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

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

data_ram-16_scale
_database_code_depnum_ccdc_archive 'CCDC 1897108'
loop_
_audit_author_name
_audit_author_address
'Richard Manzano'
;Australian National University
Australia
;
_audit_update_record             
;
2019-02-14 deposited with the CCDC.	2019-04-23 downloaded from the CCDC.
;
_audit_creation_date             2018-09-05
_audit_creation_method           
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
a.hill@anu.edu.au
richard.manzano@anu.edu.au
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C24 H31 B N6 O2 W'
_chemical_formula_sum            'C24 H31 B N6 O2 W'
_chemical_formula_weight         630.21
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C24 H31 B1 N6 O2 W1'
_chemical_oxdiff_usercomment     'Red crystal blocks'
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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   15.2849(2)
_cell_length_b                   16.5974(2)
_cell_length_c                   20.0536(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5087.39(10)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    36889
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      29.4570
_cell_measurement_theta_min      3.5460
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    4.574
_exptl_absorpt_correction_T_max  0.724
_exptl_absorpt_correction_T_min  0.512
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.646
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2496
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
13 -3 23 0.0835
1 -4 28 0.0767
-16 -4 19 0.0787
3 5 -27 0.0423
20 -9 0 0.1016
15 -16 -2 0.1121
-18 -12 -5 0.1120
-21 -4 -4 0.1083
-12 19 3 0.1470
9 20 6 0.0964

_exptl_crystal_preparation       
'Red crystals were obtained from vapour-vapour diffusion of pentane into a DCM solution'
_exptl_crystal_recrystallization_method 
'Red crystals were obtained from vapour-vapour diffusion of n-pentane into a DCM solution'
_exptl_crystal_size_max          0.318
_exptl_crystal_size_mid          0.244
_exptl_crystal_size_min          0.125
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
12.6936 -2.7034 22.6174 -0.2108 0.7136 0.6681
1.1267 -4.4104 27.7340 -0.2806 0.9478 0.1518
-15.6447 -4.2282 18.7600 -0.2149 0.7237 -0.6558
3.2245 4.6836 -27.3825 0.2837 -0.9576 0.0506
19.7586 -9.3195 0.3829 -0.4311 -0.1269 0.8933
15.3741 -16.3105 -1.9269 -0.7134 -0.2107 0.6683
-17.8635 -12.2892 -5.4336 -0.4745 -0.1413 -0.8689
-21.0542 -3.8572 -3.7942 -0.1159 -0.0352 -0.9926
-12.3429 19.0130 3.0004 0.8197 0.2423 -0.5191
9.2486 20.4852 6.2815 0.8349 0.2477 0.4916

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0518
_diffrn_reflns_av_unetI/netI     0.0251
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            106944
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.694
_diffrn_reflns_theta_min         3.352
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3744
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -39.00  62.00   1.00   10.00    --  -11.22  57.00  30.00  101
  2  ω    -87.00  21.00   1.00   10.00    --  -11.22 -77.00 120.00  108
  3  ω    -39.00  62.00   1.00   10.00    --  -11.22  57.00 -60.00  101
  4  ω    -83.00  17.00   1.00   10.00    --  -11.22 -57.00-120.00  100
  5  ω    -20.00  30.00   1.00   10.00    --  -11.22 -99.00 -30.00   50
  6  ω    -86.00  13.00   1.00   10.00    --  -11.22 -37.00 -30.00   99
  7  ω     34.00  98.00   1.00   10.00    --   11.30-178.00-180.00   64
  8  ω     -1.00  42.00   1.00   10.00    --   11.30-121.00-126.00   43
  9  ω    -61.00  39.00   1.00   10.00    --   11.30 -57.00-180.00  100
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, Atlas'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0016968000
_diffrn_orient_matrix_UB_12      0.0425278000
_diffrn_orient_matrix_UB_13      -0.0032845000
_diffrn_orient_matrix_UB_21      -0.0053236000
_diffrn_orient_matrix_UB_22      0.0037664000
_diffrn_orient_matrix_UB_23      0.0349882000
_diffrn_orient_matrix_UB_31      0.0460759000
_diffrn_orient_matrix_UB_32      0.0019926000
_diffrn_orient_matrix_UB_33      0.0039182000
_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'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5341
_reflns_number_total             6535
_reflns_odcompleteness_completeness 99.64
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.730
_refine_diff_density_min         -0.475
_refine_diff_density_rms         0.097
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         6535
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0366
_refine_ls_R_factor_gt           0.0246
_refine_ls_restrained_S_all      1.053
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0145P)²+6.5612P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0437
_refine_ls_wR_factor_ref         0.0468
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 B1(H1)
2.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C14(H14), C17(H17)
2.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C19(H19A,H19B,H19C),
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,
 H23C), C24(H24A,H24B,H24C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.41515(2) 0.67940(2) 0.64109(2) 0.01603(4) Uani 1 1 d . . . . .
O1 O 0.43592(14) 0.75827(13) 0.78259(10) 0.0333(5) Uani 1 1 d . . . . .
O2 O 0.21679(13) 0.72801(14) 0.65083(11) 0.0372(5) Uani 1 1 d . . . . .
N1 N 0.44404(14) 0.79395(12) 0.58130(11) 0.0185(4) Uani 1 1 d . . . . .
N2 N 0.48937(13) 0.78681(12) 0.52233(11) 0.0166(4) Uani 1 1 d . . . . .
N3 N 0.55705(14) 0.65888(12) 0.62583(10) 0.0163(4) Uani 1 1 d . . . . .
N4 N 0.59622(13) 0.68554(12) 0.56813(11) 0.0172(4) Uani 1 1 d . . . . .
N5 N 0.41038(14) 0.62430(12) 0.54117(11) 0.0186(4) Uani 1 1 d . . . . .
N6 N 0.47388(14) 0.63991(12) 0.49444(10) 0.0181(4) Uani 1 1 d . . . . .
C1 C 0.38357(17) 0.59352(15) 0.69357(13) 0.0201(5) Uani 1 1 d . . . . .
C2 C 0.35795(17) 0.53501(16) 0.73800(14) 0.0223(6) Uani 1 1 d . . . . .
C3 C 0.33890(17) 0.48083(16) 0.77565(14) 0.0228(6) Uani 1 1 d . . . . .
C4 C 0.32357(17) 0.41259(16) 0.82123(14) 0.0223(6) Uani 1 1 d . . . . .
C5 C 0.43026(17) 0.73233(15) 0.72955(14) 0.0218(6) Uani 1 1 d . . . . .
C6 C 0.28914(18) 0.71026(17) 0.64612(14) 0.0233(6) Uani 1 1 d . . . . .
C7 C 0.3408(2) 0.43951(19) 0.89278(15) 0.0329(7) Uani 1 1 d . . . . .
H7A H 0.400544 0.456740 0.896944 0.049 Uiso 1 1 calc GR . . . .
H7B H 0.330262 0.395343 0.922621 0.049 Uiso 1 1 calc GR . . . .
H7C H 0.302563 0.483399 0.903804 0.049 Uiso 1 1 calc GR . . . .
C8 C 0.3878(2) 0.34601(18) 0.80207(18) 0.0376(8) Uani 1 1 d . . . . .
H8A H 0.375964 0.328505 0.757334 0.056 Uiso 1 1 calc GR . . . .
H8B H 0.381222 0.301383 0.832109 0.056 Uiso 1 1 calc GR . . . .
H8C H 0.446495 0.366279 0.804703 0.056 Uiso 1 1 calc GR . . . .
C9 C 0.22961(19) 0.3824(2) 0.81416(16) 0.0366(8) Uani 1 1 d . . . . .
H9A H 0.189752 0.425866 0.822735 0.055 Uiso 1 1 calc GR . . . .
H9B H 0.219424 0.339769 0.845581 0.055 Uiso 1 1 calc GR . . . .
H9C H 0.220619 0.362541 0.769718 0.055 Uiso 1 1 calc GR . . . .
C10 C 0.41345(16) 0.86993(14) 0.58325(13) 0.0173(5) Uani 1 1 d . . . . .
C11 C 0.43690(16) 0.91006(15) 0.52520(13) 0.0195(5) Uani 1 1 d . . . . .
H11 H 0.423090 0.962885 0.513871 0.023 Uiso 1 1 calc R . . . .
C12 C 0.48463(16) 0.85624(15) 0.48769(13) 0.0176(5) Uani 1 1 d . . . . .
C13 C 0.62124(18) 0.63590(15) 0.66689(14) 0.0207(6) Uani 1 1 d . . . . .
C14 C 0.70186(18) 0.64814(16) 0.63604(14) 0.0232(6) Uani 1 1 d . . . . .
H14 H 0.756756 0.636825 0.653705 0.028 Uiso 1 1 calc R . . . .
C15 C 0.68417(17) 0.68017(15) 0.57448(14) 0.0215(5) Uani 1 1 d . . . . .
C16 C 0.36245(17) 0.56282(16) 0.51713(14) 0.0229(6) Uani 1 1 d . . . . .
C17 C 0.39613(18) 0.53832(16) 0.45608(14) 0.0253(6) Uani 1 1 d . . . . .
H17 H 0.375723 0.496441 0.429476 0.030 Uiso 1 1 calc R . . . .
C18 C 0.46573(18) 0.58839(15) 0.44283(13) 0.0216(6) Uani 1 1 d . . . . .
C19 C 0.36262(18) 0.90132(16) 0.64118(14) 0.0253(6) Uani 1 1 d . . . . .
H19A H 0.304189 0.880179 0.639724 0.038 Uiso 1 1 calc GR . . . .
H19B H 0.360574 0.959075 0.639188 0.038 Uiso 1 1 calc GR . . . .
H19C H 0.390383 0.884894 0.681913 0.038 Uiso 1 1 calc GR . . . .
C20 C 0.52494(19) 0.86641(16) 0.42025(14) 0.0263(6) Uani 1 1 d . . . . .
H20A H 0.587259 0.860520 0.423632 0.039 Uiso 1 1 calc GR . . . .
H20B H 0.511289 0.919028 0.403299 0.039 Uiso 1 1 calc GR . . . .
H20C H 0.502134 0.826226 0.390529 0.039 Uiso 1 1 calc GR . . . .
C21 C 0.60395(19) 0.60360(17) 0.73523(14) 0.0289(6) Uani 1 1 d . . . . .
H21A H 0.586772 0.646903 0.764139 0.043 Uiso 1 1 calc GR . . . .
H21B H 0.656102 0.578790 0.752274 0.043 Uiso 1 1 calc GR . . . .
H21C H 0.557891 0.564358 0.733168 0.043 Uiso 1 1 calc GR . . . .
C22 C 0.74550(19) 0.70815(18) 0.52123(15) 0.0313(7) Uani 1 1 d . . . . .
H22A H 0.735020 0.678159 0.481086 0.047 Uiso 1 1 calc GR . . . .
H22B H 0.804755 0.699811 0.535537 0.047 Uiso 1 1 calc GR . . . .
H22C H 0.736125 0.764443 0.512878 0.047 Uiso 1 1 calc GR . . . .
C23 C 0.28501(19) 0.53018(18) 0.55334(16) 0.0321(7) Uani 1 1 d . . . . .
H23A H 0.302384 0.513082 0.597115 0.048 Uiso 1 1 calc GR . . . .
H23B H 0.261632 0.485102 0.529218 0.048 Uiso 1 1 calc GR . . . .
H23C H 0.241149 0.571341 0.557019 0.048 Uiso 1 1 calc GR . . . .
C24 C 0.5242(2) 0.58998(18) 0.38305(15) 0.0316(7) Uani 1 1 d . . . . .
H24A H 0.505983 0.632322 0.353548 0.047 Uiso 1 1 calc GR . . . .
H24B H 0.520802 0.539214 0.360268 0.047 Uiso 1 1 calc GR . . . .
H24C H 0.583434 0.599444 0.396974 0.047 Uiso 1 1 calc GR . . . .
B1 B 0.54003(19) 0.70797(17) 0.50703(15) 0.0189(6) Uani 1 1 d . . . . .
H1 H 0.577395 0.715394 0.467794 0.023 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 N1 2.291(2) . ?
W1 N3 2.217(2) . ?
W1 N5 2.204(2) . ?
W1 C1 1.836(3) . ?
W1 C5 1.993(3) . ?
W1 C6 1.996(3) . ?
O1 C5 1.151(3) . ?
O2 C6 1.148(3) . ?
N1 N2 1.376(3) . ?
N1 C10 1.346(3) . ?
N2 C12 1.348(3) . ?
N2 B1 1.551(3) . ?
N3 N4 1.376(3) . ?
N3 C13 1.336(3) . ?
N4 C15 1.353(3) . ?
N4 B1 1.542(4) . ?
N5 N6 1.374(3) . ?
N5 C16 1.345(3) . ?
N6 C18 1.348(3) . ?
N6 B1 1.537(4) . ?
C1 C2 1.375(4) . ?
C2 C3 1.210(4) . ?
C3 C4 1.474(4) . ?
C4 C7 1.526(4) . ?
C4 C8 1.527(4) . ?
C4 C9 1.528(4) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 C11 1.388(4) . ?
C10 C19 1.492(4) . ?
C11 H11 0.9300 . ?
C11 C12 1.377(4) . ?
C12 C20 1.496(4) . ?
C13 C14 1.394(4) . ?
C13 C21 1.495(4) . ?
C14 H14 0.9300 . ?
C14 C15 1.371(4) . ?
C15 C22 1.495(4) . ?
C16 C17 1.389(4) . ?
C16 C23 1.491(4) . ?
C17 H17 0.9300 . ?
C17 C18 1.376(4) . ?
C18 C24 1.496(4) . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
B1 H1 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 W1 N1 82.33(7) . . ?
N5 W1 N1 82.81(8) . . ?
N5 W1 N3 80.97(8) . . ?
C1 W1 N1 174.19(10) . . ?
C1 W1 N3 102.54(10) . . ?
C1 W1 N5 100.97(10) . . ?
C1 W1 C5 82.09(11) . . ?
C1 W1 C6 85.21(11) . . ?
C5 W1 N1 94.46(9) . . ?
C5 W1 N3 94.43(9) . . ?
C5 W1 N5 174.91(9) . . ?
C5 W1 C6 87.34(11) . . ?
C6 W1 N1 89.97(9) . . ?
C6 W1 N3 172.21(9) . . ?
C6 W1 N5 96.93(10) . . ?
N2 N1 W1 118.39(15) . . ?
C10 N1 W1 134.09(17) . . ?
C10 N1 N2 106.3(2) . . ?
N1 N2 B1 119.6(2) . . ?
C12 N2 N1 110.0(2) . . ?
C12 N2 B1 130.3(2) . . ?
N4 N3 W1 119.50(15) . . ?
C13 N3 W1 132.62(18) . . ?
C13 N3 N4 106.9(2) . . ?
N3 N4 B1 120.2(2) . . ?
C15 N4 N3 109.4(2) . . ?
C15 N4 B1 130.1(2) . . ?
N6 N5 W1 121.24(15) . . ?
C16 N5 W1 131.19(18) . . ?
C16 N5 N6 106.5(2) . . ?
N5 N6 B1 119.4(2) . . ?
C18 N6 N5 109.8(2) . . ?
C18 N6 B1 130.8(2) . . ?
C2 C1 W1 174.0(2) . . ?
C3 C2 C1 176.4(3) . . ?
C2 C3 C4 175.1(3) . . ?
C3 C4 C7 109.3(2) . . ?
C3 C4 C8 107.3(2) . . ?
C3 C4 C9 110.1(2) . . ?
C7 C4 C8 109.7(2) . . ?
C7 C4 C9 110.2(2) . . ?
C8 C4 C9 110.1(2) . . ?
O1 C5 W1 175.1(2) . . ?
O2 C6 W1 178.2(3) . . ?
C4 C7 H7A 109.5 . . ?
C4 C7 H7B 109.5 . . ?
C4 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C4 C8 H8A 109.5 . . ?
C4 C8 H8B 109.5 . . ?
C4 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C4 C9 H9A 109.5 . . ?
C4 C9 H9B 109.5 . . ?
C4 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N1 C10 C11 109.6(2) . . ?
N1 C10 C19 122.1(2) . . ?
C11 C10 C19 128.3(2) . . ?
C10 C11 H11 126.8 . . ?
C12 C11 C10 106.5(2) . . ?
C12 C11 H11 126.8 . . ?
N2 C12 C11 107.6(2) . . ?
N2 C12 C20 122.7(2) . . ?
C11 C12 C20 129.7(2) . . ?
N3 C13 C14 109.5(2) . . ?
N3 C13 C21 122.5(2) . . ?
C14 C13 C21 128.0(3) . . ?
C13 C14 H14 126.8 . . ?
C15 C14 C13 106.4(2) . . ?
C15 C14 H14 126.8 . . ?
N4 C15 C14 107.8(2) . . ?
N4 C15 C22 122.4(2) . . ?
C14 C15 C22 129.8(3) . . ?
N5 C16 C17 109.6(2) . . ?
N5 C16 C23 122.2(3) . . ?
C17 C16 C23 128.1(3) . . ?
C16 C17 H17 126.9 . . ?
C18 C17 C16 106.3(2) . . ?
C18 C17 H17 126.9 . . ?
N6 C18 C17 107.8(2) . . ?
N6 C18 C24 123.3(2) . . ?
C17 C18 C24 128.9(3) . . ?
C10 C19 H19A 109.5 . . ?
C10 C19 H19B 109.5 . . ?
C10 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C12 C20 H20A 109.5 . . ?
C12 C20 H20B 109.5 . . ?
C12 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C13 C21 H21A 109.5 . . ?
C13 C21 H21B 109.5 . . ?
C13 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C15 C22 H22A 109.5 . . ?
C15 C22 H22B 109.5 . . ?
C15 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C16 C23 H23A 109.5 . . ?
C16 C23 H23B 109.5 . . ?
C16 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C18 C24 H24A 109.5 . . ?
C18 C24 H24B 109.5 . . ?
C18 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N2 B1 H1 110.1 . . ?
N4 B1 N2 108.9(2) . . ?
N4 B1 H1 110.1 . . ?
N6 B1 N2 108.9(2) . . ?
N6 B1 N4 108.6(2) . . ?
N6 B1 H1 110.1 . . ?


_ins_header                      
;
TITL RAM-16_scale in Pbca 
REM Pbca (#61 in standard setting)
CELL 0.71073  15.284889  16.597387  20.053558  90.0000  90.0000  90.0000
ZERR    8.00   0.000183   0.000183   0.000249   0.0000   0.0000   0.0000
LATT  1
SYMM -x+1/2,-y, z+1/2 
SYMM -x, y+1/2,-z+1/2 
SYMM  x+1/2,-y+1/2,-z 
SFAC C H B N O W
UNIT 192.00 248.00 8.00 48.00 16.00 8.00
TREF
HKLF 4
END
;
_olex2_date_sample_submission    2018-09-05
_olex2_submission_original_sample_id W(C3)(CO)2(Tp*)
_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 1.116
_oxdiff_exptl_absorpt_empirical_full_min 0.926

####################################################################### 
# 
# 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_ram-069_scale
_database_code_depnum_ccdc_archive 'CCDC 1897689'
loop_
_audit_author_name
_audit_author_address
'Richard Manzano'
;Australian National University
Australia
;
_audit_update_record             
;
2019-02-18 deposited with the CCDC.	2019-04-23 downloaded from the CCDC.
;
_audit_creation_date             2019-02-18
_audit_creation_method           
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
a.hill@anu.edu.au
richard.manzano@anu.edu.au

# start Validation Reply Form
_vrf_PLAT213_ram-069_scale       
;
PROBLEM: Atom C1              has ADP max/min Ratio .....        4.1 oblate
RESPONSE: Despite multiple collections, the crystal supplied were found to be of 
consistently poor quality, which reduced the quality of the final model. 
However, the identity of the structure was clearly established.
;
_vrf_PLAT342_ram-069_scale       
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.02516 Ang.  
RESPONSE: Despite multiple collections, the crystal supplied were found to be of 
consistently poor quality, which reduced the quality of the final model. 
However, the identity of the structure was clearly established.
;
# end Validation Reply Form

_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C30 H31 B Fe N6 O2 W'
_chemical_formula_sum            'C30 H31 B Fe N6 O2 W'
_chemical_formula_weight         758.12
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C30 H31 B1 N6 O2 Fe1 W1'
_chemical_oxdiff_usercomment     'red needle'
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'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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                   10.0081(3)
_cell_length_b                   15.9662(5)
_cell_length_c                   18.8514(8)
_cell_angle_alpha                90
_cell_angle_beta                 92.404(4)
_cell_angle_gamma                90
_cell_volume                     3009.64(18)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4611
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      71.7550
_cell_measurement_theta_min      3.6140
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    11.125
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79017
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.673
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1496
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 -3 -12 0.0183
-5 6 -1 0.0417
5 -6 1 0.0227
-5 -7 -1 0.0301
5 7 1 0.0361
-1 -8 7 0.0115
1 8 -7 0.0125
-1 3 12 0.0083

_exptl_crystal_preparation       ?
_exptl_crystal_recrystallization_method 
'Red crystals grown from vapour-vapour diffusion of hexane into a DCM solution'
_exptl_crystal_size_max          0.084
_exptl_crystal_size_mid          0.037
_exptl_crystal_size_min          0.024
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
0.9913 -3.0130 -11.9889 0.2259 0.9558 -0.3049
-5.0046 5.9894 -0.9964 -0.7497 0.1814 0.5874
5.0046 -5.9894 0.9964 0.7497 -0.1814 -0.5874
-4.9925 -7.0047 -0.9599 -0.7676 0.1651 -0.6660
4.9925 7.0047 0.9599 0.7676 -0.1651 0.6660
-0.9856 -7.9885 7.0226 -0.2088 -0.5621 -0.7613
0.9856 7.9885 -7.0226 0.2088 0.5621 0.7613
-0.9913 3.0130 11.9889 -0.2259 -0.9558 0.3049

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0681
_diffrn_reflns_av_unetI/netI     0.0645
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            20882
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        66.584
_diffrn_reflns_theta_max         66.584
_diffrn_reflns_theta_min         4.696
_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 0.998
_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     29.00  94.00   1.00   18.00    --   35.53-133.00  51.00   65
  2  ω    -34.00 105.00   1.00   18.00    --   35.53   0.00  60.00  139
  3  ω      0.00  28.00   1.00   18.00    --   35.53  92.00 -40.49   28
  4  ω    -32.00  52.00   1.00   18.00    --   35.53 -57.00  30.00   84
  5  ω      9.00 103.00   1.00   18.00    --   35.53  77.00-120.00   94
  6  ω     23.00  89.00   1.00   18.00    --   35.53-125.00-180.00   66
  7  ω     38.00 116.00   1.00   65.00    --  108.00-111.00-120.00   78
  8  ω     40.00  98.00   1.00   65.00    --  108.00 -45.00 -60.00   58
  9  ω     40.00 135.00   1.00   65.00    --  108.00 -77.00  90.00   95
 10  ω     40.00  98.00   1.00   65.00    --  108.00 -45.00  60.00   58
 11  ω     40.00  98.00   1.00   65.00    --  108.00 -45.00-180.00   58
 12  ω     40.00  98.00   1.00   65.00    --  108.00 -45.00   0.00   58
 13  ω     38.00 116.00   1.00   65.00    --  108.00-111.00  60.00   78
 14  ω     40.00  98.00   1.00   65.00    --  108.00 -45.00-120.00   58
 15  ω     91.00 176.00   1.00   65.00    --  108.00  45.00-180.00   85
 16  ω     40.00 135.00   1.00   65.00    --  108.00 -77.00 -90.00   95
 17  ω     38.00  90.00   1.00   65.00    --  108.00 -30.00 150.00   52
 18  ω     39.00 177.00   1.00   65.00    --  108.00   0.00 -30.00  138
 19  ω    -34.00  54.00   1.00   18.00    --   35.53 -38.00-150.00   88
 20  ω     -2.00  24.00   1.00   18.00    --   35.53  96.00  69.29   26
 21  ω      6.00  95.00   1.00   18.00    --   35.53  19.00-150.00   89
 22  ω      9.00 103.00   1.00   18.00    --   35.53  77.00 120.00   94
;
_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      0.1529072000
_diffrn_orient_matrix_UB_12      0.0014985000
_diffrn_orient_matrix_UB_13      -0.0065726000
_diffrn_orient_matrix_UB_21      -0.0188079000
_diffrn_orient_matrix_UB_22      0.0010095000
_diffrn_orient_matrix_UB_23      -0.0815323000
_diffrn_orient_matrix_UB_31      -0.0021296000
_diffrn_orient_matrix_UB_32      0.0964550000
_diffrn_orient_matrix_UB_33      0.0010137000
_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                4533
_reflns_number_total             5301
_reflns_odcompleteness_completeness 99.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         4.997
_refine_diff_density_min         -3.160
_refine_diff_density_rms         0.231
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.299
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     368
_refine_ls_number_reflns         5301
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1014
_refine_ls_R_factor_gt           0.0886
_refine_ls_restrained_S_all      1.299
_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)+(0.0181P)²+109.4603P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1925
_refine_ls_wR_factor_ref         0.1972
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(N4) = Uanis(N6)
Uanis(C2) = Uanis(C1)
3.a Aromatic/amide H refined with riding coordinates:
 C22(H22), C27(H27), C7(H7), C11(H11), C17(H17), C8(H8), C10(H10), C14(H14),
 C15(H15), C9(H9), C12(H12), C13(H13)
3.b Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C29(H29A,H29B,H29C), C25(H25A,H25B,H25C), C19(H19A,H19B,
 H19C), C20(H20A,H20B,H20C), C30(H30A,H30B,H30C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.28849(6) 0.35387(4) 0.65012(3) 0.01681(19) Uani 1 1 d . . . . .
Fe1 Fe 0.7335(3) 0.63644(16) 0.81048(16) 0.0342(6) Uani 1 1 d . . . . .
N5 N 0.2750(12) 0.2170(7) 0.6696(6) 0.018(2) Uani 1 1 d . . . . .
N1 N 0.1150(12) 0.3273(7) 0.5721(7) 0.019(3) Uani 1 1 d . . . . .
N6 N 0.2526(11) 0.1624(6) 0.6144(6) 0.0148(17) Uani 1 1 d . . . . .
O2 O 0.0837(13) 0.4014(8) 0.7660(7) 0.044(3) Uani 1 1 d . . . . .
C21 C 0.5153(14) 0.3425(9) 0.5312(8) 0.022(3) Uani 1 1 d . . . . .
O1 O 0.2909(12) 0.5429(6) 0.6042(6) 0.033(3) Uani 1 1 d . . . . .
C1 C 0.4189(17) 0.3900(9) 0.7146(8) 0.026(2) Uani 1 1 d . . . . .
C5 C 0.2884(15) 0.4738(10) 0.6201(8) 0.024(3) Uani 1 1 d . . . . .
C22 C 0.5422(15) 0.2956(10) 0.4719(9) 0.030(4) Uani 1 1 d . . . . .
H22 H 0.611708 0.304088 0.441535 0.036 Uiso 1 1 calc R . . . .
N3 N 0.4054(11) 0.3119(7) 0.5602(6) 0.018(2) Uani 1 1 d . . . . .
N2 N 0.1173(12) 0.2547(7) 0.5315(6) 0.020(3) Uani 1 1 d . . . . .
C28 C 0.2464(14) 0.0842(8) 0.6414(8) 0.020(3) Uani 1 1 d . . . . .
C27 C 0.2613(16) 0.0879(9) 0.7127(8) 0.026(3) Uani 1 1 d . . . . .
H27 H 0.259490 0.043352 0.744366 0.031 Uiso 1 1 calc R . . . .
N4 N 0.3644(11) 0.2440(6) 0.5200(6) 0.0148(17) Uani 1 1 d . . . . .
C18 C 0.0053(16) 0.2509(10) 0.4895(8) 0.027(3) Uani 1 1 d . . . . .
C6 C 0.1613(18) 0.3830(10) 0.7232(10) 0.035(4) Uani 1 1 d . . . . .
C16 C 0.0025(15) 0.3675(10) 0.5529(8) 0.028(3) Uani 1 1 d . . . . .
C23 C 0.4477(17) 0.2350(10) 0.4666(8) 0.029(4) Uani 1 1 d . . . . .
C26 C 0.2803(15) 0.1732(8) 0.7294(8) 0.021(3) Uani 1 1 d . . . . .
C24 C 0.5883(15) 0.4173(11) 0.5618(9) 0.031(4) Uani 1 1 d . . . . .
H24A H 0.623080 0.404284 0.608739 0.047 Uiso 1 1 calc GR . . . .
H24B H 0.527848 0.463798 0.563919 0.047 Uiso 1 1 calc GR . . . .
H24C H 0.660767 0.431577 0.532238 0.047 Uiso 1 1 calc GR . . . .
C4 C 0.6823(14) 0.5191(9) 0.8377(9) 0.026(3) Uani 1 1 d . . . . .
C29 C 0.301(2) 0.2121(11) 0.8007(8) 0.038(4) Uani 1 1 d . . . . .
H29A H 0.370349 0.253387 0.799180 0.058 Uiso 1 1 calc GR . . . .
H29B H 0.325843 0.169741 0.834786 0.058 Uiso 1 1 calc GR . . . .
H29C H 0.219257 0.238393 0.814018 0.058 Uiso 1 1 calc GR . . . .
C25 C 0.4292(19) 0.1669(10) 0.4124(9) 0.039(4) Uani 1 1 d . . . . .
H25A H 0.495738 0.172384 0.377434 0.058 Uiso 1 1 calc GR . . . .
H25B H 0.341789 0.171459 0.389713 0.058 Uiso 1 1 calc GR . . . .
H25C H 0.438229 0.113379 0.435208 0.058 Uiso 1 1 calc GR . . . .
C2 C 0.5092(16) 0.4295(8) 0.7601(8) 0.026(2) Uani 1 1 d . . . . .
B1 B 0.2389(17) 0.1950(10) 0.5382(8) 0.019(3) Uani 1 1 d . . . . .
C19 C -0.0383(18) 0.4475(11) 0.5869(10) 0.041(4) Uani 1 1 d . . . . .
H19A H -0.062965 0.436576 0.634671 0.061 Uiso 1 1 calc GR . . . .
H19B H -0.113183 0.471047 0.560384 0.061 Uiso 1 1 calc GR . . . .
H19C H 0.035080 0.486257 0.587454 0.061 Uiso 1 1 calc GR . . . .
C3 C 0.5914(16) 0.4703(10) 0.7969(8) 0.028(3) Uani 1 1 d . . . . .
C7 C 0.6511(19) 0.5765(12) 0.8926(10) 0.044(5) Uani 1 1 d . . . . .
H7 H 0.566910 0.584936 0.910410 0.052 Uiso 1 1 calc R . . . .
C20 C -0.0202(18) 0.1794(11) 0.4391(9) 0.040(4) Uani 1 1 d . . . . .
H20A H 0.031391 0.187145 0.397766 0.060 Uiso 1 1 calc GR . . . .
H20B H -0.113541 0.177627 0.425209 0.060 Uiso 1 1 calc GR . . . .
H20C H 0.005258 0.127798 0.461968 0.060 Uiso 1 1 calc GR . . . .
C30 C 0.2286(18) 0.0090(10) 0.5952(9) 0.032(4) Uani 1 1 d . . . . .
H30A H 0.158863 0.019417 0.559777 0.049 Uiso 1 1 calc GR . . . .
H30B H 0.204825 -0.038200 0.623569 0.049 Uiso 1 1 calc GR . . . .
H30C H 0.310638 -0.002589 0.572487 0.049 Uiso 1 1 calc GR . . . .
C11 C 0.630(3) 0.6629(16) 0.7189(17) 0.093(11) Uani 1 1 d . . . . .
H11 H 0.574552 0.625534 0.693620 0.111 Uiso 1 1 calc R . . . .
C17 C -0.0691(17) 0.3209(11) 0.5017(10) 0.038(4) Uani 1 1 d . . . . .
H17 H -0.151395 0.334735 0.479994 0.045 Uiso 1 1 calc R . . . .
C8 C 0.768(2) 0.6180(14) 0.9151(12) 0.057(6) Uani 1 1 d . . . . .
H8 H 0.774632 0.658840 0.950302 0.068 Uiso 1 1 calc R . . . .
C10 C 0.8240(15) 0.5248(11) 0.8291(10) 0.036(4) Uani 1 1 d . . . . .
H10 H 0.873443 0.492868 0.798310 0.044 Uiso 1 1 calc R . . . .
C14 C 0.706(3) 0.7621(14) 0.7967(18) 0.087(10) Uani 1 1 d . . . . .
H14 H 0.709442 0.801770 0.832890 0.105 Uiso 1 1 calc R . . . .
C15 C 0.593(3) 0.7170(15) 0.770(2) 0.099(12) Uani 1 1 d . . . . .
H15 H 0.507100 0.723360 0.785925 0.119 Uiso 1 1 calc R . . . .
C9 C 0.8755(19) 0.5883(13) 0.8764(12) 0.055(6) Uani 1 1 d . . . . .
H9 H 0.963744 0.606631 0.880635 0.066 Uiso 1 1 calc R . . . .
C12 C 0.766(3) 0.6752(15) 0.7122(16) 0.078(8) Uani 1 1 d . . . . .
H12 H 0.818819 0.646636 0.680935 0.093 Uiso 1 1 calc R . . . .
C13 C 0.808(3) 0.7353(15) 0.7580(18) 0.088(10) Uani 1 1 d . . . . .
H13 H 0.895646 0.755263 0.762399 0.105 Uiso 1 1 calc R . . . .
H1 H 0.225(14) 0.144(10) 0.502(7) 0.02(4) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 N5 2.222(11) . ?
W1 N1 2.269(12) . ?
W1 C1 1.838(17) . ?
W1 C5 1.997(16) . ?
W1 N3 2.205(11) . ?
W1 C6 1.970(18) . ?
Fe1 C4 2.015(16) . ?
Fe1 C7 2.025(19) . ?
Fe1 C11 2.02(2) . ?
Fe1 C8 2.01(2) . ?
Fe1 C10 2.024(17) . ?
Fe1 C14 2.04(2) . ?
Fe1 C15 2.02(2) . ?
Fe1 C9 2.00(2) . ?
Fe1 C12 1.99(3) . ?
Fe1 C13 2.02(2) . ?
N5 N6 1.368(15) . ?
N5 C26 1.325(18) . ?
N1 N2 1.389(16) . ?
N1 C16 1.333(18) . ?
N6 C28 1.351(17) . ?
N6 B1 1.530(19) . ?
O2 C6 1.18(2) . ?
C21 C22 1.38(2) . ?
C21 N3 1.341(17) . ?
C21 C24 1.50(2) . ?
O1 C5 1.144(19) . ?
C1 C2 1.37(2) . ?
C22 C23 1.35(2) . ?
N3 N4 1.375(15) . ?
N2 C18 1.345(19) . ?
N2 B1 1.55(2) . ?
C28 C27 1.35(2) . ?
C28 C30 1.49(2) . ?
C27 C26 1.41(2) . ?
N4 C23 1.341(18) . ?
N4 B1 1.530(19) . ?
C18 C20 1.50(2) . ?
C18 C17 1.37(2) . ?
C16 C19 1.49(2) . ?
C16 C17 1.39(2) . ?
C23 C25 1.50(2) . ?
C26 C29 1.49(2) . ?
C4 C3 1.40(2) . ?
C4 C7 1.43(2) . ?
C4 C10 1.44(2) . ?
C2 C3 1.24(2) . ?
C7 C8 1.40(3) . ?
C11 C15 1.36(4) . ?
C11 C12 1.39(4) . ?
C8 C9 1.40(3) . ?
C10 C9 1.43(3) . ?
C14 C15 1.41(4) . ?
C14 C13 1.35(4) . ?
C12 C13 1.35(4) . ?

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
N5 W1 N1 82.7(4) . . ?
C1 W1 N5 104.2(5) . . ?
C1 W1 N1 172.0(5) . . ?
C1 W1 C5 83.0(6) . . ?
C1 W1 N3 102.7(6) . . ?
C1 W1 C6 85.7(7) . . ?
C5 W1 N5 172.4(5) . . ?
C5 W1 N1 90.3(5) . . ?
C5 W1 N3 93.9(5) . . ?
N3 W1 N5 82.3(4) . . ?
N3 W1 N1 82.0(4) . . ?
C6 W1 N5 94.1(5) . . ?
C6 W1 N1 89.9(6) . . ?
C6 W1 C5 88.8(6) . . ?
C6 W1 N3 171.5(6) . . ?
C4 Fe1 C7 41.4(7) . . ?
C4 Fe1 C11 106.6(9) . . ?
C4 Fe1 C10 41.7(6) . . ?
C4 Fe1 C14 155.9(9) . . ?
C4 Fe1 C15 120.4(9) . . ?
C4 Fe1 C13 162.5(11) . . ?
C7 Fe1 C14 120.4(11) . . ?
C7 Fe1 C15 106.8(12) . . ?
C11 Fe1 C7 122.7(11) . . ?
C11 Fe1 C10 122.9(10) . . ?
C11 Fe1 C14 67.9(12) . . ?
C11 Fe1 C15 39.2(13) . . ?
C11 Fe1 C13 66.9(12) . . ?
C8 Fe1 C4 69.5(8) . . ?
C8 Fe1 C7 40.6(7) . . ?
C8 Fe1 C11 158.5(13) . . ?
C8 Fe1 C10 69.1(8) . . ?
C8 Fe1 C14 106.6(12) . . ?
C8 Fe1 C15 123.3(13) . . ?
C8 Fe1 C13 122.7(12) . . ?
C10 Fe1 C7 69.2(8) . . ?
C10 Fe1 C14 160.9(10) . . ?
C10 Fe1 C15 157.2(10) . . ?
C15 Fe1 C14 40.6(11) . . ?
C9 Fe1 C4 70.5(7) . . ?
C9 Fe1 C7 69.2(9) . . ?
C9 Fe1 C11 159.5(13) . . ?
C9 Fe1 C8 41.0(9) . . ?
C9 Fe1 C10 41.7(7) . . ?
C9 Fe1 C14 123.0(11) . . ?
C9 Fe1 C15 159.7(12) . . ?
C9 Fe1 C13 109.5(11) . . ?
C12 Fe1 C4 125.4(9) . . ?
C12 Fe1 C7 160.9(11) . . ?
C12 Fe1 C11 40.4(12) . . ?
C12 Fe1 C8 158.4(11) . . ?
C12 Fe1 C10 110.3(9) . . ?
C12 Fe1 C14 66.5(12) . . ?
C12 Fe1 C15 65.9(13) . . ?
C12 Fe1 C9 123.9(11) . . ?
C12 Fe1 C13 39.2(11) . . ?
C13 Fe1 C7 156.0(11) . . ?
C13 Fe1 C10 126.8(10) . . ?
C13 Fe1 C14 38.8(11) . . ?
C13 Fe1 C15 65.6(12) . . ?
N6 N5 W1 120.6(8) . . ?
C26 N5 W1 131.2(9) . . ?
C26 N5 N6 108.1(11) . . ?
N2 N1 W1 118.9(8) . . ?
C16 N1 W1 134.4(10) . . ?
C16 N1 N2 106.6(12) . . ?
N5 N6 B1 120.2(10) . . ?
C28 N6 N5 108.1(11) . . ?
C28 N6 B1 131.7(12) . . ?
C22 C21 C24 129.3(13) . . ?
N3 C21 C22 108.8(13) . . ?
N3 C21 C24 121.9(13) . . ?
C2 C1 W1 170.9(12) . . ?
O1 C5 W1 178.2(15) . . ?
C23 C22 C21 106.8(13) . . ?
C21 N3 W1 132.3(9) . . ?
C21 N3 N4 107.1(11) . . ?
N4 N3 W1 120.5(8) . . ?
N1 N2 B1 120.0(11) . . ?
C18 N2 N1 109.3(12) . . ?
C18 N2 B1 130.8(12) . . ?
N6 C28 C30 122.0(13) . . ?
C27 C28 N6 109.3(12) . . ?
C27 C28 C30 128.7(13) . . ?
C28 C27 C26 105.9(13) . . ?
N3 N4 B1 120.6(11) . . ?
C23 N4 N3 108.5(11) . . ?
C23 N4 B1 130.9(12) . . ?
N2 C18 C20 121.5(15) . . ?
N2 C18 C17 108.1(14) . . ?
C17 C18 C20 130.4(15) . . ?
O2 C6 W1 178.7(17) . . ?
N1 C16 C19 122.6(15) . . ?
N1 C16 C17 109.5(14) . . ?
C17 C16 C19 127.7(15) . . ?
C22 C23 C25 129.4(14) . . ?
N4 C23 C22 108.8(14) . . ?
N4 C23 C25 121.8(14) . . ?
N5 C26 C27 108.6(13) . . ?
N5 C26 C29 123.2(13) . . ?
C27 C26 C29 128.2(14) . . ?
C3 C4 Fe1 122.8(12) . . ?
C3 C4 C7 126.8(15) . . ?
C3 C4 C10 126.4(15) . . ?
C7 C4 Fe1 69.7(10) . . ?
C7 C4 C10 106.8(14) . . ?
C10 C4 Fe1 69.5(9) . . ?
C3 C2 C1 174.7(16) . . ?
N6 B1 N2 109.0(11) . . ?
N6 B1 N4 110.0(12) . . ?
N4 B1 N2 108.5(12) . . ?
C2 C3 C4 177.9(17) . . ?
C4 C7 Fe1 69.0(10) . . ?
C8 C7 Fe1 69.2(12) . . ?
C8 C7 C4 108.6(17) . . ?
C15 C11 Fe1 70.5(16) . . ?
C15 C11 C12 105(3) . . ?
C12 C11 Fe1 68.7(15) . . ?
C18 C17 C16 106.5(14) . . ?
C7 C8 Fe1 70.2(12) . . ?
C7 C8 C9 109.4(18) . . ?
C9 C8 Fe1 69.2(13) . . ?
C4 C10 Fe1 68.8(9) . . ?
C9 C10 Fe1 68.3(11) . . ?
C9 C10 C4 107.8(16) . . ?
C15 C14 Fe1 69.1(13) . . ?
C13 C14 Fe1 69.9(14) . . ?
C13 C14 C15 105(3) . . ?
C11 C15 Fe1 70.3(14) . . ?
C11 C15 C14 110(3) . . ?
C14 C15 Fe1 70.3(14) . . ?
C8 C9 Fe1 69.9(13) . . ?
C8 C9 C10 107.5(16) . . ?
C10 C9 Fe1 70.0(10) . . ?
C11 C12 Fe1 70.9(15) . . ?
C13 C12 Fe1 71.6(17) . . ?
C13 C12 C11 109(3) . . ?
C14 C13 Fe1 71.3(15) . . ?
C12 C13 Fe1 69.2(14) . . ?
C12 C13 C14 110(3) . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.258 0.401 0.444 17.1 0.0 ?
2 0.242 0.901 0.056 17.1 0.0 ?
3 0.758 0.099 0.944 17.1 0.0 ?
4 0.742 0.599 0.556 17.1 0.0 ?


_ins_header                      
;
TITL RAM-069_scale in P2(1)/n 
REM P2(1)/n (#14 in standard setting)
CELL 1.54184  10.008106  15.966216  18.851428  90.0000  92.4042  90.0000
ZERR    4.00   0.000331   0.000527   0.000752   0.0000   0.0036   0.0000
LATT  1
SYMM -x+1/2, y+1/2,-z+1/2 
SFAC C H B N O Fe W
UNIT 120.00 124.00 4.00 24.00 8.00 4.00 4.00
TREF
HKLF 4
END
;
_olex2_submission_original_sample_id WC3Fc(CO)2(Tp*)
_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 1.252
_oxdiff_exptl_absorpt_empirical_full_min 0.849


####################################################################### 
# 
# 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_platon_sq
_database_code_depnum_ccdc_archive 'CCDC 1897316'
loop_
_audit_author_name
_audit_author_address
'Richard Manzano'
;Australian National University
Australia
;
_audit_update_record             
;
2019-02-15 deposited with the CCDC.	2019-04-23 downloaded from the CCDC.
;
_audit_creation_date             2018-09-12
_audit_creation_method           
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
a.hill@anu.edu.au
richard.manzano@anu.edu.au
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C38 H37 B N6 O2 Si W'
_chemical_formula_sum            'C38 H37 B N6 O2 Si W'
_chemical_formula_weight         832.48
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C40 H40 B1 Cl4 N6 O2 Si1 W'
_chemical_oxdiff_usercomment     
'Grown from slow evaporation of DCM/EtOH solution at 0 degrees celcius'
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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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                   15.9396(9)
_cell_length_b                   12.8019(8)
_cell_length_c                   19.6756(10)
_cell_angle_alpha                90
_cell_angle_beta                 95.280(6)
_cell_angle_gamma                90
_cell_volume                     3997.9(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5563
_cell_measurement_temperature    149.99(11)
_cell_measurement_theta_max      28.0440
_cell_measurement_theta_min      3.7910
_shelx_estimated_absorpt_T_max   0.800
_shelx_estimated_absorpt_T_min   0.662
_exptl_absorpt_coefficient_mu    2.957
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98209
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.383
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1664
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-8 5 26 0.0307
6 3 -27 0.0275
2 -16 12 0.0727
-2 16 -12 0.0727
7 -17 -6 0.0809
4 -9 -24 0.0594
-3 9 24 0.0363
22 1 2 0.0449
-22 0 1 0.0278

_exptl_crystal_preparation       ?
_exptl_crystal_recrystallization_method 
'Grown from slow evaporationg of a chloroform/ethanol solution at 0 degrees celcius'
_exptl_crystal_size_max          0.152
_exptl_crystal_size_mid          0.097
_exptl_crystal_size_min          0.079
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
-7.9998 5.0001 26.0019 0.0457 0.2136 -0.9907
5.9998 3.0004 -27.0015 -0.1306 -0.6099 0.7864
2.0001 -16.0009 11.9997 0.2296 0.9629 0.0912
-2.0001 16.0009 -11.9997 -0.2296 -0.9629 -0.0912
7.0000 -17.0008 -6.0015 0.1795 0.6976 0.7063
3.9995 -9.0003 -24.0021 -0.1938 0.0353 0.9841
-2.9995 9.0003 24.0021 0.2363 -0.0407 -0.9710
22.0012 1.0002 2.0002 0.9646 -0.1348 0.2020
-22.0011 -0.0001 1.0000 -0.9194 0.1339 -0.3153

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0529
_diffrn_reflns_av_unetI/netI     0.0845
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            21582
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.270
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.99(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3744
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_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    -80.00  14.00   1.00  290.00    --  -11.22 -57.00  90.00   94
  2  ω     -5.00  30.00   1.00  290.00    --  -11.22  57.00-150.00   35
  3  ω    -92.00 -34.00   1.00  290.00    --  -11.22 178.00-150.00   58
  4  ω     70.00  95.00   1.00  290.00    --   11.46 178.00 -30.00   25
;
_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      0.0424443000
_diffrn_orient_matrix_UB_12      0.0018076000
_diffrn_orient_matrix_UB_13      0.0144696000
_diffrn_orient_matrix_UB_21      -0.0053583000
_diffrn_orient_matrix_UB_22      -0.0488774000
_diffrn_orient_matrix_UB_23      0.0159641000
_diffrn_orient_matrix_UB_31      0.0130070000
_diffrn_orient_matrix_UB_32      -0.0259114000
_diffrn_orient_matrix_UB_33      -0.0291151000
_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'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5970
_reflns_number_total             8152
_reflns_odcompleteness_completeness 99.70
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (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         1.384
_refine_diff_density_min         -0.573
_refine_diff_density_rms         0.126
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         8152
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0723
_refine_ls_R_factor_gt           0.0458
_refine_ls_restrained_S_all      1.000
_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)+(0.0309P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0797
_refine_ls_wR_factor_ref         0.0882
_refine_special_details          SQUEEZE
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C28(H28), C25(H25), C19(H19), C20(H20), C31(H31), C23(H23), C22(H22),
 C21(H21), C7(H7), C14(H14), C17(H17), C9(H9), C8(H8), C10(H10), C11(H11),
 C15(H15), C16(H16), C13(H13)
2.b Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C37(H37A,H37B,
 H37C), C34(H34A,H34B,H34C), C38(H38A,H38B,H38C)
;
_atom_sites_solution_hydrogens   mixed
_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 0.13373(2) 0.66885(2) 0.83946(2) 0.02496(8) Uani 1 1 d . . . . .
Si1 Si 0.31217(9) 0.41495(13) 0.62308(8) 0.0336(4) Uani 1 1 d . . . . .
N3 N 0.1181(2) 0.5408(3) 0.9116(2) 0.0241(10) Uani 1 1 d . . . . .
O1 O -0.0349(2) 0.6221(3) 0.74726(19) 0.0412(10) Uani 1 1 d . . . . .
N1 N 0.0644(2) 0.7581(3) 0.9166(2) 0.0262(10) Uani 1 1 d . . . . .
N2 N 0.0905(2) 0.7477(3) 0.9851(2) 0.0259(10) Uani 1 1 d . . . . .
O2 O 0.1513(3) 0.8677(4) 0.7468(2) 0.0543(12) Uani 1 1 d . . . . .
N6 N 0.2407(3) 0.6927(3) 0.9815(2) 0.0309(11) Uani 1 1 d . . . . .
N5 N 0.2442(3) 0.7040(4) 0.9116(2) 0.0313(11) Uani 1 1 d . . . . .
N4 N 0.1280(2) 0.5582(3) 0.9816(2) 0.0255(10) Uani 1 1 d . . . . .
C5 C 0.1442(3) 0.7959(5) 0.7820(3) 0.0351(14) Uani 1 1 d . . . . .
C24 C 0.0052(3) 0.8326(4) 0.9121(3) 0.0279(12) Uani 1 1 d . . . . .
C4 C 0.0259(3) 0.6389(4) 0.7822(3) 0.0281(13) Uani 1 1 d . . . . .
C2 C 0.2202(3) 0.5451(4) 0.7222(3) 0.0283(13) Uani 1 1 d . . . . .
C1 C 0.1850(3) 0.5989(4) 0.7738(3) 0.0294(13) Uani 1 1 d . . . . .
C33 C -0.0380(3) 0.8675(5) 0.8446(3) 0.0400(15) Uani 1 1 d . . . . .
H33A H 0.001514 0.907723 0.819693 0.060 Uiso 1 1 calc GR . . . .
H33B H -0.086608 0.911312 0.852579 0.060 Uiso 1 1 calc GR . . . .
H33C H -0.057207 0.806170 0.817717 0.060 Uiso 1 1 calc GR . . . .
C27 C 0.0966(3) 0.4409(4) 0.9028(3) 0.0280(13) Uani 1 1 d . . . . .
C26 C 0.0466(3) 0.8152(4) 1.0211(3) 0.0293(13) Uani 1 1 d . . . . .
C35 C 0.0795(3) 0.3946(5) 0.8326(3) 0.0357(14) Uani 1 1 d . . . . .
H35A H 0.028848 0.426715 0.809464 0.053 Uiso 1 1 calc GR . . . .
H35B H 0.070808 0.319099 0.836403 0.053 Uiso 1 1 calc GR . . . .
H35C H 0.127652 0.407808 0.806269 0.053 Uiso 1 1 calc GR . . . .
C29 C 0.1110(3) 0.4694(4) 1.0136(3) 0.0271(13) Uani 1 1 d . . . . .
C3 C 0.2528(3) 0.4951(5) 0.6806(3) 0.0336(14) Uani 1 1 d . . . . .
C28 C 0.0922(3) 0.3946(5) 0.9657(3) 0.0323(14) Uani 1 1 d . . . . .
H28 H 0.078545 0.323757 0.973882 0.039 Uiso 1 1 calc R . . . .
C30 C 0.3246(3) 0.7296(5) 0.9032(3) 0.0438(16) Uani 1 1 d . . . . .
C18 C 0.2580(3) 0.4236(5) 0.5343(3) 0.0316(14) Uani 1 1 d . . . . .
C25 C -0.0089(3) 0.8681(4) 0.9762(3) 0.0294(13) Uani 1 1 d . . . . .
H25 H -0.049018 0.918903 0.987107 0.035 Uiso 1 1 calc R . . . .
C36 C 0.1159(3) 0.4598(5) 1.0898(3) 0.0373(15) Uani 1 1 d . . . . .
H36A H 0.174034 0.471489 1.109034 0.056 Uiso 1 1 calc GR . . . .
H36B H 0.097819 0.389668 1.102161 0.056 Uiso 1 1 calc GR . . . .
H36C H 0.078938 0.511944 1.108096 0.056 Uiso 1 1 calc GR . . . .
C19 C 0.2388(3) 0.5197(5) 0.5064(3) 0.0371(14) Uani 1 1 d . . . . .
H19 H 0.251908 0.580989 0.532566 0.045 Uiso 1 1 calc R . . . .
C12 C 0.4196(3) 0.4756(5) 0.6267(3) 0.0364(15) Uani 1 1 d . . . . .
C6 C 0.3140(4) 0.2775(5) 0.6550(3) 0.0398(15) Uani 1 1 d . . . . .
C37 C 0.3526(4) 0.7499(6) 0.8335(3) 0.063(2) Uani 1 1 d . . . . .
H37A H 0.337498 0.690154 0.803743 0.094 Uiso 1 1 calc GR . . . .
H37B H 0.413766 0.759955 0.837137 0.094 Uiso 1 1 calc GR . . . .
H37C H 0.324685 0.812898 0.814214 0.094 Uiso 1 1 calc GR . . . .
C34 C 0.0613(4) 0.8250(5) 1.0973(3) 0.0390(15) Uani 1 1 d . . . . .
H34A H 0.060323 0.755530 1.118100 0.059 Uiso 1 1 calc GR . . . .
H34B H 0.016859 0.868321 1.114113 0.059 Uiso 1 1 calc GR . . . .
H34C H 0.116207 0.857706 1.109475 0.059 Uiso 1 1 calc GR . . . .
C20 C 0.2387(4) 0.3360(5) 0.4943(3) 0.0411(15) Uani 1 1 d . . . . .
H20 H 0.251913 0.268545 0.512411 0.049 Uiso 1 1 calc R . . . .
B1 B 0.1559(4) 0.6654(5) 1.0093(3) 0.0290(14) Uani 1 1 d . . . . .
C31 C 0.3706(4) 0.7342(6) 0.9659(3) 0.0525(19) Uani 1 1 d . . . . .
H31 H 0.428903 0.750246 0.973873 0.063 Uiso 1 1 calc R . . . .
C32 C 0.3176(4) 0.7116(5) 1.0144(3) 0.0425(16) Uani 1 1 d . . . . .
C23 C 0.1804(3) 0.4444(5) 0.4019(3) 0.0413(16) Uani 1 1 d . . . . .
H23 H 0.153054 0.451370 0.357207 0.050 Uiso 1 1 calc R . . . .
C38 C 0.3331(4) 0.7059(6) 1.0903(3) 0.058(2) Uani 1 1 d . . . . .
H38A H 0.298707 0.758539 1.110967 0.087 Uiso 1 1 calc GR . . . .
H38B H 0.392832 0.719204 1.104008 0.087 Uiso 1 1 calc GR . . . .
H38C H 0.317976 0.636245 1.105886 0.087 Uiso 1 1 calc GR . . . .
C22 C 0.2008(4) 0.3453(5) 0.4292(3) 0.0485(18) Uani 1 1 d . . . . .
H22 H 0.188227 0.284536 0.402488 0.058 Uiso 1 1 calc R . . . .
C21 C 0.2002(4) 0.5285(5) 0.4398(3) 0.0424(16) Uani 1 1 d . . . . .
H21 H 0.187805 0.595911 0.421338 0.051 Uiso 1 1 calc R . . . .
C7 C 0.2631(4) 0.2437(6) 0.7035(3) 0.0499(18) Uani 1 1 d . . . . .
H7 H 0.226698 0.292535 0.722223 0.060 Uiso 1 1 calc R . . . .
C14 C 0.4771(4) 0.4456(6) 0.5826(4) 0.060(2) Uani 1 1 d . . . . .
H14 H 0.462408 0.393068 0.549480 0.072 Uiso 1 1 calc R . . . .
C17 C 0.5791(4) 0.5675(7) 0.6300(4) 0.071(2) Uani 1 1 d . . . . .
H17 H 0.633409 0.598469 0.631216 0.086 Uiso 1 1 calc R . . . .
C9 C 0.2632(5) 0.1428(6) 0.7258(3) 0.060(2) Uani 1 1 d . . . . .
H9 H 0.227263 0.122976 0.759483 0.073 Uiso 1 1 calc R . . . .
C8 C 0.3664(5) 0.2031(6) 0.6296(4) 0.068(2) Uani 1 1 d . . . . .
H8 H 0.403728 0.223389 0.597075 0.082 Uiso 1 1 calc R . . . .
C10 C 0.3653(5) 0.1008(7) 0.6507(4) 0.086(3) Uani 1 1 d . . . . .
H10 H 0.399961 0.050704 0.631213 0.103 Uiso 1 1 calc R . . . .
C11 C 0.3141(5) 0.0704(6) 0.7001(4) 0.070(2) Uani 1 1 d . . . . .
H11 H 0.314464 0.000190 0.715836 0.084 Uiso 1 1 calc R . . . .
C15 C 0.5222(5) 0.5997(7) 0.6732(5) 0.090(3) Uani 1 1 d . . . . .
H15 H 0.536650 0.654438 0.704730 0.107 Uiso 1 1 calc R . . . .
C16 C 0.5562(4) 0.4909(7) 0.5857(4) 0.073(2) Uani 1 1 d . . . . .
H16 H 0.595403 0.466968 0.555591 0.087 Uiso 1 1 calc R . . . .
C13 C 0.4435(4) 0.5533(7) 0.6716(4) 0.071(2) Uani 1 1 d . . . . .
H13 H 0.405163 0.576360 0.702646 0.085 Uiso 1 1 calc R . . . .
H1 H 0.162(3) 0.658(4) 1.066(2) 0.032(14) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 N3 2.198(4) . ?
W1 N1 2.266(4) . ?
W1 N5 2.203(4) . ?
W1 C5 1.996(6) . ?
W1 C4 2.004(6) . ?
W1 C1 1.826(5) . ?
Si1 C3 1.851(6) . ?
Si1 C18 1.880(6) . ?
Si1 C12 1.876(6) . ?
Si1 C6 1.868(6) . ?
N3 N4 1.390(5) . ?
N3 C27 1.331(6) . ?
O1 C4 1.155(6) . ?
N1 N2 1.380(5) . ?
N1 C24 1.339(6) . ?
N2 C26 1.352(6) . ?
N2 B1 1.529(8) . ?
O2 C5 1.163(7) . ?
N6 N5 1.390(6) . ?
N6 B1 1.544(7) . ?
N6 C32 1.353(7) . ?
N5 C30 1.348(7) . ?
N4 C29 1.339(6) . ?
N4 B1 1.528(8) . ?
C24 C33 1.506(7) . ?
C24 C25 1.379(7) . ?
C2 C1 1.386(7) . ?
C2 C3 1.195(7) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C27 C35 1.505(7) . ?
C27 C28 1.378(7) . ?
C26 C25 1.370(7) . ?
C26 C34 1.501(7) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C29 C28 1.358(7) . ?
C29 C36 1.499(7) . ?
C28 H28 0.9500 . ?
C30 C37 1.504(8) . ?
C30 C31 1.377(8) . ?
C18 C19 1.370(8) . ?
C18 C20 1.388(8) . ?
C25 H25 0.9500 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C19 H19 0.9500 . ?
C19 C21 1.400(8) . ?
C12 C14 1.374(7) . ?
C12 C13 1.362(9) . ?
C6 C7 1.378(8) . ?
C6 C8 1.389(8) . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C20 H20 0.9500 . ?
C20 C22 1.370(8) . ?
B1 H1 1.12(5) . ?
C31 H31 0.9500 . ?
C31 C32 1.363(8) . ?
C32 C38 1.494(8) . ?
C23 H23 0.9500 . ?
C23 C22 1.405(9) . ?
C23 C21 1.331(8) . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C22 H22 0.9500 . ?
C21 H21 0.9500 . ?
C7 H7 0.9500 . ?
C7 C9 1.363(9) . ?
C14 H14 0.9500 . ?
C14 C16 1.384(9) . ?
C17 H17 0.9500 . ?
C17 C15 1.363(10) . ?
C17 C16 1.340(10) . ?
C9 H9 0.9500 . ?
C9 C11 1.360(9) . ?
C8 H8 0.9500 . ?
C8 C10 1.375(10) . ?
C10 H10 0.9500 . ?
C10 C11 1.381(9) . ?
C11 H11 0.9500 . ?
C15 H15 0.9500 . ?
C15 C13 1.386(9) . ?
C16 H16 0.9500 . ?
C13 H13 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 W1 N1 81.50(15) . . ?
N3 W1 N5 82.40(16) . . ?
N5 W1 N1 82.86(15) . . ?
C5 W1 N3 173.61(18) . . ?
C5 W1 N1 92.27(18) . . ?
C5 W1 N5 95.5(2) . . ?
C5 W1 C4 87.1(2) . . ?
C4 W1 N3 94.47(18) . . ?
C4 W1 N1 91.56(17) . . ?
C4 W1 N5 173.94(16) . . ?
C1 W1 N3 100.1(2) . . ?
C1 W1 N1 176.9(2) . . ?
C1 W1 N5 100.0(2) . . ?
C1 W1 C5 86.2(2) . . ?
C1 W1 C4 85.7(2) . . ?
C3 Si1 C18 108.6(2) . . ?
C3 Si1 C12 105.3(3) . . ?
C3 Si1 C6 108.0(3) . . ?
C12 Si1 C18 110.5(2) . . ?
C6 Si1 C18 111.1(3) . . ?
C6 Si1 C12 113.0(3) . . ?
N4 N3 W1 120.7(3) . . ?
C27 N3 W1 132.5(3) . . ?
C27 N3 N4 106.7(4) . . ?
N2 N1 W1 118.9(3) . . ?
C24 N1 W1 134.3(3) . . ?
C24 N1 N2 106.3(4) . . ?
N1 N2 B1 120.4(4) . . ?
C26 N2 N1 109.1(4) . . ?
C26 N2 B1 130.4(4) . . ?
N5 N6 B1 119.3(4) . . ?
C32 N6 N5 109.8(4) . . ?
C32 N6 B1 130.9(5) . . ?
N6 N5 W1 121.0(3) . . ?
C30 N5 W1 133.1(4) . . ?
C30 N5 N6 105.7(5) . . ?
N3 N4 B1 120.0(4) . . ?
C29 N4 N3 108.7(4) . . ?
C29 N4 B1 131.3(4) . . ?
O2 C5 W1 177.6(5) . . ?
N1 C24 C33 122.2(5) . . ?
N1 C24 C25 110.3(5) . . ?
C25 C24 C33 127.5(5) . . ?
O1 C4 W1 177.8(4) . . ?
C3 C2 C1 176.2(6) . . ?
C2 C1 W1 177.3(4) . . ?
C24 C33 H33A 109.5 . . ?
C24 C33 H33B 109.5 . . ?
C24 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
N3 C27 C35 121.3(5) . . ?
N3 C27 C28 109.3(5) . . ?
C28 C27 C35 129.4(5) . . ?
N2 C26 C25 108.2(5) . . ?
N2 C26 C34 122.5(5) . . ?
C25 C26 C34 129.3(5) . . ?
C27 C35 H35A 109.5 . . ?
C27 C35 H35B 109.5 . . ?
C27 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
N4 C29 C28 108.2(4) . . ?
N4 C29 C36 123.1(5) . . ?
C28 C29 C36 128.7(5) . . ?
C2 C3 Si1 174.1(5) . . ?
C27 C28 H28 126.4 . . ?
C29 C28 C27 107.1(5) . . ?
C29 C28 H28 126.4 . . ?
N5 C30 C37 121.3(5) . . ?
N5 C30 C31 109.6(5) . . ?
C31 C30 C37 129.1(5) . . ?
C19 C18 Si1 119.4(5) . . ?
C19 C18 C20 118.0(5) . . ?
C20 C18 Si1 122.5(5) . . ?
C24 C25 H25 127.0 . . ?
C26 C25 C24 106.1(5) . . ?
C26 C25 H25 127.0 . . ?
C29 C36 H36A 109.5 . . ?
C29 C36 H36B 109.5 . . ?
C29 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C18 C19 H19 119.7 . . ?
C18 C19 C21 120.6(6) . . ?
C21 C19 H19 119.7 . . ?
C14 C12 Si1 121.4(5) . . ?
C13 C12 Si1 121.8(4) . . ?
C13 C12 C14 116.9(6) . . ?
C7 C6 Si1 122.5(5) . . ?
C7 C6 C8 116.4(6) . . ?
C8 C6 Si1 121.1(5) . . ?
C30 C37 H37A 109.5 . . ?
C30 C37 H37B 109.5 . . ?
C30 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C26 C34 H34A 109.5 . . ?
C26 C34 H34B 109.5 . . ?
C26 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C18 C20 H20 119.5 . . ?
C22 C20 C18 121.0(6) . . ?
C22 C20 H20 119.5 . . ?
N2 B1 N6 109.1(5) . . ?
N2 B1 H1 112(2) . . ?
N6 B1 H1 112(2) . . ?
N4 B1 N2 109.9(5) . . ?
N4 B1 N6 108.2(4) . . ?
N4 B1 H1 106(3) . . ?
C30 C31 H31 126.2 . . ?
C32 C31 C30 107.7(5) . . ?
C32 C31 H31 126.2 . . ?
N6 C32 C31 107.2(5) . . ?
N6 C32 C38 121.9(5) . . ?
C31 C32 C38 130.8(6) . . ?
C22 C23 H23 120.6 . . ?
C21 C23 H23 120.6 . . ?
C21 C23 C22 118.8(6) . . ?
C32 C38 H38A 109.5 . . ?
C32 C38 H38B 109.5 . . ?
C32 C38 H38C 109.5 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C20 C22 C23 120.2(6) . . ?
C20 C22 H22 119.9 . . ?
C23 C22 H22 119.9 . . ?
C19 C21 H21 119.3 . . ?
C23 C21 C19 121.4(6) . . ?
C23 C21 H21 119.3 . . ?
C6 C7 H7 118.8 . . ?
C9 C7 C6 122.5(6) . . ?
C9 C7 H7 118.8 . . ?
C12 C14 H14 119.6 . . ?
C12 C14 C16 120.8(7) . . ?
C16 C14 H14 119.6 . . ?
C15 C17 H17 121.0 . . ?
C16 C17 H17 121.0 . . ?
C16 C17 C15 118.0(7) . . ?
C7 C9 H9 119.7 . . ?
C11 C9 C7 120.6(7) . . ?
C11 C9 H9 119.7 . . ?
C6 C8 H8 119.3 . . ?
C10 C8 C6 121.3(6) . . ?
C10 C8 H8 119.3 . . ?
C8 C10 H10 119.8 . . ?
C8 C10 C11 120.4(7) . . ?
C11 C10 H10 119.8 . . ?
C9 C11 C10 118.7(7) . . ?
C9 C11 H11 120.7 . . ?
C10 C11 H11 120.7 . . ?
C17 C15 H15 119.7 . . ?
C17 C15 C13 120.6(8) . . ?
C13 C15 H15 119.7 . . ?
C14 C16 H16 119.1 . . ?
C17 C16 C14 121.9(6) . . ?
C17 C16 H16 119.1 . . ?
C12 C13 C15 121.8(6) . . ?
C12 C13 H13 119.1 . . ?
C15 C13 H13 119.1 . . ?


_ins_header                      
;
TITL RAM-40scale in P2(1)/c 
REM P2(1)/c (#14 in standard setting)
CELL 0.71073  15.939619  12.801930  19.675554  90.0000  95.2799  90.0000
ZERR    4.00   0.000943   0.000834   0.000989   0.0000   0.0057   0.0000
LATT  1
SYMM -x, y+1/2,-z+1/2 
SFAC C H B N O Si Cl W
UNIT 160.00 160.00 4.00 24.00 8.00 4.00 16.00 4.00
TREF
HKLF 4
END
;
_olex2_submission_original_sample_id RAM-40
_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 1.077
_oxdiff_exptl_absorpt_empirical_full_min 0.955

####################################################################### 
# 
# 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_wccccph3scale
_database_code_depnum_ccdc_archive 'CCDC 1897314'
loop_
_audit_author_name
_audit_author_address
'Richard Manzano'
;Australian National University
Australia
;
#Added by publCIF
_audit_update_record             
;
2019-02-15 deposited with the CCDC.	2019-04-23 downloaded from the CCDC.
;
_audit_creation_date             2018-09-11
_audit_creation_method           
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/4
loop_
_audit_author_email
a.hill@anu.edu.au
richard.manzano@anu.edu.au
_chemical_name_common            ?
_chemical_name_systematic        W(CCCCPh3)(CO)2Tp*
_chemical_formula_moiety         'C39 H37 B N6 O2 W, C H2 Cl2'
_chemical_formula_sum            'C40 H39 B Cl2 N6 O2 W'
_chemical_formula_weight         901.33
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C39 H36 B1 N6 O2 W1'
_chemical_oxdiff_usercomment     
'Crystal grown from v/v diffusion of heptane into DCM'
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'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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           15
_space_group_name_H-M_alt        'I 1 2/a 1'
_space_group_name_Hall           '-I 2ya'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'

_cell_length_a                   19.0666(2)
_cell_length_b                   12.8247(2)
_cell_length_c                   34.3229(5)
_cell_angle_alpha                90
_cell_angle_beta                 104.8000(10)
_cell_angle_gamma                90
_cell_volume                     8114.3(2)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    15259
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      73.6500
_cell_measurement_theta_min      4.6250
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    6.812
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87531
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.476
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             3600
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-12 -1 8 0.0127
12 1 -8 0.0127
-3 8 -6 0.0670
4 -7 5 0.0533
5 0 -22 0.0267
-5 0 22 0.0055

_exptl_crystal_preparation       ?
_exptl_crystal_recrystallization_method 
'Crystals were grown from vapour-vapour diffusion of heptane into a dichloromethane solution.'
_exptl_crystal_size_max          0.147
_exptl_crystal_size_mid          0.052
_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
-12.0007 -0.9926 8.0636 -0.6272 -0.7124 -0.2599
12.0007 0.9926 -8.0636 0.6272 0.7124 0.2599
-3.0074 8.0099 -5.9518 -0.2388 -0.2631 0.9871
4.0074 -7.0094 4.9484 0.2996 0.2966 -0.8576
4.9745 -0.0117 -21.9696 -0.3404 0.8652 0.3646
-4.9745 0.0117 21.9696 0.3404 -0.8652 -0.3646

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0375
_diffrn_reflns_av_unetI/netI     0.0317
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            26020
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.713
_diffrn_reflns_theta_min         3.695
_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 0.999
_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    -21.00  54.00   1.00   10.00    --   36.95 -38.00 150.00   75
  2  ω     48.00  89.00   1.00   10.00    --   36.95  57.00  90.00   41
  3  ω     74.00 100.00   1.00   10.00    --   36.95  57.00  30.00   26
  4  ω     20.00  97.00   1.00   10.00    --   36.95  57.00 150.00   77
  5  ω     20.00  59.00   1.00   10.00    --   36.95  57.00  30.00   39
  6  ω     56.00  88.00   1.00   10.00    --   36.95-125.00 -90.00   32
  7  ω     24.00  97.00   1.00   10.00    --   36.95  38.00 -30.00   73
  8  ω     64.00  96.00   1.00   10.00    --   36.95  19.00 -90.00   32
  9  ω     42.00 115.00   1.00   40.00    --  111.00-111.00-150.00   73
 10  ω     89.00 114.00   1.00   40.00    --  111.00-111.00 150.00   25
 11  ω     69.00 178.00   1.00   40.00    --  111.00  12.00-180.00  109
 12  ω    104.00 141.00   1.00   40.00    --  111.00  64.00  60.00   37
 13  ω     78.00 104.00   1.00   40.00    --  111.00 -19.00 125.43   26
 14  ω    111.00 176.00   1.00   40.00    --  111.00  64.00 150.00   65
 15  ω     96.00 122.00   1.00   40.00    --  111.00 -50.00  90.00   26
 16  ω     85.00 116.00   1.00   40.00    --  111.00 -38.00  30.00   31
 17  ω     43.00  71.00   1.00   40.00    --  111.00 -38.00  30.00   28
 18  ω    136.00 172.00   1.00   40.00    --  111.00 111.00-180.00   36
 19  ω     94.00 178.00   1.00   40.00    --  111.00  64.00  90.00   84
 20  ω    131.00 175.00   1.00   40.00    --  111.00  38.00-150.00   44
 21  ω     63.00 104.00   1.00   40.00    --  111.00-111.00 -90.00   41
 22  ω     49.00  74.00   1.00   40.00    --  111.00 -77.00 -30.00   25
 23  ω    106.00 136.00   1.00   40.00    --  111.00 -77.00 -30.00   30
 24  ω     99.00 130.00   1.00   40.00    --  111.00 -64.00 120.00   31
 25  ω     83.00 127.00   1.00   40.00    --  111.00 -64.00-180.00   44
 26  ω     62.00 104.00   1.00   40.00    --  111.00 -64.00  90.00   42
 27  ω    120.00 177.00   1.00   40.00    --  111.00 111.00  60.00   57
 28  ω     78.00 117.00   1.00   40.00    --  111.00 -92.00 -90.00   39
 29  ω     51.00 110.00   1.00   40.00    --  111.00-111.00  60.00   59
;
_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      0.0718864000
_diffrn_orient_matrix_UB_12      0.0207748000
_diffrn_orient_matrix_UB_13      0.0317597000
_diffrn_orient_matrix_UB_21      0.0426172000
_diffrn_orient_matrix_UB_22      -0.0389248000
_diffrn_orient_matrix_UB_23      -0.0297123000
_diffrn_orient_matrix_UB_31      0.0014498000
_diffrn_orient_matrix_UB_32      0.1116491000
_diffrn_orient_matrix_UB_33      -0.0163282000
_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                7353
_reflns_number_total             8115
_reflns_odcompleteness_completeness 97.81
_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 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.973
_refine_diff_density_min         -1.567
_refine_diff_density_rms         0.088
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     489
_refine_ls_number_reflns         8115
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0315
_refine_ls_R_factor_gt           0.0282
_refine_ls_restrained_S_all      1.053
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0387P)²+21.7003P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0734
_refine_ls_wR_factor_ref         0.0757
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl2-C101 = Cl10-C101
 1.7 with sigma of 0.01
3. Others
 Sof(H10c)=Sof(H10d)=Sof(Cl2)=1-FVAR(1)
 Sof(Cl10)=Sof(H10a)=Sof(H10b)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C101(H10a,H10b), C101(H10c,H10d)
4.b Aromatic/amide H refined with riding coordinates:
 C26(H26), C24(H18), C32(H31), C23(H17), C14(H12), C20(H14), C22(H16), C18(H8),
  C21(H15), C8(H20), C17(H9), C16(H10), C29(H36), C15(H11), C9(H21), C12(H24),
 C10(H22), C11(H23)
4.c Idealised Me refined as rotating group:
 C35(H29a,H29b,H29c), C34(H28a,H28b,H28c), C39(H34a,H34b,H34c), C37(H39a,H39b,
 H39c), C36(H38a,H38b,H38c), C38(H33a,H33b,H33c)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.60797(2) 0.91784(2) 0.31442(2) 0.01832(5) Uani 1 1 d . . . . .
O2 O 0.49305(12) 0.8633(2) 0.23328(7) 0.0339(5) Uani 1 1 d . . . . .
N2 N 0.74986(12) 1.00014(18) 0.29137(7) 0.0188(4) Uani 1 1 d . . . . .
N4 N 0.75621(12) 0.81203(18) 0.31254(7) 0.0190(4) Uani 1 1 d . . . . .
N3 N 0.68389(12) 0.79174(18) 0.30858(7) 0.0201(5) Uani 1 1 d . . . . .
N1 N 0.67575(12) 1.01029(18) 0.28052(7) 0.0192(4) Uani 1 1 d . . . . .
N5 N 0.69873(13) 0.96036(19) 0.36658(7) 0.0220(5) Uani 1 1 d . . . . .
N6 N 0.76954(13) 0.95272(19) 0.36415(7) 0.0209(5) Uani 1 1 d . . . . .
O1 O 0.51368(16) 1.1149(2) 0.32202(10) 0.0498(7) Uani 1 1 d . . . . .
C27 C 0.77913(16) 1.0662(2) 0.26918(9) 0.0207(5) Uani 1 1 d . . . . .
C13 C 0.34347(15) 0.6777(2) 0.37695(8) 0.0210(5) Uani 1 1 d . . . . .
C32 C 0.78994(16) 0.7232(2) 0.30666(9) 0.0225(6) Uani 1 1 d . . . . .
C25 C 0.65972(16) 1.0833(2) 0.25164(9) 0.0213(6) Uani 1 1 d . . . . .
C6 C 0.53511(15) 0.8828(2) 0.26245(9) 0.0239(6) Uani 1 1 d . . . . .
C3 C 0.46339(15) 0.7447(2) 0.37424(8) 0.0220(5) Uani 1 1 d . . . . .
C4 C 0.42507(15) 0.6831(2) 0.39896(8) 0.0205(5) Uani 1 1 d . . . . .
C26 C 0.72320(16) 1.1193(2) 0.24331(9) 0.0227(5) Uani 1 1 d . . . . .
H26 H 0.727148 1.168957 0.224225 0.027 Uiso 1 1 calc R . . . .
C30 C 0.67356(16) 0.6895(2) 0.30066(9) 0.0234(6) Uani 1 1 d . . . . .
C37 C 0.81477(17) 0.9770(2) 0.40021(9) 0.0272(6) Uani 1 1 d . . . . .
C29 C 0.85896(17) 1.0766(3) 0.27406(10) 0.0293(7) Uani 1 1 d . . . . .
H29A H 0.881047 1.106703 0.299877 0.044 Uiso 1 1 calc GR . . . .
H29B H 0.867606 1.120687 0.253173 0.044 Uiso 1 1 calc GR . . . .
H29C H 0.879506 1.008951 0.272247 0.044 Uiso 1 1 calc GR . . . .
C18 C 0.30774(16) 0.7683(2) 0.36095(9) 0.0233(6) Uani 1 1 d . . . . .
H18 H 0.334189 0.829378 0.361331 0.028 Uiso 1 1 calc R . . . .
C28 C 0.58397(17) 1.1201(3) 0.23331(10) 0.0323(7) Uani 1 1 d . . . . .
H28A H 0.552880 1.060949 0.224928 0.048 Uiso 1 1 calc GR . . . .
H28B H 0.583428 1.163242 0.210393 0.048 Uiso 1 1 calc GR . . . .
H28C H 0.567011 1.159520 0.252857 0.048 Uiso 1 1 calc GR . . . .
C5 C 0.54892(17) 1.0443(3) 0.31906(10) 0.0305(7) Uani 1 1 d . . . . .
C2 C 0.50048(15) 0.7949(2) 0.35720(8) 0.0218(5) Uani 1 1 d . . . . .
C1 C 0.54798(15) 0.8469(2) 0.33944(9) 0.0223(5) Uani 1 1 d . . . . .
C31 C 0.73923(16) 0.6441(2) 0.29910(9) 0.0253(6) Uani 1 1 d . . . . .
H31 H 0.747233 0.574440 0.293997 0.030 Uiso 1 1 calc R . . . .
C19 C 0.45934(17) 0.5731(2) 0.40555(9) 0.0244(6) Uani 1 1 d . . . . .
C7 C 0.43600(16) 0.7410(2) 0.43971(8) 0.0231(6) Uani 1 1 d . . . . .
C17 C 0.23294(17) 0.7695(2) 0.34430(9) 0.0268(6) Uani 1 1 d . . . . .
H17 H 0.209838 0.831075 0.333830 0.032 Uiso 1 1 calc R . . . .
C12 C 0.38015(17) 0.7547(3) 0.45821(9) 0.0291(6) Uani 1 1 d . . . . .
H12 H 0.334318 0.728092 0.446295 0.035 Uiso 1 1 calc R . . . .
C14 C 0.30323(19) 0.5862(2) 0.37529(10) 0.0300(7) Uani 1 1 d . . . . .
H14 H 0.326225 0.524293 0.385337 0.036 Uiso 1 1 calc R . . . .
C16 C 0.19312(17) 0.6787(3) 0.34342(10) 0.0301(6) Uani 1 1 d . . . . .
H16 H 0.143116 0.679053 0.332740 0.036 Uiso 1 1 calc R . . . .
C8 C 0.50493(17) 0.7797(3) 0.45875(9) 0.0303(6) Uani 1 1 d . . . . .
H8 H 0.543389 0.768974 0.447134 0.036 Uiso 1 1 calc R . . . .
C15 C 0.2284(2) 0.5878(3) 0.35853(12) 0.0364(8) Uani 1 1 d . . . . .
H15 H 0.201888 0.526562 0.357538 0.044 Uiso 1 1 calc R . . . .
C34 C 0.86897(17) 0.7178(3) 0.30849(12) 0.0338(7) Uani 1 1 d . . . . .
H34A H 0.879454 0.763409 0.288525 0.051 Uiso 1 1 calc GR . . . .
H34B H 0.881598 0.647577 0.303377 0.051 Uiso 1 1 calc GR . . . .
H34C H 0.896667 0.738956 0.334753 0.051 Uiso 1 1 calc GR . . . .
C20 C 0.4864(2) 0.5265(3) 0.37575(11) 0.0357(7) Uani 1 1 d . . . . .
H20 H 0.485363 0.562995 0.352199 0.043 Uiso 1 1 calc R . . . .
C9 C 0.51621(19) 0.8336(3) 0.49468(10) 0.0361(7) Uani 1 1 d . . . . .
H9 H 0.561989 0.860139 0.506788 0.043 Uiso 1 1 calc R . . . .
C35 C 0.70062(19) 0.9906(3) 0.40417(9) 0.0308(7) Uani 1 1 d . . . . .
C10 C 0.45977(19) 0.8485(3) 0.51281(10) 0.0335(7) Uani 1 1 d . . . . .
H10 H 0.467369 0.885132 0.536913 0.040 Uiso 1 1 calc R . . . .
C36 C 0.7724(2) 1.0008(3) 0.42635(10) 0.0341(7) Uani 1 1 d . . . . .
H36 H 0.788740 1.019820 0.453307 0.041 Uiso 1 1 calc R . . . .
C39 C 0.89546(18) 0.9750(3) 0.40804(10) 0.0342(7) Uani 1 1 d . . . . .
H39A H 0.911553 0.904233 0.407257 0.051 Uiso 1 1 calc GR . . . .
H39B H 0.916821 1.004250 0.434110 0.051 Uiso 1 1 calc GR . . . .
H39C H 0.909904 1.015075 0.387786 0.051 Uiso 1 1 calc GR . . . .
C11 C 0.39237(19) 0.8084(3) 0.49467(10) 0.0336(7) Uani 1 1 d . . . . .
H11 H 0.354497 0.817184 0.506894 0.040 Uiso 1 1 calc R . . . .
B1 B 0.78675(17) 0.9216(2) 0.32416(10) 0.0206(6) Uani 1 1 d . . . . .
C38 C 0.6332(2) 1.0076(4) 0.41805(12) 0.0456(9) Uani 1 1 d . . . . .
H38A H 0.609794 1.070487 0.406293 0.068 Uiso 1 1 calc GR . . . .
H38B H 0.645664 1.013446 0.446890 0.068 Uiso 1 1 calc GR . . . .
H38C H 0.600931 0.949609 0.409883 0.068 Uiso 1 1 calc GR . . . .
C21 C 0.5151(2) 0.4260(3) 0.38067(13) 0.0440(9) Uani 1 1 d . . . . .
H21 H 0.532734 0.395641 0.360475 0.053 Uiso 1 1 calc R . . . .
C24 C 0.4615(2) 0.5168(3) 0.44034(11) 0.0409(8) Uani 1 1 d . . . . .
H24 H 0.443733 0.546472 0.460643 0.049 Uiso 1 1 calc R . . . .
C22 C 0.5172(2) 0.3721(3) 0.41554(13) 0.0492(10) Uani 1 1 d . . . . .
H22 H 0.537082 0.305520 0.419181 0.059 Uiso 1 1 calc R . . . .
C23 C 0.4898(3) 0.4165(3) 0.44512(13) 0.0534(11) Uani 1 1 d . . . . .
H23 H 0.490353 0.379174 0.468412 0.064 Uiso 1 1 calc R . . . .
Cl11 Cl 0.66431(13) 0.6436(2) 0.41499(8) 0.0767(8) Uani 0.578(4) 1 d D . P A 1
C101 C 0.7289(4) 0.7237(6) 0.4150(2) 0.117(3) Uani 1 1 d D . . . .
H10A H 0.725976 0.778305 0.434093 0.141 Uiso 0.578(4) 1 calc R . P A 1
H10B H 0.717525 0.756117 0.388581 0.141 Uiso 0.578(4) 1 calc R . P A 1
H10C H 0.698224 0.669638 0.399734 0.141 Uiso 0.422(4) 1 calc R . P A 2
H10D H 0.721686 0.787034 0.398992 0.141 Uiso 0.422(4) 1 calc R . P A 2
Cl10 Cl 0.81554(12) 0.68740(15) 0.42507(9) 0.1202(8) Uani 1 1 d . . . . .
C33 C 0.60121(17) 0.6384(3) 0.29468(12) 0.0334(7) Uani 1 1 d . . . . .
H33A H 0.581042 0.655473 0.316796 0.050 Uiso 1 1 calc GR . . . .
H33B H 0.606770 0.564131 0.293421 0.050 Uiso 1 1 calc GR . . . .
H33C H 0.569334 0.662573 0.269973 0.050 Uiso 1 1 calc GR . . . .
Cl20 Cl 0.7044(3) 0.7466(5) 0.46295(19) 0.141(3) Uani 0.422(4) 1 d D . P A 2
H1 H 0.848(2) 0.921(3) 0.3281(11) 0.023(9) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 N3 2.213(2) . ?
W1 N1 2.280(2) . ?
W1 N5 2.217(2) . ?
W1 C6 2.012(3) . ?
W1 C5 2.004(3) . ?
W1 C1 1.837(3) . ?
CL11a C101 1.604(7) . ?
O2 C6 1.139(4) . ?
N2 N1 1.372(3) . ?
N2 C27 1.351(4) . ?
N2 B1 1.540(4) . ?
N4 N3 1.375(3) . ?
N4 C32 1.348(4) . ?
N4 B1 1.534(4) . ?
N3 C30 1.343(4) . ?
N1 C25 1.341(4) . ?
N5 N6 1.377(3) . ?
N5 C35 1.339(4) . ?
N6 C37 1.351(4) . ?
N6 B1 1.543(4) . ?
O1 C5 1.148(4) . ?
C27 C26 1.381(4) . ?
C27 C29 1.494(4) . ?
C13 C4 1.548(4) . ?
C13 C18 1.388(4) . ?
C13 C14 1.394(4) . ?
C32 C31 1.380(4) . ?
C32 C34 1.494(4) . ?
C25 C26 1.392(4) . ?
C25 C28 1.496(4) . ?
C3 C4 1.482(4) . ?
C3 C2 1.211(4) . ?
C4 C19 1.547(4) . ?
C4 C7 1.550(4) . ?
C26 H26 0.9300 . ?
C30 C31 1.395(4) . ?
C30 C33 1.494(4) . ?
C37 C36 1.386(5) . ?
C37 C39 1.493(4) . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C18 H18 0.9300 . ?
C18 C17 1.394(4) . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C2 C1 1.385(4) . ?
C31 H31 0.9300 . ?
C19 C20 1.393(5) . ?
C19 C24 1.387(5) . ?
C7 C12 1.383(4) . ?
C7 C8 1.400(4) . ?
C17 H17 0.9300 . ?
C17 C16 1.387(5) . ?
C12 H12 0.9300 . ?
C12 C11 1.395(4) . ?
C14 H14 0.9300 . ?
C14 C15 1.396(5) . ?
C16 H16 0.9300 . ?
C16 C15 1.379(5) . ?
C8 H8 0.9300 . ?
C8 C9 1.382(5) . ?
C15 H15 0.9300 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C20 H20 0.9300 . ?
C20 C21 1.392(5) . ?
C9 H9 0.9300 . ?
C9 C10 1.387(5) . ?
C35 C36 1.393(5) . ?
C35 C38 1.496(5) . ?
C10 H10 0.9300 . ?
C10 C11 1.377(5) . ?
C36 H36 0.9300 . ?
C39 H39A 0.9600 . ?
C39 H39B 0.9600 . ?
C39 H39C 0.9600 . ?
C11 H11 0.9300 . ?
B1 H1 1.15(4) . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
C21 H21 0.9300 . ?
C21 C22 1.374(6) . ?
C24 H24 0.9300 . ?
C24 C23 1.388(5) . ?
C22 H22 0.9300 . ?
C22 C23 1.378(6) . ?
C23 H23 0.9300 . ?
C101 H10A 0.9700 . ?
C101 H10B 0.9700 . ?
C101 H10C 0.9700 . ?
C101 H10D 0.9700 . ?
C101 Cl10 1.666(8) . ?
C101 Cl20 1.845(8) . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
CL11a C101 H10A 106.6 . . ?
N3 W1 N1 82.22(8) . . ?
H10Aa C101 H10B 106.6 . . ?
CL11a C101 H10B 106.6 . . ?
CL20b C101 H10C 109.9 . . ?
H10Cb C101 H10D 108.3 . . ?
CL20b C101 H10D 109.9 . . ?
N3 W1 N5 81.91(9) . . ?
CL11a C101 Cl10 122.8(5) . . ?
N5 W1 N1 81.77(9) . . ?
C6 W1 N3 94.36(10) . . ?
C6 W1 N1 90.95(10) . . ?
C6 W1 N5 172.19(10) . . ?
C5 W1 N3 172.90(11) . . ?
C5 W1 N1 91.31(11) . . ?
C5 W1 N5 94.32(11) . . ?
C5 W1 C6 88.65(13) . . ?
C1 W1 N3 100.38(11) . . ?
C1 W1 N1 176.23(10) . . ?
C1 W1 N5 101.25(11) . . ?
C1 W1 C6 86.14(12) . . ?
C1 W1 C5 86.22(13) . . ?
N1 N2 B1 120.5(2) . . ?
C27 N2 N1 109.4(2) . . ?
C27 N2 B1 130.1(2) . . ?
N3 N4 B1 120.2(2) . . ?
C32 N4 N3 109.3(2) . . ?
C32 N4 B1 130.4(2) . . ?
N4 N3 W1 121.00(17) . . ?
C30 N3 W1 131.8(2) . . ?
C30 N3 N4 107.2(2) . . ?
N2 N1 W1 119.39(17) . . ?
C25 N1 W1 133.51(19) . . ?
C25 N1 N2 106.9(2) . . ?
N6 N5 W1 120.58(17) . . ?
C35 N5 W1 132.3(2) . . ?
C35 N5 N6 107.1(2) . . ?
N5 N6 B1 120.4(2) . . ?
C37 N6 N5 109.5(2) . . ?
C37 N6 B1 130.0(3) . . ?
N2 C27 C26 108.0(3) . . ?
N2 C27 C29 123.3(3) . . ?
C26 C27 C29 128.7(3) . . ?
C18 C13 C4 119.1(2) . . ?
C18 C13 C14 118.6(3) . . ?
C14 C13 C4 122.1(3) . . ?
N4 C32 C31 108.1(3) . . ?
N4 C32 C34 123.2(3) . . ?
C31 C32 C34 128.6(3) . . ?
N1 C25 C26 109.7(3) . . ?
N1 C25 C28 122.9(3) . . ?
C26 C25 C28 127.3(3) . . ?
O2 C6 W1 179.0(3) . . ?
C2 C3 C4 173.7(3) . . ?
C13 C4 C7 110.4(2) . . ?
C3 C4 C13 109.0(2) . . ?
C3 C4 C19 108.6(2) . . ?
C3 C4 C7 106.8(2) . . ?
C19 C4 C13 111.4(2) . . ?
C19 C4 C7 110.5(2) . . ?
C27 C26 C25 105.9(3) . . ?
C27 C26 H26 127.1 . . ?
C25 C26 H26 127.1 . . ?
N3 C30 C31 109.2(3) . . ?
N3 C30 C33 122.6(3) . . ?
C31 C30 C33 128.1(3) . . ?
N6 C37 C36 107.6(3) . . ?
N6 C37 C39 123.2(3) . . ?
C36 C37 C39 129.1(3) . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C13 C18 H18 119.4 . . ?
C13 C18 C17 121.3(3) . . ?
C17 C18 H18 119.4 . . ?
C25 C28 H28A 109.5 . . ?
C25 C28 H28B 109.5 . . ?
C25 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
O1 C5 W1 178.1(3) . . ?
C3 C2 C1 175.0(3) . . ?
C2 C1 W1 177.8(2) . . ?
C32 C31 C30 106.1(3) . . ?
C32 C31 H31 126.9 . . ?
C30 C31 H31 126.9 . . ?
C20 C19 C4 120.4(3) . . ?
C24 C19 C4 121.3(3) . . ?
C24 C19 C20 118.3(3) . . ?
C12 C7 C4 122.2(3) . . ?
C12 C7 C8 118.8(3) . . ?
C8 C7 C4 119.0(3) . . ?
C18 C17 H17 120.1 . . ?
C16 C17 C18 119.7(3) . . ?
C16 C17 H17 120.1 . . ?
C7 C12 H12 119.9 . . ?
C7 C12 C11 120.2(3) . . ?
C11 C12 H12 119.9 . . ?
C13 C14 H14 120.0 . . ?
C13 C14 C15 119.9(3) . . ?
C15 C14 H14 120.0 . . ?
C17 C16 H16 120.3 . . ?
C15 C16 C17 119.4(3) . . ?
C15 C16 H16 120.3 . . ?
C7 C8 H8 119.8 . . ?
C9 C8 C7 120.5(3) . . ?
C9 C8 H8 119.8 . . ?
C14 C15 H15 119.5 . . ?
C16 C15 C14 121.1(3) . . ?
C16 C15 H15 119.5 . . ?
C32 C34 H34A 109.5 . . ?
C32 C34 H34B 109.5 . . ?
C32 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C19 C20 H20 119.5 . . ?
C21 C20 C19 121.0(3) . . ?
C21 C20 H20 119.5 . . ?
C8 C9 H9 119.8 . . ?
C8 C9 C10 120.5(3) . . ?
C10 C9 H9 119.8 . . ?
N5 C35 C36 109.6(3) . . ?
N5 C35 C38 122.3(3) . . ?
C36 C35 C38 128.1(3) . . ?
C9 C10 H10 120.4 . . ?
C11 C10 C9 119.2(3) . . ?
C11 C10 H10 120.4 . . ?
C37 C36 C35 106.2(3) . . ?
C37 C36 H36 126.9 . . ?
C35 C36 H36 126.9 . . ?
C37 C39 H39A 109.5 . . ?
C37 C39 H39B 109.5 . . ?
C37 C39 H39C 109.5 . . ?
H39A C39 H39B 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C12 C11 H11 119.6 . . ?
C10 C11 C12 120.9(3) . . ?
C10 C11 H11 119.6 . . ?
N2 B1 N6 108.6(2) . . ?
N2 B1 H1 110.6(18) . . ?
N4 B1 N2 109.7(2) . . ?
N4 B1 N6 108.4(2) . . ?
N4 B1 H1 109.5(17) . . ?
N6 B1 H1 110.0(18) . . ?
C35 C38 H38A 109.5 . . ?
C35 C38 H38B 109.5 . . ?
C35 C38 H38C 109.5 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C20 C21 H21 120.2 . . ?
C22 C21 C20 119.6(4) . . ?
C22 C21 H21 120.2 . . ?
C19 C24 H24 119.7 . . ?
C19 C24 C23 120.6(4) . . ?
C23 C24 H24 119.7 . . ?
C21 C22 H22 119.9 . . ?
C21 C22 C23 120.1(4) . . ?
C23 C22 H22 119.9 . . ?
C24 C23 H23 119.8 . . ?
C22 C23 C24 120.4(4) . . ?
C22 C23 H23 119.8 . . ?
Cl10 C101 H10A 106.6 . . ?
Cl10 C101 H10B 106.6 . . ?
Cl10 C101 H10C 109.9 . . ?
Cl10 C101 H10D 109.9 . . ?
Cl10 C101 Cl20 108.8(4) . . ?
C30 C33 H33A 109.5 . . ?
C30 C33 H33B 109.5 . . ?
C30 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?

_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 0.250 -0.094 0.000 157.2 36.1 ?
2 0.250 0.594 0.500 157.2 35.3 ?
3 0.750 0.406 0.500 157.2 36.1 ?
4 0.750 0.094 1.000 157.2 35.3 ?


_ins_header                      
'TITL WCCCCPh3scale in Ia REM Ia (#9 in standard setting) CELL 1.54184 19.066561 12.824714 34.322878 90.0000 104.7999 90.0000 ZERR 8.00 0.000245 0.000153 0.000484 0.0000 0.0014 0.0000 LATT -2 SYMM x+1/2,-y, z SFAC C H B N O W UNIT 312.00 288.00 8.00 48.00 16.00 8.00 TREF HKLF 4 END'
_olex2_submission_original_sample_id WCCCCPh3
_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 1.310
_oxdiff_exptl_absorpt_empirical_full_min 0.809

####################################################################### 
# 
# 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_ram-43_scale
_database_code_depnum_ccdc_archive 'CCDC 1897317'
loop_
_audit_author_name
_audit_author_address
'Richard Manzano'
;Australian National University
Australia
;
#Added by publCIF



_audit_update_record             
;
2019-02-15 deposited with the CCDC.	2019-04-23 downloaded from the CCDC.
;
_audit_creation_date             2018-02-14
_audit_creation_method           
;
Olex2 1.2
(compiled Aug 10 2017 17:28:52 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2016/4
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C38 H37 B Ge N6 O2 W, C H Cl3'
_chemical_formula_sum            'C39 H38 B Cl3 Ge N6 O2 W'
_chemical_formula_weight         996.35
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C38 H36 B1 Ge1 N6 O2 W1'
_chemical_oxdiff_usercomment     
'Crystals grown from chloroform/ethanol evaporation at 0 degrees celcius'
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'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge -1.0885 0.8855 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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/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                   15.9977(2)
_cell_length_b                   12.82720(10)
_cell_length_c                   19.7393(2)
_cell_angle_alpha                90
_cell_angle_beta                 95.3800(10)
_cell_angle_gamma                90
_cell_volume                     4032.77(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    29820
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      73.7150
_cell_measurement_theta_min      4.1170
_shelx_estimated_absorpt_T_max   0.733
_shelx_estimated_absorpt_T_min   0.292
_exptl_absorpt_coefficient_mu    8.275
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66225
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)

Empirical absorption correction using spherical harmonics,

 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.641
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1968
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 2 -13 0.0323
2 -2 -12 0.0298
-2 3 12 0.0371
-1 -2 13 0.0323
-1 8 0 0.0994
1 -8 0 0.0994
-10 0 0 0.0245
10 0 1 0.0141
-9 1 -5 0.0251
-7 -3 9 0.0298

_exptl_crystal_preparation       ?
_exptl_crystal_recrystallization_method 
'Crystals were grown from slow evaporation of a ethanol/chloroform solution at 0 degrees celcius.'
_exptl_crystal_size_max          0.197
_exptl_crystal_size_mid          0.065
_exptl_crystal_size_min          0.04
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
1.0009 2.0019 -12.9938 -0.0481 -0.2015 1.0212
1.9967 -1.9995 -11.9977 -0.1872 -0.5931 0.7473
-1.9956 2.9999 11.9984 0.1974 0.7018 -0.6972
-1.0009 -2.0019 12.9938 0.0481 0.2015 -1.0212
-0.9911 8.0027 0.0062 0.1778 0.8595 0.4033
0.9911 -8.0027 -0.0062 -0.1778 -0.8595 -0.4033
-10.0024 -0.0004 0.0074 0.9619 -0.1024 0.0243
10.0026 0.0003 0.9922 -0.9640 0.1354 -0.0953
-9.0017 1.0004 -4.9905 0.8866 -0.1485 0.4271
-7.0040 -3.0021 8.9993 0.6235 -0.1007 -0.7726

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0350
_diffrn_reflns_av_unetI/netI     0.0203
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            59421
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.885
_diffrn_reflns_theta_min         4.116
_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 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):



  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames

#--------------------------------------------------------------------------

  1  ω     -3.00  38.00   1.00    2.50    --   37.04 -57.00 -30.00   41

  2  ω      6.00  40.00   1.00    2.50    --   37.04 -57.00 -60.00   34

  3  ω     44.00  71.00   1.00    2.50    --   37.04 -99.00   0.00   27

  4  ω     43.00  89.00   1.00    2.50    --   37.04-125.00   0.00   46

  5  ω     54.00  83.00   1.00    2.50    --   37.04-125.00  90.00   29

  6  ω     29.00  82.00   1.00    2.50    --   37.04-125.00 -30.00   53

  7  ω     49.00  89.00   1.00    2.50    --   37.04-125.00 -90.00   40

  8  ω     83.00 109.00   1.00   10.00    --  111.00 -77.00 -60.00   26

  9  ω    115.00 141.00   1.00   10.00    --  111.00 -92.00 -90.00   26

 10  ω    112.00 138.00   1.00   10.00    --  111.00 -77.00-150.00   26

 11  ω    121.00 146.00   1.00   10.00    --  111.00 -92.00-150.00   25

 12  ω    102.00 136.00   1.00   10.00    --  111.00 -25.00-150.00   34

 13  ω     86.00 124.00   1.00   10.00    --  111.00 -38.00 -90.00   38

 14  ω     87.00 126.00   1.00   10.00    --  111.00 -46.00-162.59   39

 15  ω     75.00 109.00   1.00   10.00    --  111.00-111.00 -90.00   34

 16  ω     91.00 116.00   1.00   10.00    --  111.00-111.00 -30.00   25

 17  ω     81.00 116.00   1.00   10.00    --  111.00-111.00  60.00   35

 18  ω     84.00 113.00   1.00   10.00    --  111.00-111.00 120.00   29

 19  ω     87.00 113.00   1.00   10.00    --  111.00 -77.00  60.00   26

 20  ω    103.00 130.00   1.00   10.00    --  111.00 -64.00  60.00   27

 21  ω     85.00 114.00   1.00   10.00    --  111.00 -50.00  30.00   29

 22  ω     76.00 112.00   1.00   10.00    --  111.00 -38.00  60.00   36

 23  ω     73.00 119.00   1.00   10.00    --  111.00 -64.00  30.00   46

 24  ω     73.00 116.00   1.00   10.00    --  111.00-111.00  90.00   43

 25  ω     75.00 100.00   1.00   10.00    --  111.00-111.00 150.00   25

 26  ω     73.00 105.00   1.00   10.00    --  111.00 -77.00 150.00   32

 27  ω     57.00  93.00   1.00   10.00    --  111.00 -50.00 120.00   36

 28  ω     46.00  71.00   1.00   10.00    --  111.00 -77.00  60.00   25

 29  ω     63.00 116.00   1.00   10.00    --  111.00-111.00  30.00   53

 30  ω     63.00  91.00   1.00   10.00    --  111.00 -38.00   0.00   28

 31  ω     66.00 131.00   1.00   10.00    --  111.00 -64.00 -60.00   65

 32  ω     65.00 113.00   1.00   10.00    --  111.00-111.00 -60.00   48

 33  ω     63.00  92.00   1.00   10.00    --  111.00 -77.00-150.00   29

 34  ω     62.00 114.00   1.00   10.00    --  111.00-111.00-180.00   52

 35  ω     56.00 116.00   1.00   10.00    --  111.00-111.00-120.00   60

 36  ω     50.00  80.00   1.00   10.00    --  111.00 -92.00 -90.00   30

 37  ω     46.00  88.00   1.00   10.00    --  111.00 -50.00 -60.00   42

 38  ω     47.00  73.00   1.00   10.00    --  111.00 -38.00 -90.00   26

 39  ω     44.00  95.00   1.00   10.00    --  111.00 -50.00-120.00   51

 40  ω     56.00 145.00   1.00   10.00    --  111.00 -12.00-180.00   89

 41  ω    150.00 177.00   1.00   10.00    --  111.00  50.00 -90.00   27

 42  ω    147.00 172.00   1.00   10.00    --  111.00 111.00 -90.00   25

 43  ω    128.00 176.00   1.00   10.00    --  111.00  77.00-180.00   48

 44  ω    110.00 136.00   1.00   10.00    --  111.00  77.00 -60.00   26

 45  ω     97.00 124.00   1.00   10.00    --  111.00  64.00 -60.00   27

 46  ω     92.00 126.00   1.00   10.00    --  111.00  38.00   0.00   34

 47  ω    137.00 163.00   1.00   10.00    --  111.00  38.00  30.00   26

 48  ω    125.00 174.00   1.00   10.00    --  111.00  77.00  30.00   49

 49  ω    129.00 176.00   1.00   10.00    --  111.00  25.00 150.00   47

 50  ω    107.00 133.00   1.00   10.00    --  111.00  25.00  30.00   26

 51  ω     93.00 127.00   1.00   10.00    --  111.00  38.00  30.00   34

 52  ω     90.00 118.00   1.00   10.00    --  111.00  77.00  30.00   28

 53  ω     87.00 112.00   1.00   10.00    --  111.00  25.00 150.00   25

 54  ω     42.00 135.00   1.00   10.00    --  111.00 -25.00  90.00   93

 55  ω     79.00 104.00   1.00    2.50    --   37.04  38.00  90.00   25

 56  ω     41.00 149.00   1.00   10.00    --  111.00 -14.00 -27.32  108

 57  ω     94.00 142.00   1.00   10.00    --  111.00  50.00 -90.00   48

 58  ω     69.00  99.00   1.00    2.50    --   37.04  57.00 -90.00   30

 59  ω     66.00 101.00   1.00    2.50    --   37.04  57.00-150.00   35

 60  ω     41.00  75.00   1.00    2.50    --   37.04  57.00-180.00   34

 61  ω     22.00 104.00   1.00    2.50    --   37.04  57.00-120.00   82

 62  ω     44.00  87.00   1.00   10.00    --  111.00 -50.00-180.00   43

 63  ω     69.00 141.00   1.00   10.00    --  111.00  12.00 -90.00   72

 64  ω     42.00  67.00   1.00   10.00    --  111.00-111.00 -90.00   25

 65  ω     47.00  94.00   1.00   10.00    --  111.00 -92.00-150.00   47

 66  ω     46.00  73.00   1.00   10.00    --  111.00 -77.00-180.00   27

 67  ω     48.00  80.00   1.00   10.00    --  111.00 -25.00-150.00   32

 68  ω     21.00  65.00   1.00    2.50    --   37.04  57.00-150.00   44

 69  ω     22.00  48.00   1.00    2.50    --   37.04  57.00 -90.00   26

 70  ω    -30.00  21.00   1.00    2.50    --   37.04 -57.00  60.00   51

 71  ω     25.00  84.00   1.00    2.50    --   37.04-125.00 150.00   59

 72  ω     42.00  67.00   1.00   10.00    --  111.00-111.00 150.00   25

 73  ω     20.00  57.00   1.00    2.50    --   37.04  38.00  90.00   37

 74  ω     -1.00  32.00   1.00    2.50    --  -37.04  38.00 120.00   33

 75  ω    -66.00 -41.00   1.00    2.50    --  -37.04 -57.00  30.00   25

 76  ω    -34.00  61.00   1.00    2.50    --   37.04 -19.00 -90.00   95

 77  ω    -48.00   0.00   1.00    2.50    --  -37.04  57.00-180.00   48

 78  ω    -65.00 -40.00   1.00    2.50    --  -37.04 -38.00-180.00   25

 79  ω    112.00 137.00   1.00   10.00    --  111.00 178.00-180.00   25

 80  ω    118.00 144.00   1.00   10.00    --  111.00 178.00  30.00   26
;
_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      -0.0961683000
_diffrn_orient_matrix_UB_12      0.0103029000
_diffrn_orient_matrix_UB_13      -0.0021221000
_diffrn_orient_matrix_UB_21      0.0102588000
_diffrn_orient_matrix_UB_22      0.1086404000
_diffrn_orient_matrix_UB_23      0.0330319000
_diffrn_orient_matrix_UB_31      -0.0024841000
_diffrn_orient_matrix_UB_32      0.0501378000
_diffrn_orient_matrix_UB_33      -0.0710552000
_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                7495
_reflns_number_total             8148
_reflns_odcompleteness_completeness 98.93
_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 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         1.843
_refine_diff_density_min         -0.878
_refine_diff_density_rms         0.112
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     524
_refine_ls_number_reflns         8148
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0388
_refine_ls_R_factor_gt           0.0358
_refine_ls_restrained_S_all      1.034
_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)+(0.0627P)²+6.7078P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0953
_refine_ls_wR_factor_ref         0.0989
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl2-C100
 1.75 with sigma of 0.02
 Cl3-C100 = Cl1-C100 = Cl2-C100
 1.75 with sigma of 0.02
 Cl6-C200 = Cl5-C200
 1.75 with sigma of 0.02
3. Others
 Fixed Sof: Cl3(0.5) Cl2(0.5) Cl5(0.5) Cl6(0.5) Cl1(0.5) Cl4(0.5) C100(0.5)
 H100(0.5) C200(0.5) H200(0.5)
4.a Ternary CH refined with riding coordinates:
 C100(H100), C200(H200)
4.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C13(H13), C14(H14), C15(H15),
 C16(H16), C17(H17), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C25(H25),
  C30(H30), C35(H35)
4.c Idealised Me refined as rotating group:
 C27(H27a,H27b,H27c), C28(H28a,H28b,H28c), C32(H32a,H32b,H32c), C33(H33a,H33b,
 H33c), C37(H37a,H37b,H37c), C38(H38a,H38b,H38c)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.86802(2) 0.32929(2) 0.16016(2) 0.02861(7) Uani 1 1 d . . . . .
Ge1 Ge 0.68635(3) 0.58612(4) 0.37712(2) 0.03622(11) Uani 1 1 d . . . . .
O1 O 1.03506(19) 0.3778(3) 0.25212(15) 0.0481(7) Uani 1 1 d . . . . .
O2 O 0.8517(2) 0.1303(3) 0.25208(18) 0.0598(9) Uani 1 1 d . . . . .
N1 N 0.93748(18) 0.2406(2) 0.08303(14) 0.0282(6) Uani 1 1 d . . . . .
N2 N 0.91131(19) 0.2511(2) 0.01497(14) 0.0292(6) Uani 1 1 d . . . . .
N3 N 0.88259(19) 0.4577(2) 0.08805(14) 0.0304(6) Uani 1 1 d . . . . .
N4 N 0.87304(19) 0.4411(2) 0.01878(14) 0.0304(6) Uani 1 1 d . . . . .
N5 N 0.7576(2) 0.2935(3) 0.08751(16) 0.0350(6) Uani 1 1 d . . . . .
N6 N 0.7613(2) 0.3048(3) 0.01852(16) 0.0350(6) Uani 1 1 d . . . . .
C1 C 0.8162(2) 0.4000(3) 0.22613(18) 0.0348(7) Uani 1 1 d . . . . .
C2 C 0.7809(2) 0.4532(3) 0.27699(19) 0.0349(7) Uani 1 1 d . . . . .
C3 C 0.7484(2) 0.5045(3) 0.3178(2) 0.0404(8) Uani 1 1 d . . . . .
C4 C 0.9756(2) 0.3611(3) 0.21757(18) 0.0344(7) Uani 1 1 d . . . . .
C5 C 0.8577(3) 0.2007(3) 0.2174(2) 0.0394(8) Uani 1 1 d . . . . .
C6 C 0.6845(3) 0.7299(4) 0.3443(2) 0.0439(9) Uani 1 1 d . . . . .
C7 C 0.7358(3) 0.7616(4) 0.2960(2) 0.0523(11) Uani 1 1 d . . . . .
H7 H 0.771085 0.712133 0.276971 0.063 Uiso 1 1 calc R . . . .
C8 C 0.7368(4) 0.8648(5) 0.2748(3) 0.0652(14) Uani 1 1 d . . . . .
H8 H 0.773548 0.885421 0.242141 0.078 Uiso 1 1 calc R . . . .
C9 C 0.6855(4) 0.9370(5) 0.3006(3) 0.0697(15) Uani 1 1 d . . . . .
H9 H 0.686008 1.007471 0.285728 0.084 Uiso 1 1 calc R . . . .
C10 C 0.6328(5) 0.9062(6) 0.3485(4) 0.086(2) Uani 1 1 d . . . . .
H10 H 0.596371 0.955399 0.366497 0.104 Uiso 1 1 calc R . . . .
C11 C 0.6332(4) 0.8040(4) 0.3703(3) 0.0679(15) Uani 1 1 d . . . . .
H11 H 0.597430 0.783969 0.403819 0.081 Uiso 1 1 calc R . . . .
C12 C 0.7425(2) 0.5782(3) 0.46868(19) 0.0348(7) Uani 1 1 d . . . . .
C13 C 0.7602(3) 0.6667(3) 0.5083(2) 0.0461(10) Uani 1 1 d . . . . .
H13 H 0.745650 0.733735 0.490380 0.055 Uiso 1 1 calc R . . . .
C14 C 0.7988(3) 0.6574(4) 0.5738(2) 0.0502(11) Uani 1 1 d . . . . .
H14 H 0.810223 0.718110 0.600627 0.060 Uiso 1 1 calc R . . . .
C15 C 0.8210(3) 0.5600(4) 0.6005(2) 0.0456(9) Uani 1 1 d . . . . .
H15 H 0.847823 0.554021 0.645407 0.055 Uiso 1 1 calc R . . . .
C16 C 0.8041(3) 0.4732(4) 0.5620(2) 0.0457(9) Uani 1 1 d . . . . .
H16 H 0.819065 0.406495 0.580232 0.055 Uiso 1 1 calc R . . . .
C17 C 0.7649(3) 0.4815(3) 0.4957(2) 0.0419(9) Uani 1 1 d . . . . .
H17 H 0.753555 0.420412 0.469248 0.050 Uiso 1 1 calc R . . . .
C18 C 0.5764(2) 0.5205(4) 0.3734(2) 0.0430(9) Uani 1 1 d . . . . .
C19 C 0.5542(3) 0.4416(5) 0.3278(3) 0.0664(15) Uani 1 1 d . . . . .
H19 H 0.592439 0.420671 0.296443 0.080 Uiso 1 1 calc R . . . .
C20 C 0.4766(4) 0.3922(6) 0.3270(4) 0.085(2) Uani 1 1 d . . . . .
H20 H 0.463061 0.336048 0.296558 0.102 Uiso 1 1 calc R . . . .
C21 C 0.4202(4) 0.4249(6) 0.3704(3) 0.0768(18) Uani 1 1 d . . . . .
H21 H 0.367173 0.391469 0.369947 0.092 Uiso 1 1 calc R . . . .
C22 C 0.4397(3) 0.5052(6) 0.4141(3) 0.0722(16) Uani 1 1 d . . . . .
H22 H 0.399294 0.530298 0.442483 0.087 Uiso 1 1 calc R . . . .
C23 C 0.5190(3) 0.5504(5) 0.4170(3) 0.0631(13) Uani 1 1 d . . . . .
H23 H 0.533627 0.602971 0.449842 0.076 Uiso 1 1 calc R . . . .
C24 C 0.9978(2) 0.1674(3) 0.0880(2) 0.0329(7) Uani 1 1 d . . . . .
C25 C 1.0109(2) 0.1310(3) 0.0231(2) 0.0356(8) Uani 1 1 d . . . . .
H25 H 1.050285 0.079796 0.011996 0.043 Uiso 1 1 calc R . . . .
C26 C 0.9550(3) 0.1844(3) -0.02149(19) 0.0331(7) Uani 1 1 d . . . . .
C27 C 1.0402(3) 0.1318(4) 0.1546(2) 0.0451(9) Uani 1 1 d . . . . .
H27A H 1.057455 0.192604 0.182554 0.068 Uiso 1 1 calc GR . . . .
H27B H 1.089784 0.090292 0.146643 0.068 Uiso 1 1 calc GR . . . .
H27C H 1.001250 0.089189 0.178245 0.068 Uiso 1 1 calc GR . . . .
C28 C 0.9404(3) 0.1741(3) -0.0971(2) 0.0441(10) Uani 1 1 d . . . . .
H28A H 0.885211 0.142547 -0.109234 0.066 Uiso 1 1 calc GR . . . .
H28B H 0.984067 0.129675 -0.113573 0.066 Uiso 1 1 calc GR . . . .
H28C H 0.942343 0.243152 -0.118075 0.066 Uiso 1 1 calc GR . . . .
C29 C 0.9041(2) 0.5583(3) 0.09734(19) 0.0338(7) Uani 1 1 d . . . . .
C30 C 0.9081(2) 0.6056(3) 0.0349(2) 0.0364(8) Uani 1 1 d . . . . .
H30 H 0.921616 0.676430 0.026931 0.044 Uiso 1 1 calc R . . . .
C31 C 0.8887(2) 0.5298(3) -0.01361(19) 0.0333(7) Uani 1 1 d . . . . .
C32 C 0.9201(3) 0.6050(3) 0.1667(2) 0.0440(9) Uani 1 1 d . . . . .
H32A H 0.874363 0.586179 0.194084 0.066 Uiso 1 1 calc GR . . . .
H32B H 0.923201 0.681040 0.162864 0.066 Uiso 1 1 calc GR . . . .
H32C H 0.973361 0.578388 0.188701 0.066 Uiso 1 1 calc GR . . . .
C33 C 0.8840(3) 0.5398(3) -0.0891(2) 0.0436(9) Uani 1 1 d . . . . .
H33A H 0.928615 0.497962 -0.106480 0.065 Uiso 1 1 calc GR . . . .
H33B H 0.891186 0.613085 -0.101310 0.065 Uiso 1 1 calc GR . . . .
H33C H 0.829264 0.514944 -0.109054 0.065 Uiso 1 1 calc GR . . . .
C34 C 0.6786(3) 0.2665(4) 0.0971(2) 0.0498(10) Uani 1 1 d . . . . .
C35 C 0.6317(3) 0.2609(5) 0.0336(3) 0.0587(12) Uani 1 1 d . . . . .
H35 H 0.573924 0.243447 0.025313 0.070 Uiso 1 1 calc R . . . .
C36 C 0.6858(3) 0.2856(4) -0.0144(2) 0.0464(9) Uani 1 1 d . . . . .
C37 C 0.6506(3) 0.2455(6) 0.1658(3) 0.0712(17) Uani 1 1 d . . . . .
H37A H 0.679083 0.183156 0.185175 0.107 Uiso 1 1 calc GR . . . .
H37B H 0.589747 0.234272 0.161844 0.107 Uiso 1 1 calc GR . . . .
H37C H 0.664625 0.305327 0.195653 0.107 Uiso 1 1 calc GR . . . .
C38 C 0.6691(3) 0.2902(5) -0.0906(2) 0.0589(12) Uani 1 1 d . . . . .
H38A H 0.678650 0.361403 -0.106192 0.088 Uiso 1 1 calc GR . . . .
H38B H 0.610780 0.270124 -0.103899 0.088 Uiso 1 1 calc GR . . . .
H38C H 0.707009 0.242233 -0.111268 0.088 Uiso 1 1 calc GR . . . .
B1 B 0.8452(3) 0.3334(3) -0.0093(2) 0.0321(8) Uani 1 1 d . . . . .
H1 H 0.838(3) 0.335(4) -0.058(3) 0.045(14) Uiso 1 1 d . . . . .
Cl3 Cl 0.6747(3) 0.6456(3) 0.1538(2) 0.0954(11) Uani 0.5 1 d D . P A 1
Cl2 Cl 0.5556(3) 0.4836(4) 0.1226(3) 0.1082(13) Uani 0.5 1 d D . P A 1
Cl5 Cl 0.5714(4) 0.5899(5) 0.1842(2) 0.137(2) Uani 0.5 1 d D . P B 2
Cl6 Cl 0.5355(3) 0.5920(9) 0.0412(3) 0.208(5) Uani 0.5 1 d D . P B 2
Cl1 Cl 0.6638(2) 0.5542(3) 0.02172(18) 0.0802(8) Uani 0.5 1 d D . P A 1
Cl4 Cl 0.7024(3) 0.5668(5) 0.0983(5) 0.161(3) Uani 0.5 1 d . . P B 2
C100 C 0.6493(7) 0.5337(9) 0.1070(6) 0.070(3) Uani 0.5 1 d D . P A 1
H100 H 0.692014 0.480403 0.123619 0.084 Uiso 0.5 1 calc R . P A 1
C200 C 0.6108(10) 0.614(4) 0.1088(8) 0.31(3) Uani 0.5 1 d D . P B 2
H200 H 0.619360 0.691209 0.108689 0.376 Uiso 0.5 1 calc R . 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 N1 2.273(3) . ?
W1 N3 2.204(3) . ?
W1 N5 2.217(3) . ?
W1 C1 1.846(4) . ?
W1 C4 2.012(4) . ?
W1 C5 2.014(4) . ?
CL1a C100 1.741(11) . ?
CL3a C100 1.734(11) . ?
CL2a C100 1.686(10) . ?
C100a H100 1.0000 . ?
CL6b C200 1.735(17) . ?
CL4b C200 1.62(3) . ?
CL5b C200 1.697(15) . ?
C200b H200 1.0000 . ?
Ge1 C3 1.915(4) . ?
Ge1 C6 1.955(5) . ?
Ge1 C12 1.944(4) . ?
Ge1 C18 1.945(4) . ?
O1 C4 1.138(5) . ?
O2 C5 1.143(5) . ?
N1 N2 1.376(4) . ?
N1 C24 1.343(5) . ?
N2 C26 1.354(4) . ?
N2 B1 1.538(5) . ?
N3 N4 1.378(4) . ?
N3 C29 1.344(5) . ?
N4 C31 1.340(5) . ?
N4 B1 1.539(5) . ?
N5 N6 1.376(4) . ?
N5 C34 1.340(5) . ?
N6 C36 1.341(5) . ?
N6 B1 1.541(5) . ?
C1 C2 1.378(5) . ?
C2 C3 1.197(6) . ?
C6 C7 1.375(6) . ?
C6 C11 1.385(7) . ?
C7 H7 0.9500 . ?
C7 C8 1.389(8) . ?
C8 H8 0.9500 . ?
C8 C9 1.367(9) . ?
C9 H9 0.9500 . ?
C9 C10 1.383(9) . ?
C10 H10 0.9500 . ?
C10 C11 1.379(9) . ?
C11 H11 0.9500 . ?
C12 C13 1.393(6) . ?
C12 C17 1.384(6) . ?
C13 H13 0.9500 . ?
C13 C14 1.384(7) . ?
C14 H14 0.9500 . ?
C14 C15 1.390(7) . ?
C15 H15 0.9500 . ?
C15 C16 1.360(6) . ?
C16 H16 0.9500 . ?
C16 C17 1.401(6) . ?
C17 H17 0.9500 . ?
C18 C19 1.378(7) . ?
C18 C23 1.371(6) . ?
C19 H19 0.9500 . ?
C19 C20 1.392(8) . ?
C20 H20 0.9500 . ?
C20 C21 1.367(10) . ?
C21 H21 0.9500 . ?
C21 C22 1.361(10) . ?
C22 H22 0.9500 . ?
C22 C23 1.391(8) . ?
C23 H23 0.9500 . ?
C24 C25 1.398(5) . ?
C24 C27 1.493(5) . ?
C25 H25 0.9500 . ?
C25 C26 1.377(6) . ?
C26 C28 1.495(5) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 C30 1.381(5) . ?
C29 C32 1.495(5) . ?
C30 H30 0.9500 . ?
C30 C31 1.380(5) . ?
C31 C33 1.490(5) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 C35 1.400(7) . ?
C34 C37 1.494(7) . ?
C35 H35 0.9500 . ?
C35 C36 1.380(7) . ?
C36 C38 1.503(6) . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
B1 H1 0.97(5) . ?

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
CL2a C100a Cl3 112.7(7) . . ?
N3 W1 N1 81.57(10) . . ?
N3 W1 N5 82.14(12) . . ?
CL4b C200b Cl5 117.4(17) . . ?
CL4b C200b Cl6 114.4(18) . . ?
N5 W1 N1 82.70(11) . . ?
C1 W1 N1 177.05(14) . . ?
CL5b C200b Cl6 110.9(11) . . ?
CL3a C100a Cl1 110.1(6) . . ?
C1 W1 N3 99.81(14) . . ?
C1 W1 N5 100.05(14) . . ?
CL2a C100a Cl1 115.9(7) . . ?
C1 W1 C4 85.43(15) . . ?
CL2a C100a H100 105.8 . . ?
CL1a C100a H100 105.8 . . ?
CL3a C100a H100 105.8 . . ?
CL5b C200b H200 104.1 . . ?
C1 W1 C5 86.59(16) . . ?
C4 W1 N1 91.88(12) . . ?
CL4b C200b H200 104.1 . . ?
CL6b C200b H200 104.1 . . ?
C4 W1 N3 94.34(13) . . ?
C4 W1 N5 173.90(13) . . ?
C4 W1 C5 87.75(16) . . ?
C5 W1 N1 92.11(13) . . ?
C5 W1 N3 173.39(13) . . ?
C5 W1 N5 95.21(15) . . ?
C3 Ge1 C6 107.81(18) . . ?
C3 Ge1 C12 108.58(17) . . ?
C3 Ge1 C18 105.00(18) . . ?
C12 Ge1 C6 110.44(17) . . ?
C12 Ge1 C18 110.50(17) . . ?
C18 Ge1 C6 114.20(19) . . ?
N2 N1 W1 118.8(2) . . ?
C24 N1 W1 134.0(2) . . ?
C24 N1 N2 106.9(3) . . ?
N1 N2 B1 120.5(3) . . ?
C26 N2 N1 109.4(3) . . ?
C26 N2 B1 130.0(3) . . ?
N4 N3 W1 121.1(2) . . ?
C29 N3 W1 132.1(2) . . ?
C29 N3 N4 106.7(3) . . ?
N3 N4 B1 119.8(3) . . ?
C31 N4 N3 109.5(3) . . ?
C31 N4 B1 130.6(3) . . ?
N6 N5 W1 120.8(2) . . ?
C34 N5 W1 131.9(3) . . ?
C34 N5 N6 107.2(3) . . ?
N5 N6 B1 119.8(3) . . ?
C36 N6 N5 109.9(3) . . ?
C36 N6 B1 130.3(3) . . ?
C2 C1 W1 177.5(3) . . ?
C3 C2 C1 175.4(4) . . ?
C2 C3 Ge1 174.3(4) . . ?
O1 C4 W1 177.4(3) . . ?
O2 C5 W1 177.3(4) . . ?
C7 C6 Ge1 121.1(4) . . ?
C7 C6 C11 117.8(5) . . ?
C11 C6 Ge1 121.0(4) . . ?
C6 C7 H7 119.5 . . ?
C6 C7 C8 121.0(5) . . ?
C8 C7 H7 119.5 . . ?
C7 C8 H8 119.7 . . ?
C9 C8 C7 120.6(5) . . ?
C9 C8 H8 119.7 . . ?
C8 C9 H9 120.4 . . ?
C8 C9 C10 119.1(6) . . ?
C10 C9 H9 120.4 . . ?
C9 C10 H10 120.0 . . ?
C11 C10 C9 120.0(6) . . ?
C11 C10 H10 120.0 . . ?
C6 C11 H11 119.3 . . ?
C10 C11 C6 121.5(6) . . ?
C10 C11 H11 119.3 . . ?
C13 C12 Ge1 122.1(3) . . ?
C17 C12 Ge1 119.1(3) . . ?
C17 C12 C13 118.8(4) . . ?
C12 C13 H13 119.9 . . ?
C14 C13 C12 120.2(4) . . ?
C14 C13 H13 119.9 . . ?
C13 C14 H14 119.7 . . ?
C13 C14 C15 120.6(4) . . ?
C15 C14 H14 119.7 . . ?
C14 C15 H15 120.2 . . ?
C16 C15 C14 119.5(4) . . ?
C16 C15 H15 120.2 . . ?
C15 C16 H16 119.7 . . ?
C15 C16 C17 120.5(4) . . ?
C17 C16 H16 119.7 . . ?
C12 C17 C16 120.3(4) . . ?
C12 C17 H17 119.8 . . ?
C16 C17 H17 119.8 . . ?
C19 C18 Ge1 121.3(3) . . ?
C23 C18 Ge1 120.8(4) . . ?
C23 C18 C19 117.9(5) . . ?
C18 C19 H19 119.4 . . ?
C18 C19 C20 121.2(5) . . ?
C20 C19 H19 119.4 . . ?
C19 C20 H20 120.2 . . ?
C21 C20 C19 119.5(6) . . ?
C21 C20 H20 120.2 . . ?
C20 C21 H21 119.9 . . ?
C22 C21 C20 120.3(5) . . ?
C22 C21 H21 119.9 . . ?
C21 C22 H22 120.2 . . ?
C21 C22 C23 119.6(5) . . ?
C23 C22 H22 120.2 . . ?
C18 C23 C22 121.4(6) . . ?
C18 C23 H23 119.3 . . ?
C22 C23 H23 119.3 . . ?
N1 C24 C25 109.6(3) . . ?
N1 C24 C27 122.8(3) . . ?
C25 C24 C27 127.6(4) . . ?
C24 C25 H25 127.0 . . ?
C26 C25 C24 106.0(3) . . ?
C26 C25 H25 127.0 . . ?
N2 C26 C25 108.1(3) . . ?
N2 C26 C28 123.2(4) . . ?
C25 C26 C28 128.7(4) . . ?
C24 C27 H27A 109.5 . . ?
C24 C27 H27B 109.5 . . ?
C24 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
N3 C29 C30 109.5(3) . . ?
N3 C29 C32 122.0(3) . . ?
C30 C29 C32 128.5(4) . . ?
C29 C30 H30 126.8 . . ?
C31 C30 C29 106.4(3) . . ?
C31 C30 H30 126.8 . . ?
N4 C31 C30 107.9(3) . . ?
N4 C31 C33 123.8(3) . . ?
C30 C31 C33 128.3(4) . . ?
C29 C32 H32A 109.5 . . ?
C29 C32 H32B 109.5 . . ?
C29 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
N5 C34 C35 108.7(4) . . ?
N5 C34 C37 122.8(4) . . ?
C35 C34 C37 128.5(4) . . ?
C34 C35 H35 126.7 . . ?
C36 C35 C34 106.6(4) . . ?
C36 C35 H35 126.7 . . ?
N6 C36 C35 107.7(4) . . ?
N6 C36 C38 123.1(4) . . ?
C35 C36 C38 129.3(4) . . ?
C34 C37 H37A 109.5 . . ?
C34 C37 H37B 109.5 . . ?
C34 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C36 C38 H38A 109.5 . . ?
C36 C38 H38B 109.5 . . ?
C36 C38 H38C 109.5 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
N2 B1 N4 109.7(3) . . ?
N2 B1 N6 108.8(3) . . ?
N2 B1 H1 110(3) . . ?
N4 B1 N6 108.5(3) . . ?
N4 B1 H1 110(3) . . ?
N6 B1 H1 109(3) . . ?


_ins_header                      
;
TITL RAM-43_scale in P2(1)/c 

REM P2(1)/c (#14 in standard setting)

CELL 1.54184  15.997741  12.827151  19.739328  90.0000  95.3795  90.0000

ZERR    4.00   0.000155   0.000127   0.000151   0.0000   0.0008   0.0000

LATT  1

SYMM -x, y+1/2,-z+1/2 

SFAC C H B N O Ge W

UNIT 152.00 144.00 4.00 24.00 8.00 4.00 4.00

TREF

HKLF 4

END
;
_olex2_submission_original_sample_id RAM-43
_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 1.473
_oxdiff_exptl_absorpt_empirical_full_min 0.719

####################################################################### 
# 
# 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_ram-138scaleabscorrect3
_database_code_depnum_ccdc_archive 'CCDC 1897700'
loop_
_audit_author_name
_audit_author_address
'Richard Manzano'
;Australian National University
Australia
;
_audit_update_record             
;
2019-02-18 deposited with the CCDC.	2019-04-23 downloaded from the CCDC.
;
_audit_creation_date             2019-02-18
_audit_creation_method           
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
a.hill@anu.edu.au
richard.manzano@anu.edu.au

# start Validation Reply Form
_vrf_PLAT342_ram-138scaleabscorrect3 
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.02055 Ang.  
RESPONSE: Low bond percision due to poor quality crystal data.
;
# end Validation Reply Form

_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C52 H54 Au2 B2 Cl2 N12 O4 Si W2, C H Cl3'
_chemical_formula_sum            'C53 H55 Au2 B2 Cl5 N12 O4 Si W2'
_chemical_formula_weight         1912.68
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C63 H65 Au2 B2 Cl5 N12 O4 Si1 W2'
_chemical_oxdiff_usercomment     
'Brown needles grown from chloroform/pentane vdiffusion'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Au Au -4.4197 7.2980 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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                   12.7417(2)
_cell_length_b                   15.7262(3)
_cell_length_c                   17.5006(3)
_cell_angle_alpha                100.499(2)
_cell_angle_beta                 111.095(2)
_cell_angle_gamma                99.537(2)
_cell_volume                     3113.06(10)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    17573
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.5140
_cell_measurement_theta_min      2.7800
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    17.908
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.849
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    2.040
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1808
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
4 8 -6 0.0227
-4 -8 6 0.0350
5 -3 6 0.0665
-5 3 -6 0.0665
-4 8 5 0.0193
3 -8 -5 0.0140

_exptl_crystal_preparation       ?
_exptl_crystal_recrystallization_method 
'Crystals were grown from vapour-vapour diffusion of hexane in to a chloroform solution.'
_exptl_crystal_size_max          0.137
_exptl_crystal_size_mid          0.078
_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
3.9945 7.9777 -6.0227 -0.0115 1.0105 -0.0047
-3.9945 -7.9777 6.0227 0.0115 -1.0105 0.0047
4.9804 -2.9805 6.0161 -0.0486 0.0022 1.0002
-4.9804 2.9805 -6.0161 0.0486 -0.0022 -1.0002
-4.0016 8.0096 4.9539 -0.9384 0.2993 -0.1000
3.0041 -8.0097 -4.9555 0.9099 -0.3669 -0.0117

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0373
_diffrn_reflns_av_unetI/netI     0.0387
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            40111
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        66.590
_diffrn_reflns_theta_max         66.590
_diffrn_reflns_theta_min         3.498
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(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 1.000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     19.00  55.00   1.00    3.73    --   37.04 -38.00   0.00   36
  2  ω     22.00  54.00   1.00    3.73    --   37.04 -57.00   0.00   32
  3  ω     30.00  74.00   1.00    3.73    --   37.04 -99.00 -30.00   44
  4  ω     61.00  89.00   1.00    3.73    --   37.04-125.00 -90.00   28
  5  ω     34.00  74.00   1.00    3.73    --   37.04-125.00 -30.00   40
  6  ω     23.00  50.00   1.00    3.73    --   37.04 -77.00  90.00   27
  7  ω     39.00  90.00   1.00    3.73    --   37.04-125.00 120.00   51
  8  ω     88.00 116.00   1.00   14.89    --  111.00-111.00 150.00   28
  9  ω     80.00 135.00   1.00   14.89    --  111.00 -92.00 150.00   55
 10  ω     78.00 111.00   1.00   14.89    --  111.00-111.00  30.00   33
 11  ω     93.00 132.00   1.00   14.89    --  111.00 -77.00  30.00   39
 12  ω    101.00 126.00   1.00   14.89    --  111.00 -50.00 -30.00   25
 13  ω    102.00 136.00   1.00   14.89    --  111.00 -25.00 -90.00   34
 14  ω    127.00 156.00   1.00   14.89    --  111.00 -12.00-120.00   29
 15  ω    127.00 154.00   1.00   14.89    --  111.00   0.00-150.00   27
 16  ω    117.00 144.00   1.00   14.89    --  111.00  50.00-120.00   27
 17  ω    123.00 150.00   1.00   14.89    --  111.00  64.00 -90.00   27
 18  ω    140.00 165.00   1.00   14.89    --  111.00 111.00 -60.00   25
 19  ω    103.00 130.00   1.00   14.89    --  111.00 111.00   0.00   27
 20  ω    144.00 177.00   1.00   14.89    --  111.00  55.00  85.00   33
 21  ω    149.00 174.00   1.00   14.89    --  111.00  25.00 150.00   25
 22  ω    121.00 148.00   1.00   14.89    --  111.00  12.00  90.00   27
 23  ω    111.00 136.00   1.00   14.89    --  111.00  55.00  85.00   25
 24  ω     92.00 141.00   1.00   14.89    --  111.00  25.00 150.00   49
 25  ω     76.00 124.00   1.00   14.89    --  111.00 -64.00  30.00   48
 26  ω     93.00 138.00   1.00   14.89    --  111.00 -92.00 -60.00   45
 27  ω    100.00 134.00   1.00   14.89    --  111.00 -25.00-150.00   34
 28  ω    113.00 146.00   1.00   14.89    --  111.00 -12.00-180.00   33
 29  ω    103.00 128.00   1.00   14.89    --  111.00 -50.00-180.00   25
 30  ω     96.00 123.00   1.00   14.89    --  111.00 -12.00-120.00   27
 31  ω     88.00 136.00   1.00   14.89    --  111.00  25.00-150.00   48
 32  ω     97.00 178.00   1.00   14.89    --  111.00  50.00-150.00   81
 33  ω     97.00 122.00   1.00   14.89    --  111.00  50.00 -60.00   25
 34  ω     95.00 127.00   1.00   14.89    --  111.00  50.00 -90.00   32
 35  ω     89.00 157.00   1.00   14.89    --  111.00  25.00-180.00   68
 36  ω     90.00 130.00   1.00   14.89    --  111.00 -64.00-180.00   40
 37  ω     82.00 116.00   1.00   14.89    --  111.00-111.00-120.00   34
 38  ω     70.00 105.00   1.00   14.89    --  111.00 -64.00 -60.00   35
 39  ω     66.00 116.00   1.00   14.89    --  111.00-111.00 -30.00   50
 40  ω     78.00 110.00   1.00   14.89    --  111.00-111.00  60.00   32
 41  ω     67.00  92.00   1.00   14.89    --  111.00 -92.00 120.00   25
 42  ω     64.00 124.00   1.00   14.89    --  111.00 -64.00 150.00   60
 43  ω     58.00  98.00   1.00   14.89    --  111.00 -77.00 150.00   40
 44  ω     58.00 103.00   1.00   14.89    --  111.00-111.00 120.00   45
 45  ω     57.00 103.00   1.00   14.89    --  111.00 -77.00 107.29   46
 46  ω     59.00  92.00   1.00   14.89    --  111.00 -25.00 150.00   33
 47  ω     46.00  77.00   1.00   14.89    --  111.00 -50.00 150.00   31
 48  ω     44.00  79.00   1.00   14.89    --  111.00 -50.00 120.00   35
 49  ω     42.00  75.00   1.00   14.89    --  111.00 -92.00 150.00   33
 50  ω     43.00  98.00   1.00   14.89    --  111.00-111.00  90.00   55
 51  ω     44.00  71.00   1.00   14.89    --  111.00-111.00 150.00   27
 52  ω     46.00 102.00   1.00   14.89    --  111.00 -38.00  30.00   56
 53  ω     62.00  98.00   1.00   14.89    --  111.00 -77.00 -60.00   36
 54  ω     66.00  92.00   1.00   14.89    --  111.00 -25.00 -90.00   26
 55  ω     73.00 100.00   1.00   14.89    --  111.00   0.00-150.00   27
 56  ω     57.00 100.00   1.00   14.89    --  111.00 -55.00 -57.00   43
 57  ω     46.00 126.00   1.00   14.89    --  111.00 -38.00 -90.00   80
 58  ω     50.00 101.00   1.00   14.89    --  111.00-111.00 -60.00   51
 59  ω     45.00  72.00   1.00   14.89    --  111.00 -92.00 -60.00   27
 60  ω     43.00  74.00   1.00   14.89    --  111.00 -50.00 -90.00   31
 61  ω     41.00  89.00   1.00   14.89    --  111.00 -12.00-180.00   48
 62  ω     45.00 103.00   1.00    3.73    --   37.04  57.00-180.00   58
 63  ω     14.00  98.00   1.00    3.73    --   37.04  77.00   0.00   84
 64  ω     44.00  99.00   1.00    3.73    --   37.04  57.00 150.00   55
 65  ω      2.00  27.00   1.00    3.73    --   37.04 -99.00 -30.00   25
 66  ω      1.00  50.00   1.00    3.73    --   37.04 -99.00-120.00   49
 67  ω    -15.00  28.00   1.00    3.73    --   37.04 -57.00-120.00   43
 68  ω    -30.00  12.00   1.00    3.73    --   37.04 -57.00   0.00   42
 69  ω    -29.00  -4.00   1.00    3.73    --   37.04 -57.00 -30.00   25
 70  ω    -26.00  66.00   1.00    3.73    --   37.04 -19.00   0.00   92
 71  ω     41.00  68.00   1.00   14.89    --  111.00 -25.00 120.00   27
 72  ω    -21.00  40.00   1.00    3.73    --   37.04 -38.00 -90.00   61
 73  ω    107.00 132.00   1.00   14.89    --  111.00 178.00 -90.00   25
 74  ω     97.00 122.00   1.00   14.89    --  111.00 178.00 -30.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0286856000
_diffrn_orient_matrix_UB_12      -0.0636413000
_diffrn_orient_matrix_UB_13      -0.0633616000
_diffrn_orient_matrix_UB_21      0.0677754000
_diffrn_orient_matrix_UB_22      0.0809122000
_diffrn_orient_matrix_UB_23      -0.0156603000
_diffrn_orient_matrix_UB_31      0.1118807000
_diffrn_orient_matrix_UB_32      -0.0016318000
_diffrn_orient_matrix_UB_33      0.0728226000
_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                9706
_reflns_number_total             10989
_reflns_odcompleteness_completeness 98.70
_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 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         7.529
_refine_diff_density_min         -5.307
_refine_diff_density_rms         0.293
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     742
_refine_ls_number_reflns         10989
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0714
_refine_ls_R_factor_gt           0.0644
_refine_ls_restrained_S_all      1.018
_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)+(0.1087P)²+66.5357P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1813
_refine_ls_wR_factor_ref         0.1893
_refine_special_details          'Olex solvent mask'
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 B1(H1), B2(H2), C101(H101)
2.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C18(H18), C19(H19),
 C20(H20), C21(H21), C22(H22), C24(H24), C29(H29), C34(H34), C39(H39), C44(H44),
  C49(H49)
2.c Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C31(H31A,H31B,H31C), C32(H32A,H32B,
 H32C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C41(H41A,H41B,H41C), C42(H42A,
 H42B,H42C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C51(H51A,H51B,H51C),
 C52(H52A,H52B,H52C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Au1 Au 0.95940(5) 0.82615(4) 0.69234(3) 0.04038(16) Uani 1 1 d . . . . .
Au2 Au 0.79626(5) 0.38898(4) 0.79626(4) 0.03996(16) Uani 1 1 d . . . . .
Cl1 Cl 1.1293(4) 0.9340(4) 0.7445(3) 0.0837(16) Uani 1 1 d . . . . .
Cl2 Cl 0.9496(3) 0.3847(3) 0.7609(3) 0.0578(9) Uani 1 1 d . . . . .
Si1 Si 0.6793(3) 0.70520(19) 0.86503(19) 0.0280(6) Uani 1 1 d . . . . .
O1 O 0.5502(10) 0.7155(10) 0.5135(8) 0.069(4) Uani 1 1 d . . . . .
O2 O 0.7242(9) 0.5224(7) 0.6204(8) 0.054(3) Uani 1 1 d . . . . .
O3 O 0.4050(9) 0.2778(8) 0.6669(7) 0.057(3) Uani 1 1 d . . . . .
O4 O 0.5141(11) 0.4086(8) 0.9356(9) 0.063(3) Uani 1 1 d . . . . .
N1 N 0.7322(8) 0.5923(7) 0.4267(6) 0.033(2) Uani 1 1 d . . . . .
N2 N 0.7962(8) 0.6046(7) 0.3799(6) 0.029(2) Uani 1 1 d . . . . .
N3 N 0.8500(9) 0.7855(7) 0.4907(6) 0.033(2) Uani 1 1 d . . . . .
N4 N 0.9053(8) 0.7648(6) 0.4391(5) 0.0270(19) Uani 1 1 d . . . . .
N5 N 0.9612(9) 0.6496(6) 0.5638(6) 0.031(2) Uani 1 1 d . . . . .
N6 N 0.9966(8) 0.6498(6) 0.4990(6) 0.029(2) Uani 1 1 d . . . . .
N7 N 0.5262(8) 0.1859(7) 0.8615(6) 0.030(2) Uani 1 1 d . . . . .
N8 N 0.5859(8) 0.1239(6) 0.8893(6) 0.0279(19) Uani 1 1 d . . . . .
N9 N 0.6788(9) 0.1890(7) 0.7702(6) 0.030(2) Uani 1 1 d . . . . .
N10 N 0.7139(8) 0.1246(6) 0.8112(6) 0.0277(19) Uani 1 1 d . . . . .
N11 N 0.7705(8) 0.2946(7) 0.9499(6) 0.030(2) Uani 1 1 d . . . . .
N12 N 0.7911(8) 0.2162(7) 0.9612(6) 0.030(2) Uani 1 1 d . . . . .
C1 C 0.8036(11) 0.7376(8) 0.6645(8) 0.037(3) Uani 1 1 d . . . . .
C2 C 0.7618(10) 0.7359(7) 0.7277(7) 0.029(2) Uani 1 1 d . . . . .
C3 C 0.7227(12) 0.7296(8) 0.7806(8) 0.037(3) Uani 1 1 d . . . . .
C4 C 0.6643(10) 0.4190(8) 0.8282(8) 0.034(3) Uani 1 1 d . . . . .
C5 C 0.6612(11) 0.5059(8) 0.8395(8) 0.038(3) Uani 1 1 d . . . . .
C6 C 0.6661(11) 0.5861(9) 0.8515(8) 0.038(3) Uani 1 1 d . . . . .
C7 C 0.6408(14) 0.7059(10) 0.5251(8) 0.046(3) Uani 1 1 d . . . . .
C8 C 0.7517(12) 0.5797(10) 0.5938(9) 0.043(3) Uani 1 1 d . . . . .
C9 C 0.4887(12) 0.2873(8) 0.7280(8) 0.036(3) Uani 1 1 d . . . . .
C10 C 0.5483(14) 0.3719(11) 0.9021(9) 0.049(4) Uani 1 1 d . . . . .
C11 C 0.7935(10) 0.7658(8) 0.9717(7) 0.030(2) Uani 1 1 d . . . . .
C12 C 0.8079(11) 0.8575(9) 1.0045(8) 0.038(3) Uani 1 1 d . . . . .
H12 H 0.760719 0.888048 0.971925 0.045 Uiso 1 1 calc R . . . .
C13 C 0.8659(12) 0.7233(10) 1.0228(9) 0.042(3) Uani 1 1 d . . . . .
H13 H 0.858155 0.662529 1.003183 0.051 Uiso 1 1 calc R . . . .
C14 C 0.8907(14) 0.9027(10) 1.0840(10) 0.054(4) Uani 1 1 d . . . . .
H14 H 0.898043 0.963075 1.105064 0.065 Uiso 1 1 calc R . . . .
C15 C 0.9516(13) 0.7711(13) 1.1047(10) 0.055(4) Uani 1 1 d . . . . .
H15 H 0.999733 0.742249 1.138771 0.066 Uiso 1 1 calc R . . . .
C16 C 0.9619(12) 0.8600(11) 1.1322(9) 0.048(3) Uani 1 1 d . . . . .
H16 H 1.018891 0.892151 1.185159 0.058 Uiso 1 1 calc R . . . .
C17 C 0.5375(11) 0.7292(8) 0.8520(8) 0.034(3) Uani 1 1 d . . . . .
C18 C 0.4985(13) 0.7290(9) 0.9172(9) 0.043(3) Uani 1 1 d . . . . .
H18 H 0.546321 0.719439 0.967605 0.051 Uiso 1 1 calc R . . . .
C19 C 0.4629(13) 0.7432(9) 0.7774(9) 0.045(3) Uani 1 1 d . . . . .
H19 H 0.484731 0.742994 0.732038 0.054 Uiso 1 1 calc R . . . .
C20 C 0.3919(12) 0.7423(10) 0.9088(10) 0.049(3) Uani 1 1 d . . . . .
H20 H 0.367317 0.740051 0.952572 0.058 Uiso 1 1 calc R . . . .
C21 C 0.3547(12) 0.7578(11) 0.7710(11) 0.055(4) Uani 1 1 d . . . . .
H21 H 0.304651 0.766711 0.720960 0.066 Uiso 1 1 calc R . . . .
C22 C 0.3222(13) 0.7589(11) 0.8369(12) 0.058(4) Uani 1 1 d . . . . .
H22 H 0.251629 0.771139 0.832672 0.070 Uiso 1 1 calc R . . . .
C23 C 0.6330(11) 0.5304(10) 0.3770(10) 0.045(3) Uani 1 1 d . . . . .
C24 C 0.6329(11) 0.5043(9) 0.2969(9) 0.042(3) Uani 1 1 d . . . . .
H24 H 0.574414 0.462234 0.250052 0.050 Uiso 1 1 calc R . . . .
C25 C 0.7340(11) 0.5517(8) 0.2998(8) 0.035(3) Uani 1 1 d . . . . .
C26 C 0.5398(13) 0.4980(14) 0.4055(12) 0.064(5) Uani 1 1 d . . . . .
H26A H 0.573177 0.479457 0.456385 0.097 Uiso 1 1 calc GR . . . .
H26B H 0.482080 0.448386 0.361867 0.097 Uiso 1 1 calc GR . . . .
H26C H 0.504236 0.545445 0.416643 0.097 Uiso 1 1 calc GR . . . .
C27 C 0.7761(12) 0.5529(11) 0.2298(8) 0.048(3) Uani 1 1 d . . . . .
H27A H 0.787609 0.612080 0.221962 0.072 Uiso 1 1 calc GR . . . .
H27B H 0.719234 0.511798 0.178084 0.072 Uiso 1 1 calc GR . . . .
H27C H 0.848190 0.535703 0.244734 0.072 Uiso 1 1 calc GR . . . .
C28 C 0.8387(13) 0.8698(9) 0.4914(8) 0.042(3) Uani 1 1 d . . . . .
C29 C 0.8835(13) 0.9017(9) 0.4380(9) 0.042(3) Uani 1 1 d . . . . .
H29 H 0.885141 0.957219 0.426508 0.051 Uiso 1 1 calc R . . . .
C30 C 0.9254(11) 0.8344(9) 0.4048(8) 0.035(3) Uani 1 1 d . . . . .
C31 C 0.7832(18) 0.9156(11) 0.5435(11) 0.063(5) Uani 1 1 d . . . . .
H31A H 0.708579 0.877948 0.531299 0.094 Uiso 1 1 calc GR . . . .
H31B H 0.773662 0.971044 0.529873 0.094 Uiso 1 1 calc GR . . . .
H31C H 0.831779 0.927199 0.602684 0.094 Uiso 1 1 calc GR . . . .
C32 C 0.9803(12) 0.8315(11) 0.3433(10) 0.047(3) Uani 1 1 d . . . . .
H32A H 1.051781 0.814081 0.365637 0.070 Uiso 1 1 calc GR . . . .
H32B H 0.996122 0.889530 0.333742 0.070 Uiso 1 1 calc GR . . . .
H32C H 0.928786 0.788913 0.290734 0.070 Uiso 1 1 calc GR . . . .
C33 C 1.0402(11) 0.6229(8) 0.6248(8) 0.035(3) Uani 1 1 d . . . . .
C34 C 1.1249(11) 0.6062(9) 0.5965(9) 0.044(3) Uani 1 1 d . . . . .
H34 H 1.189479 0.586654 0.625080 0.053 Uiso 1 1 calc R . . . .
C35 C 1.0959(10) 0.6237(8) 0.5182(8) 0.036(3) Uani 1 1 d . . . . .
C36 C 1.0316(12) 0.6143(10) 0.7042(9) 0.048(3) Uani 1 1 d . . . . .
H36A H 0.995531 0.658451 0.722113 0.072 Uiso 1 1 calc GR . . . .
H36B H 1.108052 0.623086 0.747095 0.072 Uiso 1 1 calc GR . . . .
H36C H 0.985694 0.555738 0.695706 0.072 Uiso 1 1 calc GR . . . .
C37 C 1.1608(12) 0.6203(11) 0.4624(9) 0.050(4) Uani 1 1 d . . . . .
H37A H 1.116116 0.574291 0.410712 0.076 Uiso 1 1 calc GR . . . .
H37B H 1.234015 0.607656 0.491022 0.076 Uiso 1 1 calc GR . . . .
H37C H 1.174263 0.676925 0.449580 0.076 Uiso 1 1 calc GR . . . .
C38 C 0.4159(11) 0.1564(10) 0.8528(8) 0.041(3) Uani 1 1 d . . . . .
C39 C 0.4036(11) 0.0775(10) 0.8740(8) 0.042(3) Uani 1 1 d . . . . .
H39 H 0.336141 0.043956 0.873929 0.050 Uiso 1 1 calc R . . . .
C40 C 0.5090(12) 0.0563(9) 0.8955(8) 0.040(3) Uani 1 1 d . . . . .
C41 C 0.3217(12) 0.2029(12) 0.8227(11) 0.054(4) Uani 1 1 d . . . . .
H41A H 0.350220 0.265286 0.851900 0.081 Uiso 1 1 calc GR . . . .
H41B H 0.256751 0.177311 0.833961 0.081 Uiso 1 1 calc GR . . . .
H41C H 0.297419 0.195992 0.762714 0.081 Uiso 1 1 calc GR . . . .
C42 C 0.5453(15) -0.0252(10) 0.9194(11) 0.056(4) Uani 1 1 d . . . . .
H42A H 0.586892 -0.046615 0.886994 0.084 Uiso 1 1 calc GR . . . .
H42B H 0.477536 -0.071172 0.907685 0.084 Uiso 1 1 calc GR . . . .
H42C H 0.594626 -0.009670 0.978841 0.084 Uiso 1 1 calc GR . . . .
C43 C 0.6786(12) 0.1634(9) 0.6921(8) 0.040(3) Uani 1 1 d . . . . .
C44 C 0.7127(13) 0.0852(10) 0.6842(9) 0.047(3) Uani 1 1 d . . . . .
H44 H 0.720554 0.054114 0.636832 0.056 Uiso 1 1 calc R . . . .
C45 C 0.7331(11) 0.0611(10) 0.7585(9) 0.042(3) Uani 1 1 d . . . . .
C46 C 0.6404(15) 0.2134(12) 0.6255(10) 0.053(4) Uani 1 1 d . . . . .
H46A H 0.558882 0.209708 0.608403 0.079 Uiso 1 1 calc GR . . . .
H46B H 0.654503 0.187363 0.577182 0.079 Uiso 1 1 calc GR . . . .
H46C H 0.683392 0.274870 0.648336 0.079 Uiso 1 1 calc GR . . . .
C47 C 0.7670(16) -0.0197(10) 0.7842(12) 0.057(4) Uani 1 1 d . . . . .
H47A H 0.827204 -0.001505 0.840502 0.086 Uiso 1 1 calc GR . . . .
H47B H 0.795024 -0.049407 0.745349 0.086 Uiso 1 1 calc GR . . . .
H47C H 0.700619 -0.059717 0.783137 0.086 Uiso 1 1 calc GR . . . .
C48 C 0.8512(11) 0.3620(9) 1.0162(8) 0.039(3) Uani 1 1 d . . . . .
C49 C 0.9257(11) 0.3226(11) 1.0704(8) 0.048(4) Uani 1 1 d . . . . .
H49 H 0.989729 0.352424 1.120591 0.057 Uiso 1 1 calc R . . . .
C50 C 0.8876(11) 0.2325(10) 1.0364(7) 0.038(3) Uani 1 1 d . . . . .
C51 C 0.8578(16) 0.4593(12) 1.0268(10) 0.068(5) Uani 1 1 d . . . . .
H51A H 0.870387 0.477089 0.980553 0.101 Uiso 1 1 calc GR . . . .
H51B H 0.920960 0.492751 1.079389 0.101 Uiso 1 1 calc GR . . . .
H51C H 0.786248 0.470525 1.027367 0.101 Uiso 1 1 calc GR . . . .
C52 C 0.9333(13) 0.1580(12) 1.0672(9) 0.054(4) Uani 1 1 d . . . . .
H52A H 0.871124 0.114346 1.067370 0.081 Uiso 1 1 calc GR . . . .
H52B H 0.992556 0.181240 1.123751 0.081 Uiso 1 1 calc GR . . . .
H52C H 0.965644 0.130610 1.030298 0.081 Uiso 1 1 calc GR . . . .
B1 B 0.9195(11) 0.6693(8) 0.4168(8) 0.028(3) Uani 1 1 d . . . . .
H1 H 0.954506 0.663114 0.375237 0.034 Uiso 1 1 calc R . . . .
B2 B 0.7107(12) 0.1289(9) 0.8982(9) 0.032(3) Uani 1 1 d . . . . .
H2 H 0.735647 0.078323 0.918166 0.038 Uiso 1 1 calc R . . . .
W1 W 0.80118(4) 0.68708(4) 0.55544(3) 0.02970(15) Uani 1 1 d . . . A 1
W2 W 0.62393(4) 0.29797(3) 0.83408(3) 0.02787(15) Uani 1 1 d . . . B 1
Cl3 Cl 0.6026(5) -0.0358(3) 0.3442(3) 0.0818(14) Uani 1 1 d . . . . .
Cl4 Cl 0.5517(6) 0.1338(4) 0.3779(4) 0.0926(17) Uani 1 1 d . . . . .
Cl10 Cl 0.7897(4) 0.1237(3) 0.4397(3) 0.0748(12) Uani 1 1 d . . . . .
C101 C 0.6529(19) 0.0756(14) 0.3581(12) 0.072(5) Uani 1 1 d . . . . .
H101 H 0.657314 0.084144 0.305119 0.086 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Au1 Cl1 2.278(4) . ?
Au1 C1 2.063(13) . ?
Au1 W1 2.7822(7) . ?
Au2 Cl2 2.259(3) . ?
Au2 C4 2.051(11) . ?
Au2 W2 2.7672(7) . ?
Si1 C3 1.834(13) . ?
Si1 C6 1.815(13) . ?
Si1 C11 1.857(12) . ?
Si1 C17 1.849(13) . ?
O1 C7 1.139(18) . ?
O2 C8 1.148(18) . ?
O3 C9 1.172(17) . ?
O4 C10 1.004(19) . ?
N1 N2 1.363(14) . ?
N1 C23 1.340(16) . ?
N1 W1 2.234(9) . ?
N2 C25 1.358(15) . ?
N2 B1 1.557(15) . ?
N3 N4 1.358(13) . ?
N3 C28 1.355(17) . ?
N3 W1 2.212(11) . ?
N4 C30 1.372(16) . ?
N4 B1 1.538(15) . ?
N5 N6 1.363(14) . ?
N5 C33 1.364(15) . ?
N5 W1 2.178(10) . ?
N6 C35 1.341(15) . ?
N6 B1 1.540(16) . ?
N7 N8 1.385(13) . ?
N7 C38 1.349(16) . ?
N7 W2 2.212(10) . ?
N8 C40 1.370(16) . ?
N8 B2 1.528(16) . ?
N9 N10 1.387(13) . ?
N9 C43 1.351(15) . ?
N9 W2 2.222(10) . ?
N10 C45 1.348(16) . ?
N10 B2 1.528(15) . ?
N11 N12 1.337(14) . ?
N11 C48 1.364(16) . ?
N11 W2 2.224(9) . ?
N12 C50 1.384(15) . ?
N12 B2 1.523(17) . ?
C1 C2 1.392(18) . ?
C1 W1 1.916(14) . ?
C2 C3 1.210(18) . ?
C4 C5 1.355(18) . ?
C4 W2 1.919(13) . ?
C5 C6 1.227(19) . ?
C7 W1 2.006(16) . ?
C8 W1 2.016(16) . ?
C9 W2 1.982(13) . ?
C10 W2 2.096(19) . ?
C11 C12 1.407(18) . ?
C11 C13 1.388(18) . ?
C12 C14 1.37(2) . ?
C13 C15 1.42(2) . ?
C14 C16 1.36(2) . ?
C15 C16 1.36(2) . ?
C17 C18 1.399(17) . ?
C17 C19 1.392(19) . ?
C18 C20 1.37(2) . ?
C19 C21 1.40(2) . ?
C20 C22 1.35(2) . ?
C21 C22 1.36(3) . ?
C23 C24 1.39(2) . ?
C23 C26 1.496(19) . ?
C24 C25 1.36(2) . ?
C25 C27 1.505(19) . ?
C28 C29 1.38(2) . ?
C28 C31 1.498(18) . ?
C29 C30 1.388(18) . ?
C30 C32 1.478(18) . ?
C33 C34 1.38(2) . ?
C33 C36 1.461(19) . ?
C34 C35 1.38(2) . ?
C35 C37 1.49(2) . ?
C38 C39 1.36(2) . ?
C38 C41 1.494(19) . ?
C39 C40 1.374(19) . ?
C40 C42 1.51(2) . ?
C43 C44 1.37(2) . ?
C43 C46 1.505(19) . ?
C44 C45 1.37(2) . ?
C45 C47 1.50(2) . ?
C48 C49 1.39(2) . ?
C48 C51 1.49(2) . ?
C49 C50 1.36(2) . ?
C50 C52 1.49(2) . ?
Cl3 C101 1.70(2) . ?
Cl4 C101 1.79(2) . ?
Cl10 C101 1.74(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
Cl1 Au1 W1 146.35(12) . . ?
C1 Au1 Cl1 170.1(4) . . ?
C1 Au1 W1 43.5(4) . . ?
Cl2 Au2 W2 147.51(12) . . ?
C4 Au2 Cl2 168.6(4) . . ?
C4 Au2 W2 43.9(4) . . ?
C3 Si1 C11 111.3(6) . . ?
C3 Si1 C17 111.4(6) . . ?
C6 Si1 C3 104.1(6) . . ?
C6 Si1 C11 108.6(6) . . ?
C6 Si1 C17 109.6(6) . . ?
C17 Si1 C11 111.5(5) . . ?
N2 N1 W1 115.9(7) . . ?
C23 N1 N2 108.1(10) . . ?
C23 N1 W1 135.4(9) . . ?
N1 N2 B1 123.2(9) . . ?
C25 N2 N1 108.4(10) . . ?
C25 N2 B1 128.4(10) . . ?
N4 N3 W1 119.6(7) . . ?
C28 N3 N4 107.0(10) . . ?
C28 N3 W1 133.3(8) . . ?
N3 N4 C30 109.8(9) . . ?
N3 N4 B1 119.9(9) . . ?
C30 N4 B1 129.5(9) . . ?
N6 N5 C33 108.1(10) . . ?
N6 N5 W1 119.9(7) . . ?
C33 N5 W1 131.9(9) . . ?
N5 N6 B1 120.4(9) . . ?
C35 N6 N5 109.0(10) . . ?
C35 N6 B1 130.3(10) . . ?
N8 N7 W2 116.2(7) . . ?
C38 N7 N8 107.3(10) . . ?
C38 N7 W2 136.2(9) . . ?
N7 N8 B2 123.1(9) . . ?
C40 N8 N7 107.7(10) . . ?
C40 N8 B2 128.7(10) . . ?
N10 N9 W2 119.2(7) . . ?
C43 N9 N10 106.2(10) . . ?
C43 N9 W2 134.3(9) . . ?
N9 N10 B2 119.2(9) . . ?
C45 N10 N9 109.3(10) . . ?
C45 N10 B2 131.0(11) . . ?
N12 N11 C48 109.3(10) . . ?
N12 N11 W2 119.7(7) . . ?
C48 N11 W2 130.9(9) . . ?
N11 N12 C50 108.3(10) . . ?
N11 N12 B2 120.6(9) . . ?
C50 N12 B2 131.1(11) . . ?
C2 C1 Au1 119.2(9) . . ?
C2 C1 W1 151.6(10) . . ?
W1 C1 Au1 88.6(6) . . ?
C3 C2 C1 176.5(13) . . ?
C2 C3 Si1 169.6(12) . . ?
C5 C4 Au2 115.1(9) . . ?
C5 C4 W2 156.1(10) . . ?
W2 C4 Au2 88.3(5) . . ?
C6 C5 C4 175.8(14) . . ?
C5 C6 Si1 176.1(12) . . ?
O1 C7 W1 174.9(12) . . ?
O2 C8 W1 175.5(12) . . ?
O3 C9 W2 176.1(12) . . ?
O4 C10 W2 178.4(16) . . ?
C12 C11 Si1 120.4(9) . . ?
C13 C11 Si1 122.2(10) . . ?
C13 C11 C12 117.4(12) . . ?
C14 C12 C11 120.9(13) . . ?
C11 C13 C15 121.0(13) . . ?
C16 C14 C12 120.7(15) . . ?
C16 C15 C13 118.7(13) . . ?
C14 C16 C15 121.4(14) . . ?
C18 C17 Si1 119.9(11) . . ?
C19 C17 Si1 122.8(10) . . ?
C19 C17 C18 117.2(13) . . ?
C20 C18 C17 121.9(14) . . ?
C17 C19 C21 119.7(14) . . ?
C22 C20 C18 120.1(14) . . ?
C22 C21 C19 120.7(15) . . ?
C20 C22 C21 120.4(15) . . ?
N1 C23 C24 108.2(12) . . ?
N1 C23 C26 124.3(14) . . ?
C24 C23 C26 127.5(13) . . ?
C25 C24 C23 107.2(11) . . ?
N2 C25 C27 122.4(12) . . ?
C24 C25 N2 108.1(12) . . ?
C24 C25 C27 129.5(12) . . ?
N3 C28 C29 109.7(11) . . ?
N3 C28 C31 121.8(13) . . ?
C29 C28 C31 128.5(13) . . ?
C28 C29 C30 106.5(12) . . ?
N4 C30 C29 107.0(11) . . ?
N4 C30 C32 123.2(11) . . ?
C29 C30 C32 129.9(13) . . ?
N5 C33 C34 107.4(11) . . ?
N5 C33 C36 124.1(12) . . ?
C34 C33 C36 128.4(12) . . ?
C35 C34 C33 107.3(11) . . ?
N6 C35 C34 108.1(12) . . ?
N6 C35 C37 122.8(12) . . ?
C34 C35 C37 129.0(12) . . ?
N7 C38 C39 109.6(11) . . ?
N7 C38 C41 124.8(13) . . ?
C39 C38 C41 125.6(12) . . ?
C38 C39 C40 107.4(11) . . ?
N8 C40 C39 107.9(12) . . ?
N8 C40 C42 121.0(12) . . ?
C39 C40 C42 131.1(13) . . ?
N9 C43 C44 109.2(12) . . ?
N9 C43 C46 123.2(12) . . ?
C44 C43 C46 127.5(12) . . ?
C45 C44 C43 107.7(12) . . ?
N10 C45 C44 107.5(12) . . ?
N10 C45 C47 121.4(13) . . ?
C44 C45 C47 131.0(13) . . ?
N11 C48 C49 107.1(12) . . ?
N11 C48 C51 125.6(12) . . ?
C49 C48 C51 127.3(12) . . ?
C50 C49 C48 107.6(11) . . ?
N12 C50 C52 121.5(13) . . ?
C49 C50 N12 107.7(12) . . ?
C49 C50 C52 130.8(13) . . ?
N4 B1 N2 107.2(9) . . ?
N4 B1 N6 108.4(8) . . ?
N6 B1 N2 109.6(10) . . ?
N10 B2 N8 108.3(10) . . ?
N12 B2 N8 109.9(9) . . ?
N12 B2 N10 109.7(10) . . ?
N1 W1 Au1 155.9(3) . . ?
N3 W1 Au1 78.3(3) . . ?
N3 W1 N1 83.6(4) . . ?
N5 W1 Au1 80.8(3) . . ?
N5 W1 N1 82.0(4) . . ?
N5 W1 N3 85.7(4) . . ?
C1 W1 Au1 47.9(4) . . ?
C1 W1 N1 156.2(5) . . ?
C1 W1 N3 115.0(4) . . ?
C1 W1 N5 112.7(4) . . ?
C1 W1 C7 77.8(5) . . ?
C1 W1 C8 76.1(5) . . ?
C7 W1 Au1 109.6(4) . . ?
C7 W1 N1 86.9(5) . . ?
C7 W1 N3 92.9(5) . . ?
C7 W1 N5 168.9(5) . . ?
C7 W1 C8 89.1(6) . . ?
C8 W1 Au1 111.3(4) . . ?
C8 W1 N1 85.6(5) . . ?
C8 W1 N3 168.9(5) . . ?
C8 W1 N5 90.3(4) . . ?
N7 W2 Au2 157.3(2) . . ?
N7 W2 N9 82.6(4) . . ?
N7 W2 N11 84.0(4) . . ?
N9 W2 Au2 76.7(3) . . ?
N9 W2 N11 83.9(4) . . ?
N11 W2 Au2 84.7(3) . . ?
C4 W2 Au2 47.8(3) . . ?
C4 W2 N7 154.6(4) . . ?
C4 W2 N9 122.2(4) . . ?
C4 W2 N11 102.8(5) . . ?
C4 W2 C9 83.0(5) . . ?
C4 W2 C10 73.4(5) . . ?
C9 W2 Au2 98.4(4) . . ?
C9 W2 N7 91.3(5) . . ?
C9 W2 N9 92.0(4) . . ?
C9 W2 N11 174.1(4) . . ?
C9 W2 C10 88.8(5) . . ?
C10 W2 Au2 118.6(4) . . ?
C10 W2 N7 81.8(5) . . ?
C10 W2 N9 164.4(5) . . ?
C10 W2 N11 94.1(5) . . ?
Cl3 C101 Cl4 109.5(12) . . ?
Cl3 C101 Cl10 114.6(11) . . ?
Cl10 C101 Cl4 108.7(11) . . ?

_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 0.312 0.411 0.957 11.4 0.0 ?
2 0.500 0.000 0.500 28.2 0.0 ?
3 0.688 0.589 0.043 11.4 0.0 ?


_ins_header                      
;
TITL RAM-138scaleabscorrect3 in P-1 
REM P-1 (#2 in standard setting)
CELL 1.54184  12.741684  15.726221  17.500558 100.4994 111.0946  99.5366
ZERR    2.00   0.000222   0.000343   0.000289   0.0016   0.0016   0.0016
LATT  1
SFAC C H B N O Si Cl W Au
UNIT 126.00 130.00 4.00 24.00 8.00 2.00 10.00 4.00 4.00
TREF
HKLF 4
END
;
_olex2_submission_original_sample_id W2Au2{CCC(SiPh2)(CCC}(CO)4Cl(Tp*)2
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.255
_oxdiff_exptl_absorpt_empirical_full_min 0.592


