   16.00    --  111.00 -25.00-120.00   58
 32  ω     73.00 100.00   1.00   16.00    --  111.00 178.00 150.00   27
 33  ω     42.00  87.00   1.00   16.00    --  111.00-111.00 -60.00   45
 34  ω    115.00 157.00   1.00   16.00    --  111.00 -12.00  60.00   42
 35  ω    101.00 134.00   1.00   16.00    --  111.00 111.00  60.00   33
 36  ω     47.00  74.00   1.00   16.00    --  111.00 -77.00  90.00   27
 37  ω     99.00 126.00   1.00   16.00    --  111.00  25.00-150.00   27
 38  ω     42.00 105.00   1.00   16.00    --  111.00 -12.00  60.00   63
 39  ω    105.00 130.00   1.00   16.00    --  111.00 -77.00  90.00   25
 40  ω    113.00 152.00   1.00   16.00    --  111.00  77.00   0.00   39
 41  ω    100.00 125.00   1.00   16.00    --  111.00 -50.00 120.00   25
 42  ω     43.00 109.00   1.00   16.00    --  111.00 -92.00 150.00   66
 43  ω     54.00  96.00   1.00   16.00    --  111.00 -77.00 -30.00   42
 44  ω     96.00 130.00   1.00   16.00    --  111.00  38.00 -90.00   34
 45  ω    132.00 162.00   1.00   16.00    --  111.00  38.00 -90.00   30
 46  ω     47.00  74.00   1.00   16.00    --  111.00 -64.00 150.00   27
 47  ω     94.00 121.00   1.00   16.00    --  111.00 -64.00 150.00   27
 48  ω     75.00 116.00   1.00   16.00    --  111.00-111.00  30.00   41
 49  ω     71.00 114.00   1.00   16.00    --  111.00-111.00-120.00   43
 50  ω     86.00 120.00   1.00   16.00    --  111.00 -50.00 150.00   34
 51  ω    103.00 140.00   1.00   16.00    --  111.00 -92.00 -30.00   37
 52  ω    112.00 144.00   1.00   16.00    --  111.00 178.00 -90.00   32
 53  ω     42.00  68.00   1.00   16.00    --  111.00 -92.00 -30.00   26
 54  ω     58.00  83.00   1.00   16.00    --  111.00 178.00-150.00   25
 55  ω    118.00 157.00   1.00   16.00    --  111.00  77.00  60.00   39
 56  ω     43.00  69.00   1.00   16.00    --  111.00 -38.00 120.00   26
 57  ω     90.00 130.00   1.00   16.00    --  111.00 -38.00  90.00   40
 58  ω    105.00 146.00   1.00   16.00    --  111.00 -92.00-150.00   41
 59  ω     42.00  75.00   1.00   16.00    --  111.00 -38.00 -30.00   33
 60  ω     95.00 123.00   1.00   16.00    --  111.00 -64.00 -60.00   28
 61  ω     97.00 150.00   1.00   16.00    --  111.00  38.00 -30.00   53
 62  ω     42.00  71.00   1.00   16.00    --  111.00 -92.00-150.00   29
 63  ω    101.00 128.00   1.00   16.00    --  111.00 -50.00-180.00   27
 64  ω    116.00 172.00   1.00   16.00    --  111.00  50.00  30.00   56
 65  ω    144.00 177.00   1.00   16.00    --  111.00  77.00 -90.00   33
 66  ω     88.00 120.00   1.00   16.00    --  111.00 -38.00 -30.00   32
 67  ω    101.00 169.00   1.00   16.00    --  111.00 111.00  30.00   68
 68  ω     42.00 111.00   1.00   16.00    --  111.00-111.00 150.00   69
 69  ω    100.00 130.00   1.00   16.00    --  111.00 -38.00 120.00   30
 70  ω     66.00  93.00   1.00   16.00    --  111.00 178.00 -90.00   27
 71  ω     94.00 131.00   1.00   16.00    --  111.00  77.00 -90.00   37
 72  ω     98.00 147.00   1.00   16.00    --  111.00  38.00  60.00   49
 73  ω     70.00 114.00   1.00   16.00    --  111.00-111.00 -90.00   44
 74  ω     90.00 116.00   1.00   16.00    --  111.00-111.00 -30.00   26
 75  ω     90.00 116.00   1.00   16.00    --  111.00-111.00-180.00   26
 76  ω    121.00 146.00   1.00   16.00    --  111.00 178.00 150.00   25
 77  ω     46.00  73.00   1.00   16.00    --  111.00 -64.00-180.00   27
 78  ω     88.00 128.00   1.00   16.00    --  111.00 -64.00   0.00   40
 79  ω     81.00 122.00   1.00   16.00    --  111.00 -34.00   6.69   41
 80  ω     70.00  97.00   1.00   16.00    --  111.00 178.00  30.00   27
 81  ω     97.00 122.00   1.00   16.00    --  111.00 -79.00 -14.95   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1272975000
_diffrn_orient_matrix_UB_12      0.0044532000
_diffrn_orient_matrix_UB_13      0.0216200000
_diffrn_orient_matrix_UB_21      -0.0346226000
_diffrn_orient_matrix_UB_22      -0.0042126000
_diffrn_orient_matrix_UB_23      -0.0716676000
_diffrn_orient_matrix_UB_31      0.0088798000
_diffrn_orient_matrix_UB_32      -0.0985318000
_diffrn_orient_matrix_UB_33      0.0147691000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                13010
_reflns_number_total             15029
_reflns_odcompleteness_completeness 98.47
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         1.948
_refine_diff_density_min         -2.363
_refine_diff_density_rms         0.132
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     710
_refine_ls_number_reflns         15029
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0446
_refine_ls_R_factor_gt           0.0378
_refine_ls_restrained_S_all      1.055
_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)+(0.0510P)²+4.9249P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0968
_refine_ls_wR_factor_ref         0.1018
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C2AB) = Uanis(C4AB) = Uanis(C3AB)
Uanis(C1AA) = Uanis(C2AA) = Uanis(C4AA) = Uanis(C3AA)
3. Others
 Sof(H1BC)=Sof(H1BD)=Sof(H2B)=Sof(C1AB)=Sof(H1AE)=Sof(H1AF)=Sof(C2AB)=
 Sof(H2AC)=Sof(H2AD)=Sof(C4AB)=Sof(H4AC)=Sof(H4AD)=Sof(C3AB)=Sof(H3AC)=
 Sof(H3AD)=1-FVAR(1)
 Sof(H1AA)=Sof(H1AB)=Sof(H2A)=Sof(C2AA)=Sof(H2AA)=Sof(H2AB)=Sof(C1AA)=
 Sof(H1AC)=Sof(H1AD)=Sof(C3AA)=Sof(H3AA)=Sof(H3AB)=Sof(C4AA)=Sof(H4AA)=
 Sof(H4AB)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C10(H10), C13(H13), C16(H16), C17(H17), C2(H2A),
 C2(H2B)
4.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C12(H12A,H12B), C15(H15A,
 H15B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B), C24(H24A,H24B),
 C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C30(H30A,H30B),
  C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C35(H35A,H35B), C36(H36A,
 H36B), C0AA(H0AA,H0AB), C38(H38A,H38B), C40(H40A,H40B), C41(H41A,H41B),
 C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B), C47(H47A,H47B), C49(H49A,H49B),
  C52(H52A,H52B), C53(H53A,H53B), C54(H54A,H54B), C55(H55A,H55B), C57(H57A,
 H57B), C60(H60A,H60B), C61(H61A,H61B), C62(H62A,H62B), C63(H63A,H63B),
 C67(H67A,H67B), C1(H1AA,H1AB), C1(H1BC,H1BD), C2AA(H2AA,H2AB), C1AA(H1AC,H1AD),
  C3AA(H3AA,H3AB), C4AA(H4AA,H4AB), C1AB(H1AE,H1AF), C2AB(H2AC,H2AD), C4AB(H4AC,
 H4AD), C3AB(H3AC,H3AD)
4.c Aromatic/amide H refined with riding coordinates:
 C18(H18), C43(H43), C50(H50), C58(H58), C59(H59), C66(H66), C68(H68),
 C69(H69), C72(H72), C73(H73)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_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 0.79130(2) 0.54765(2) 0.21099(2) 0.02440(6) Uani 1 1 d . . . . .
W2 W 0.84882(2) 1.03575(2) 0.22888(2) 0.02692(6) Uani 1 1 d . . . . .
Br3 Br 0.64370(5) 0.66814(3) 0.26359(3) 0.03539(12) Uani 1 1 d . . . . .
Br4 Br 0.74065(5) 0.62953(3) 0.10043(3) 0.03600(12) Uani 1 1 d . . . . .
Br5 Br 0.75084(5) 1.15543(3) 0.30518(3) 0.03355(11) Uani 1 1 d . . . . .
Br6 Br 0.94047(4) 0.62004(3) 0.25873(3) 0.03478(11) Uani 1 1 d . . . . .
Br7 Br 1.03423(5) 1.07170(3) 0.26924(3) 0.03840(12) Uani 1 1 d . . . . .
Br8 Br 0.78655(5) 1.14634(3) 0.13470(3) 0.03990(13) Uani 1 1 d . . . . .
P9 P 0.78074(10) 0.44922(7) 0.32267(5) 0.0240(2) Uani 1 1 d . . . . .
P10 P 0.85682(11) 0.92005(7) 0.33026(6) 0.0269(2) Uani 1 1 d . . . . .
P11 P 0.65346(11) 0.97400(7) 0.22603(6) 0.0287(2) Uani 1 1 d . . . . .
P108 P 0.61935(10) 0.46557(7) 0.19484(6) 0.0249(2) Uani 1 1 d . . . . .
C23 C 0.8903(4) 0.4699(3) 0.1786(2) 0.0285(9) Uani 1 1 d . . . . .
C34 C 0.9731(4) 0.4143(3) 0.1476(2) 0.0317(10) Uani 1 1 d . . . . .
C37 C 0.9130(5) 0.9604(3) 0.1785(3) 0.0353(11) Uani 1 1 d . . . . .
C3 C 0.6570(4) 0.3869(3) 0.3208(2) 0.0271(9) Uani 1 1 d . . . . .
H3A H 0.6697 0.3341 0.3513 0.033 Uiso 1 1 calc R . . . .
H3B H 0.5887 0.4194 0.3355 0.033 Uiso 1 1 calc R . . . .
C4 C 0.7530(4) 0.5017(3) 0.3992(2) 0.0277(9) Uani 1 1 d . . . . .
H4 H 0.7017 0.5537 0.3856 0.033 Uiso 1 1 calc R . . . .
C5 C 0.4807(4) 0.5210(3) 0.2179(2) 0.0283(9) Uani 1 1 d . . . . .
H5 H 0.4986 0.5518 0.2541 0.034 Uiso 1 1 calc R . . . .
C6 C 0.9040(4) 0.3641(3) 0.3346(2) 0.0264(9) Uani 1 1 d . . . . .
H6 H 0.8963 0.3275 0.3004 0.032 Uiso 1 1 calc R . . . .
C7 C 0.9014(4) 0.3045(3) 0.4011(2) 0.0277(9) Uani 1 1 d . . . . .
H7A H 0.8267 0.2831 0.4079 0.033 Uiso 1 1 calc R . . . .
H7B H 0.9143 0.3362 0.4370 0.033 Uiso 1 1 calc R . . . .
C8 C 1.0232(4) 0.3967(3) 0.3229(2) 0.0286(9) Uani 1 1 d . . . . .
H8A H 1.0247 0.4340 0.2810 0.034 Uiso 1 1 calc R . . . .
H8B H 1.0390 0.4294 0.3578 0.034 Uiso 1 1 calc R . . . .
C9 C 0.8799(5) 1.0089(3) 0.4383(2) 0.0327(10) Uani 1 1 d . . . . .
H9A H 0.9412 0.9692 0.4592 0.039 Uiso 1 1 calc R . . . .
H9B H 0.9138 1.0486 0.4045 0.039 Uiso 1 1 calc R . . . .
C10 C 1.0002(5) 0.8611(3) 0.3511(2) 0.0326(10) Uani 1 1 d . . . . .
H10 H 1.0426 0.8988 0.3734 0.039 Uiso 1 1 calc R . . . .
C12 C 0.6376(4) 0.3656(3) 0.2514(2) 0.0288(9) Uani 1 1 d . . . . .
H12A H 0.5697 0.3353 0.2515 0.035 Uiso 1 1 calc R . . . .
H12B H 0.7029 0.3292 0.2376 0.035 Uiso 1 1 calc R . . . .
C13 C 0.6379(5) 0.9162(3) 0.1537(3) 0.0353(11) Uani 1 1 d . . . . .
H13 H 0.6895 0.8633 0.1623 0.042 Uiso 1 1 calc R . . . .
C15 C 0.9952(4) 0.2289(3) 0.4008(2) 0.0309(10) Uani 1 1 d . . . . .
H15A H 0.9951 0.1929 0.4434 0.037 Uiso 1 1 calc R . . . .
H15B H 0.9779 0.1946 0.3673 0.037 Uiso 1 1 calc R . . . .
C16 C 0.7953(4) 0.9593(3) 0.4063(2) 0.0304(10) Uani 1 1 d . . . . .
H16 H 0.7322 1.0023 0.3908 0.036 Uiso 1 1 calc R . . . .
C17 C 0.6024(5) 0.4355(3) 0.1113(2) 0.0316(10) Uani 1 1 d . . . . .
H17 H 0.5738 0.4881 0.0827 0.038 Uiso 1 1 calc R . . . .
C18 C 0.9783(5) 0.3245(3) 0.1574(3) 0.0360(11) Uani 1 1 d . . . . .
H18 H 0.9275 0.2972 0.1871 0.043 Uiso 1 1 calc R . . . .
C19 C 0.7627(5) 0.8408(3) 0.3139(3) 0.0337(11) Uani 1 1 d . . . . .
H19A H 0.7938 0.8116 0.2777 0.040 Uiso 1 1 calc R . . . .
H19B H 0.7567 0.7985 0.3529 0.040 Uiso 1 1 calc R . . . .
C20 C 0.4388(5) 0.5912(3) 0.1617(2) 0.0334(10) Uani 1 1 d . . . . .
H20A H 0.5014 0.6249 0.1463 0.040 Uiso 1 1 calc R . . . .
H20B H 0.4146 0.5650 0.1249 0.040 Uiso 1 1 calc R . . . .
C21 C 1.1136(4) 0.2590(3) 0.3869(3) 0.0325(10) Uani 1 1 d . . . . .
H21A H 1.1693 0.2099 0.3838 0.039 Uiso 1 1 calc R . . . .
H21B H 1.1353 0.2873 0.4232 0.039 Uiso 1 1 calc R . . . .
C24 C 1.0720(5) 0.8409(3) 0.2905(3) 0.0367(11) Uani 1 1 d . . . . .
H24A H 1.0798 0.8934 0.2606 0.044 Uiso 1 1 calc R . . . .
H24B H 1.0333 0.8031 0.2671 0.044 Uiso 1 1 calc R . . . .
C25 C 1.1146(4) 0.3209(3) 0.3224(3) 0.0336(10) Uani 1 1 d . . . . .
H25A H 1.1895 0.3419 0.3158 0.040 Uiso 1 1 calc R . . . .
H25B H 1.1011 0.2907 0.2857 0.040 Uiso 1 1 calc R . . . .
C26 C 0.9913(5) 0.7785(3) 0.4001(3) 0.0410(13) Uani 1 1 d . . . . .
H26A H 0.9493 0.7924 0.4394 0.049 Uiso 1 1 calc R . . . .
H26B H 0.9489 0.7397 0.3799 0.049 Uiso 1 1 calc R . . . .
C27 C 0.8613(5) 0.5323(3) 0.4247(3) 0.0353(11) Uani 1 1 d . . . . .
H27A H 0.9147 0.4832 0.4405 0.042 Uiso 1 1 calc R . . . .
H27B H 0.8984 0.5668 0.3888 0.042 Uiso 1 1 calc R . . . .
C28 C 0.6446(5) 0.8871(3) 0.2960(2) 0.0325(10) Uani 1 1 d . . . . .
H28A H 0.6110 0.9109 0.3342 0.039 Uiso 1 1 calc R . . . .
H28B H 0.5950 0.8463 0.2843 0.039 Uiso 1 1 calc R . . . .
C30 C 0.7414(5) 0.8969(3) 0.4598(3) 0.0372(11) Uani 1 1 d . . . . .
H30A H 0.6875 0.8660 0.4397 0.045 Uiso 1 1 calc R . . . .
H30B H 0.8007 0.8555 0.4809 0.045 Uiso 1 1 calc R . . . .
C31 C 0.7672(5) 0.5355(4) 0.5374(3) 0.0410(12) Uani 1 1 d . . . . .
H31A H 0.7447 0.5724 0.5706 0.049 Uiso 1 1 calc R . . . .
H31B H 0.8178 0.4874 0.5580 0.049 Uiso 1 1 calc R . . . .
C32 C 0.8177(5) 1.0581(3) 0.4898(3) 0.0359(11) Uani 1 1 d . . . . .
H32A H 0.8724 1.0872 0.5108 0.043 Uiso 1 1 calc R . . . .
H32B H 0.7611 1.1011 0.4680 0.043 Uiso 1 1 calc R . . . .
C33 C 0.6898(4) 0.4501(3) 0.4555(2) 0.0331(10) Uani 1 1 d . . . . .
H33A H 0.7376 0.3982 0.4719 0.040 Uiso 1 1 calc R . . . .
H33B H 0.6197 0.4338 0.4389 0.040 Uiso 1 1 calc R . . . .
C35 C 0.5134(6) 0.8289(3) 0.0962(3) 0.0484(15) Uani 1 1 d . . . . .
H35A H 0.4354 0.8148 0.0923 0.058 Uiso 1 1 calc R . . . .
H35B H 0.5614 0.7759 0.1093 0.058 Uiso 1 1 calc R . . . .
C36 C 0.6606(5) 0.5028(4) 0.5123(3) 0.0390(11) Uani 1 1 d . . . . .
H36A H 0.6056 0.5512 0.4971 0.047 Uiso 1 1 calc R . . . .
H36B H 0.6252 0.4676 0.5485 0.047 Uiso 1 1 calc R . . . .
C0AA C 0.7157(5) 0.4023(3) 0.0800(3) 0.0376(12) Uani 1 1 d . . . . .
H0AA H 0.7698 0.4451 0.0781 0.045 Uiso 1 1 calc R . . . .
H0AB H 0.7483 0.3508 0.1073 0.045 Uiso 1 1 calc R . . . .
C38 C 0.8312(5) 0.5853(3) 0.4809(3) 0.0393(12) Uani 1 1 d . . . . .
H38A H 0.9011 0.6018 0.4976 0.047 Uiso 1 1 calc R . . . .
H38B H 0.7838 0.6372 0.4639 0.047 Uiso 1 1 calc R . . . .
C40 C 0.4947(6) 0.3528(4) 0.0402(3) 0.0445(14) Uani 1 1 d . . . . .
H40A H 0.4404 0.3103 0.0417 0.053 Uiso 1 1 calc R . . . .
H40B H 0.4628 0.4045 0.0129 0.053 Uiso 1 1 calc R . . . .
C41 C 0.5121(5) 0.3724(3) 0.1106(3) 0.0408(12) Uani 1 1 d . . . . .
H41A H 0.4399 0.3965 0.1279 0.049 Uiso 1 1 calc R . . . .
H41B H 0.5362 0.3196 0.1391 0.049 Uiso 1 1 calc R . . . .
C42 C 0.9683(5) 0.9075(3) 0.1335(3) 0.0355(11) Uani 1 1 d . . . . .
C43 C 0.9475(6) 0.8215(3) 0.1310(3) 0.0424(13) Uani 1 1 d . . . . .
H43 H 0.8952 0.7962 0.1608 0.051 Uiso 1 1 calc R . . . .
C44 C 0.5168(5) 0.8870(3) 0.1494(3) 0.0424(13) Uani 1 1 d . . . . .
H44A H 0.4955 0.8564 0.1919 0.051 Uiso 1 1 calc R . . . .
H44B H 0.4616 0.9368 0.1392 0.051 Uiso 1 1 calc R . . . .
C45 C 0.7585(6) 0.9992(4) 0.5423(3) 0.0449(13) Uani 1 1 d . . . . .
H45A H 0.8159 0.9612 0.5682 0.054 Uiso 1 1 calc R . . . .
H45B H 0.7145 1.0333 0.5719 0.054 Uiso 1 1 calc R . . . .
C46 C 0.6760(5) 0.9605(3) 0.0868(3) 0.0389(12) Uani 1 1 d . . . . .
H46A H 0.7530 0.9768 0.0901 0.047 Uiso 1 1 calc R . . . .
H46B H 0.6252 1.0122 0.0741 0.047 Uiso 1 1 calc R . . . .
C47 C 0.2831(5) 0.5281(4) 0.2684(3) 0.0451(13) Uani 1 1 d . . . . .
H47A H 0.3083 0.5539 0.3051 0.054 Uiso 1 1 calc R . . . .
H47B H 0.2197 0.4953 0.2840 0.054 Uiso 1 1 calc R . . . .
C49 C 0.5548(7) 0.8712(4) 0.0292(3) 0.0554(18) Uani 1 1 d . . . . .
H49A H 0.5011 0.9201 0.0134 0.067 Uiso 1 1 calc R . . . .
H49B H 0.5569 0.8308 -0.0024 0.067 Uiso 1 1 calc R . . . .
C50 C 1.0586(5) 0.2760(4) 0.1232(3) 0.0432(13) Uani 1 1 d . . . . .
H50 H 1.0608 0.2165 0.1299 0.052 Uiso 1 1 calc R . . . .
C52 C 0.3819(5) 0.4680(3) 0.2450(3) 0.0398(12) Uani 1 1 d . . . . .
H52A H 0.3555 0.4386 0.2106 0.048 Uiso 1 1 calc R . . . .
H52B H 0.4088 0.4254 0.2817 0.048 Uiso 1 1 calc R . . . .
C53 C 0.3389(5) 0.6498(3) 0.1848(3) 0.0406(12) Uani 1 1 d . . . . .
H53A H 0.3649 0.6803 0.2187 0.049 Uiso 1 1 calc R . . . .
H53B H 0.3115 0.6918 0.1479 0.049 Uiso 1 1 calc R . . . .
C54 C 0.2420(5) 0.5987(4) 0.2123(3) 0.0454(13) Uani 1 1 d . . . . .
H54A H 0.2109 0.5731 0.1771 0.054 Uiso 1 1 calc R . . . .
H54B H 0.1812 0.6368 0.2288 0.054 Uiso 1 1 calc R . . . .
C55 C 0.6069(6) 0.3196(3) 0.0095(3) 0.0455(15) Uani 1 1 d . . . . .
H55A H 0.5940 0.3111 -0.0357 0.055 Uiso 1 1 calc R . . . .
H55B H 0.6348 0.2648 0.0341 0.055 Uiso 1 1 calc R . . . .
C57 C 0.6965(5) 0.3825(4) 0.0101(3) 0.0429(13) Uani 1 1 d . . . . .
H57A H 0.6718 0.4353 -0.0183 0.051 Uiso 1 1 calc R . . . .
H57B H 0.7684 0.3586 -0.0077 0.051 Uiso 1 1 calc R . . . .
C58 C 1.0025(7) 0.7748(4) 0.0861(3) 0.0555(17) Uani 1 1 d . . . . .
H58 H 0.9881 0.7181 0.0862 0.067 Uiso 1 1 calc R . . . .
C59 C 1.0523(6) 0.4532(4) 0.1033(3) 0.0501(14) Uani 1 1 d . . . . .
H59 H 1.0514 0.5126 0.0969 0.060 Uiso 1 1 calc R . . . .
C60 C 0.6743(7) 0.9008(4) 0.0336(3) 0.0533(17) Uani 1 1 d . . . . .
H60A H 0.6959 0.9309 -0.0090 0.064 Uiso 1 1 calc R . . . .
H60B H 0.7299 0.8513 0.0444 0.064 Uiso 1 1 calc R . . . .
C61 C 1.1101(6) 0.7342(4) 0.4198(3) 0.0495(16) Uani 1 1 d . . . . .
H61A H 1.1488 0.7703 0.4447 0.059 Uiso 1 1 calc R . . . .
H61B H 1.1014 0.6807 0.4483 0.059 Uiso 1 1 calc R . . . .
C62 C 0.6793(6) 0.9464(4) 0.5115(3) 0.0467(13) Uani 1 1 d . . . . .
H62A H 0.6159 0.9840 0.4908 0.056 Uiso 1 1 calc R . . . .
H62B H 0.6479 0.9063 0.5460 0.056 Uiso 1 1 calc R . . . .
C63 C 1.1825(6) 0.7162(4) 0.3604(3) 0.0503(16) Uani 1 1 d . . . . .
H63A H 1.1492 0.6741 0.3387 0.060 Uiso 1 1 calc R . . . .
H63B H 1.2589 0.6924 0.3747 0.060 Uiso 1 1 calc R . . . .
C66 C 1.1356(6) 0.3154(5) 0.0789(4) 0.0568(17) Uani 1 1 d . . . . .
H66 H 1.1893 0.2828 0.0561 0.068 Uiso 1 1 calc R . . . .
C67 C 1.1909(6) 0.7981(4) 0.3113(3) 0.0491(14) Uani 1 1 d . . . . .
H67A H 1.2318 0.8378 0.3315 0.059 Uiso 1 1 calc R . . . .
H67B H 1.2342 0.7842 0.2724 0.059 Uiso 1 1 calc R . . . .
C68 C 1.1316(7) 0.4050(5) 0.0691(4) 0.0620(19) Uani 1 1 d . . . . .
H68 H 1.1825 0.4320 0.0394 0.074 Uiso 1 1 calc R . . . .
C69 C 1.0791(9) 0.8108(5) 0.0404(4) 0.077(3) Uani 1 1 d . . . . .
H69 H 1.1143 0.7794 0.0089 0.092 Uiso 1 1 calc R . . . .
C72 C 1.0474(8) 0.9429(4) 0.0871(4) 0.068(2) Uani 1 1 d . . . . .
H72 H 1.0623 0.9995 0.0866 0.082 Uiso 1 1 calc R . . . .
C73 C 1.1033(10) 0.8951(5) 0.0421(5) 0.093(4) Uani 1 1 d . . . . .
H73 H 1.1573 0.9191 0.0128 0.111 Uiso 1 1 calc R . . . .
C1 C 0.4928(5) 1.1123(3) 0.1747(3) 0.0403(12) Uani 1 1 d . . . . .
H1AA H 0.5081 1.0862 0.1347 0.048 Uiso 0.626(11) 1 calc R . P A 1
H1AB H 0.5443 1.1566 0.1744 0.048 Uiso 0.626(11) 1 calc R . P A 1
H1BC H 0.5627 1.1376 0.1598 0.048 Uiso 0.374(11) 1 calc R . P A 2
H1BD H 0.4661 1.0854 0.1389 0.048 Uiso 0.374(11) 1 calc R . P A 2
C2 C 0.5189(6) 1.0445(4) 0.2346(3) 0.0460(14) Uani 1 1 d . . . . .
H2A H 0.4620 1.0049 0.2289 0.055 Uiso 0.626(11) 1 calc R . P A 1
H2B H 0.5437 1.0803 0.2659 0.055 Uiso 0.374(11) 1 calc R . P A 2
C2AA C 0.3384(11) 1.0884(8) 0.2901(6) 0.0551(19) Uani 0.626(11) 1 d . . P A 1
H2AA H 0.3006 1.0948 0.3322 0.066 Uiso 0.626(11) 1 calc R . P A 1
H2AB H 0.3061 1.0442 0.2703 0.066 Uiso 0.626(11) 1 calc R . P A 1
C1AA C 0.4813(10) 1.0701(7) 0.2970(5) 0.0551(19) Uani 0.626(11) 1 d . . P A 1
H1AC H 0.5144 1.1216 0.3043 0.066 Uiso 0.626(11) 1 calc R . P A 1
H1AD H 0.5021 1.0250 0.3332 0.066 Uiso 0.626(11) 1 calc R . P A 1
C3AA C 0.3685(11) 1.1541(8) 0.1734(6) 0.0551(19) Uani 0.626(11) 1 d . . P A 1
H3AA H 0.3611 1.2026 0.1385 0.066 Uiso 0.626(11) 1 calc R . P A 1
H3AB H 0.3176 1.1130 0.1636 0.066 Uiso 0.626(11) 1 calc R . P A 1
C4AA C 0.3335(10) 1.1835(8) 0.2378(5) 0.0551(19) Uani 0.626(11) 1 d . . P A 1
H4AA H 0.2568 1.2132 0.2359 0.066 Uiso 0.626(11) 1 calc R . P A 1
H4AB H 0.3868 1.2208 0.2510 0.066 Uiso 0.626(11) 1 calc R . P A 1
C1AB C 0.4234(11) 1.0102(9) 0.2709(7) 0.034(3) Uani 0.374(11) 1 d . . P A 2
H1AE H 0.4472 0.9675 0.3081 0.041 Uiso 0.374(11) 1 calc R . P A 2
H1AF H 0.3724 0.9869 0.2429 0.041 Uiso 0.374(11) 1 calc R . P A 2
C2AB C 0.3565(14) 1.1184(9) 0.2985(9) 0.035(2) Uani 0.374(11) 1 d . . P A 2
H2AC H 0.3015 1.1113 0.3348 0.042 Uiso 0.374(11) 1 calc R . P A 2
H2AD H 0.4128 1.1562 0.3070 0.042 Uiso 0.374(11) 1 calc R . P A 2
C4AB C 0.2967(12) 1.1430(9) 0.2241(8) 0.035(2) Uani 0.374(11) 1 d . . P A 2
H4AC H 0.2781 1.0930 0.2057 0.042 Uiso 0.374(11) 1 calc R . P A 2
H4AD H 0.2299 1.1846 0.2237 0.042 Uiso 0.374(11) 1 calc R . P A 2
C3AB C 0.4032(13) 1.1816(9) 0.1907(8) 0.035(2) Uani 0.374(11) 1 d . . P A 2
H3AC H 0.3805 1.2189 0.1503 0.042 Uiso 0.374(11) 1 calc R . P A 2
H3AD H 0.4352 1.2159 0.2201 0.042 Uiso 0.374(11) 1 calc R . 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 Br3 2.7548(5) . ?
W1 Br4 2.4914(5) . ?
W1 Br6 2.4782(5) . ?
W1 P9 2.5787(11) . ?
W1 P108 2.5596(11) . ?
W1 C23 1.788(5) . ?
W2 Br5 2.7624(5) . ?
W2 Br7 2.4914(6) . ?
W2 Br8 2.4804(5) . ?
W2 P10 2.5579(11) . ?
W2 P11 2.5845(13) . ?
W2 C37 1.780(6) . ?
P9 C3 1.840(5) . ?
P9 C4 1.876(5) . ?
P9 C6 1.869(4) . ?
P10 C10 1.865(5) . ?
P10 C16 1.852(5) . ?
P10 C19 1.824(5) . ?
P11 C13 1.867(5) . ?
P11 C28 1.845(5) . ?
P11 C2 1.855(6) . ?
P108 C5 1.847(5) . ?
P108 C12 1.820(5) . ?
P108 C17 1.856(5) . ?
C23 C34 1.436(7) . ?
C34 C18 1.403(7) . ?
C34 C59 1.404(8) . ?
C37 C42 1.428(8) . ?
C3 C12 1.530(6) . ?
C4 C27 1.534(6) . ?
C4 C33 1.530(7) . ?
C5 C20 1.533(6) . ?
C5 C52 1.543(7) . ?
C6 C7 1.539(6) . ?
C6 C8 1.538(7) . ?
C7 C15 1.541(6) . ?
C8 C25 1.525(6) . ?
C9 C16 1.539(6) . ?
C9 C32 1.521(7) . ?
C10 C24 1.529(7) . ?
C10 C26 1.541(7) . ?
C13 C44 1.545(8) . ?
C13 C46 1.519(8) . ?
C15 C21 1.519(7) . ?
C16 C30 1.533(7) . ?
C17 C0AA 1.533(8) . ?
C17 C41 1.529(7) . ?
C18 C50 1.391(8) . ?
C19 C28 1.527(7) . ?
C20 C53 1.524(7) . ?
C21 C25 1.526(7) . ?
C24 C67 1.529(7) . ?
C26 C61 1.531(8) . ?
C27 C38 1.527(7) . ?
C30 C62 1.528(8) . ?
C31 C36 1.528(8) . ?
C31 C38 1.524(8) . ?
C32 C45 1.517(8) . ?
C33 C36 1.533(7) . ?
C35 C44 1.523(7) . ?
C35 C49 1.524(9) . ?
C0AA C57 1.531(7) . ?
C40 C41 1.535(7) . ?
C40 C55 1.517(9) . ?
C42 C43 1.416(7) . ?
C42 C72 1.406(9) . ?
C43 C58 1.366(8) . ?
C45 C62 1.515(8) . ?
C46 C60 1.541(7) . ?
C47 C52 1.532(8) . ?
C47 C54 1.534(8) . ?
C49 C60 1.530(10) . ?
C50 C66 1.389(10) . ?
C53 C54 1.510(8) . ?
C55 C57 1.520(8) . ?
C58 C69 1.381(11) . ?
C59 C68 1.380(9) . ?
C61 C63 1.502(9) . ?
C63 C67 1.533(9) . ?
C66 C68 1.400(10) . ?
C69 C73 1.398(11) . ?
C72 C73 1.380(10) . ?
C1 C2 1.523(7) . ?
C1 C3AA 1.537(12) . ?
C1 C3AB 1.505(14) . ?
C2 C1AA 1.435(12) . ?
C2 C1AB 1.434(15) . ?
C2AA C1AA 1.675(16) . ?
C2AA C4AA 1.714(17) . ?
C3AA C4AA 1.489(16) . ?
C1AB C2AB 1.96(2) . ?
C2AB C4AB 1.67(2) . ?
C4AB C3AB 1.54(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br4 W1 Br3 86.542(18) . . ?
Br4 W1 P9 162.25(3) . . ?
Br4 W1 P108 85.02(3) . . ?
Br6 W1 Br3 83.294(17) . . ?
Br6 W1 Br4 107.915(19) . . ?
Br6 W1 P9 88.33(3) . . ?
Br6 W1 P108 164.29(3) . . ?
P9 W1 Br3 88.39(3) . . ?
P108 W1 Br3 88.78(3) . . ?
P108 W1 P9 77.87(3) . . ?
C23 W1 Br3 178.29(14) . . ?
C23 W1 Br4 94.58(14) . . ?
C23 W1 Br6 95.12(14) . . ?
C23 W1 P9 90.91(15) . . ?
C23 W1 P108 92.60(15) . . ?
Br7 W2 Br5 84.659(18) . . ?
Br7 W2 P10 85.12(3) . . ?
Br7 W2 P11 161.39(3) . . ?
Br8 W2 Br5 83.949(18) . . ?
Br8 W2 Br7 107.97(2) . . ?
Br8 W2 P10 165.07(3) . . ?
Br8 W2 P11 89.04(3) . . ?
P10 W2 Br5 90.34(3) . . ?
P10 W2 P11 77.14(4) . . ?
P11 W2 Br5 89.83(3) . . ?
C37 W2 Br5 178.79(16) . . ?
C37 W2 Br7 94.98(17) . . ?
C37 W2 Br8 95.07(15) . . ?
C37 W2 P10 90.79(15) . . ?
C37 W2 P11 90.86(18) . . ?
C3 P9 W1 108.09(14) . . ?
C3 P9 C4 103.2(2) . . ?
C3 P9 C6 102.7(2) . . ?
C4 P9 W1 117.57(15) . . ?
C6 P9 W1 112.79(16) . . ?
C6 P9 C4 110.9(2) . . ?
C10 P10 W2 116.61(18) . . ?
C16 P10 W2 113.40(15) . . ?
C16 P10 C10 107.9(2) . . ?
C19 P10 W2 106.90(16) . . ?
C19 P10 C10 106.9(2) . . ?
C19 P10 C16 104.2(2) . . ?
C13 P11 W2 113.71(19) . . ?
C28 P11 W2 109.01(16) . . ?
C28 P11 C13 101.6(2) . . ?
C28 P11 C2 103.3(3) . . ?
C2 P11 W2 119.5(2) . . ?
C2 P11 C13 107.8(3) . . ?
C5 P108 W1 113.31(15) . . ?
C5 P108 C17 107.0(2) . . ?
C12 P108 W1 106.74(15) . . ?
C12 P108 C5 106.0(2) . . ?
C12 P108 C17 106.2(2) . . ?
C17 P108 W1 116.82(18) . . ?
C34 C23 W1 174.2(4) . . ?
C18 C34 C23 124.6(5) . . ?
C18 C34 C59 118.1(5) . . ?
C59 C34 C23 117.2(5) . . ?
C42 C37 W2 174.0(4) . . ?
C12 C3 P9 111.9(3) . . ?
C27 C4 P9 112.8(3) . . ?
C33 C4 P9 115.4(3) . . ?
C33 C4 C27 110.7(4) . . ?
C20 C5 P108 110.4(3) . . ?
C20 C5 C52 110.7(4) . . ?
C52 C5 P108 119.7(3) . . ?
C7 C6 P9 114.3(3) . . ?
C8 C6 P9 114.9(3) . . ?
C8 C6 C7 109.9(4) . . ?
C6 C7 C15 109.7(4) . . ?
C25 C8 C6 109.8(4) . . ?
C32 C9 C16 110.0(4) . . ?
C24 C10 P10 113.8(3) . . ?
C24 C10 C26 109.8(4) . . ?
C26 C10 P10 112.3(4) . . ?
C3 C12 P108 108.2(3) . . ?
C44 C13 P11 112.9(4) . . ?
C46 C13 P11 116.2(4) . . ?
C46 C13 C44 110.7(4) . . ?
C21 C15 C7 112.0(4) . . ?
C9 C16 P10 111.7(4) . . ?
C30 C16 P10 119.4(3) . . ?
C30 C16 C9 109.6(4) . . ?
C0AA C17 P108 113.4(3) . . ?
C41 C17 P108 112.3(4) . . ?
C41 C17 C0AA 110.9(4) . . ?
C50 C18 C34 120.6(5) . . ?
C28 C19 P10 108.3(3) . . ?
C53 C20 C5 111.1(4) . . ?
C15 C21 C25 110.6(4) . . ?
C10 C24 C67 110.6(4) . . ?
C8 C25 C21 111.7(4) . . ?
C61 C26 C10 111.4(5) . . ?
C38 C27 C4 110.6(4) . . ?
C19 C28 P11 111.6(4) . . ?
C62 C30 C16 109.7(4) . . ?
C38 C31 C36 111.1(5) . . ?
C45 C32 C9 111.8(4) . . ?
C4 C33 C36 110.8(4) . . ?
C44 C35 C49 111.7(5) . . ?
C31 C36 C33 111.8(5) . . ?
C57 C0AA C17 110.8(4) . . ?
C31 C38 C27 111.7(4) . . ?
C55 C40 C41 111.4(5) . . ?
C17 C41 C40 111.2(5) . . ?
C43 C42 C37 124.7(5) . . ?
C72 C42 C37 118.4(5) . . ?
C72 C42 C43 116.9(5) . . ?
C58 C43 C42 121.6(6) . . ?
C35 C44 C13 110.9(5) . . ?
C62 C45 C32 111.4(5) . . ?
C13 C46 C60 110.7(5) . . ?
C52 C47 C54 111.1(5) . . ?
C35 C49 C60 111.6(5) . . ?
C66 C50 C18 120.6(5) . . ?
C47 C52 C5 109.2(4) . . ?
C54 C53 C20 110.7(5) . . ?
C53 C54 C47 111.3(5) . . ?
C40 C55 C57 110.8(4) . . ?
C55 C57 C0AA 111.9(5) . . ?
C43 C58 C69 120.8(6) . . ?
C68 C59 C34 121.2(6) . . ?
C49 C60 C46 110.6(6) . . ?
C63 C61 C26 111.9(5) . . ?
C45 C62 C30 112.0(5) . . ?
C61 C63 C67 111.1(5) . . ?
C50 C66 C68 119.2(6) . . ?
C24 C67 C63 111.3(6) . . ?
C59 C68 C66 120.3(7) . . ?
C58 C69 C73 119.1(7) . . ?
C73 C72 C42 121.1(7) . . ?
C72 C73 C69 120.4(8) . . ?
C2 C1 C3AA 113.6(6) . . ?
C3AB C1 C2 111.6(7) . . ?
C1 C2 P11 113.9(4) . . ?
C1AA C2 P11 121.9(6) . . ?
C1AA C2 C1 114.8(6) . . ?
C1AB C2 P11 119.6(6) . . ?
C1AB C2 C1 117.6(7) . . ?
C1AA C2AA C4AA 98.0(9) . . ?
C2 C1AA C2AA 103.9(9) . . ?
C4AA C3AA C1 111.6(10) . . ?
C3AA C4AA C2AA 101.7(10) . . ?
C2 C1AB C2AB 96.4(9) . . ?
C4AB C2AB C1AB 88.1(10) . . ?
C3AB C4AB C2AB 94.4(12) . . ?
C1 C3AB C4AB 111.0(10) . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.252 -0.060 0.162 32.5 0.0 ?
2 0.492 0.757 0.493 163.1 43.5 ?
3 0.508 0.243 0.507 163.1 44.5 ?
4 0.748 0.060 0.838 32.5 0.0 ?


_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 1.576
_oxdiff_exptl_absorpt_empirical_full_min 0.624
####################################################################### 
# 
# 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 1515754'
_audit_update_record             
;
2016-11-08 deposited with the CCDC.
2016-12-12 downloaded from the CCDC.
;
_audit_creation_date             2016-09-27
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_shelxl_version_number           2013-3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         
'C27 H46 Br4 P2 W, C27 H48 Br4 P2 W, C H1.59 Cl2, C H1.88 Cl2'
_chemical_formula_sum            'C56 H98 Br8 Cl4 P4 W2'
_chemical_formula_weight         2044.00
_chemical_melting_point          ?
_chemical_oxdiff_formula         C29H48Br2O2P2W
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 '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                   18.5723(3)
_cell_length_b                   15.8298(3)
_cell_length_c                   25.1171(6)
_cell_angle_alpha                90
_cell_angle_beta                 100.001(2)
_cell_angle_gamma                90
_cell_volume                     7272.1(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    24976
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      28.8710
_cell_measurement_theta_min      3.5760
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    7.825
_exptl_absorpt_correction_T_max  0.55842
_exptl_absorpt_correction_T_min  0.55028
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Spherical absorption correction
 using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.867
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             3960
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 -22 -1 0.0846
7 0 32 0.0177
13 3 27 0.0145
-7 -1 -32 0.0301
-25 5 4 0.0458
3 22 0 0.0974
26 0 -4 0.0325

_exptl_crystal_preparation       ?
_exptl_crystal_recrystallization_method 
'Vapour diffusion of pentane into a conc. solution of DCM.'
_exptl_crystal_size_max          0.205
_exptl_crystal_size_mid          0.116
_exptl_crystal_size_min          0.05
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-0.9798 -21.9720 -1.0624 -0.0278 0.1846 -0.9679
7.0394 -0.0478 32.0103 0.9204 0.3854 0.0923
13.0233 2.9533 27.0104 0.7870 0.5617 0.2712
-7.0384 -0.9510 -32.0132 -0.9204 -0.3751 -0.1358
-24.9738 4.9983 4.0409 0.0757 -0.9783 0.0004
2.9764 21.9726 0.0599 0.0024 -0.1130 0.9847
25.9681 -0.0046 -4.0276 -0.0747 0.9646 0.2262

_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0730
_diffrn_reflns_av_unetI/netI     0.0434
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            109424
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         3.257
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3744
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.998
_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  30.00   1.00   70.00    --  -11.22 -99.00 150.00   50
  2  ω    -86.00  13.00   1.00   70.00    --  -11.22 -37.00 -30.00   99
  3  ω    -44.00  65.00   1.00   70.00    --  -11.22  77.00 120.00  109
  4  ω    -44.00  65.00   1.00   70.00    --  -11.22  77.00-180.00  109
  5  ω    -36.00  63.00   1.00   70.00    --  -11.22  37.00 -60.00   99
  6  ω    -86.00  13.00   1.00   70.00    --  -11.22 -37.00-120.00   99
  7  ω     35.00  80.00   1.00   70.00    --   11.30 178.00 120.00   45
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0015303000
_diffrn_orient_matrix_UB_12      -0.0001760000
_diffrn_orient_matrix_UB_13      0.0284180000
_diffrn_orient_matrix_UB_21      0.0377209000
_diffrn_orient_matrix_UB_22      -0.0102624000
_diffrn_orient_matrix_UB_23      0.0037299000
_diffrn_orient_matrix_UB_31      0.0088738000
_diffrn_orient_matrix_UB_32      0.0436094000
_diffrn_orient_matrix_UB_33      0.0009956000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10322
_reflns_number_total             12804
_reflns_odcompleteness_completeness 99.72
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         1.226
_refine_diff_density_min         -0.876
_refine_diff_density_rms         0.137
_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     705
_refine_ls_number_reflns         12804
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_gt           0.0411
_refine_ls_restrained_S_all      1.099
_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)+(0.0113P)²+41.1681P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0678
_refine_ls_wR_factor_ref         0.0721
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(Cl4A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Sof(Cl1A)=Sof(Cl2A)=1-FVAR(1)
 Sof(Cl1)=Sof(Cl2)=Sof(H9BA)=Sof(H9BB)=FVAR(1)
 Sof(H31)=Sof(Cl4A)=Sof(Cl3A)=1-FVAR(2)
 Sof(Cl3)=Sof(Cl4)=Sof(H31A)=Sof(H31B)=FVAR(2)
4.a Ternary CH refined with riding coordinates:
 C9(H9), C15(H15), C8BA(H8BA), C20(H20), C0BA(H0BA), C2AA(H2AA), C9AA(H9AA),
 C1BA(H1BA)
4.b Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C13(H13A,H13B), C10(H10A,H10B), C11(H11A,H11B), C14(H14A,
 H14B), C17(H17A,H17B), C0AA(H0AA,H0AB), C24(H24A,H24B), C25(H25A,H25B),
 C26(H26A,H26B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C32(H32A,H32B),
  C36(H36A,H36B), C37(H37A,H37B), C39(H39A,H39B), C40(H40A,H40B), C42(H42A,
 H42B), C45(H45A,H45B), C46(H46A,H46B), C8AA(H8AA,H8AB), C3AA(H3AA,H3AB),
 C7AA(H7AA,H7AB), C4AA(H4AA,H4AB), C7BA(H7BA,H7BB), C5AA(H5AA,H5AB), C6AA(H6AA,
 H6AB), C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C27(H27A,H27B),
 C2BA(H2BA,H2BB), C34(H34A,H34B), C38(H38A,H38B), C3BA(H3BA,H3BB), C43(H43A,
 H43B), C4BA(H4BA,H4BB), C5BA(H5BA,H5BB), C6BA(H6BA,H6BB), C16(H16A,H16B),
 C19(H19A,H19B), C9BA(H9BA,H9BB), C31(H31A,H31B)
4.c Aromatic/amide H refined with riding coordinates:
 C31(H31), C0CA(H0CA), C1CA(H1CA)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_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 0.07918(2) 0.10914(2) 0.24070(2) 0.01905(7) Uani 1 1 d . . . . .
W2 W 0.56567(2) -0.10937(2) 0.25172(2) 0.01807(7) Uani 1 1 d . . . . .
Br3 Br 0.43823(3) -0.18848(4) 0.25505(3) 0.02267(15) Uani 1 1 d . . . . .
Br4 Br 0.11196(4) 0.01616(4) 0.32062(3) 0.02772(16) Uani 1 1 d . . . . .
Br5 Br 0.61164(4) -0.18983(4) 0.33654(3) 0.02641(16) Uani 1 1 d . . . . .
Br6 Br 0.56923(3) -0.20162(4) 0.17242(3) 0.02430(15) Uani 1 1 d . . . . .
Br7 Br 0.07945(4) 0.01392(4) 0.16239(3) 0.03155(17) Uani 1 1 d . . . . .
Br9 Br -0.06018(4) 0.05248(4) 0.23682(3) 0.03056(17) Uani 1 1 d . . . . .
Br10 Br 0.25707(4) 0.20066(5) 0.24089(4) 0.0420(2) Uani 1 1 d . . . . .
Br1 Br 0.74633(4) -0.03093(5) 0.24565(3) 0.03766(19) Uani 1 1 d . . . . .
P2 P 0.04498(9) 0.22113(10) 0.30746(7) 0.0228(4) Uani 1 1 d . . . . .
P3 P 0.49249(9) -0.00049(10) 0.18706(7) 0.0177(4) Uani 1 1 d . . . . .
P4 P 0.53231(9) 0.00554(10) 0.31572(7) 0.0182(4) Uani 1 1 d . . . . .
P5 P 0.03032(9) 0.23161(10) 0.17733(7) 0.0218(4) Uani 1 1 d . . . . .
C12 C 0.4720(3) 0.0925(4) 0.2259(3) 0.0194(14) Uani 1 1 d . . . . .
H12A H 0.4727 0.1439 0.2035 0.023 Uiso 1 1 calc R . . . .
H12B H 0.4222 0.0867 0.2346 0.023 Uiso 1 1 calc R . . . .
C13 C 0.5265(3) 0.1025(4) 0.2776(3) 0.0208(14) Uani 1 1 d . . . . .
H13A H 0.5110 0.1491 0.2994 0.025 Uiso 1 1 calc R . . . .
H13B H 0.5751 0.1168 0.2691 0.025 Uiso 1 1 calc R . . . .
C18 C 0.1695(4) 0.1532(4) 0.2415(3) 0.0227(15) Uani 1 1 d . . . . .
C9 C 0.5982(3) 0.0266(4) 0.3787(3) 0.0247(16) Uani 1 1 d . . . . .
H9 H 0.5938 -0.0208 0.4042 0.030 Uiso 1 1 calc R . . . .
C10 C 0.5652(4) -0.0176(4) 0.0960(3) 0.0260(16) Uani 1 1 d . . . . .
H10A H 0.6072 -0.0489 0.1164 0.031 Uiso 1 1 calc R . . . .
H10B H 0.5262 -0.0588 0.0826 0.031 Uiso 1 1 calc R . . . .
C11 C 0.3649(4) -0.1001(4) 0.3856(3) 0.0290(16) Uani 1 1 d . . . . .
H11A H 0.3412 -0.1301 0.3526 0.035 Uiso 1 1 calc R . . . .
H11B H 0.3668 -0.1392 0.4166 0.035 Uiso 1 1 calc R . . . .
C1AA C 0.6527(3) -0.0626(4) 0.2485(3) 0.0248(15) Uani 1 1 d . . . . .
C14 C 0.4427(4) -0.0754(4) 0.3797(3) 0.0245(15) Uani 1 1 d . . . . .
H14A H 0.4686 -0.0512 0.4141 0.029 Uiso 1 1 calc R . . . .
H14B H 0.4698 -0.1262 0.3713 0.029 Uiso 1 1 calc R . . . .
C15 C 0.4405(3) -0.0105(4) 0.3343(3) 0.0189(14) Uani 1 1 d . . . . .
H15 H 0.4102 -0.0370 0.3018 0.023 Uiso 1 1 calc R . . . .
C17 C 0.3983(3) 0.0682(4) 0.3459(3) 0.0236(15) Uani 1 1 d . . . . .
H17A H 0.3971 0.1096 0.3162 0.028 Uiso 1 1 calc R . . . .
H17B H 0.4228 0.0950 0.3799 0.028 Uiso 1 1 calc R . . . .
C0AA C 0.3925(4) -0.1066(4) 0.1152(3) 0.0301(16) Uani 1 1 d . . . . .
H0AA H 0.4208 -0.1546 0.1335 0.036 Uiso 1 1 calc R . . . .
H0AB H 0.4136 -0.0918 0.0828 0.036 Uiso 1 1 calc R . . . .
C8BA C 0.5370(4) 0.0460(4) 0.1335(3) 0.0240(15) Uani 1 1 d . . . . .
H8BA H 0.4983 0.0796 0.1100 0.029 Uiso 1 1 calc R . . . .
C20 C 0.3985(3) -0.0309(4) 0.1535(3) 0.0196(14) Uani 1 1 d . . . . .
H20 H 0.3725 -0.0482 0.1834 0.024 Uiso 1 1 calc R . . . .
C24 C 0.3193(4) -0.0227(4) 0.3946(3) 0.0338(18) Uani 1 1 d . . . . .
H24A H 0.2683 -0.0403 0.3949 0.041 Uiso 1 1 calc R . . . .
H24B H 0.3389 0.0026 0.4303 0.041 Uiso 1 1 calc R . . . .
C25 C 0.6243(4) 0.1531(4) 0.1074(3) 0.0377(19) Uani 1 1 d . . . . .
H25A H 0.5840 0.1881 0.0879 0.045 Uiso 1 1 calc R . . . .
H25B H 0.6654 0.1911 0.1216 0.045 Uiso 1 1 calc R . . . .
C26 C 0.3203(4) 0.0427(4) 0.3510(3) 0.0323(18) Uani 1 1 d . . . . .
H26A H 0.2931 0.0934 0.3595 0.039 Uiso 1 1 calc R . . . .
H26B H 0.2951 0.0198 0.3160 0.039 Uiso 1 1 calc R . . . .
C28 C 0.5983(4) 0.1084(4) 0.1547(3) 0.0295(16) Uani 1 1 d . . . . .
H28A H 0.5802 0.1508 0.1782 0.035 Uiso 1 1 calc R . . . .
H28B H 0.6397 0.0778 0.1765 0.035 Uiso 1 1 calc R . . . .
C29 C 0.2744(4) 0.0165(5) 0.1091(3) 0.042(2) Uani 1 1 d . . . . .
H29A H 0.2541 0.0035 0.1421 0.050 Uiso 1 1 calc R . . . .
H29B H 0.2461 0.0641 0.0904 0.050 Uiso 1 1 calc R . . . .
C30 C 0.5796(4) 0.1077(5) 0.4060(3) 0.0357(18) Uani 1 1 d . . . . .
H30A H 0.5286 0.1046 0.4126 0.043 Uiso 1 1 calc R . . . .
H30B H 0.5832 0.1562 0.3817 0.043 Uiso 1 1 calc R . . . .
C32 C 0.6313(4) 0.1217(5) 0.4599(3) 0.048(2) Uani 1 1 d . . . . .
H32A H 0.6198 0.1764 0.4756 0.057 Uiso 1 1 calc R . . . .
H32B H 0.6239 0.0764 0.4855 0.057 Uiso 1 1 calc R . . . .
C36 C 0.5886(4) 0.0274(5) 0.0484(3) 0.0372(19) Uani 1 1 d . . . . .
H36A H 0.5461 0.0568 0.0271 0.045 Uiso 1 1 calc R . . . .
H36B H 0.6067 -0.0145 0.0246 0.045 Uiso 1 1 calc R . . . .
C37 C 0.3543(3) 0.0431(4) 0.1253(3) 0.0325(18) Uani 1 1 d . . . . .
H37A H 0.3579 0.0922 0.1500 0.039 Uiso 1 1 calc R . . . .
H37B H 0.3742 0.0598 0.0928 0.039 Uiso 1 1 calc R . . . .
C39 C 0.3124(4) -0.1326(5) 0.0980(4) 0.043(2) Uani 1 1 d . . . . .
H39A H 0.3094 -0.1798 0.0718 0.052 Uiso 1 1 calc R . . . .
H39B H 0.2931 -0.1529 0.1300 0.052 Uiso 1 1 calc R . . . .
C40 C 0.6772(4) 0.0287(4) 0.3704(3) 0.0338(18) Uani 1 1 d . . . . .
H40A H 0.6841 0.0756 0.3456 0.041 Uiso 1 1 calc R . . . .
H40B H 0.6893 -0.0249 0.3536 0.041 Uiso 1 1 calc R . . . .
C42 C 0.2658(4) -0.0599(5) 0.0725(3) 0.041(2) Uani 1 1 d . . . . .
H42A H 0.2803 -0.0450 0.0375 0.050 Uiso 1 1 calc R . . . .
H42B H 0.2138 -0.0774 0.0652 0.050 Uiso 1 1 calc R . . . .
C45 C 0.7283(4) 0.0409(5) 0.4245(4) 0.046(2) Uani 1 1 d . . . . .
H45A H 0.7239 -0.0080 0.4482 0.056 Uiso 1 1 calc R . . . .
H45B H 0.7795 0.0437 0.4184 0.056 Uiso 1 1 calc R . . . .
C46 C 0.6487(4) 0.0911(5) 0.0683(3) 0.040(2) Uani 1 1 d . . . . .
H46A H 0.6930 0.0610 0.0864 0.048 Uiso 1 1 calc R . . . .
H46B H 0.6615 0.1223 0.0370 0.048 Uiso 1 1 calc R . . . .
C0BA C -0.0646(3) 0.2199(4) 0.1408(3) 0.0223(15) Uani 1 1 d . . . . .
H0BA H -0.0925 0.1967 0.1682 0.027 Uiso 1 1 calc R . . . .
C8AA C -0.0088(4) 0.3034(4) 0.2670(3) 0.0319(17) Uani 1 1 d . . . . .
H8AA H -0.0592 0.2829 0.2540 0.038 Uiso 1 1 calc R . . . .
H8AB H -0.0116 0.3544 0.2894 0.038 Uiso 1 1 calc R . . . .
C2AA C 0.1259(3) 0.2800(4) 0.3430(3) 0.0239(15) Uani 1 1 d . . . . .
H2AA H 0.1481 0.3066 0.3135 0.029 Uiso 1 1 calc R . . . .
C3AA C 0.1856(4) 0.2253(4) 0.3737(3) 0.0311(17) Uani 1 1 d . . . . .
H3AA H 0.1967 0.1784 0.3503 0.037 Uiso 1 1 calc R . . . .
H3AB H 0.1692 0.2007 0.4057 0.037 Uiso 1 1 calc R . . . .
C7AA C 0.0276(4) 0.3246(4) 0.2197(3) 0.0335(18) Uani 1 1 d . . . . .
H7AA H 0.0780 0.3448 0.2329 0.040 Uiso 1 1 calc R . . . .
H7AB H 0.0003 0.3704 0.1981 0.040 Uiso 1 1 calc R . . . .
C4AA C 0.1776(4) 0.4059(5) 0.3974(3) 0.043(2) Uani 1 1 d . . . . .
H4AA H 0.1930 0.4344 0.3661 0.052 Uiso 1 1 calc R . . . .
H4AB H 0.1663 0.4501 0.4225 0.052 Uiso 1 1 calc R . . . .
C7BA C 0.1083(4) 0.3534(4) 0.3776(3) 0.0364(19) Uani 1 1 d . . . . .
H7BA H 0.0885 0.3315 0.4090 0.044 Uiso 1 1 calc R . . . .
H7BB H 0.0705 0.3897 0.3561 0.044 Uiso 1 1 calc R . . . .
C9AA C -0.0145(4) 0.1863(5) 0.3551(3) 0.0335(18) Uani 1 1 d . . . . .
H9AA H -0.0467 0.1412 0.3358 0.040 Uiso 1 1 calc R . . . .
C5AA C 0.2400(4) 0.3513(5) 0.4259(3) 0.041(2) Uani 1 1 d . . . . .
H5AA H 0.2850 0.3859 0.4344 0.050 Uiso 1 1 calc R . . . .
H5AB H 0.2278 0.3301 0.4603 0.050 Uiso 1 1 calc R . . . .
C6AA C 0.2538(4) 0.2780(5) 0.3914(3) 0.042(2) Uani 1 1 d . . . . .
H6AA H 0.2925 0.2419 0.4120 0.051 Uiso 1 1 calc R . . . .
H6AB H 0.2718 0.2992 0.3591 0.051 Uiso 1 1 calc R . . . .
C1BA C 0.0914(5) 0.2668(5) 0.1314(4) 0.053(3) Uani 1 1 d . . . . .
H1BA H 0.1352 0.2831 0.1585 0.063 Uiso 1 1 calc R . . . .
C21 C 0.7099(4) 0.1218(5) 0.4523(4) 0.049(2) Uani 1 1 d . . . . .
H21A H 0.7421 0.1269 0.4880 0.059 Uiso 1 1 calc R . . . .
H21B H 0.7189 0.1713 0.4302 0.059 Uiso 1 1 calc R . . . .
C22 C -0.1041(4) 0.3012(4) 0.1210(4) 0.043(2) Uani 1 1 d . . . . .
H22A H -0.1020 0.3410 0.1517 0.052 Uiso 1 1 calc R . . . .
H22B H -0.0791 0.3280 0.0936 0.052 Uiso 1 1 calc R . . . .
C23 C -0.0659(4) 0.2526(6) 0.3714(3) 0.050(2) Uani 1 1 d . . . . .
H23A H -0.0368 0.2965 0.3936 0.060 Uiso 1 1 calc R . . . .
H23B H -0.0929 0.2801 0.3385 0.060 Uiso 1 1 calc R . . . .
C27 C 0.0260(4) 0.1455(5) 0.4062(4) 0.045(2) Uani 1 1 d . . . . .
H27A H 0.0557 0.1887 0.4286 0.055 Uiso 1 1 calc R . . . .
H27B H 0.0596 0.1018 0.3966 0.055 Uiso 1 1 calc R . . . .
C2BA C -0.0732(4) 0.1549(4) 0.0963(3) 0.045(2) Uani 1 1 d . . . . .
H2BA H -0.0506 0.1011 0.1107 0.054 Uiso 1 1 calc R . . . .
H2BB H -0.0476 0.1744 0.0671 0.054 Uiso 1 1 calc R . . . .
C34 C -0.0270(6) 0.1051(6) 0.4390(4) 0.067(3) Uani 1 1 d . . . . .
H34A H -0.0540 0.0586 0.4178 0.081 Uiso 1 1 calc R . . . .
H34B H 0.0008 0.0807 0.4727 0.081 Uiso 1 1 calc R . . . .
C38 C 0.0760(7) 0.3478(6) 0.1033(5) 0.084(4) Uani 1 1 d . . . . .
H38A H 0.0655 0.3905 0.1297 0.100 Uiso 1 1 calc R . . . .
H38B H 0.0315 0.3416 0.0755 0.100 Uiso 1 1 calc R . . . .
C3BA C 0.1246(6) 0.2031(6) 0.1009(4) 0.076(3) Uani 1 1 d . . . . .
H3BA H 0.0866 0.1791 0.0723 0.092 Uiso 1 1 calc R . . . .
H3BB H 0.1444 0.1566 0.1255 0.092 Uiso 1 1 calc R . . . .
C43 C 0.1887(6) 0.2427(6) 0.0740(5) 0.075(3) Uani 1 1 d . . . . .
H43A H 0.2320 0.2515 0.1025 0.091 Uiso 1 1 calc R . . . .
H43B H 0.2024 0.2016 0.0478 0.091 Uiso 1 1 calc R . . . .
Cl1 Cl -0.19944(15) 0.18908(16) 0.24531(12) 0.0522(10) Uani 0.796(6) 1 d . . P
A 1
Cl2 Cl -0.2178(4) 0.3688(3) 0.2577(3) 0.0645(18) Uani 0.796(6) 1 d . . P A 1
Cl3 Cl 0.3826(4) 0.1392(3) 0.5049(2) 0.097(2) Uani 0.877(10) 1 d . . P B 1
Cl4 Cl 0.4621(3) 0.2832(3) 0.48047(16) 0.103(2) Uani 0.877(10) 1 d . . P B 1
C4BA C -0.1903(4) 0.2209(4) 0.0521(3) 0.0339(18) Uani 1 1 d . . . . .
H4BA H -0.1672 0.2428 0.0222 0.041 Uiso 1 1 calc R . . . .
H4BB H -0.2426 0.2101 0.0379 0.041 Uiso 1 1 calc R . . . .
C5BA C -0.1831(4) 0.2842(6) 0.0966(4) 0.049(2) Uani 1 1 d . . . . .
H5BA H -0.2093 0.2634 0.1251 0.059 Uiso 1 1 calc R . . . .
H5BB H -0.2065 0.3377 0.0823 0.059 Uiso 1 1 calc R . . . .
C6BA C -0.1535(5) 0.1405(5) 0.0735(4) 0.063(3) Uani 1 1 d . . . . .
H6BA H -0.1579 0.0983 0.0441 0.076 Uiso 1 1 calc R . . . .
H6BB H -0.1783 0.1176 0.1023 0.076 Uiso 1 1 calc R . . . .
C16 C -0.0803(5) 0.1691(6) 0.4527(4) 0.058(3) Uani 1 1 d . . . . .
H16A H -0.0538 0.2109 0.4782 0.070 Uiso 1 1 calc R . . . .
H16B H -0.1165 0.1404 0.4711 0.070 Uiso 1 1 calc R . . . .
C19 C -0.1201(5) 0.2147(7) 0.4033(4) 0.067(3) Uani 1 1 d . . . . .
H19A H -0.1509 0.2600 0.4147 0.081 Uiso 1 1 calc R . . . .
H19B H -0.1524 0.1746 0.3802 0.081 Uiso 1 1 calc R . . . .
C9BA C -0.2559(6) 0.2659(7) 0.2533(6) 0.095(4) Uani 1 1 d . . . . .
H9BA H -0.2760 0.2548 0.2867 0.114 Uiso 0.796(6) 1 calc R . P A 1
H9BB H -0.2973 0.2646 0.2226 0.114 Uiso 0.796(6) 1 calc R . P A 1
C31 C 0.4167(8) 0.2368(7) 0.5252(5) 0.109(5) Uani 1 1 d . . . . .
H31A H 0.3758 0.2739 0.5309 0.130 Uiso 0.877(10) 1 calc R . P B 1
H31B H 0.4501 0.2311 0.5603 0.130 Uiso 0.877(10) 1 calc R . P B 1
H31 H 0.4160 0.2296 0.5627 0.130 Uiso 0.123(10) 1 calc R . P B 2
C0CA C 0.1703(7) 0.3209(7) 0.0468(5) 0.092(4) Uani 1 1 d . . . . .
H0CA H 0.1798 0.3322 0.0115 0.110 Uiso 1 1 calc R . . . .
C1CA C 0.1371(7) 0.3799(8) 0.0765(6) 0.122(6) Uani 1 1 d . . . . .
H1CA H 0.1525 0.4372 0.0796 0.146 Uiso 1 1 calc R . . . .
Cl1A Cl -0.2525(7) 0.1993(7) 0.2982(6) 0.073(5) Uani 0.204(6) 1 d . . P A 2
Cl2A Cl -0.2083(14) 0.3516(18) 0.2399(10) 0.068(7) Uani 0.204(6) 1 d . . P A 2
Cl4A Cl 0.4153(18) 0.3120(14) 0.5139(14) 0.098(13) Uani 0.123(10) 1 d . U P B 2
Cl3A Cl 0.4196(19) 0.134(2) 0.4927(15) 0.070(10) Uani 0.123(10) 1 d . . P B 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 Br4 2.4783(7) . ?
W1 Br7 2.4788(7) . ?
W1 Br9 2.7248(7) . ?
W1 P2 2.5938(17) . ?
W1 P5 2.5717(17) . ?
W1 C18 1.813(7) . ?
W2 Br3 2.6918(6) . ?
W2 Br5 2.5016(7) . ?
W2 Br6 2.4800(7) . ?
W2 P3 2.5862(16) . ?
W2 P4 2.5734(16) . ?
W2 C1AA 1.793(6) . ?
Br10 C18 1.794(7) . ?
Br1 C1AA 1.822(6) . ?
P2 C8AA 1.837(7) . ?
P2 C2AA 1.859(6) . ?
P2 C9AA 1.849(7) . ?
P3 C12 1.842(6) . ?
P3 C8BA 1.850(7) . ?
P3 C20 1.866(6) . ?
P4 C13 1.802(6) . ?
P4 C9 1.856(7) . ?
P4 C15 1.861(6) . ?
P5 C0BA 1.850(6) . ?
P5 C7AA 1.822(7) . ?
P5 C1BA 1.840(8) . ?
C12 C13 1.510(9) . ?
C9 C30 1.523(9) . ?
C9 C40 1.518(9) . ?
C10 C8BA 1.530(9) . ?
C10 C36 1.518(9) . ?
C11 C14 1.530(9) . ?
C11 C24 1.528(9) . ?
C14 C15 1.530(9) . ?
C15 C17 1.527(8) . ?
C17 C26 1.531(9) . ?
C0AA C20 1.528(9) . ?
C0AA C39 1.531(9) . ?
C8BA C28 1.531(9) . ?
C20 C37 1.531(9) . ?
C24 C26 1.509(10) . ?
C25 C28 1.531(9) . ?
C25 C46 1.512(10) . ?
C29 C37 1.528(9) . ?
C29 C42 1.511(10) . ?
C30 C32 1.533(10) . ?
C32 C21 1.503(11) . ?
C36 C46 1.524(10) . ?
C39 C42 1.515(10) . ?
C40 C45 1.529(10) . ?
C45 C21 1.526(10) . ?
C0BA C22 1.521(9) . ?
C0BA C2BA 1.508(9) . ?
C8AA C7AA 1.505(10) . ?
C2AA C3AA 1.509(9) . ?
C2AA C7BA 1.519(9) . ?
C3AA C6AA 1.517(9) . ?
C4AA C7BA 1.541(10) . ?
C4AA C5AA 1.522(11) . ?
C9AA C23 1.522(10) . ?
C9AA C27 1.515(11) . ?
C5AA C6AA 1.495(10) . ?
C1BA C38 1.468(11) . ?
C1BA C3BA 1.464(12) . ?
C22 C5BA 1.514(10) . ?
C23 C19 1.514(12) . ?
C27 C34 1.529(10) . ?
C2BA C6BA 1.520(10) . ?
C34 C16 1.498(12) . ?
C38 C1CA 1.506(13) . ?
C3BA C43 1.597(13) . ?
C43 C0CA 1.426(14) . ?
Cl1 C9BA 1.641(11) . ?
Cl2 C9BA 1.772(12) . ?
Cl3 C31 1.714(12) . ?
Cl4 C31 1.686(12) . ?
C4BA C5BA 1.488(11) . ?
C4BA C6BA 1.500(10) . ?
C16 C19 1.513(13) . ?
C9BA Cl1A 1.536(16) . ?
C9BA Cl2A 1.69(3) . ?
C31 Cl4A 1.22(2) . ?
C31 Cl3A 1.82(3) . ?
C0CA C1CA 1.403(15) . ?

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
Br4 W1 Br7 104.34(2) . . ?
Br4 W1 Br9 86.08(2) . . ?
Br4 W1 P2 86.31(4) . . ?
Br4 W1 P5 163.67(4) . . ?
Br7 W1 Br9 84.51(2) . . ?
Br7 W1 P2 164.38(4) . . ?
Br7 W1 P5 90.94(4) . . ?
P2 W1 Br9 84.86(4) . . ?
P5 W1 Br9 89.72(4) . . ?
P5 W1 P2 77.59(6) . . ?
C18 W1 Br4 97.06(19) . . ?
C18 W1 Br7 96.5(2) . . ?
C18 W1 Br9 176.32(18) . . ?
C18 W1 P2 93.4(2) . . ?
C18 W1 P5 86.73(19) . . ?
Br5 W2 Br3 84.76(2) . . ?
Br5 W2 P3 159.80(4) . . ?
Br5 W2 P4 84.92(4) . . ?
Br6 W2 Br3 84.10(2) . . ?
Br6 W2 Br5 109.35(2) . . ?
Br6 W2 P3 88.42(4) . . ?
Br6 W2 P4 163.91(4) . . ?
P3 W2 Br3 87.74(4) . . ?
P4 W2 Br3 90.06(4) . . ?
P4 W2 P3 76.35(5) . . ?
C1AA W2 Br3 176.6(2) . . ?
C1AA W2 Br5 94.1(2) . . ?
C1AA W2 Br6 93.2(2) . . ?
C1AA W2 P3 94.3(2) . . ?
C1AA W2 P4 93.1(2) . . ?
C8AA P2 W1 107.3(2) . . ?
C8AA P2 C2AA 103.1(3) . . ?
C8AA P2 C9AA 103.9(3) . . ?
C2AA P2 W1 112.6(2) . . ?
C9AA P2 W1 117.1(2) . . ?
C9AA P2 C2AA 111.3(3) . . ?
C12 P3 W2 109.6(2) . . ?
C12 P3 C8BA 103.1(3) . . ?
C12 P3 C20 100.5(3) . . ?
C8BA P3 W2 118.0(2) . . ?
C8BA P3 C20 105.9(3) . . ?
C20 P3 W2 117.4(2) . . ?
C13 P4 W2 105.6(2) . . ?
C13 P4 C9 105.6(3) . . ?
C13 P4 C15 106.0(3) . . ?
C9 P4 W2 117.7(2) . . ?
C9 P4 C15 108.0(3) . . ?
C15 P4 W2 113.0(2) . . ?
C0BA P5 W1 115.8(2) . . ?
C7AA P5 W1 106.9(2) . . ?
C7AA P5 C0BA 104.4(3) . . ?
C7AA P5 C1BA 101.8(4) . . ?
C1BA P5 W1 115.3(2) . . ?
C1BA P5 C0BA 111.0(4) . . ?
C13 C12 P3 111.7(4) . . ?
C12 C13 P4 109.7(4) . . ?
Br10 C18 W1 177.6(4) . . ?
C30 C9 P4 111.6(5) . . ?
C40 C9 P4 113.3(5) . . ?
C40 C9 C30 110.2(5) . . ?
C36 C10 C8BA 110.6(5) . . ?
C24 C11 C14 111.5(5) . . ?
W2 C1AA Br1 171.5(4) . . ?
C15 C14 C11 110.0(5) . . ?
C14 C15 P4 111.8(4) . . ?
C17 C15 P4 117.4(4) . . ?
C17 C15 C14 110.7(5) . . ?
C15 C17 C26 109.0(5) . . ?
C20 C0AA C39 110.4(6) . . ?
C10 C8BA P3 115.5(4) . . ?
C10 C8BA C28 109.0(5) . . ?
C28 C8BA P3 113.7(5) . . ?
C0AA C20 P3 116.6(4) . . ?
C0AA C20 C37 109.6(6) . . ?
C37 C20 P3 113.3(4) . . ?
C26 C24 C11 111.5(6) . . ?
C46 C25 C28 112.1(6) . . ?
C24 C26 C17 111.9(6) . . ?
C25 C28 C8BA 110.1(6) . . ?
C42 C29 C37 112.2(6) . . ?
C9 C30 C32 111.2(6) . . ?
C21 C32 C30 111.3(7) . . ?
C10 C36 C46 110.3(6) . . ?
C29 C37 C20 109.3(6) . . ?
C42 C39 C0AA 111.8(6) . . ?
C9 C40 C45 110.2(6) . . ?
C29 C42 C39 111.0(6) . . ?
C21 C45 C40 111.1(6) . . ?
C25 C46 C36 110.9(6) . . ?
C22 C0BA P5 116.2(5) . . ?
C2BA C0BA P5 113.8(5) . . ?
C2BA C0BA C22 110.6(6) . . ?
C7AA C8AA P2 108.6(5) . . ?
C3AA C2AA P2 114.8(4) . . ?
C3AA C2AA C7BA 111.0(6) . . ?
C7BA C2AA P2 114.9(5) . . ?
C2AA C3AA C6AA 109.7(6) . . ?
C8AA C7AA P5 110.1(5) . . ?
C5AA C4AA C7BA 111.8(6) . . ?
C2AA C7BA C4AA 110.3(6) . . ?
C23 C9AA P2 116.2(6) . . ?
C27 C9AA P2 114.3(5) . . ?
C27 C9AA C23 107.9(6) . . ?
C6AA C5AA C4AA 111.2(7) . . ?
C5AA C6AA C3AA 112.2(6) . . ?
C38 C1BA P5 118.4(6) . . ?
C3BA C1BA P5 118.7(6) . . ?
C3BA C1BA C38 114.6(8) . . ?
C32 C21 C45 110.9(6) . . ?
C5BA C22 C0BA 111.1(6) . . ?
C19 C23 C9AA 112.0(7) . . ?
C9AA C27 C34 111.3(7) . . ?
C0BA C2BA C6BA 110.6(7) . . ?
C16 C34 C27 110.7(7) . . ?
C1BA C38 C1CA 114.2(9) . . ?
C1BA C3BA C43 111.3(8) . . ?
C0CA C43 C3BA 114.2(9) . . ?
C5BA C4BA C6BA 109.0(7) . . ?
C4BA C5BA C22 112.2(6) . . ?
C4BA C6BA C2BA 111.3(6) . . ?
C34 C16 C19 112.5(8) . . ?
C16 C19 C23 110.4(7) . . ?
Cl1 C9BA Cl2 115.6(6) . . ?
Cl1A C9BA Cl2A 138.0(13) . . ?
Cl4 C31 Cl3 113.3(7) . . ?
Cl4A C31 Cl3A 140(2) . . ?
C1CA C0CA C43 114.5(10) . . ?
C0CA C1CA C38 116.6(10) . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 0.000 133.1 28.7 ?
2 0.000 0.500 0.500 133.1 28.7 ?
3 0.156 0.006 0.459 40.0 0.0 ?
4 0.156 0.494 0.959 40.0 0.0 ?
5 0.143 -0.027 0.655 10.6 0.0 ?
6 0.143 0.527 0.155 10.6 0.0 ?
7 0.500 0.000 0.500 11.7 0.0 ?
8 0.500 0.500 0.000 11.7 0.0 ?
9 0.844 0.506 0.041 40.0 1.3 ?
10 0.844 0.994 0.541 40.0 1.3 ?
11 0.857 0.027 0.345 10.6 0.0 ?
12 0.857 0.473 0.845 10.6 0.0 ?



_ins_header                      
;
TITL RK11_scaled2 in P2(1)/c 
REM P2(1)/c (#14 in standard setting)
CELL 0.71073  18.572260  15.829825  25.117115  90.0000 100.0005  90.0000
ZERR   11.00   0.000338   0.000265   0.000636   0.0000   0.0021   0.0000
LATT  1
SYMM -x, y+1/2,-z+1/2 
SFAC C H O P Br W
UNIT 319.00 528.00 22.00 22.00 22.00 11.00
TREF
HKLF 4
END
;
_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 1.496
_oxdiff_exptl_absorpt_empirical_full_min 0.852

