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

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

data_3
_database_code_depnum_ccdc_archive 'CCDC 1481874'
_audit_update_record             
;
2016-06-21 deposited with the CCDC.
2016-07-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C53 H50 F6 Fe N3 O6 P3 S2 Si'
_chemical_formula_weight         1179.93

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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

_cell_length_a                   13.8465(10)
_cell_length_b                   14.2314(8)
_cell_length_c                   15.3249(12)
_cell_angle_alpha                73.403(5)
_cell_angle_beta                 79.675(4)
_cell_angle_gamma                70.236(4)
_cell_volume                     2712.1(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    117414
_cell_measurement_theta_min      2.19
_cell_measurement_theta_max      25.68

_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.445
_exptl_crystal_F_000             1216
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_exptl_absorpt_coefficient_mu    0.538
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.875
_exptl_absorpt_correction_T_max  1.095
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_special_details           'crystal-to-detector distance 33 mm'
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method       
'2 φ and 12 ω scans with 2° steps (707 frames)'
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            117414
_diffrn_reflns_av_unetI/netI     0.1004
_diffrn_reflns_av_R_equivalents  0.0731
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.192
_diffrn_reflns_theta_max         25.682
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             10290
_reflns_number_gt                6157
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  
'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)'

_refine_special_details          
;
 Structure solved by intrinsic phasing and subsequent difference Fourier
 synthesis. One of the trifluoromethanesulfonate counter-ions is disordered
 over two positions sharing two O and two F atoms, which were refined
 with occupancy parameters constrained to sum to unity and restraints
 on bond lengths and displacement parameters. All non-hydrogen atoms 
 were refined with anisotropic displacement parameters. The H atoms
 were introduced at calculated positions and were treated as riding atoms
 with an isotropic displacement parameter equal to 1.2 times that of the
 parent atom (1.5 for CH₃, with optimized geometry). 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0726P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10290
_refine_ls_number_parameters     716
_refine_ls_number_restraints     134
_refine_ls_R_factor_all          0.1114
_refine_ls_R_factor_gt           0.0572
_refine_ls_wR_factor_ref         0.1528
_refine_ls_wR_factor_gt          0.1342
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_restrained_S_all      1.090
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.68923(4) 0.75021(4) 0.73562(4) 0.03326(17) Uani 1 1 d . . . . .
P1 P 0.58273(8) 0.67114(8) 0.84180(7) 0.0335(3) Uani 1 1 d . . . . .
P2 P 0.75885(8) 0.60784(8) 0.67348(7) 0.0333(3) Uani 1 1 d . . . . .
P3 P 0.81705(8) 0.69560(8) 0.83218(8) 0.0360(3) Uani 1 1 d . . . . .
Si1 Si 0.78076(8) 0.48476(8) 0.87379(8) 0.0376(3) Uani 1 1 d . . . . .
S1 S 0.72078(8) 0.95026(8) 0.32712(8) 0.0427(3) Uani 1 1 d . . . . .
O1 O 0.6513(2) 0.9282(2) 0.2818(2) 0.0557(8) Uani 1 1 d . . . . .
O2 O 0.7183(2) 0.9064(2) 0.4245(2) 0.0507(8) Uani 1 1 d . . . . .
O3 O 0.7227(2) 1.0553(2) 0.2997(2) 0.0512(8) Uani 1 1 d . . . . .
N1 N 0.5835(3) 0.8100(2) 0.6487(2) 0.0368(8) Uani 1 1 d . . . . .
N2 N 0.7710(3) 0.8255(2) 0.6433(2) 0.0386(8) Uani 1 1 d . . . . .
N3 N 0.6348(2) 0.8793(3) 0.7747(2) 0.0407(8) Uani 1 1 d . . . . .
F1 F 0.8626(2) 0.9078(2) 0.1941(2) 0.0741(8) Uani 1 1 d . . . . .
F2 F 0.8598(2) 0.77805(19) 0.3058(2) 0.0682(8) Uani 1 1 d . . . . .
F3 F 0.9220(2) 0.8909(2) 0.3199(2) 0.0711(8) Uani 1 1 d . . . . .
C1 C 0.6534(3) 0.5591(3) 0.9245(3) 0.0369(9) Uani 1 1 d . . . . .
H1A H 0.6103 0.5127 0.9501 0.044 Uiso 1 1 calc R U . . .
H1B H 0.6657 0.5822 0.9754 0.044 Uiso 1 1 calc R U . . .
C2 C 0.7619(3) 0.4865(3) 0.7560(3) 0.0379(10) Uani 1 1 d . . . . .
H2A H 0.8184 0.4306 0.7353 0.045 Uiso 1 1 calc R U . . .
H2B H 0.6963 0.4722 0.7577 0.045 Uiso 1 1 calc R U . . .
C3 C 0.8757(3) 0.5559(3) 0.8663(3) 0.0384(10) Uani 1 1 d . . . . .
H3A H 0.9028 0.5372 0.9266 0.046 Uiso 1 1 calc R U . . .
H3B H 0.9344 0.5345 0.8214 0.046 Uiso 1 1 calc R U . . .
C4 C 0.4984(3) 0.6238(3) 0.7968(3) 0.0355(9) Uani 1 1 d . . . . .
C5 C 0.5067(3) 0.5207(3) 0.8124(3) 0.0389(10) Uani 1 1 d . . . . .
H5 H 0.5588 0.4701 0.8480 0.047 Uiso 1 1 calc R U . . .
C6 C 0.4399(3) 0.4902(3) 0.7769(3) 0.0506(12) Uani 1 1 d . . . . .
H6 H 0.4472 0.4191 0.7877 0.061 Uiso 1 1 calc R U . . .
C7 C 0.3637(4) 0.5619(4) 0.7263(4) 0.0565(13) Uani 1 1 d . . . . .
H7 H 0.3181 0.5405 0.7024 0.068 Uiso 1 1 calc R U . . .
C8 C 0.3526(3) 0.6662(4) 0.7098(3) 0.0507(12) Uani 1 1 d . . . . .
H8 H 0.2999 0.7164 0.6746 0.061 Uiso 1 1 calc R U . . .
C9 C 0.4198(3) 0.6953(3) 0.7455(3) 0.0412(10) Uani 1 1 d . . . . .
H9 H 0.4120 0.7665 0.7348 0.049 Uiso 1 1 calc R U . . .
C10 C 0.4846(3) 0.7495(3) 0.9120(3) 0.0362(9) Uani 1 1 d . . . . .
C11 C 0.4653(3) 0.7093(3) 1.0058(3) 0.0426(10) Uani 1 1 d . . . . .
H11 H 0.5042 0.6412 1.0334 0.051 Uiso 1 1 calc R U . . .
C12 C 0.3906(3) 0.7670(3) 1.0589(3) 0.0482(11) Uani 1 1 d . . . . .
H12 H 0.3777 0.7382 1.1223 0.058 Uiso 1 1 calc R U . . .
C13 C 0.3349(3) 0.8669(4) 1.0194(3) 0.0518(12) Uani 1 1 d . . . . .
H13 H 0.2843 0.9072 1.0558 0.062 Uiso 1 1 calc R U . . .
C14 C 0.3530(3) 0.9078(3) 0.9267(3) 0.0444(10) Uani 1 1 d . . . . .
H14 H 0.3143 0.9761 0.8994 0.053 Uiso 1 1 calc R U . . .
C15 C 0.4276(3) 0.8492(3) 0.8737(3) 0.0405(10) Uani 1 1 d . . . . .
H15 H 0.4397 0.8780 0.8102 0.049 Uiso 1 1 calc R U . . .
C16 C 0.6931(3) 0.6066(3) 0.5800(3) 0.0362(9) Uani 1 1 d . . . . .
C17 C 0.6563(3) 0.5258(3) 0.5835(3) 0.0411(10) Uani 1 1 d . . . . .
H17 H 0.6624 0.4704 0.6365 0.049 Uiso 1 1 calc R U . . .
C18 C 0.6110(3) 0.5257(3) 0.5104(3) 0.0489(11) Uani 1 1 d . . . . .
H18 H 0.5862 0.4700 0.5137 0.059 Uiso 1 1 calc R U . . .
C19 C 0.6010(3) 0.6049(3) 0.4330(3) 0.0492(11) Uani 1 1 d . . . . .
H19 H 0.5689 0.6043 0.3833 0.059 Uiso 1 1 calc R U . . .
C20 C 0.6380(3) 0.6854(3) 0.4278(3) 0.0465(11) Uani 1 1 d . . . . .
H20 H 0.6323 0.7400 0.3741 0.056 Uiso 1 1 calc R U . . .
C21 C 0.6838(3) 0.6866(3) 0.5013(3) 0.0403(10) Uani 1 1 d . . . . .
H21 H 0.7087 0.7423 0.4977 0.048 Uiso 1 1 calc R U . . .
C22 C 0.8939(3) 0.5847(3) 0.6233(3) 0.0368(10) Uani 1 1 d . . . . .
C23 C 0.9719(3) 0.4979(3) 0.6574(3) 0.0465(11) Uani 1 1 d . . . . .
H23 H 0.9561 0.4463 0.7075 0.056 Uiso 1 1 calc R U . . .
C24 C 1.0731(3) 0.4844(4) 0.6199(4) 0.0565(13) Uani 1 1 d . . . . .
H24 H 1.1261 0.4246 0.6449 0.068 Uiso 1 1 calc R U . . .
C25 C 1.0966(4) 0.5578(4) 0.5466(4) 0.0600(14) Uani 1 1 d . . . . .
H25 H 1.1662 0.5495 0.5220 0.072 Uiso 1 1 calc R U . . .
C26 C 1.0197(4) 0.6433(4) 0.5088(3) 0.0552(13) Uani 1 1 d . . . . .
H26 H 1.0361 0.6928 0.4569 0.066 Uiso 1 1 calc R U . . .
C27 C 0.9185(3) 0.6576(3) 0.5461(3) 0.0450(11) Uani 1 1 d . . . . .
H27 H 0.8656 0.7166 0.5197 0.054 Uiso 1 1 calc R U . . .
C28 C 0.9215(3) 0.7510(3) 0.7831(3) 0.0366(9) Uani 1 1 d . . . . .
C29 C 1.0069(3) 0.7040(3) 0.7306(3) 0.0454(11) Uani 1 1 d . . . . .
H29 H 1.0163 0.6365 0.7252 0.055 Uiso 1 1 calc R U . . .
C30 C 1.0789(3) 0.7542(4) 0.6858(3) 0.0519(12) Uani 1 1 d . . . . .
H30 H 1.1367 0.7216 0.6494 0.062 Uiso 1 1 calc R U . . .
C31 C 1.0660(3) 0.8513(4) 0.6945(3) 0.0534(12) Uani 1 1 d . . . . .
H31 H 1.1163 0.8848 0.6653 0.064 Uiso 1 1 calc R U . . .
C32 C 0.9813(3) 0.9009(3) 0.7448(3) 0.0486(11) Uani 1 1 d . . . . .
H32 H 0.9728 0.9683 0.7497 0.058 Uiso 1 1 calc R U . . .
C33 C 0.9088(3) 0.8520(3) 0.7881(3) 0.0441(11) Uani 1 1 d . . . . .
H33 H 0.8495 0.8868 0.8217 0.053 Uiso 1 1 calc R U . . .
C34 C 0.7889(3) 0.7262(3) 0.9445(3) 0.0420(10) Uani 1 1 d . . . . .
C35 C 0.8697(4) 0.7004(4) 0.9981(3) 0.0535(12) Uani 1 1 d . . . . .
H35 H 0.9383 0.6707 0.9746 0.064 Uiso 1 1 calc R U . . .
C36 C 0.8520(4) 0.7173(4) 1.0846(3) 0.0660(15) Uani 1 1 d . . . . .
H36 H 0.9085 0.7012 1.1192 0.079 Uiso 1 1 calc R U . . .
C37 C 0.7535(4) 0.7574(5) 1.1210(4) 0.0726(16) Uani 1 1 d . . . . .
H37 H 0.7409 0.7666 1.1815 0.087 Uiso 1 1 calc R U . . .
C38 C 0.6735(4) 0.7838(5) 1.0688(4) 0.0701(16) Uani 1 1 d . . . . .
H38 H 0.6051 0.8125 1.0932 0.084 Uiso 1 1 calc R U . . .
C39 C 0.6908(3) 0.7693(3) 0.9806(3) 0.0514(12) Uani 1 1 d . . . . .
H39 H 0.6343 0.7894 0.9450 0.062 Uiso 1 1 calc R U . . .
C40 C 0.8231(3) 0.3510(3) 0.9445(3) 0.0401(10) Uani 1 1 d . . . . .
C41 C 0.7955(4) 0.3264(4) 1.0391(3) 0.0570(13) Uani 1 1 d . . . . .
H41 H 0.7535 0.3794 1.0679 0.068 Uiso 1 1 calc R U . . .
C42 C 0.8281(4) 0.2271(4) 1.0907(3) 0.0637(14) Uani 1 1 d . . . . .
H42 H 0.8071 0.2118 1.1543 0.076 Uiso 1 1 calc R U . . .
C43 C 0.8904(4) 0.1502(4) 1.0513(4) 0.0591(13) Uani 1 1 d . . . . .
H43 H 0.9155 0.0823 1.0880 0.071 Uiso 1 1 calc R U . . .
C44 C 0.9168(4) 0.1707(3) 0.9592(4) 0.0572(13) Uani 1 1 d . . . . .
H44 H 0.9588 0.1167 0.9316 0.069 Uiso 1 1 calc R U . . .
C45 C 0.8829(3) 0.2692(3) 0.9065(3) 0.0505(12) Uani 1 1 d . . . . .
H45 H 0.9005 0.2820 0.8423 0.061 Uiso 1 1 calc R U . . .
C46 C 0.5298(3) 0.8444(3) 0.5925(3) 0.0436(10) Uani 1 1 d . . . . .
C47 C 0.4623(4) 0.8833(4) 0.5188(3) 0.0616(14) Uani 1 1 d . . . . .
H47A H 0.5029 0.8971 0.4599 0.092 Uiso 1 1 calc R U . . .
H47B H 0.4093 0.9471 0.5270 0.092 Uiso 1 1 calc R U . . .
H47C H 0.4294 0.8319 0.5199 0.092 Uiso 1 1 calc R U . . .
C48 C 0.8158(3) 0.8751(3) 0.5932(3) 0.0456(11) Uani 1 1 d . . . . .
C49 C 0.8764(4) 0.9358(4) 0.5295(3) 0.0655(15) Uani 1 1 d . . . . .
H49A H 0.9062 0.9665 0.5634 0.098 Uiso 1 1 calc R U . . .
H49B H 0.8319 0.9904 0.4858 0.098 Uiso 1 1 calc R U . . .
H49C H 0.9318 0.8913 0.4966 0.098 Uiso 1 1 calc R U . . .
C50 C 0.6032(3) 0.9591(4) 0.7870(3) 0.0493(12) Uani 1 1 d . . . . .
C51 C 0.5575(4) 1.0606(4) 0.8063(5) 0.085(2) Uani 1 1 d . . . . .
H51A H 0.4967 1.0986 0.7723 0.127 Uiso 1 1 calc R U . . .
H51B H 0.6080 1.0987 0.7877 0.127 Uiso 1 1 calc R U . . .
H51C H 0.5370 1.0527 0.8720 0.127 Uiso 1 1 calc R U . . .
C52 C 0.8473(3) 0.8782(3) 0.2844(3) 0.0505(11) Uani 1 1 d . . . . .
S2A S 0.7574(2) 1.22147(19) 0.69894(18) 0.0530(7) Uani 0.610(5) 1 d D U P A 1
O4A O 0.6526(4) 1.2824(5) 0.7097(4) 0.0613(17) Uani 0.610(5) 1 d D U P A 1
F6A F 0.8698(4) 1.1430(4) 0.5624(4) 0.0642(14) Uani 0.610(5) 1 d D U P A 1
C53A C 0.7709(5) 1.1904(5) 0.5890(5) 0.0660(17) Uani 0.610(5) 1 d D U P A 1
S2B S 0.7999(5) 1.1900(5) 0.6792(4) 0.1001(17) Uani 0.390(5) 1 d D U P A 2
O4B O 0.8851(7) 1.1379(7) 0.6217(7) 0.067(2) Uani 0.390(5) 1 d D U P A 2
F6B F 0.6203(8) 1.2633(9) 0.6770(8) 0.112(3) Uani 0.390(5) 1 d D U P A 2
C53B C 0.6919(7) 1.2245(6) 0.6142(4) 0.050(2) Uani 0.390(5) 1 d D U P A 2
O5 O 0.7881(3) 1.1199(2) 0.7613(2) 0.0716(10) Uani 1 1 d D U . . .
O6 O 0.8288(3) 1.2767(2) 0.6823(3) 0.0710(10) Uani 1 1 d D U . . .
F4 F 0.7280(4) 1.2741(3) 0.5279(3) 0.1253(14) Uani 1 1 d D U . . .
F5 F 0.7056(3) 1.1325(3) 0.5967(3) 0.1290(14) Uani 1 1 d D U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 1.953(4) . ?
Fe1 N3 1.958(3) . ?
Fe1 N1 1.963(4) . ?
Fe1 P3 2.2972(12) . ?
Fe1 P1 2.3031(12) . ?
Fe1 P2 2.3224(11) . ?
P1 C1 1.828(4) . ?
P1 C4 1.839(4) . ?
P1 C10 1.840(4) . ?
P2 C2 1.818(4) . ?
P2 C16 1.836(4) . ?
P2 C22 1.846(4) . ?
P3 C28 1.823(4) . ?
P3 C3 1.831(4) . ?
P3 C34 1.838(4) . ?
Si1 C40 1.853(4) . ?
Si1 C2 1.861(4) . ?
Si1 C3 1.883(4) . ?
Si1 C1 1.884(4) . ?
S1 O3 1.440(3) . ?
S1 O1 1.441(3) . ?
S1 O2 1.443(3) . ?
S1 C52 1.819(5) . ?
N1 C46 1.129(5) . ?
N2 C48 1.135(5) . ?
N3 C50 1.128(5) . ?
F1 C52 1.326(5) . ?
F2 C52 1.326(5) . ?
F3 C52 1.334(5) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.385(5) . ?
C4 C9 1.392(6) . ?
C5 C6 1.389(6) . ?
C5 H5 0.9500 . ?
C6 C7 1.367(6) . ?
C6 H6 0.9500 . ?
C7 C8 1.391(6) . ?
C7 H7 0.9500 . ?
C8 C9 1.382(5) . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?
C10 C15 1.383(5) . ?
C10 C11 1.400(6) . ?
C11 C12 1.383(6) . ?
C11 H11 0.9500 . ?
C12 C13 1.385(6) . ?
C12 H12 0.9500 . ?
C13 C14 1.385(6) . ?
C13 H13 0.9500 . ?
C14 C15 1.388(5) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C16 C17 1.392(5) . ?
C16 C21 1.392(6) . ?
C17 C18 1.379(6) . ?
C17 H17 0.9500 . ?
C18 C19 1.374(6) . ?
C18 H18 0.9500 . ?
C19 C20 1.383(6) . ?
C19 H19 0.9500 . ?
C20 C21 1.395(6) . ?
C20 H20 0.9500 . ?
C21 H21 0.9500 . ?
C22 C23 1.377(6) . ?
C22 C27 1.408(6) . ?
C23 C24 1.386(6) . ?
C23 H23 0.9500 . ?
C24 C25 1.374(7) . ?
C24 H24 0.9500 . ?
C25 C26 1.376(7) . ?
C25 H25 0.9500 . ?
C26 C27 1.386(6) . ?
C26 H26 0.9500 . ?
C27 H27 0.9500 . ?
C28 C29 1.388(6) . ?
C28 C33 1.410(5) . ?
C29 C30 1.390(6) . ?
C29 H29 0.9500 . ?
C30 C31 1.375(6) . ?
C30 H30 0.9500 . ?
C31 C32 1.377(6) . ?
C31 H31 0.9500 . ?
C32 C33 1.379(6) . ?
C32 H32 0.9500 . ?
C33 H33 0.9500 . ?
C34 C39 1.374(6) . ?
C34 C35 1.393(6) . ?
C35 C36 1.378(6) . ?
C35 H35 0.9500 . ?
C36 C37 1.372(7) . ?
C36 H36 0.9500 . ?
C37 C38 1.368(7) . ?
C37 H37 0.9500 . ?
C38 C39 1.392(6) . ?
C38 H38 0.9500 . ?
C39 H39 0.9500 . ?
C40 C45 1.394(6) . ?
C40 C41 1.404(6) . ?
C41 C42 1.373(6) . ?
C41 H41 0.9500 . ?
C42 C43 1.363(7) . ?
C42 H42 0.9500 . ?
C43 C44 1.365(7) . ?
C43 H43 0.9500 . ?
C44 C45 1.372(6) . ?
C44 H44 0.9500 . ?
C45 H45 0.9500 . ?
C46 C47 1.459(6) . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 C49 1.455(6) . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C50 C51 1.461(6) . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
S2A O6 1.407(4) . ?
S2A O4A 1.425(6) . ?
S2A O5 1.457(4) . ?
S2A C53A 1.824(6) . ?
F6A C53A 1.352(7) . ?
C53A F4 1.317(7) . ?
C53A F5 1.385(6) . ?
S2B O5 1.387(6) . ?
S2B O6 1.435(6) . ?
S2B O4B 1.458(8) . ?
S2B C53B 1.796(8) . ?
F6B C53B 1.344(8) . ?
C53B F5 1.354(7) . ?
C53B F4 1.403(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
N2 Fe1 N3 83.22(14) . . ?
N2 Fe1 N1 85.75(14) . . ?
N3 Fe1 N1 86.84(13) . . ?
N2 Fe1 P3 89.49(10) . . ?
N3 Fe1 P3 89.29(10) . . ?
N1 Fe1 P3 174.20(10) . . ?
N2 Fe1 P1 175.99(10) . . ?
N3 Fe1 P1 94.16(10) . . ?
N1 Fe1 P1 91.07(10) . . ?
P3 Fe1 P1 93.53(4) . . ?
N2 Fe1 P2 90.87(10) . . ?
N3 Fe1 P2 173.62(11) . . ?
N1 Fe1 P2 90.34(10) . . ?
P3 Fe1 P2 93.07(4) . . ?
P1 Fe1 P2 91.61(4) . . ?
C1 P1 C4 104.65(18) . . ?
C1 P1 C10 104.65(19) . . ?
C4 P1 C10 98.85(17) . . ?
C1 P1 Fe1 112.90(13) . . ?
C4 P1 Fe1 116.51(13) . . ?
C10 P1 Fe1 117.44(13) . . ?
C2 P2 C16 103.97(18) . . ?
C2 P2 C22 102.81(19) . . ?
C16 P2 C22 102.27(18) . . ?
C2 P2 Fe1 113.61(13) . . ?
C16 P2 Fe1 116.16(13) . . ?
C22 P2 Fe1 116.25(12) . . ?
C28 P3 C3 106.92(18) . . ?
C28 P3 C34 100.53(18) . . ?
C3 P3 C34 100.23(19) . . ?
C28 P3 Fe1 112.06(14) . . ?
C3 P3 Fe1 115.02(13) . . ?
C34 P3 Fe1 120.25(14) . . ?
C40 Si1 C2 110.99(18) . . ?
C40 Si1 C3 111.96(18) . . ?
C2 Si1 C3 108.86(18) . . ?
C40 Si1 C1 110.40(18) . . ?
C2 Si1 C1 107.03(18) . . ?
C3 Si1 C1 107.41(18) . . ?
O3 S1 O1 115.12(19) . . ?
O3 S1 O2 114.54(19) . . ?
O1 S1 O2 114.57(18) . . ?
O3 S1 C52 103.80(19) . . ?
O1 S1 C52 103.3(2) . . ?
O2 S1 C52 103.3(2) . . ?
C46 N1 Fe1 173.7(3) . . ?
C48 N2 Fe1 174.7(4) . . ?
C50 N3 Fe1 172.2(4) . . ?
P1 C1 Si1 113.3(2) . . ?
P1 C1 H1A 108.9 . . ?
Si1 C1 H1A 108.9 . . ?
P1 C1 H1B 108.9 . . ?
Si1 C1 H1B 108.9 . . ?
H1A C1 H1B 107.7 . . ?
P2 C2 Si1 113.7(2) . . ?
P2 C2 H2A 108.8 . . ?
Si1 C2 H2A 108.8 . . ?
P2 C2 H2B 108.8 . . ?
Si1 C2 H2B 108.8 . . ?
H2A C2 H2B 107.7 . . ?
P3 C3 Si1 111.9(2) . . ?
P3 C3 H3A 109.2 . . ?
Si1 C3 H3A 109.2 . . ?
P3 C3 H3B 109.2 . . ?
Si1 C3 H3B 109.2 . . ?
H3A C3 H3B 107.9 . . ?
C5 C4 C9 117.5(4) . . ?
C5 C4 P1 123.9(3) . . ?
C9 C4 P1 118.5(3) . . ?
C4 C5 C6 121.0(4) . . ?
C4 C5 H5 119.5 . . ?
C6 C5 H5 119.5 . . ?
C7 C6 C5 120.4(4) . . ?
C7 C6 H6 119.8 . . ?
C5 C6 H6 119.8 . . ?
C6 C7 C8 120.2(4) . . ?
C6 C7 H7 119.9 . . ?
C8 C7 H7 119.9 . . ?
C9 C8 C7 118.7(4) . . ?
C9 C8 H8 120.6 . . ?
C7 C8 H8 120.6 . . ?
C8 C9 C4 122.2(4) . . ?
C8 C9 H9 118.9 . . ?
C4 C9 H9 118.9 . . ?
C15 C10 C11 118.3(4) . . ?
C15 C10 P1 121.1(3) . . ?
C11 C10 P1 120.7(3) . . ?
C12 C11 C10 121.2(4) . . ?
C12 C11 H11 119.4 . . ?
C10 C11 H11 119.4 . . ?
C11 C12 C13 119.7(4) . . ?
C11 C12 H12 120.2 . . ?
C13 C12 H12 120.2 . . ?
C12 C13 C14 119.9(4) . . ?
C12 C13 H13 120.1 . . ?
C14 C13 H13 120.1 . . ?
C13 C14 C15 120.1(4) . . ?
C13 C14 H14 119.9 . . ?
C15 C14 H14 119.9 . . ?
C10 C15 C14 120.9(4) . . ?
C10 C15 H15 119.5 . . ?
C14 C15 H15 119.5 . . ?
C17 C16 C21 118.7(4) . . ?
C17 C16 P2 122.1(3) . . ?
C21 C16 P2 119.2(3) . . ?
C18 C17 C16 120.4(4) . . ?
C18 C17 H17 119.8 . . ?
C16 C17 H17 119.8 . . ?
C19 C18 C17 121.0(4) . . ?
C19 C18 H18 119.5 . . ?
C17 C18 H18 119.5 . . ?
C18 C19 C20 119.5(4) . . ?
C18 C19 H19 120.2 . . ?
C20 C19 H19 120.2 . . ?
C19 C20 C21 120.0(4) . . ?
C19 C20 H20 120.0 . . ?
C21 C20 H20 120.0 . . ?
C16 C21 C20 120.4(4) . . ?
C16 C21 H21 119.8 . . ?
C20 C21 H21 119.8 . . ?
C23 C22 C27 118.3(4) . . ?
C23 C22 P2 122.7(3) . . ?
C27 C22 P2 119.1(3) . . ?
C22 C23 C24 121.2(5) . . ?
C22 C23 H23 119.4 . . ?
C24 C23 H23 119.4 . . ?
C25 C24 C23 119.9(5) . . ?
C25 C24 H24 120.1 . . ?
C23 C24 H24 120.1 . . ?
C24 C25 C26 120.2(4) . . ?
C24 C25 H25 119.9 . . ?
C26 C25 H25 119.9 . . ?
C25 C26 C27 120.2(5) . . ?
C25 C26 H26 119.9 . . ?
C27 C26 H26 119.9 . . ?
C26 C27 C22 120.1(4) . . ?
C26 C27 H27 119.9 . . ?
C22 C27 H27 119.9 . . ?
C29 C28 C33 118.1(4) . . ?
C29 C28 P3 122.8(3) . . ?
C33 C28 P3 118.5(3) . . ?
C28 C29 C30 120.9(4) . . ?
C28 C29 H29 119.5 . . ?
C30 C29 H29 119.5 . . ?
C31 C30 C29 119.5(4) . . ?
C31 C30 H30 120.2 . . ?
C29 C30 H30 120.2 . . ?
C30 C31 C32 121.1(4) . . ?
C30 C31 H31 119.5 . . ?
C32 C31 H31 119.5 . . ?
C31 C32 C33 119.6(4) . . ?
C31 C32 H32 120.2 . . ?
C33 C32 H32 120.2 . . ?
C32 C33 C28 120.8(4) . . ?
C32 C33 H33 119.6 . . ?
C28 C33 H33 119.6 . . ?
C39 C34 C35 117.8(4) . . ?
C39 C34 P3 123.1(3) . . ?
C35 C34 P3 119.0(3) . . ?
C36 C35 C34 121.2(4) . . ?
C36 C35 H35 119.4 . . ?
C34 C35 H35 119.4 . . ?
C37 C36 C35 120.5(5) . . ?
C37 C36 H36 119.8 . . ?
C35 C36 H36 119.8 . . ?
C38 C37 C36 118.9(5) . . ?
C38 C37 H37 120.6 . . ?
C36 C37 H37 120.6 . . ?
C37 C38 C39 121.1(5) . . ?
C37 C38 H38 119.5 . . ?
C39 C38 H38 119.5 . . ?
C34 C39 C38 120.5(4) . . ?
C34 C39 H39 119.8 . . ?
C38 C39 H39 119.8 . . ?
C45 C40 C41 116.4(4) . . ?
C45 C40 Si1 121.8(3) . . ?
C41 C40 Si1 121.8(3) . . ?
C42 C41 C40 121.1(4) . . ?
C42 C41 H41 119.4 . . ?
C40 C41 H41 119.4 . . ?
C43 C42 C41 120.5(5) . . ?
C43 C42 H42 119.7 . . ?
C41 C42 H42 119.7 . . ?
C42 C43 C44 120.0(4) . . ?
C42 C43 H43 120.0 . . ?
C44 C43 H43 120.0 . . ?
C43 C44 C45 120.1(5) . . ?
C43 C44 H44 119.9 . . ?
C45 C44 H44 119.9 . . ?
C44 C45 C40 121.8(5) . . ?
C44 C45 H45 119.1 . . ?
C40 C45 H45 119.1 . . ?
N1 C46 C47 176.9(5) . . ?
C46 C47 H47A 109.5 . . ?
C46 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
C46 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
N2 C48 C49 178.1(5) . . ?
C48 C49 H49A 109.5 . . ?
C48 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
C48 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
N3 C50 C51 176.7(5) . . ?
C50 C51 H51A 109.5 . . ?
C50 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
C50 C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
F2 C52 F1 107.3(4) . . ?
F2 C52 F3 106.9(4) . . ?
F1 C52 F3 107.8(4) . . ?
F2 C52 S1 111.8(3) . . ?
F1 C52 S1 111.6(3) . . ?
F3 C52 S1 111.1(3) . . ?
O6 S2A O4A 114.2(3) . . ?
O6 S2A O5 114.8(3) . . ?
O4A S2A O5 117.1(3) . . ?
O6 S2A C53A 100.9(3) . . ?
O4A S2A C53A 104.6(4) . . ?
O5 S2A C53A 102.3(3) . . ?
F4 C53A F6A 112.9(6) . . ?
F4 C53A F5 101.2(5) . . ?
F6A C53A F5 113.2(5) . . ?
F4 C53A S2A 109.4(4) . . ?
F6A C53A S2A 112.4(5) . . ?
F5 C53A S2A 107.0(5) . . ?
O5 S2B O6 117.5(5) . . ?
O5 S2B O4B 108.5(6) . . ?
O6 S2B O4B 102.9(5) . . ?
O5 S2B C53B 110.4(4) . . ?
O6 S2B C53B 113.5(5) . . ?
O4B S2B C53B 102.5(7) . . ?
F6B C53B F5 123.9(8) . . ?
F6B C53B F4 130.1(8) . . ?
F5 C53B F4 98.5(5) . . ?
F6B C53B S2B 95.9(7) . . ?
F5 C53B S2B 99.7(6) . . ?
F4 C53B S2B 102.0(5) . . ?

_refine_diff_density_max         2.100
_refine_diff_density_min         -0.749
_refine_diff_density_rms         0.077

_shelxl_version_number           2014-3


####################################################################### 
# 
# 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_3prime
_database_code_depnum_ccdc_archive 'CCDC 1481875'
_audit_update_record             
;
2016-06-21 deposited with the CCDC.
2016-07-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C50 H44 F6 Fe N3 O9 P3 S2 Si'
_chemical_formula_weight         1185.85

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'
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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   13.2856(5)
_cell_length_b                   23.6456(9)
_cell_length_c                   17.1543(4)
_cell_angle_alpha                90
_cell_angle_beta                 102.994(2)
_cell_angle_gamma                90
_cell_volume                     5251.0(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    194968
_cell_measurement_theta_min      2.11
_cell_measurement_theta_max      25.68

_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            'translucent light orange'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.500
_exptl_crystal_F_000             2432
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_exptl_absorpt_coefficient_mu    0.560
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.848
_exptl_absorpt_correction_T_max  0.904
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_special_details           'crystal-to-detector distance 30 mm'
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method       
'two φ and seven ω scans with 2° steps (488 frames)'
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            194968
_diffrn_reflns_av_unetI/netI     0.0330
_diffrn_reflns_av_R_equivalents  0.0244
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.110
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             9959
_reflns_number_gt                8074
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  
'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)'

_refine_special_details          
;
 Structure solved by intrinsic phasing and subsequent difference Fourier
 synthesis. All non-hydrogen atoms were refined with anisotropic
 displacement parameters. The H atoms were introduced at calculated
 positions and were treated as riding atoms with an isotropic displacement
 parameter equal to 1.2 times that of the parent atom (1.5 for CH₃, with
 optimized geometry). 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0440P)²+3.1971P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9959
_refine_ls_number_parameters     679
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0517
_refine_ls_R_factor_gt           0.0374
_refine_ls_wR_factor_ref         0.0954
_refine_ls_wR_factor_gt          0.0899
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_restrained_S_all      1.026
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.21848(2) 0.47567(2) 0.24073(2) 0.02525(9) Uani 1 1 d . . . . .
P1 P 0.27453(4) 0.38582(2) 0.24892(3) 0.02799(13) Uani 1 1 d . . . . .
P2 P 0.12532(4) 0.45843(2) 0.33288(3) 0.02749(13) Uani 1 1 d . . . . .
P3 P 0.36172(4) 0.50027(2) 0.33355(3) 0.02794(13) Uani 1 1 d . . . . .
Si1 Si 0.30938(5) 0.40495(3) 0.42019(3) 0.02884(14) Uani 1 1 d . . . . .
S1 S 0.29251(7) 0.68125(3) 0.06507(5) 0.0598(2) Uani 1 1 d . . . . .
S2 S 0.84544(5) 0.58167(3) 0.09540(4) 0.04342(16) Uani 1 1 d . . . . .
O1 O 0.30279(12) 0.36443(6) 0.34155(9) 0.0346(4) Uani 1 1 d . . . . .
O2 O 0.19447(12) 0.43232(7) 0.41468(9) 0.0319(3) Uani 1 1 d . . . . .
O3 O 0.38372(12) 0.45889(7) 0.41147(9) 0.0334(4) Uani 1 1 d . . . . .
O4 O 0.2629(2) 0.63127(9) 0.10228(16) 0.0838(8) Uani 1 1 d . . . . .
O5 O 0.2494(2) 0.73306(10) 0.08554(18) 0.0978(9) Uani 1 1 d . . . . .
O6 O 0.29373(19) 0.67428(10) -0.01779(13) 0.0727(6) Uani 1 1 d . . . . .
O7 O 0.94395(18) 0.60473(14) 0.13005(15) 0.0939(9) Uani 1 1 d . . . . .
O8 O 0.81179(18) 0.53795(9) 0.14128(12) 0.0640(6) Uani 1 1 d . . . . .
O9 O 0.82744(16) 0.57074(8) 0.01085(11) 0.0544(5) Uani 1 1 d . . . . .
N1 N 0.09559(14) 0.45873(8) 0.15601(11) 0.0317(4) Uani 1 1 d . . . . .
N2 N 0.17514(14) 0.55500(8) 0.23423(10) 0.0292(4) Uani 1 1 d . . . . .
N3 N 0.28426(14) 0.49403(8) 0.15228(11) 0.0304(4) Uani 1 1 d . . . . .
F1 F 0.4430(3) 0.69473(11) 0.19045(13) 0.1236(10) Uani 1 1 d . . . . .
F2 F 0.47918(17) 0.64090(10) 0.10113(14) 0.0933(7) Uani 1 1 d . . . . .
F3 F 0.47200(18) 0.73106(10) 0.08480(14) 0.0993(8) Uani 1 1 d . . . . .
F4 F 0.6615(2) 0.62317(17) 0.06301(15) 0.1469(15) Uani 1 1 d . . . . .
F5 F 0.7808(3) 0.68393(11) 0.06544(16) 0.1550(16) Uani 1 1 d . . . . .
F6 F 0.7531(2) 0.65137(10) 0.17458(12) 0.1129(9) Uani 1 1 d . . . . .
C1 C 0.18638(17) 0.33081(10) 0.20156(14) 0.0348(5) Uani 1 1 d . . . . .
C2 C 0.1589(2) 0.28616(11) 0.24600(18) 0.0504(7) Uani 1 1 d . . . . .
H2 H 0.1883 0.2833 0.3017 0.061 Uiso 1 1 calc R U . . .
C3 C 0.0888(3) 0.24631(14) 0.2084(2) 0.0720(10) Uani 1 1 d . . . . .
H3 H 0.0698 0.2160 0.2386 0.086 Uiso 1 1 calc R U . . .
C4 C 0.0460(3) 0.24978(14) 0.1281(3) 0.0755(11) Uani 1 1 d . . . . .
H4 H -0.0035 0.2226 0.1033 0.091 Uiso 1 1 calc R U . . .
C5 C 0.0748(2) 0.29280(14) 0.0830(2) 0.0625(9) Uani 1 1 d . . . . .
H5 H 0.0461 0.2947 0.0271 0.075 Uiso 1 1 calc R U . . .
C6 C 0.1458(2) 0.33318(11) 0.11966(16) 0.0441(6) Uani 1 1 d . . . . .
H6 H 0.1665 0.3624 0.0887 0.053 Uiso 1 1 calc R U . . .
C7 C 0.39324(17) 0.36817(9) 0.21783(13) 0.0299(5) Uani 1 1 d . . . . .
C8 C 0.47407(19) 0.34121(11) 0.27047(15) 0.0413(6) Uani 1 1 d . . . . .
H8 H 0.4683 0.3333 0.3236 0.050 Uiso 1 1 calc R U . . .
C9 C 0.5628(2) 0.32581(12) 0.24604(17) 0.0504(7) Uani 1 1 d . . . . .
H9 H 0.6174 0.3072 0.2823 0.061 Uiso 1 1 calc R U . . .
C10 C 0.57188(19) 0.33739(12) 0.16942(18) 0.0476(7) Uani 1 1 d . . . . .
H10 H 0.6330 0.3271 0.1530 0.057 Uiso 1 1 calc R U . . .
C11 C 0.4926(2) 0.36390(11) 0.11628(16) 0.0434(6) Uani 1 1 d . . . . .
H11 H 0.4994 0.3719 0.0635 0.052 Uiso 1 1 calc R U . . .
C12 C 0.40253(19) 0.37892(10) 0.13996(14) 0.0363(5) Uani 1 1 d . . . . .
H12 H 0.3474 0.3965 0.1029 0.044 Uiso 1 1 calc R U . . .
C13 C 0.02160(17) 0.40615(10) 0.31107(14) 0.0324(5) Uani 1 1 d . . . . .
C14 C -0.06853(18) 0.41585(11) 0.25307(16) 0.0433(6) Uani 1 1 d . . . . .
H14 H -0.0758 0.4497 0.2224 0.052 Uiso 1 1 calc R U . . .
C15 C -0.1477(2) 0.37638(13) 0.2399(2) 0.0585(8) Uani 1 1 d . . . . .
H15 H -0.2083 0.3831 0.1995 0.070 Uiso 1 1 calc R U . . .
C16 C -0.1393(2) 0.32767(13) 0.2845(2) 0.0614(8) Uani 1 1 d . . . . .
H16 H -0.1942 0.3010 0.2752 0.074 Uiso 1 1 calc R U . . .
C17 C -0.0515(2) 0.31754(12) 0.34261(19) 0.0538(7) Uani 1 1 d . . . . .
H17 H -0.0460 0.2841 0.3739 0.065 Uiso 1 1 calc R U . . .
C18 C 0.0295(2) 0.35632(10) 0.35570(15) 0.0403(6) Uani 1 1 d . . . . .
H18 H 0.0906 0.3488 0.3953 0.048 Uiso 1 1 calc R U . . .
C19 C 0.06403(17) 0.51740(9) 0.37166(13) 0.0312(5) Uani 1 1 d . . . . .
C20 C 0.0895(2) 0.53004(11) 0.45292(15) 0.0436(6) Uani 1 1 d . . . . .
H20 H 0.1408 0.5087 0.4883 0.052 Uiso 1 1 calc R U . . .
C21 C 0.0392(3) 0.57432(12) 0.48209(17) 0.0558(8) Uani 1 1 d . . . . .
H21 H 0.0577 0.5837 0.5373 0.067 Uiso 1 1 calc R U . . .
C22 C -0.0365(2) 0.60443(12) 0.43196(18) 0.0542(8) Uani 1 1 d . . . . .
H22 H -0.0712 0.6340 0.4527 0.065 Uiso 1 1 calc R U . . .
C23 C -0.0627(2) 0.59192(12) 0.35142(18) 0.0509(7) Uani 1 1 d . . . . .
H23 H -0.1159 0.6126 0.3168 0.061 Uiso 1 1 calc R U . . .
C24 C -0.01143(19) 0.54912(11) 0.32095(15) 0.0402(6) Uani 1 1 d . . . . .
H24 H -0.0279 0.5414 0.2652 0.048 Uiso 1 1 calc R U . . .
C25 C 0.35950(17) 0.56967(10) 0.37847(13) 0.0323(5) Uani 1 1 d . . . . .
C26 C 0.3259(2) 0.57581(12) 0.44854(16) 0.0526(7) Uani 1 1 d . . . . .
H26 H 0.3102 0.5433 0.4761 0.063 Uiso 1 1 calc R U . . .
C27 C 0.3150(3) 0.62941(14) 0.47897(19) 0.0697(9) Uani 1 1 d . . . . .
H27 H 0.2911 0.6331 0.5269 0.084 Uiso 1 1 calc R U . . .
C28 C 0.3382(2) 0.67671(13) 0.44092(18) 0.0576(8) Uani 1 1 d . . . . .
H28 H 0.3300 0.7132 0.4620 0.069 Uiso 1 1 calc R U . . .
C29 C 0.3734(2) 0.67111(11) 0.37182(18) 0.0523(7) Uani 1 1 d . . . . .
H29 H 0.3912 0.7038 0.3456 0.063 Uiso 1 1 calc R U . . .
C30 C 0.3831(2) 0.61820(11) 0.34063(17) 0.0478(6) Uani 1 1 d . . . . .
H30 H 0.4063 0.6149 0.2923 0.057 Uiso 1 1 calc R U . . .
C31 C 0.48609(17) 0.49780(10) 0.30604(14) 0.0326(5) Uani 1 1 d . . . . .
C32 C 0.50560(19) 0.52974(11) 0.24243(14) 0.0380(5) Uani 1 1 d . . . . .
H32 H 0.4527 0.5530 0.2121 0.046 Uiso 1 1 calc R U . . .
C33 C 0.6018(2) 0.52780(12) 0.22323(16) 0.0463(6) Uani 1 1 d . . . . .
H33 H 0.6144 0.5496 0.1799 0.056 Uiso 1 1 calc R U . . .
C34 C 0.6790(2) 0.49410(13) 0.26718(19) 0.0533(7) Uani 1 1 d . . . . .
H34 H 0.7448 0.4927 0.2541 0.064 Uiso 1 1 calc R U . . .
C35 C 0.6605(2) 0.46257(12) 0.32970(19) 0.0538(7) Uani 1 1 d . . . . .
H35 H 0.7139 0.4395 0.3598 0.065 Uiso 1 1 calc R U . . .
C36 C 0.56485(19) 0.46402(11) 0.34943(16) 0.0425(6) Uani 1 1 d . . . . .
H36 H 0.5531 0.4419 0.3927 0.051 Uiso 1 1 calc R U . . .
C37 C 0.34202(17) 0.36235(10) 0.51041(13) 0.0324(5) Uani 1 1 d . . . . .
C38 C 0.3349(2) 0.38462(11) 0.58491(14) 0.0408(6) Uani 1 1 d . . . . .
H38 H 0.3240 0.4240 0.5902 0.049 Uiso 1 1 calc R U . . .
C39 C 0.3436(2) 0.34933(13) 0.65069(15) 0.0487(7) Uani 1 1 d . . . . .
H39 H 0.3414 0.3649 0.7013 0.058 Uiso 1 1 calc R U . . .
C40 C 0.3554(2) 0.29229(12) 0.64307(16) 0.0546(8) Uani 1 1 d . . . . .
H40 H 0.3590 0.2683 0.6880 0.066 Uiso 1 1 calc R U . . .
C41 C 0.3622(3) 0.26977(12) 0.57131(18) 0.0633(9) Uani 1 1 d . . . . .
H41 H 0.3717 0.2302 0.5667 0.076 Uiso 1 1 calc R U . . .
C42 C 0.3551(2) 0.30429(12) 0.50486(16) 0.0529(7) Uani 1 1 d . . . . .
H42 H 0.3593 0.2881 0.4550 0.063 Uiso 1 1 calc R U . . .
C43 C 0.02805(18) 0.44855(11) 0.10440(15) 0.0365(5) Uani 1 1 d . . . . .
C44 C -0.05897(19) 0.43354(13) 0.03928(16) 0.0487(7) Uani 1 1 d . . . . .
H44A H -0.0331 0.4180 -0.0055 0.073 Uiso 1 1 calc R U . . .
H44B H -0.1005 0.4673 0.0215 0.073 Uiso 1 1 calc R U . . .
H44C H -0.1018 0.4051 0.0581 0.073 Uiso 1 1 calc R U . . .
C45 C 0.15634(18) 0.60187(10) 0.23047(13) 0.0334(5) Uani 1 1 d . . . . .
C46 C 0.1331(2) 0.66227(11) 0.22866(17) 0.0474(6) Uani 1 1 d . . . . .
H46A H 0.1370 0.6758 0.2833 0.071 Uiso 1 1 calc R U . . .
H46B H 0.0634 0.6688 0.1961 0.071 Uiso 1 1 calc R U . . .
H46C H 0.1834 0.6828 0.2054 0.071 Uiso 1 1 calc R U . . .
C47 C 0.31268(18) 0.50729(10) 0.09711(14) 0.0355(5) Uani 1 1 d . . . . .
C48 C 0.3542(2) 0.52286(13) 0.02821(15) 0.0495(7) Uani 1 1 d . . . . .
H48A H 0.4294 0.5183 0.0416 0.074 Uiso 1 1 calc R U . . .
H48B H 0.3368 0.5624 0.0139 0.074 Uiso 1 1 calc R U . . .
H48C H 0.3241 0.4984 -0.0171 0.074 Uiso 1 1 calc R U . . .
C49 C 0.4252(3) 0.68765(14) 0.11238(18) 0.0680(9) Uani 1 1 d . . . . .
C50 C 0.7582(4) 0.63862(17) 0.10043(19) 0.0802(12) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 1.958(2) . ?
Fe1 N3 1.9624(18) . ?
Fe1 N1 1.967(2) . ?
Fe1 P1 2.2452(6) . ?
Fe1 P2 2.2532(6) . ?
Fe1 P3 2.2656(6) . ?
P1 O1 1.6288(15) . ?
P1 C1 1.815(2) . ?
P1 C7 1.823(2) . ?
P2 O2 1.6169(16) . ?
P2 C19 1.815(2) . ?
P2 C13 1.826(2) . ?
P3 O3 1.6290(16) . ?
P3 C25 1.816(2) . ?
P3 C31 1.819(2) . ?
Si1 O3 1.6405(16) . ?
Si1 O1 1.6409(16) . ?
Si1 O2 1.6412(16) . ?
Si1 C37 1.816(2) . ?
S1 O5 1.429(2) . ?
S1 O6 1.435(2) . ?
S1 O4 1.439(2) . ?
S1 C49 1.773(4) . ?
S2 O7 1.419(2) . ?
S2 O8 1.430(2) . ?
S2 O9 1.4392(19) . ?
S2 C50 1.791(4) . ?
N1 C43 1.136(3) . ?
N2 C45 1.135(3) . ?
N3 C47 1.139(3) . ?
F1 C49 1.317(4) . ?
F2 C49 1.355(4) . ?
F3 C49 1.340(4) . ?
F4 C50 1.351(5) . ?
F5 C50 1.296(5) . ?
F6 C50 1.324(3) . ?
C1 C6 1.388(4) . ?
C1 C2 1.398(3) . ?
C2 C3 1.379(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.368(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.383(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.389(4) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C12 1.392(3) . ?
C7 C8 1.392(3) . ?
C8 C9 1.386(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.374(4) . ?
C9 H9 0.9500 . ?
C10 C11 1.379(4) . ?
C10 H10 0.9500 . ?
C11 C12 1.394(3) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 C14 1.393(3) . ?
C13 C18 1.396(3) . ?
C14 C15 1.386(4) . ?
C14 H14 0.9500 . ?
C15 C16 1.374(4) . ?
C15 H15 0.9500 . ?
C16 C17 1.375(4) . ?
C16 H16 0.9500 . ?
C17 C18 1.393(4) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 C24 1.390(3) . ?
C19 C20 1.391(3) . ?
C20 C21 1.394(4) . ?
C20 H20 0.9500 . ?
C21 C22 1.367(4) . ?
C21 H21 0.9500 . ?
C22 C23 1.379(4) . ?
C22 H22 0.9500 . ?
C23 C24 1.386(4) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 C26 1.381(3) . ?
C25 C30 1.388(3) . ?
C26 C27 1.391(4) . ?
C26 H26 0.9500 . ?
C27 C28 1.365(4) . ?
C27 H27 0.9500 . ?
C28 C29 1.375(4) . ?
C28 H28 0.9500 . ?
C29 C30 1.378(4) . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?
C31 C36 1.392(3) . ?
C31 C32 1.399(3) . ?
C32 C33 1.390(3) . ?
C32 H32 0.9500 . ?
C33 C34 1.381(4) . ?
C33 H33 0.9500 . ?
C34 C35 1.373(4) . ?
C34 H34 0.9500 . ?
C35 C36 1.388(4) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C37 C42 1.390(4) . ?
C37 C38 1.405(3) . ?
C38 C39 1.387(3) . ?
C38 H38 0.9500 . ?
C39 C40 1.367(4) . ?
C39 H39 0.9500 . ?
C40 C41 1.362(4) . ?
C40 H40 0.9500 . ?
C41 C42 1.388(4) . ?
C41 H41 0.9500 . ?
C42 H42 0.9500 . ?
C43 C44 1.459(3) . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 C46 1.460(3) . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 C48 1.459(3) . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 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
N2 Fe1 N3 85.43(7) . . ?
N2 Fe1 N1 88.19(8) . . ?
N3 Fe1 N1 85.06(7) . . ?
N2 Fe1 P1 177.79(6) . . ?
N3 Fe1 P1 93.37(6) . . ?
N1 Fe1 P1 93.56(6) . . ?
N2 Fe1 P2 90.71(5) . . ?
N3 Fe1 P2 173.16(6) . . ?
N1 Fe1 P2 89.19(6) . . ?
P1 Fe1 P2 90.67(2) . . ?
N2 Fe1 P3 89.07(6) . . ?
N3 Fe1 P3 92.11(6) . . ?
N1 Fe1 P3 176.21(6) . . ?
P1 Fe1 P3 89.12(2) . . ?
P2 Fe1 P3 93.47(2) . . ?
O1 P1 C1 101.43(10) . . ?
O1 P1 C7 100.92(9) . . ?
C1 P1 C7 102.62(10) . . ?
O1 P1 Fe1 110.81(6) . . ?
C1 P1 Fe1 118.59(8) . . ?
C7 P1 Fe1 119.65(7) . . ?
O2 P2 C19 100.92(9) . . ?
O2 P2 C13 100.06(10) . . ?
C19 P2 C13 102.42(10) . . ?
O2 P2 Fe1 112.54(6) . . ?
C19 P2 Fe1 118.73(7) . . ?
C13 P2 Fe1 119.14(7) . . ?
O3 P3 C25 102.22(10) . . ?
O3 P3 C31 100.82(10) . . ?
C25 P3 C31 103.98(10) . . ?
O3 P3 Fe1 112.94(6) . . ?
C25 P3 Fe1 116.04(7) . . ?
C31 P3 Fe1 118.55(8) . . ?
O3 Si1 O1 107.52(8) . . ?
O3 Si1 O2 105.04(8) . . ?
O1 Si1 O2 107.82(8) . . ?
O3 Si1 C37 118.41(9) . . ?
O1 Si1 C37 109.59(10) . . ?
O2 Si1 C37 107.98(9) . . ?
O5 S1 O6 115.87(16) . . ?
O5 S1 O4 115.46(14) . . ?
O6 S1 O4 114.22(15) . . ?
O5 S1 C49 103.10(18) . . ?
O6 S1 C49 103.40(15) . . ?
O4 S1 C49 102.11(16) . . ?
O7 S2 O8 114.84(15) . . ?
O7 S2 O9 114.82(14) . . ?
O8 S2 O9 115.02(13) . . ?
O7 S2 C50 103.7(2) . . ?
O8 S2 C50 103.36(17) . . ?
O9 S2 C50 102.76(14) . . ?
P1 O1 Si1 125.36(10) . . ?
P2 O2 Si1 122.69(9) . . ?
P3 O3 Si1 122.76(9) . . ?
C43 N1 Fe1 176.35(19) . . ?
C45 N2 Fe1 175.63(19) . . ?
C47 N3 Fe1 172.69(19) . . ?
C6 C1 C2 119.5(2) . . ?
C6 C1 P1 119.26(19) . . ?
C2 C1 P1 121.2(2) . . ?
C3 C2 C1 119.5(3) . . ?
C3 C2 H2 120.2 . . ?
C1 C2 H2 120.2 . . ?
C4 C3 C2 120.9(3) . . ?
C4 C3 H3 119.6 . . ?
C2 C3 H3 119.6 . . ?
C3 C4 C5 120.2(3) . . ?
C3 C4 H4 119.9 . . ?
C5 C4 H4 119.9 . . ?
C4 C5 C6 119.8(3) . . ?
C4 C5 H5 120.1 . . ?
C6 C5 H5 120.1 . . ?
C1 C6 C5 120.0(3) . . ?
C1 C6 H6 120.0 . . ?
C5 C6 H6 120.0 . . ?
C12 C7 C8 118.9(2) . . ?
C12 C7 P1 120.53(17) . . ?
C8 C7 P1 120.45(17) . . ?
C9 C8 C7 120.6(2) . . ?
C9 C8 H8 119.7 . . ?
C7 C8 H8 119.7 . . ?
C10 C9 C8 120.0(3) . . ?
C10 C9 H9 120.0 . . ?
C8 C9 H9 120.0 . . ?
C9 C10 C11 120.3(2) . . ?
C9 C10 H10 119.8 . . ?
C11 C10 H10 119.8 . . ?
C10 C11 C12 120.1(2) . . ?
C10 C11 H11 120.0 . . ?
C12 C11 H11 120.0 . . ?
C7 C12 C11 120.0(2) . . ?
C7 C12 H12 120.0 . . ?
C11 C12 H12 120.0 . . ?
C14 C13 C18 118.5(2) . . ?
C14 C13 P2 121.51(18) . . ?
C18 C13 P2 119.90(19) . . ?
C15 C14 C13 120.3(3) . . ?
C15 C14 H14 119.8 . . ?
C13 C14 H14 119.8 . . ?
C16 C15 C14 120.7(3) . . ?
C16 C15 H15 119.7 . . ?
C14 C15 H15 119.7 . . ?
C15 C16 C17 120.0(3) . . ?
C15 C16 H16 120.0 . . ?
C17 C16 H16 120.0 . . ?
C16 C17 C18 120.1(3) . . ?
C16 C17 H17 120.0 . . ?
C18 C17 H17 120.0 . . ?
C17 C18 C13 120.4(3) . . ?
C17 C18 H18 119.8 . . ?
C13 C18 H18 119.8 . . ?
C24 C19 C20 119.3(2) . . ?
C24 C19 P2 120.34(18) . . ?
C20 C19 P2 120.29(18) . . ?
C19 C20 C21 119.5(3) . . ?
C19 C20 H20 120.2 . . ?
C21 C20 H20 120.2 . . ?
C22 C21 C20 120.6(3) . . ?
C22 C21 H21 119.7 . . ?
C20 C21 H21 119.7 . . ?
C21 C22 C23 120.2(2) . . ?
C21 C22 H22 119.9 . . ?
C23 C22 H22 119.9 . . ?
C22 C23 C24 120.0(3) . . ?
C22 C23 H23 120.0 . . ?
C24 C23 H23 120.0 . . ?
C23 C24 C19 120.3(2) . . ?
C23 C24 H24 119.9 . . ?
C19 C24 H24 119.9 . . ?
C26 C25 C30 118.1(2) . . ?
C26 C25 P3 120.25(19) . . ?
C30 C25 P3 121.44(18) . . ?
C25 C26 C27 120.3(3) . . ?
C25 C26 H26 119.9 . . ?
C27 C26 H26 119.9 . . ?
C28 C27 C26 120.9(3) . . ?
C28 C27 H27 119.5 . . ?
C26 C27 H27 119.5 . . ?
C27 C28 C29 119.4(3) . . ?
C27 C28 H28 120.3 . . ?
C29 C28 H28 120.3 . . ?
C28 C29 C30 120.1(3) . . ?
C28 C29 H29 120.0 . . ?
C30 C29 H29 120.0 . . ?
C29 C30 C25 121.2(3) . . ?
C29 C30 H30 119.4 . . ?
C25 C30 H30 119.4 . . ?
C36 C31 C32 118.6(2) . . ?
C36 C31 P3 119.84(18) . . ?
C32 C31 P3 121.58(18) . . ?
C33 C32 C31 120.6(2) . . ?
C33 C32 H32 119.7 . . ?
C31 C32 H32 119.7 . . ?
C34 C33 C32 119.9(3) . . ?
C34 C33 H33 120.0 . . ?
C32 C33 H33 120.0 . . ?
C35 C34 C33 119.9(2) . . ?
C35 C34 H34 120.0 . . ?
C33 C34 H34 120.0 . . ?
C34 C35 C36 120.8(3) . . ?
C34 C35 H35 119.6 . . ?
C36 C35 H35 119.6 . . ?
C35 C36 C31 120.2(3) . . ?
C35 C36 H36 119.9 . . ?
C31 C36 H36 119.9 . . ?
C42 C37 C38 117.9(2) . . ?
C42 C37 Si1 119.95(18) . . ?
C38 C37 Si1 121.03(18) . . ?
C39 C38 C37 120.3(2) . . ?
C39 C38 H38 119.9 . . ?
C37 C38 H38 119.9 . . ?
C40 C39 C38 120.4(3) . . ?
C40 C39 H39 119.8 . . ?
C38 C39 H39 119.8 . . ?
C41 C40 C39 120.3(2) . . ?
C41 C40 H40 119.9 . . ?
C39 C40 H40 119.9 . . ?
C40 C41 C42 120.4(3) . . ?
C40 C41 H41 119.8 . . ?
C42 C41 H41 119.8 . . ?
C41 C42 C37 120.7(3) . . ?
C41 C42 H42 119.6 . . ?
C37 C42 H42 119.6 . . ?
N1 C43 C44 178.0(3) . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
N2 C45 C46 178.0(3) . . ?
C45 C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C45 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
N3 C47 C48 177.0(3) . . ?
C47 C48 H48A 109.5 . . ?
C47 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C47 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
F1 C49 F3 105.7(3) . . ?
F1 C49 F2 105.6(3) . . ?
F3 C49 F2 105.8(3) . . ?
F1 C49 S1 114.1(3) . . ?
F3 C49 S1 113.3(2) . . ?
F2 C49 S1 111.6(2) . . ?
F5 C50 F6 108.9(3) . . ?
F5 C50 F4 107.3(3) . . ?
F6 C50 F4 105.6(3) . . ?
F5 C50 S2 112.3(3) . . ?
F6 C50 S2 113.0(2) . . ?
F4 C50 S2 109.3(3) . . ?

_refine_diff_density_max         0.397
_refine_diff_density_min         -0.483
_refine_diff_density_rms         0.067

_shelxl_version_number           2014-3


####################################################################### 
# 
# 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_4
_database_code_depnum_ccdc_archive 'CCDC 1481876'
_audit_update_record             
;
2016-06-21 deposited with the CCDC.
2016-07-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C45 H41 Cl2 Co P3 Si'
_chemical_formula_weight         832.61

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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   13.5425(9)
_cell_length_b                   13.5858(5)
_cell_length_c                   24.5419(17)
_cell_angle_alpha                90
_cell_angle_beta                 105.036(4)
_cell_angle_gamma                90
_cell_volume                     4360.8(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    121962
_cell_measurement_theta_min      2.16
_cell_measurement_theta_max      25.68

_exptl_crystal_description       platelet
_exptl_crystal_colour            'translucent blue'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.268
_exptl_crystal_F_000             1724
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_exptl_absorpt_coefficient_mu    0.683
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.846
_exptl_absorpt_correction_T_max  0.973
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_special_details           'crystal-to-detector distance 30 mm'
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method       
'two φ and four ω scans with 2° steps (390 frames)'
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            121962
_diffrn_reflns_av_unetI/netI     0.0848
_diffrn_reflns_av_R_equivalents  0.0579
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         2.161
_diffrn_reflns_theta_max         25.682
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             8275
_reflns_number_gt                5168
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  
'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)'

_refine_special_details          
;
 Structure solved by intrinsic phasing and subsequent difference Fourier
 synthesis. All non-hydrogen atoms were refined with anisotropic
 displacement parameters. The H atoms were introduced at calculated
 positions and were treated as riding atoms with an isotropic displacement
 parameter equal to 1.2 times that of the parent atom. Some voids in the
 lattice likely indicate the presence of other, unresolved solvent molecules.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0474P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8275
_refine_ls_number_parameters     469
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0942
_refine_ls_R_factor_gt           0.0505
_refine_ls_wR_factor_ref         0.1120
_refine_ls_wR_factor_gt          0.1010
_refine_ls_goodness_of_fit_ref   0.983
_refine_ls_restrained_S_all      0.983
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.67112(3) 1.25562(3) 0.62227(2) 0.02811(12) Uani 1 1 d . . . . .
P1 P 0.73695(7) 1.40274(6) 0.66757(4) 0.0288(2) Uani 1 1 d . . . . .
P2 P 0.52116(6) 1.22768(6) 0.65114(4) 0.0290(2) Uani 1 1 d . . . . .
P3 P 0.39177(7) 1.47067(7) 0.75100(5) 0.0396(3) Uani 1 1 d . . . . .
Cl1 Cl 0.76134(7) 1.14072(7) 0.67891(4) 0.0435(2) Uani 1 1 d . . . . .
Cl2 Cl 0.65167(7) 1.25269(7) 0.53021(4) 0.0452(2) Uani 1 1 d . . . . .
Si1 Si 0.60653(7) 1.36511(6) 0.75938(4) 0.0295(2) Uani 1 1 d . . . . .
C1 C 0.7304(2) 1.3936(2) 0.74038(14) 0.0311(8) Uani 1 1 d . . . . .
H1A H 0.7558 1.4568 0.7588 0.037 Uiso 1 1 calc R U . . .
H1B H 0.7802 1.3425 0.7586 0.037 Uiso 1 1 calc R U . . .
C2 C 0.5481(3) 1.2443(2) 0.72737(14) 0.0324(8) Uani 1 1 d . . . . .
H2A H 0.5947 1.1906 0.7454 0.039 Uiso 1 1 calc R U . . .
H2B H 0.4832 1.2350 0.7381 0.039 Uiso 1 1 calc R U . . .
C3 C 0.5173(3) 1.4702(2) 0.73543(17) 0.0355(8) Uani 1 1 d . . . . .
H3A H 0.5534 1.5309 0.7518 0.043 Uiso 1 1 calc R U . . .
H3B H 0.5052 1.4753 0.6940 0.043 Uiso 1 1 calc R U . . .
C4 C 0.8718(3) 1.4263(3) 0.67302(15) 0.0361(8) Uani 1 1 d . . . . .
C5 C 0.9076(3) 1.5161(3) 0.65947(18) 0.0493(10) Uani 1 1 d . . . . .
H5 H 0.8613 1.5687 0.6465 0.059 Uiso 1 1 calc R U . . .
C6 C 1.0124(3) 1.5293(3) 0.6650(2) 0.0623(13) Uani 1 1 d . . . . .
H6 H 1.0369 1.5908 0.6555 0.075 Uiso 1 1 calc R U . . .
C7 C 1.0799(3) 1.4537(4) 0.6840(2) 0.0618(13) Uani 1 1 d . . . . .
H7 H 1.1510 1.4634 0.6884 0.074 Uiso 1 1 calc R U . . .
C8 C 1.0445(3) 1.3643(3) 0.69669(19) 0.0557(12) Uani 1 1 d . . . . .
H8 H 1.0910 1.3116 0.7091 0.067 Uiso 1 1 calc R U . . .
C9 C 0.9409(3) 1.3507(3) 0.69143(17) 0.0447(10) Uani 1 1 d . . . . .
H9 H 0.9171 1.2886 0.7006 0.054 Uiso 1 1 calc R U . . .
C10 C 0.6704(2) 1.5140(2) 0.63845(15) 0.0298(8) Uani 1 1 d . . . . .
C11 C 0.6687(3) 1.5990(2) 0.67041(17) 0.0413(9) Uani 1 1 d . . . . .
H11 H 0.7046 1.6005 0.7092 0.050 Uiso 1 1 calc R U . . .
C12 C 0.6144(3) 1.6809(3) 0.64525(18) 0.0470(10) Uani 1 1 d . . . . .
H12 H 0.6125 1.7381 0.6672 0.056 Uiso 1 1 calc R U . . .
C13 C 0.5644(3) 1.6801(3) 0.58998(19) 0.0561(12) Uani 1 1 d . . . . .
H13 H 0.5284 1.7370 0.5731 0.067 Uiso 1 1 calc R U . . .
C14 C 0.5653(4) 1.5971(3) 0.5580(2) 0.0734(16) Uani 1 1 d . . . . .
H14 H 0.5288 1.5963 0.5193 0.088 Uiso 1 1 calc R U . . .
C15 C 0.6193(3) 1.5151(3) 0.58213(18) 0.0530(11) Uani 1 1 d . . . . .
H15 H 0.6213 1.4587 0.5596 0.064 Uiso 1 1 calc R U . . .
C16 C 0.4838(3) 1.0996(2) 0.63500(15) 0.0322(8) Uani 1 1 d . . . . .
C17 C 0.4740(3) 1.0300(3) 0.67455(17) 0.0428(9) Uani 1 1 d . . . . .
H17 H 0.4893 1.0468 0.7134 0.051 Uiso 1 1 calc R U . . .
C18 C 0.4416(3) 0.9355(3) 0.6568(2) 0.0526(11) Uani 1 1 d . . . . .
H18 H 0.4349 0.8877 0.6839 0.063 Uiso 1 1 calc R U . . .
C19 C 0.4193(3) 0.9104(3) 0.60117(19) 0.0488(11) Uani 1 1 d . . . . .
H19 H 0.3964 0.8457 0.5896 0.059 Uiso 1 1 calc R U . . .
C20 C 0.4299(3) 0.9785(3) 0.56193(18) 0.0509(11) Uani 1 1 d . . . . .
H20 H 0.4153 0.9608 0.5232 0.061 Uiso 1 1 calc R U . . .
C21 C 0.4619(3) 1.0731(3) 0.57873(17) 0.0439(10) Uani 1 1 d . . . . .
H21 H 0.4689 1.1202 0.5514 0.053 Uiso 1 1 calc R U . . .
C22 C 0.4021(3) 1.2913(2) 0.62029(16) 0.0350(8) Uani 1 1 d . . . . .
C23 C 0.3121(3) 1.2644(3) 0.63219(18) 0.0511(10) Uani 1 1 d . . . . .
H23 H 0.3126 1.2131 0.6586 0.061 Uiso 1 1 calc R U . . .
C24 C 0.2203(3) 1.3108(3) 0.6064(2) 0.0571(12) Uani 1 1 d . . . . .
H24 H 0.1589 1.2915 0.6154 0.069 Uiso 1 1 calc R U . . .
C25 C 0.2187(4) 1.3826(4) 0.5689(3) 0.0856(19) Uani 1 1 d . . . . .
H25 H 0.1560 1.4134 0.5503 0.103 Uiso 1 1 calc R U . . .
C26 C 0.3083(4) 1.4115(5) 0.5575(3) 0.135(3) Uani 1 1 d . . . . .
H26 H 0.3078 1.4637 0.5317 0.162 Uiso 1 1 calc R U . . .
C27 C 0.3990(3) 1.3654(4) 0.5832(3) 0.0866(19) Uani 1 1 d . . . . .
H27 H 0.4604 1.3861 0.5748 0.104 Uiso 1 1 calc R U . . .
C28 C 0.3343(3) 1.5824(3) 0.7121(2) 0.0459(10) Uani 1 1 d . . . . .
C29 C 0.2780(3) 1.6492(3) 0.7339(2) 0.0585(12) Uani 1 1 d . . . . .
H29 H 0.2745 1.6427 0.7718 0.070 Uiso 1 1 calc R U . . .
C30 C 0.2264(3) 1.7258(3) 0.7009(3) 0.0717(16) Uani 1 1 d . . . . .
H30 H 0.1876 1.7706 0.7167 0.086 Uiso 1 1 calc R U . . .
C31 C 0.2302(3) 1.7379(3) 0.6472(3) 0.0707(15) Uani 1 1 d . . . . .
H31 H 0.1947 1.7905 0.6250 0.085 Uiso 1 1 calc R U . . .
C32 C 0.2866(4) 1.6728(4) 0.6252(3) 0.0902(19) Uani 1 1 d . . . . .
H32 H 0.2890 1.6796 0.5870 0.108 Uiso 1 1 calc R U . . .
C33 C 0.3399(4) 1.5975(4) 0.6574(3) 0.0839(18) Uani 1 1 d . . . . .
H33 H 0.3813 1.5552 0.6417 0.101 Uiso 1 1 calc R U . . .
C34 C 0.4173(3) 1.5137(3) 0.82454(18) 0.0431(10) Uani 1 1 d . . . . .
C35 C 0.5048(3) 1.5604(3) 0.8543(2) 0.0559(12) Uani 1 1 d . . . . .
H35 H 0.5577 1.5734 0.8363 0.067 Uiso 1 1 calc R U . . .
C36 C 0.5177(4) 1.5888(4) 0.9093(2) 0.0734(15) Uani 1 1 d . . . . .
H36 H 0.5787 1.6210 0.9292 0.088 Uiso 1 1 calc R U . . .
C37 C 0.4404(5) 1.5699(4) 0.9356(2) 0.0774(16) Uani 1 1 d . . . . .
H37 H 0.4490 1.5881 0.9739 0.093 Uiso 1 1 calc R U . . .
C38 C 0.3528(5) 1.5258(4) 0.9068(3) 0.0772(16) Uani 1 1 d . . . . .
H38 H 0.2994 1.5147 0.9246 0.093 Uiso 1 1 calc R U . . .
C39 C 0.3409(3) 1.4969(3) 0.8516(2) 0.0584(13) Uani 1 1 d . . . . .
H39 H 0.2796 1.4650 0.8319 0.070 Uiso 1 1 calc R U . . .
C40 C 0.6411(3) 1.3477(2) 0.83747(16) 0.0362(8) Uani 1 1 d . . . . .
C41 C 0.5785(4) 1.2967(4) 0.8636(2) 0.0766(16) Uani 1 1 d . . . . .
H41 H 0.5168 1.2690 0.8413 0.092 Uiso 1 1 calc R U . . .
C42 C 0.6030(6) 1.2848(4) 0.9216(2) 0.106(2) Uani 1 1 d . . . . .
H42 H 0.5580 1.2496 0.9384 0.128 Uiso 1 1 calc R U . . .
C43 C 0.6916(5) 1.3231(4) 0.9548(2) 0.0840(18) Uani 1 1 d . . . . .
H43 H 0.7085 1.3141 0.9945 0.101 Uiso 1 1 calc R U . . .
C44 C 0.7555(4) 1.3746(4) 0.9304(2) 0.0707(14) Uani 1 1 d . . . . .
H44 H 0.8174 1.4014 0.9531 0.085 Uiso 1 1 calc R U . . .
C45 C 0.7300(3) 1.3874(3) 0.87258(18) 0.0549(11) Uani 1 1 d . . . . .
H45 H 0.7744 1.4246 0.8562 0.066 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 Cl2 2.2061(10) . ?
Co1 Cl1 2.2318(10) . ?
Co1 P1 2.3476(10) . ?
Co1 P2 2.3489(10) . ?
P1 C10 1.810(3) . ?
P1 C1 1.816(3) . ?
P1 C4 1.825(4) . ?
P2 C22 1.813(3) . ?
P2 C2 1.825(3) . ?
P2 C16 1.827(3) . ?
P3 C3 1.836(3) . ?
P3 C34 1.842(4) . ?
P3 C28 1.853(4) . ?
Si1 C3 1.864(3) . ?
Si1 C40 1.866(4) . ?
Si1 C1 1.894(3) . ?
Si1 C2 1.901(3) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C9 1.385(5) . ?
C4 C5 1.385(5) . ?
C5 C6 1.401(5) . ?
C5 H5 0.9500 . ?
C6 C7 1.373(6) . ?
C6 H6 0.9500 . ?
C7 C8 1.371(6) . ?
C7 H7 0.9500 . ?
C8 C9 1.387(5) . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?
C10 C15 1.376(5) . ?
C10 C11 1.398(5) . ?
C11 C12 1.387(5) . ?
C11 H11 0.9500 . ?
C12 C13 1.350(6) . ?
C12 H12 0.9500 . ?
C13 C14 1.376(6) . ?
C13 H13 0.9500 . ?
C14 C15 1.379(5) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C16 C21 1.383(5) . ?
C16 C17 1.386(5) . ?
C17 C18 1.390(5) . ?
C17 H17 0.9500 . ?
C18 C19 1.363(6) . ?
C18 H18 0.9500 . ?
C19 C20 1.370(6) . ?
C19 H19 0.9500 . ?
C20 C21 1.385(5) . ?
C20 H20 0.9500 . ?
C21 H21 0.9500 . ?
C22 C27 1.350(5) . ?
C22 C23 1.374(5) . ?
C23 C24 1.391(5) . ?
C23 H23 0.9500 . ?
C24 C25 1.338(6) . ?
C24 H24 0.9500 . ?
C25 C26 1.372(7) . ?
C25 H25 0.9500 . ?
C26 C27 1.378(6) . ?
C26 H26 0.9500 . ?
C27 H27 0.9500 . ?
C28 C29 1.379(5) . ?
C28 C33 1.379(6) . ?
C29 C30 1.391(6) . ?
C29 H29 0.9500 . ?
C30 C31 1.343(7) . ?
C30 H30 0.9500 . ?
C31 C32 1.367(7) . ?
C31 H31 0.9500 . ?
C32 C33 1.378(6) . ?
C32 H32 0.9500 . ?
C33 H33 0.9500 . ?
C34 C35 1.376(5) . ?
C34 C39 1.386(5) . ?
C35 C36 1.371(6) . ?
C35 H35 0.9500 . ?
C36 C37 1.388(7) . ?
C36 H36 0.9500 . ?
C37 C38 1.353(7) . ?
C37 H37 0.9500 . ?
C38 C39 1.378(7) . ?
C38 H38 0.9500 . ?
C39 H39 0.9500 . ?
C40 C41 1.376(6) . ?
C40 C45 1.394(5) . ?
C41 C42 1.383(7) . ?
C41 H41 0.9500 . ?
C42 C43 1.366(8) . ?
C42 H42 0.9500 . ?
C43 C44 1.366(7) . ?
C43 H43 0.9500 . ?
C44 C45 1.382(6) . ?
C44 H44 0.9500 . ?
C45 H45 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
Cl2 Co1 Cl1 121.73(4) . . ?
Cl2 Co1 P1 115.48(4) . . ?
Cl1 Co1 P1 102.78(4) . . ?
Cl2 Co1 P2 115.04(4) . . ?
Cl1 Co1 P2 94.33(4) . . ?
P1 Co1 P2 104.27(3) . . ?
C10 P1 C1 107.42(16) . . ?
C10 P1 C4 105.60(16) . . ?
C1 P1 C4 104.08(16) . . ?
C10 P1 Co1 115.80(11) . . ?
C1 P1 Co1 107.34(11) . . ?
C4 P1 Co1 115.72(12) . . ?
C22 P2 C2 106.80(16) . . ?
C22 P2 C16 101.40(16) . . ?
C2 P2 C16 108.11(16) . . ?
C22 P2 Co1 122.80(12) . . ?
C2 P2 Co1 109.30(11) . . ?
C16 P2 Co1 107.51(11) . . ?
C3 P3 C34 104.86(18) . . ?
C3 P3 C28 100.56(17) . . ?
C34 P3 C28 101.07(18) . . ?
C3 Si1 C40 112.99(16) . . ?
C3 Si1 C1 108.02(15) . . ?
C40 Si1 C1 106.03(16) . . ?
C3 Si1 C2 111.37(16) . . ?
C40 Si1 C2 106.35(15) . . ?
C1 Si1 C2 112.00(15) . . ?
P1 C1 Si1 121.91(18) . . ?
P1 C1 H1A 106.9 . . ?
Si1 C1 H1A 106.9 . . ?
P1 C1 H1B 106.9 . . ?
Si1 C1 H1B 106.9 . . ?
H1A C1 H1B 106.7 . . ?
P2 C2 Si1 118.80(18) . . ?
P2 C2 H2A 107.6 . . ?
Si1 C2 H2A 107.6 . . ?
P2 C2 H2B 107.6 . . ?
Si1 C2 H2B 107.6 . . ?
H2A C2 H2B 107.0 . . ?
P3 C3 Si1 119.79(19) . . ?
P3 C3 H3A 107.4 . . ?
Si1 C3 H3A 107.4 . . ?
P3 C3 H3B 107.4 . . ?
Si1 C3 H3B 107.4 . . ?
H3A C3 H3B 106.9 . . ?
C9 C4 C5 118.8(3) . . ?
C9 C4 P1 118.2(3) . . ?
C5 C4 P1 122.9(3) . . ?
C4 C5 C6 119.9(4) . . ?
C4 C5 H5 120.1 . . ?
C6 C5 H5 120.1 . . ?
C7 C6 C5 120.4(4) . . ?
C7 C6 H6 119.8 . . ?
C5 C6 H6 119.8 . . ?
C8 C7 C6 119.9(4) . . ?
C8 C7 H7 120.0 . . ?
C6 C7 H7 120.0 . . ?
C7 C8 C9 120.1(4) . . ?
C7 C8 H8 120.0 . . ?
C9 C8 H8 120.0 . . ?
C4 C9 C8 120.9(4) . . ?
C4 C9 H9 119.5 . . ?
C8 C9 H9 119.5 . . ?
C15 C10 C11 118.5(3) . . ?
C15 C10 P1 118.3(3) . . ?
C11 C10 P1 123.1(3) . . ?
C12 C11 C10 119.7(4) . . ?
C12 C11 H11 120.1 . . ?
C10 C11 H11 120.1 . . ?
C13 C12 C11 120.7(4) . . ?
C13 C12 H12 119.6 . . ?
C11 C12 H12 119.6 . . ?
C12 C13 C14 120.2(4) . . ?
C12 C13 H13 119.9 . . ?
C14 C13 H13 119.9 . . ?
C13 C14 C15 119.9(4) . . ?
C13 C14 H14 120.0 . . ?
C15 C14 H14 120.0 . . ?
C10 C15 C14 120.8(4) . . ?
C10 C15 H15 119.6 . . ?
C14 C15 H15 119.6 . . ?
C21 C16 C17 119.2(3) . . ?
C21 C16 P2 116.1(3) . . ?
C17 C16 P2 124.7(3) . . ?
C16 C17 C18 119.4(4) . . ?
C16 C17 H17 120.3 . . ?
C18 C17 H17 120.3 . . ?
C19 C18 C17 121.0(4) . . ?
C19 C18 H18 119.5 . . ?
C17 C18 H18 119.5 . . ?
C18 C19 C20 119.9(4) . . ?
C18 C19 H19 120.0 . . ?
C20 C19 H19 120.0 . . ?
C19 C20 C21 120.0(4) . . ?
C19 C20 H20 120.0 . . ?
C21 C20 H20 120.0 . . ?
C16 C21 C20 120.5(4) . . ?
C16 C21 H21 119.7 . . ?
C20 C21 H21 119.7 . . ?
C27 C22 C23 117.8(4) . . ?
C27 C22 P2 120.4(3) . . ?
C23 C22 P2 121.7(3) . . ?
C22 C23 C24 121.4(4) . . ?
C22 C23 H23 119.3 . . ?
C24 C23 H23 119.3 . . ?
C25 C24 C23 119.8(4) . . ?
C25 C24 H24 120.1 . . ?
C23 C24 H24 120.1 . . ?
C24 C25 C26 119.5(5) . . ?
C24 C25 H25 120.3 . . ?
C26 C25 H25 120.3 . . ?
C25 C26 C27 120.5(5) . . ?
C25 C26 H26 119.8 . . ?
C27 C26 H26 119.8 . . ?
C22 C27 C26 121.1(4) . . ?
C22 C27 H27 119.5 . . ?
C26 C27 H27 119.5 . . ?
C29 C28 C33 117.0(4) . . ?
C29 C28 P3 122.7(4) . . ?
C33 C28 P3 120.1(3) . . ?
C28 C29 C30 120.8(5) . . ?
C28 C29 H29 119.6 . . ?
C30 C29 H29 119.6 . . ?
C31 C30 C29 121.4(5) . . ?
C31 C30 H30 119.3 . . ?
C29 C30 H30 119.3 . . ?
C30 C31 C32 118.4(5) . . ?
C30 C31 H31 120.8 . . ?
C32 C31 H31 120.8 . . ?
C31 C32 C33 121.1(6) . . ?
C31 C32 H32 119.4 . . ?
C33 C32 H32 119.4 . . ?
C32 C33 C28 121.1(5) . . ?
C32 C33 H33 119.5 . . ?
C28 C33 H33 119.5 . . ?
C35 C34 C39 117.9(4) . . ?
C35 C34 P3 125.7(3) . . ?
C39 C34 P3 116.4(3) . . ?
C36 C35 C34 121.6(4) . . ?
C36 C35 H35 119.2 . . ?
C34 C35 H35 119.2 . . ?
C35 C36 C37 119.2(5) . . ?
C35 C36 H36 120.4 . . ?
C37 C36 H36 120.4 . . ?
C38 C37 C36 120.2(5) . . ?
C38 C37 H37 119.9 . . ?
C36 C37 H37 119.9 . . ?
C37 C38 C39 120.2(5) . . ?
C37 C38 H38 119.9 . . ?
C39 C38 H38 119.9 . . ?
C38 C39 C34 120.9(5) . . ?
C38 C39 H39 119.6 . . ?
C34 C39 H39 119.6 . . ?
C41 C40 C45 116.4(4) . . ?
C41 C40 Si1 121.5(3) . . ?
C45 C40 Si1 122.2(3) . . ?
C40 C41 C42 121.7(5) . . ?
C40 C41 H41 119.1 . . ?
C42 C41 H41 119.1 . . ?
C43 C42 C41 120.5(5) . . ?
C43 C42 H42 119.7 . . ?
C41 C42 H42 119.7 . . ?
C42 C43 C44 119.5(5) . . ?
C42 C43 H43 120.2 . . ?
C44 C43 H43 120.2 . . ?
C43 C44 C45 119.7(5) . . ?
C43 C44 H44 120.1 . . ?
C45 C44 H44 120.1 . . ?
C44 C45 C40 122.1(4) . . ?
C44 C45 H45 118.9 . . ?
C40 C45 H45 118.9 . . ?

_refine_diff_density_max         0.538
_refine_diff_density_min         -0.400
_refine_diff_density_rms         0.075

_shelxl_version_number           2014-3


####################################################################### 
# 
# 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_4prime
_database_code_depnum_ccdc_archive 'CCDC 1481877'
_audit_update_record             
;
2016-06-21 deposited with the CCDC.
2016-07-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C42 H35 Cl2 Co O3 P3 Si'
_chemical_formula_weight         838.53

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   9.8162(3)
_cell_length_b                   20.6578(7)
_cell_length_c                   19.1760(7)
_cell_angle_alpha                90
_cell_angle_beta                 101.210(2)
_cell_angle_gamma                90
_cell_volume                     3814.3(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    128536
_cell_measurement_theta_min      2.93
_cell_measurement_theta_max      25.68

_exptl_crystal_description       irregular
_exptl_crystal_colour            'dark orange'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.460
_exptl_crystal_F_000             1724
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_exptl_absorpt_coefficient_mu    0.787
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.714
_exptl_absorpt_correction_T_max  0.903
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_special_details           'crystal-to-detector distance 33 mm'
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method       
'two φ and five ω scans with 2° steps (489 frames)'
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            128536
_diffrn_reflns_av_unetI/netI     0.0540
_diffrn_reflns_av_R_equivalents  0.0474
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.929
_diffrn_reflns_theta_max         25.680
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             7220
_reflns_number_gt                5649
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  
'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)'

_refine_special_details          
;
 Structure solved by intrinsic phasing and subsequent difference Fourier
 synthesis. The phenyl ring bound to Si1 is disordered over two positions
 sharing atoms C37 (bound to Si1) and C40 (para position); these positions
 were given occupancy parameters constrained to sum to unity; one of them
 (A) was refined as an idealized hexagon and the other (B) with restraints on
 bond lengths and angles. All non-hydrogen atoms were refined with anisotropic
 displacement parameters. The H atoms were introduced at calculated
 positions and were treated as riding atoms with an isotropic displacement
 parameter equal to 1.2 times that of the parent atom. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0466P)²+2.2366P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7220
_refine_ls_number_parameters     494
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.0570
_refine_ls_R_factor_gt           0.0386
_refine_ls_wR_factor_ref         0.1058
_refine_ls_wR_factor_gt          0.0991
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_restrained_S_all      1.132
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.80434(3) 0.69112(2) 0.79415(2) 0.02480(11) Uani 1 1 d . . . . .
Cl1 Cl 0.95848(7) 0.65508(4) 0.88945(4) 0.04015(19) Uani 1 1 d . . . . .
Cl2 Cl 0.91287(8) 0.78712(3) 0.80636(4) 0.04160(19) Uani 1 1 d . . . . .
P1 P 0.84721(7) 0.63625(3) 0.69780(4) 0.02659(16) Uani 1 1 d . . . . .
P2 P 0.67344(7) 0.61324(3) 0.82203(4) 0.02718(16) Uani 1 1 d . . . . .
P3 P 0.62487(7) 0.74467(3) 0.73391(4) 0.02799(16) Uani 1 1 d . . . . .
Si1 Si 0.54880(7) 0.61986(4) 0.67398(4) 0.02982(18) Uani 1 1 d . . . . .
O1 O 0.69948(17) 0.61013(9) 0.65050(9) 0.0318(4) Uani 1 1 d . . . . .
O2 O 0.55754(18) 0.58938(9) 0.75370(10) 0.0334(4) Uani 1 1 d . . . . .
O3 O 0.51908(18) 0.69765(9) 0.67956(10) 0.0311(4) Uani 1 1 d . . . . .
C1 C 0.9245(3) 0.67391(13) 0.62930(14) 0.0303(6) Uani 1 1 d . . . . .
C2 C 0.8664(3) 0.66998(15) 0.55749(15) 0.0405(7) Uani 1 1 d . . . . .
H2 H 0.7812 0.6477 0.5424 0.049 Uiso 1 1 calc R U . . .
C3 C 0.9329(4) 0.69874(17) 0.50752(17) 0.0519(9) Uani 1 1 d . . . . .
H3 H 0.8928 0.6961 0.4583 0.062 Uiso 1 1 calc R U . . .
C4 C 1.0572(4) 0.73108(18) 0.52942(19) 0.0549(9) Uani 1 1 d . . . . .
H4 H 1.1024 0.7505 0.4952 0.066 Uiso 1 1 calc R U . . .
C5 C 1.1159(3) 0.73528(16) 0.60094(18) 0.0476(8) Uani 1 1 d . . . . .
H5 H 1.2017 0.7572 0.6158 0.057 Uiso 1 1 calc R U . . .
C6 C 1.0493(3) 0.70738(14) 0.65088(16) 0.0378(7) Uani 1 1 d . . . . .
H6 H 1.0887 0.7110 0.7000 0.045 Uiso 1 1 calc R U . . .
C7 C 0.9469(3) 0.56202(13) 0.71126(14) 0.0283(6) Uani 1 1 d . . . . .
C8 C 0.9061(3) 0.50627(14) 0.67228(15) 0.0337(6) Uani 1 1 d . . . . .
H8 H 0.8222 0.5060 0.6378 0.040 Uiso 1 1 calc R U . . .
C9 C 0.9873(3) 0.45104(14) 0.68354(16) 0.0398(7) Uani 1 1 d . . . . .
H9 H 0.9589 0.4130 0.6569 0.048 Uiso 1 1 calc R U . . .
C10 C 1.1090(3) 0.45112(15) 0.73328(18) 0.0454(8) Uani 1 1 d . . . . .
H10 H 1.1647 0.4132 0.7408 0.055 Uiso 1 1 calc R U . . .
C11 C 1.1500(3) 0.50601(15) 0.7720(2) 0.0523(9) Uani 1 1 d . . . . .
H11 H 1.2341 0.5059 0.8063 0.063 Uiso 1 1 calc R U . . .
C12 C 1.0697(3) 0.56168(14) 0.76159(16) 0.0397(7) Uani 1 1 d . . . . .
H12 H 1.0986 0.5994 0.7887 0.048 Uiso 1 1 calc R U . . .
C13 C 0.7436(3) 0.53502(13) 0.85482(15) 0.0298(6) Uani 1 1 d . . . . .
C14 C 0.7459(3) 0.48328(14) 0.80885(17) 0.0371(7) Uani 1 1 d . . . . .
H14 H 0.7092 0.4883 0.7595 0.044 Uiso 1 1 calc R U . . .
C15 C 0.8018(3) 0.42407(15) 0.8348(2) 0.0483(8) Uani 1 1 d . . . . .
H15 H 0.8046 0.3890 0.8031 0.058 Uiso 1 1 calc R U . . .
C16 C 0.8533(3) 0.41641(16) 0.9067(2) 0.0493(9) Uani 1 1 d . . . . .
H16 H 0.8917 0.3760 0.9242 0.059 Uiso 1 1 calc R U . . .
C17 C 0.8492(3) 0.46722(16) 0.95324(18) 0.0439(8) Uani 1 1 d . . . . .
H17 H 0.8824 0.4614 1.0028 0.053 Uiso 1 1 calc R U . . .
C18 C 0.7962(3) 0.52671(14) 0.92730(15) 0.0342(6) Uani 1 1 d . . . . .
H18 H 0.7958 0.5620 0.9591 0.041 Uiso 1 1 calc R U . . .
C19 C 0.5679(3) 0.63749(14) 0.88495(14) 0.0314(6) Uani 1 1 d . . . . .
C20 C 0.4414(3) 0.60654(17) 0.88451(17) 0.0458(8) Uani 1 1 d . . . . .
H20 H 0.4138 0.5711 0.8534 0.055 Uiso 1 1 calc R U . . .
C21 C 0.3567(3) 0.6277(2) 0.9294(2) 0.0597(10) Uani 1 1 d . . . . .
H21 H 0.2702 0.6069 0.9288 0.072 Uiso 1 1 calc R U . . .
C22 C 0.3960(4) 0.6784(2) 0.97486(19) 0.0574(10) Uani 1 1 d . . . . .
H22 H 0.3366 0.6925 1.0054 0.069 Uiso 1 1 calc R U . . .
C23 C 0.5214(4) 0.70919(18) 0.97657(17) 0.0496(8) Uani 1 1 d . . . . .
H23 H 0.5483 0.7442 1.0084 0.059 Uiso 1 1 calc R U . . .
C24 C 0.6085(3) 0.68889(14) 0.93146(15) 0.0358(7) Uani 1 1 d . . . . .
H24 H 0.6949 0.7099 0.9324 0.043 Uiso 1 1 calc R U . . .
C25 C 0.5106(3) 0.77836(14) 0.78842(15) 0.0349(6) Uani 1 1 d . . . . .
C26 C 0.5574(4) 0.83055(16) 0.83271(17) 0.0485(8) Uani 1 1 d . . . . .
H26 H 0.6481 0.8474 0.8346 0.058 Uiso 1 1 calc R U . . .
C27 C 0.4704(5) 0.8578(2) 0.8742(2) 0.0674(11) Uani 1 1 d . . . . .
H27 H 0.5015 0.8935 0.9043 0.081 Uiso 1 1 calc R U . . .
C28 C 0.3394(4) 0.8329(2) 0.8715(2) 0.0740(13) Uani 1 1 d . . . . .
H28 H 0.2801 0.8518 0.8996 0.089 Uiso 1 1 calc R U . . .
C29 C 0.2938(4) 0.7814(2) 0.82906(19) 0.0637(11) Uani 1 1 d . . . . .
H29 H 0.2037 0.7642 0.8281 0.076 Uiso 1 1 calc R U . . .
C30 C 0.3786(3) 0.75401(17) 0.78726(16) 0.0440(8) Uani 1 1 d . . . . .
H30 H 0.3460 0.7182 0.7575 0.053 Uiso 1 1 calc R U . . .
C31 C 0.6426(3) 0.81271(13) 0.67553(14) 0.0299(6) Uani 1 1 d . . . . .
C32 C 0.5342(3) 0.85780(14) 0.66034(15) 0.0352(7) Uani 1 1 d . . . . .
H32 H 0.4545 0.8530 0.6812 0.042 Uiso 1 1 calc R U . . .
C33 C 0.5425(3) 0.90929(14) 0.61521(15) 0.0372(7) Uani 1 1 d . . . . .
H33 H 0.4687 0.9397 0.6052 0.045 Uiso 1 1 calc R U . . .
C34 C 0.6579(3) 0.91647(14) 0.58463(16) 0.0378(7) Uani 1 1 d . . . . .
H34 H 0.6639 0.9521 0.5540 0.045 Uiso 1 1 calc R U . . .
C35 C 0.7647(3) 0.87184(15) 0.59860(15) 0.0385(7) Uani 1 1 d . . . . .
H35 H 0.8435 0.8766 0.5771 0.046 Uiso 1 1 calc R U . . .
C36 C 0.7575(3) 0.82012(14) 0.64390(15) 0.0343(6) Uani 1 1 d . . . . .
H36 H 0.8313 0.7897 0.6533 0.041 Uiso 1 1 calc R U . . .
C37 C 0.4145(2) 0.57867(12) 0.61027(12) 0.0391(7) Uani 1 1 d DG . . . .
C38A C 0.2784(3) 0.57963(18) 0.62082(16) 0.0434(17) Uani 0.487(4) 1 d G . P . .
H38A H 0.2549 0.6040 0.6593 0.052 Uiso 0.487(4) 1 d R U P . .
C39A C 0.1760(2) 0.5452(2) 0.57545(19) 0.055(2) Uani 0.487(4) 1 d G . P . .
H39A H 0.0816 0.5459 0.5827 0.066 Uiso 0.487(4) 1 d R U P . .
C40 C 0.2098(3) 0.50984(15) 0.51953(15) 0.0720(12) Uani 1 1 d DG . . . .
H40 H 0.1389 0.4862 0.4883 0.086 Uiso 1 1 d R U . . .
C41A C 0.3459(3) 0.50887(18) 0.50898(16) 0.0509(19) Uani 0.487(4) 1 d G . P . .
H41A H 0.3694 0.4845 0.4705 0.061 Uiso 0.487(4) 1 d R U P . .
C42A C 0.4483(2) 0.54329(18) 0.55434(17) 0.0439(17) Uani 0.487(4) 1 d G . P . .
H42A H 0.5427 0.5427 0.5471 0.053 Uiso 0.487(4) 1 d R U P . .
C38B C 0.3248(5) 0.6073(2) 0.5567(2) 0.0501(18) Uani 0.513(4) 1 d D . P . .
H38B H 0.3436 0.6513 0.5462 0.060 Uiso 0.513(4) 1 d R U P . .
C39B C 0.2132(5) 0.5773(3) 0.5148(3) 0.0559(19) Uani 0.513(4) 1 d D . P . .
H39B H 0.1571 0.5991 0.4752 0.067 Uiso 0.513(4) 1 d R U P . .
C41B C 0.2655(6) 0.4816(3) 0.5843(3) 0.0516(18) Uani 0.513(4) 1 d D . P . .
H41B H 0.2411 0.4382 0.5947 0.062 Uiso 0.513(4) 1 d R U P . .
C42B C 0.3740(6) 0.5137(3) 0.6288(3) 0.0477(17) Uani 0.513(4) 1 d D . P . .
H42B H 0.4264 0.4924 0.6698 0.057 Uiso 0.513(4) 1 d R U P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 P2 2.1893(8) . ?
Co1 P3 2.2070(8) . ?
Co1 Cl2 2.2418(8) . ?
Co1 Cl1 2.2600(8) . ?
Co1 P1 2.2755(8) . ?
P1 O1 1.6448(18) . ?
P1 C7 1.810(3) . ?
P1 C1 1.815(3) . ?
P2 O2 1.6354(18) . ?
P2 C19 1.807(3) . ?
P2 C13 1.820(3) . ?
P3 O3 1.6392(19) . ?
P3 C25 1.814(3) . ?
P3 C31 1.826(3) . ?
Si1 O1 1.6401(19) . ?
Si1 O2 1.640(2) . ?
Si1 O3 1.6405(19) . ?
Si1 C37 1.8244(19) . ?
C1 C2 1.387(4) . ?
C1 C6 1.397(4) . ?
C2 C3 1.393(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.382(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.383(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.386(4) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C8 1.389(4) . ?
C7 C12 1.390(4) . ?
C8 C9 1.385(4) . ?
C8 H8 0.9500 . ?
C9 C10 1.376(4) . ?
C9 H9 0.9500 . ?
C10 C11 1.372(4) . ?
C10 H10 0.9500 . ?
C11 C12 1.386(4) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 C14 1.388(4) . ?
C13 C18 1.396(4) . ?
C14 C15 1.393(4) . ?
C14 H14 0.9500 . ?
C15 C16 1.382(5) . ?
C15 H15 0.9500 . ?
C16 C17 1.384(5) . ?
C16 H16 0.9500 . ?
C17 C18 1.388(4) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 C24 1.394(4) . ?
C19 C20 1.395(4) . ?
C20 C21 1.380(5) . ?
C20 H20 0.9500 . ?
C21 C22 1.370(6) . ?
C21 H21 0.9500 . ?
C22 C23 1.380(5) . ?
C22 H22 0.9500 . ?
C23 C24 1.394(4) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 C30 1.387(4) . ?
C25 C26 1.394(4) . ?
C26 C27 1.394(5) . ?
C26 H26 0.9500 . ?
C27 C28 1.378(6) . ?
C27 H27 0.9500 . ?
C28 C29 1.361(6) . ?
C28 H28 0.9500 . ?
C29 C30 1.383(5) . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?
C31 C36 1.388(4) . ?
C31 C32 1.402(4) . ?
C32 C33 1.384(4) . ?
C32 H32 0.9500 . ?
C33 C34 1.381(4) . ?
C33 H33 0.9500 . ?
C34 C35 1.383(4) . ?
C34 H34 0.9500 . ?
C35 C36 1.387(4) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C37 C38B 1.352(5) . ?
C37 C38A 1.3900 . ?
C37 C42A 1.3900 . ?
C37 C42B 1.464(5) . ?
C38A C39A 1.3900 . ?
C38A H38A 0.9572 . ?
C39A C40 1.3900 . ?
C39A H39A 0.9637 . ?
C40 C41B 1.385(5) . ?
C40 C41A 1.3900 . ?
C40 C39B 1.397(6) . ?
C40 H40 0.9590 . ?
C41A C42A 1.3900 . ?
C41A H41A 0.9571 . ?
C42A H42A 0.9637 . ?
C38B C39B 1.373(6) . ?
C38B H38B 0.9583 . ?
C39B H39B 0.9593 . ?
C41B C42B 1.396(6) . ?
C41B H41B 0.9579 . ?
C42B H42B 0.9592 . ?

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
P2 Co1 P3 92.84(3) . . ?
P2 Co1 Cl2 156.09(3) . . ?
P3 Co1 Cl2 85.76(3) . . ?
P2 Co1 Cl1 83.85(3) . . ?
P3 Co1 Cl1 158.30(3) . . ?
Cl2 Co1 Cl1 88.69(3) . . ?
P2 Co1 P1 92.42(3) . . ?
P3 Co1 P1 94.56(3) . . ?
Cl2 Co1 P1 111.49(3) . . ?
Cl1 Co1 P1 106.98(3) . . ?
O1 P1 C7 101.24(11) . . ?
O1 P1 C1 100.91(11) . . ?
C7 P1 C1 100.12(12) . . ?
O1 P1 Co1 109.20(7) . . ?
C7 P1 Co1 119.10(9) . . ?
C1 P1 Co1 122.92(9) . . ?
O2 P2 C19 102.64(11) . . ?
O2 P2 C13 99.60(11) . . ?
C19 P2 C13 104.06(13) . . ?
O2 P2 Co1 112.07(7) . . ?
C19 P2 Co1 113.53(10) . . ?
C13 P2 Co1 122.43(9) . . ?
O3 P3 C25 101.97(12) . . ?
O3 P3 C31 100.99(11) . . ?
C25 P3 C31 101.62(13) . . ?
O3 P3 Co1 112.23(7) . . ?
C25 P3 Co1 114.25(9) . . ?
C31 P3 Co1 123.02(9) . . ?
O1 Si1 O2 108.80(10) . . ?
O1 Si1 O3 108.62(10) . . ?
O2 Si1 O3 107.03(10) . . ?
O1 Si1 C37 109.38(11) . . ?
O2 Si1 C37 110.19(11) . . ?
O3 Si1 C37 112.71(11) . . ?
Si1 O1 P1 123.63(11) . . ?
P2 O2 Si1 122.23(11) . . ?
P3 O3 Si1 121.55(11) . . ?
C2 C1 C6 119.4(3) . . ?
C2 C1 P1 123.0(2) . . ?
C6 C1 P1 117.6(2) . . ?
C1 C2 C3 120.1(3) . . ?
C1 C2 H2 120.0 . . ?
C3 C2 H2 120.0 . . ?
C4 C3 C2 120.1(3) . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
C3 C4 C5 120.3(3) . . ?
C3 C4 H4 119.9 . . ?
C5 C4 H4 119.9 . . ?
C4 C5 C6 119.8(3) . . ?
C4 C5 H5 120.1 . . ?
C6 C5 H5 120.1 . . ?
C5 C6 C1 120.4(3) . . ?
C5 C6 H6 119.8 . . ?
C1 C6 H6 119.8 . . ?
C8 C7 C12 119.3(3) . . ?
C8 C7 P1 122.3(2) . . ?
C12 C7 P1 118.4(2) . . ?
C9 C8 C7 120.2(3) . . ?
C9 C8 H8 119.9 . . ?
C7 C8 H8 119.9 . . ?
C10 C9 C8 120.2(3) . . ?
C10 C9 H9 119.9 . . ?
C8 C9 H9 119.9 . . ?
C11 C10 C9 120.0(3) . . ?
C11 C10 H10 120.0 . . ?
C9 C10 H10 120.0 . . ?
C10 C11 C12 120.6(3) . . ?
C10 C11 H11 119.7 . . ?
C12 C11 H11 119.7 . . ?
C11 C12 C7 119.8(3) . . ?
C11 C12 H12 120.1 . . ?
C7 C12 H12 120.1 . . ?
C14 C13 C18 119.3(3) . . ?
C14 C13 P2 121.1(2) . . ?
C18 C13 P2 119.7(2) . . ?
C13 C14 C15 120.2(3) . . ?
C13 C14 H14 119.9 . . ?
C15 C14 H14 119.9 . . ?
C16 C15 C14 119.9(3) . . ?
C16 C15 H15 120.0 . . ?
C14 C15 H15 120.0 . . ?
C15 C16 C17 120.4(3) . . ?
C15 C16 H16 119.8 . . ?
C17 C16 H16 119.8 . . ?
C16 C17 C18 119.7(3) . . ?
C16 C17 H17 120.1 . . ?
C18 C17 H17 120.1 . . ?
C17 C18 C13 120.4(3) . . ?
C17 C18 H18 119.8 . . ?
C13 C18 H18 119.8 . . ?
C24 C19 C20 119.8(3) . . ?
C24 C19 P2 120.6(2) . . ?
C20 C19 P2 119.6(2) . . ?
C21 C20 C19 119.7(3) . . ?
C21 C20 H20 120.2 . . ?
C19 C20 H20 120.2 . . ?
C22 C21 C20 120.6(3) . . ?
C22 C21 H21 119.7 . . ?
C20 C21 H21 119.7 . . ?
C21 C22 C23 120.5(3) . . ?
C21 C22 H22 119.7 . . ?
C23 C22 H22 119.7 . . ?
C22 C23 C24 119.9(3) . . ?
C22 C23 H23 120.0 . . ?
C24 C23 H23 120.0 . . ?
C23 C24 C19 119.5(3) . . ?
C23 C24 H24 120.3 . . ?
C19 C24 H24 120.3 . . ?
C30 C25 C26 119.1(3) . . ?
C30 C25 P3 122.2(2) . . ?
C26 C25 P3 118.7(2) . . ?
C25 C26 C27 119.6(4) . . ?
C25 C26 H26 120.2 . . ?
C27 C26 H26 120.2 . . ?
C28 C27 C26 119.9(4) . . ?
C28 C27 H27 120.0 . . ?
C26 C27 H27 120.0 . . ?
C29 C28 C27 120.7(3) . . ?
C29 C28 H28 119.6 . . ?
C27 C28 H28 119.6 . . ?
C28 C29 C30 120.1(4) . . ?
C28 C29 H29 119.9 . . ?
C30 C29 H29 119.9 . . ?
C29 C30 C25 120.5(4) . . ?
C29 C30 H30 119.7 . . ?
C25 C30 H30 119.7 . . ?
C36 C31 C32 119.0(3) . . ?
C36 C31 P3 122.4(2) . . ?
C32 C31 P3 118.7(2) . . ?
C33 C32 C31 120.4(3) . . ?
C33 C32 H32 119.8 . . ?
C31 C32 H32 119.8 . . ?
C34 C33 C32 120.0(3) . . ?
C34 C33 H33 120.0 . . ?
C32 C33 H33 120.0 . . ?
C33 C34 C35 120.0(3) . . ?
C33 C34 H34 120.0 . . ?
C35 C34 H34 120.0 . . ?
C34 C35 C36 120.4(3) . . ?
C34 C35 H35 119.8 . . ?
C36 C35 H35 119.8 . . ?
C35 C36 C31 120.2(3) . . ?
C35 C36 H36 119.9 . . ?
C31 C36 H36 119.9 . . ?
C38A C37 C42A 120.0 . . ?
C38B C37 C42B 114.7(3) . . ?
C38B C37 Si1 125.8(3) . . ?
C38A C37 Si1 119.07(15) . . ?
C42A C37 Si1 120.81(15) . . ?
C42B C37 Si1 117.4(2) . . ?
C37 C38A C39A 120.0 . . ?
C37 C38A H38A 120.1 . . ?
C39A C38A H38A 119.9 . . ?
C40 C39A C38A 120.0 . . ?
C40 C39A H39A 119.9 . . ?
C38A C39A H39A 120.1 . . ?
C39A C40 C41A 120.0 . . ?
C41B C40 C39B 117.9(3) . . ?
C41B C40 H40 117.2 . . ?
C39A C40 H40 119.8 . . ?
C41A C40 H40 120.2 . . ?
C39B C40 H40 119.5 . . ?
C40 C41A C42A 120.0 . . ?
C40 C41A H41A 120.2 . . ?
C42A C41A H41A 119.8 . . ?
C41A C42A C37 120.0 . . ?
C41A C42A H42A 120.1 . . ?
C37 C42A H42A 119.9 . . ?
C37 C38B C39B 125.1(4) . . ?
C37 C38B H38B 116.8 . . ?
C39B C38B H38B 118.1 . . ?
C38B C39B C40 116.0(4) . . ?
C38B C39B H39B 121.4 . . ?
C40 C39B H39B 120.2 . . ?
C40 C41B C42B 118.0(4) . . ?
C40 C41B H41B 120.6 . . ?
C42B C41B H41B 120.6 . . ?
C41B C42B C37 119.9(4) . . ?
C41B C42B H42B 120.5 . . ?
C37 C42B H42B 119.5 . . ?

_refine_diff_density_max         0.761
_refine_diff_density_min         -0.813
_refine_diff_density_rms         0.073

_shelxl_version_number           2014-3


####################################################################### 
# 
# 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_5-3THF
_database_code_depnum_ccdc_archive 'CCDC 1481878'
_audit_update_record             
;
2016-06-21 deposited with the CCDC.
2016-07-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C57 H65 Br Cu O3 P3 Si'
_chemical_formula_weight         1062.54

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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_H-M_alt        'P n'
_space_group_name_Hall           'P -2yac'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x+1/2, -y, z+1/2'

_cell_length_a                   10.2468(8)
_cell_length_b                   14.6429(11)
_cell_length_c                   17.7472(7)
_cell_angle_alpha                90
_cell_angle_beta                 97.487(4)
_cell_angle_gamma                90
_cell_volume                     2640.1(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    87659
_cell_measurement_theta_min      3.01
_cell_measurement_theta_max      25.68

_exptl_crystal_description       platelet
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.337
_exptl_crystal_F_000             1108
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.08
_exptl_absorpt_coefficient_mu    1.327
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.791
_exptl_absorpt_correction_T_max  1.300
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_special_details           'crystal-to-detector distance 30 mm'
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method       
'two φ and six ω scans with 2° steps (457 frames)'
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            87659
_diffrn_reflns_av_unetI/netI     0.0421
_diffrn_reflns_av_R_equivalents  0.1012
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.014
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             9799
_reflns_number_gt                8535
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.997
_reflns_Friedel_fraction_max     0.998
_reflns_Friedel_fraction_full    0.998

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  
'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)'

_refine_special_details          
;
 Structure solved by intrinsic phasing and subsequent difference Fourier
 synthesis. All non-hydrogen atoms were refined with anisotropic
 displacement parameters, with restraints for some bond lengths and
 displacement parameters in two THF solvent molecules. The H atoms
 were introduced at calculated positions and were treated as riding atoms
 with an isotropic displacement parameter equal to 1.2 times that of the
 parent atom.
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1192P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.479(14)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         9799
_refine_ls_number_parameters     596
_refine_ls_number_restraints     47
_refine_ls_R_factor_all          0.0697
_refine_ls_R_factor_gt           0.0596
_refine_ls_wR_factor_ref         0.1614
_refine_ls_wR_factor_gt          0.1550
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_restrained_S_all      1.070
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.63301(8) 0.43495(6) 0.43547(5) 0.0339(2) Uani 1 1 d . . . . .
Br1 Br 0.74072(7) 0.51803(6) 0.54356(5) 0.0487(3) Uani 1 1 d . . . . .
P1 P 0.5684(2) 0.50814(14) 0.32295(11) 0.0350(4) Uani 1 1 d . . . . .
P2 P 0.43653(18) 0.37114(14) 0.45346(11) 0.0345(4) Uani 1 1 d . . . . .
P3 P 0.74267(19) 0.31143(14) 0.39566(11) 0.0357(4) Uani 1 1 d . . . . .
Si1 Si 0.4757(2) 0.30936(16) 0.28951(11) 0.0357(5) Uani 1 1 d . . . . .
O1 O 0.0875(17) 0.0061(7) 0.8408(6) 0.124(5) Uani 1 1 d D . . . .
O2 O 0.3664(12) 0.8957(7) 0.6404(7) 0.105(3) Uani 1 1 d . . . . .
O3 O 0.165(2) -0.0141(11) 0.4186(11) 0.168(5) Uani 1 1 d D U . . .
C1 C 0.5376(9) 0.4195(6) 0.2496(4) 0.0396(17) Uani 1 1 d . . . . .
H1A H 0.6200 0.4070 0.2279 0.048 Uiso 1 1 calc R U . . .
H1B H 0.4715 0.4420 0.2081 0.048 Uiso 1 1 calc R U . . .
C2 C 0.3558(8) 0.3358(6) 0.3588(5) 0.0413(18) Uani 1 1 d . . . . .
H2A H 0.2961 0.3852 0.3375 0.050 Uiso 1 1 calc R U . . .
H2B H 0.3015 0.2810 0.3646 0.050 Uiso 1 1 calc R U . . .
C3 C 0.6174(8) 0.2408(5) 0.3392(5) 0.0389(16) Uani 1 1 d . . . . .
H3A H 0.5828 0.1957 0.3731 0.047 Uiso 1 1 calc R U . . .
H3B H 0.6595 0.2067 0.3007 0.047 Uiso 1 1 calc R U . . .
C4 C 0.4140(8) 0.5721(6) 0.3161(4) 0.0380(17) Uani 1 1 d . . . . .
C5 C 0.3307(9) 0.5860(7) 0.2491(6) 0.051(2) Uani 1 1 d . . . . .
H5 H 0.3509 0.5589 0.2034 0.061 Uiso 1 1 calc R U . . .
C6 C 0.2185(10) 0.6387(8) 0.2481(7) 0.065(3) Uani 1 1 d . . . . .
H6 H 0.1613 0.6469 0.2020 0.078 Uiso 1 1 calc R U . . .
C7 C 0.1897(11) 0.6792(9) 0.3135(8) 0.071(3) Uani 1 1 d . . . . .
H7 H 0.1136 0.7165 0.3124 0.085 Uiso 1 1 calc R U . . .
C8 C 0.2715(11) 0.6660(7) 0.3816(7) 0.061(3) Uani 1 1 d . . . . .
H8 H 0.2509 0.6935 0.4271 0.073 Uiso 1 1 calc R U . . .
C9 C 0.3830(9) 0.6124(6) 0.3827(5) 0.047(2) Uani 1 1 d . . . . .
H9 H 0.4389 0.6030 0.4291 0.057 Uiso 1 1 calc R U . . .
C10 C 0.6744(8) 0.5938(6) 0.2860(5) 0.0404(18) Uani 1 1 d . . . . .
C11 C 0.6785(10) 0.6086(7) 0.2089(5) 0.050(2) Uani 1 1 d . . . . .
H11 H 0.6245 0.5738 0.1719 0.060 Uiso 1 1 calc R U . . .
C12 C 0.7625(10) 0.6746(7) 0.1869(6) 0.058(3) Uani 1 1 d . . . . .
H12 H 0.7704 0.6823 0.1345 0.070 Uiso 1 1 calc R U . . .
C13 C 0.8331(10) 0.7281(8) 0.2388(7) 0.062(3) Uani 1 1 d . . . . .
H13 H 0.8861 0.7755 0.2223 0.075 Uiso 1 1 calc R U . . .
C14 C 0.8297(10) 0.7153(7) 0.3151(6) 0.059(2) Uani 1 1 d . . . . .
H14 H 0.8820 0.7523 0.3513 0.071 Uiso 1 1 calc R U . . .
C15 C 0.7490(9) 0.6475(7) 0.3394(5) 0.049(2) Uani 1 1 d . . . . .
H15 H 0.7454 0.6383 0.3921 0.059 Uiso 1 1 calc R U . . .
C16 C 0.3124(8) 0.4384(6) 0.4936(4) 0.0377(17) Uani 1 1 d . . . . .
C17 C 0.1785(9) 0.4339(6) 0.4677(5) 0.0455(19) Uani 1 1 d . . . . .
H17 H 0.1472 0.3908 0.4296 0.055 Uiso 1 1 calc R U . . .
C18 C 0.0896(9) 0.4920(7) 0.4972(5) 0.046(2) Uani 1 1 d . . . . .
H18 H -0.0016 0.4888 0.4789 0.055 Uiso 1 1 calc R U . . .
C19 C 0.1354(9) 0.5549(6) 0.5535(5) 0.049(2) Uani 1 1 d . . . . .
H19 H 0.0757 0.5955 0.5731 0.058 Uiso 1 1 calc R U . . .
C20 C 0.2684(9) 0.5579(6) 0.5807(5) 0.047(2) Uani 1 1 d . . . . .
H20 H 0.2994 0.5997 0.6199 0.056 Uiso 1 1 calc R U . . .
C21 C 0.3563(9) 0.5007(6) 0.5513(5) 0.0432(19) Uani 1 1 d . . . . .
H21 H 0.4473 0.5035 0.5704 0.052 Uiso 1 1 calc R U . . .
C22 C 0.4463(8) 0.2663(6) 0.5091(4) 0.0390(17) Uani 1 1 d . . . . .
C23 C 0.3452(10) 0.2022(7) 0.5049(5) 0.051(2) Uani 1 1 d . . . . .
H23 H 0.2649 0.2129 0.4729 0.062 Uiso 1 1 calc R U . . .
C24 C 0.3620(13) 0.1216(7) 0.5479(6) 0.068(3) Uani 1 1 d . . . . .
H24 H 0.2930 0.0779 0.5449 0.081 Uiso 1 1 calc R U . . .
C25 C 0.4798(12) 0.1056(8) 0.5952(6) 0.066(3) Uani 1 1 d . . . . .
H25 H 0.4916 0.0507 0.6239 0.079 Uiso 1 1 calc R U . . .
C26 C 0.5789(10) 0.1698(7) 0.5999(5) 0.055(2) Uani 1 1 d . . . . .
H26 H 0.6588 0.1595 0.6323 0.066 Uiso 1 1 calc R U . . .
C27 C 0.5624(9) 0.2498(7) 0.5572(5) 0.046(2) Uani 1 1 d . . . . .
H27 H 0.6313 0.2936 0.5610 0.055 Uiso 1 1 calc R U . . .
C28 C 0.8311(8) 0.2314(6) 0.4630(5) 0.0406(18) Uani 1 1 d . . . . .
C29 C 0.8244(10) 0.1376(6) 0.4550(5) 0.049(2) Uani 1 1 d . . . . .
H29 H 0.7728 0.1120 0.4118 0.059 Uiso 1 1 calc R U . . .
C30 C 0.8922(12) 0.0794(8) 0.5093(6) 0.066(3) Uani 1 1 d . . . . .
H30 H 0.8893 0.0151 0.5022 0.079 Uiso 1 1 calc R U . . .
C31 C 0.9630(11) 0.1167(8) 0.5728(6) 0.066(3) Uani 1 1 d . . . . .
H31 H 1.0067 0.0783 0.6112 0.079 Uiso 1 1 calc R U . . .
C32 C 0.9705(11) 0.2101(9) 0.5807(6) 0.069(3) Uani 1 1 d . . . . .
H32 H 1.0230 0.2354 0.6237 0.083 Uiso 1 1 calc R U . . .
C33 C 0.9040(9) 0.2674(7) 0.5281(5) 0.051(2) Uani 1 1 d . . . . .
H33 H 0.9076 0.3316 0.5359 0.062 Uiso 1 1 calc R U . . .
C34 C 0.8633(8) 0.3350(6) 0.3309(4) 0.0384(17) Uani 1 1 d . . . . .
C35 C 0.9210(9) 0.2672(7) 0.2909(5) 0.048(2) Uani 1 1 d . . . . .
H35 H 0.8970 0.2052 0.2971 0.058 Uiso 1 1 calc R U . . .
C36 C 1.0123(10) 0.2881(8) 0.2425(6) 0.057(2) Uani 1 1 d . . . . .
H36 H 1.0509 0.2408 0.2161 0.068 Uiso 1 1 calc R U . . .
C37 C 1.0469(9) 0.3783(8) 0.2327(5) 0.054(2) Uani 1 1 d . . . . .
H37 H 1.1088 0.3930 0.1991 0.065 Uiso 1 1 calc R U . . .
C38 C 0.9924(9) 0.4462(7) 0.2711(6) 0.050(2) Uani 1 1 d . . . . .
H38 H 1.0157 0.5082 0.2644 0.060 Uiso 1 1 calc R U . . .
C39 C 0.9025(8) 0.4235(6) 0.3202(5) 0.0417(18) Uani 1 1 d . . . . .
H39 H 0.8665 0.4710 0.3475 0.050 Uiso 1 1 calc R U . . .
C40 C 0.3864(8) 0.2367(6) 0.2134(5) 0.0398(18) Uani 1 1 d . . . . .
C41 C 0.3281(9) 0.2713(7) 0.1439(5) 0.051(2) Uani 1 1 d . . . . .
H41 H 0.3389 0.3339 0.1323 0.061 Uiso 1 1 calc R U . . .
C42 C 0.2548(11) 0.2154(9) 0.0916(6) 0.065(3) Uani 1 1 d . . . . .
H42 H 0.2183 0.2404 0.0441 0.078 Uiso 1 1 calc R U . . .
C43 C 0.2334(11) 0.1268(8) 0.1060(6) 0.064(3) Uani 1 1 d . . . . .
H43 H 0.1805 0.0901 0.0699 0.076 Uiso 1 1 calc R U . . .
C44 C 0.2903(12) 0.0903(8) 0.1745(6) 0.063(3) Uani 1 1 d . . . . .
H44 H 0.2779 0.0276 0.1852 0.075 Uiso 1 1 calc R U . . .
C45 C 0.3645(10) 0.1441(7) 0.2267(5) 0.053(2) Uani 1 1 d . . . . .
H45 H 0.4022 0.1178 0.2735 0.064 Uiso 1 1 calc R U . . .
C46 C 0.069(2) 0.0722(9) 0.7823(8) 0.099(5) Uani 1 1 d . . . . .
H46A H 0.0148 0.0459 0.7371 0.119 Uiso 1 1 calc R U . . .
H46B H 0.1549 0.0902 0.7675 0.119 Uiso 1 1 calc R U . . .
C47 C 0.0027(15) 0.1522(10) 0.8083(7) 0.084(4) Uani 1 1 d D . . . .
H47A H -0.0930 0.1505 0.7908 0.101 Uiso 1 1 calc R U . . .
H47B H 0.0399 0.2093 0.7900 0.101 Uiso 1 1 calc R U . . .
C48 C 0.030(2) 0.1448(11) 0.8925(7) 0.114(6) Uani 1 1 d D . . . .
H48A H -0.0474 0.1647 0.9163 0.137 Uiso 1 1 calc R U . . .
H48B H 0.1065 0.1829 0.9124 0.137 Uiso 1 1 calc R U . . .
C49 C 0.058(3) 0.0463(12) 0.9082(7) 0.140(9) Uani 1 1 d D . . . .
H49A H 0.1338 0.0398 0.9487 0.168 Uiso 1 1 calc R U . . .
H49B H -0.0193 0.0162 0.9253 0.168 Uiso 1 1 calc R U . . .
C50 C 0.2500(16) 0.9317(11) 0.6619(10) 0.097(4) Uani 1 1 d D . . . .
H50A H 0.2505 0.9992 0.6576 0.116 Uiso 1 1 calc R U . . .
H50B H 0.2430 0.9155 0.7154 0.116 Uiso 1 1 calc R U . . .
C51 C 0.1352(15) 0.8930(9) 0.6105(10) 0.101(5) Uani 1 1 d D . . . .
H51A H 0.1118 0.9313 0.5648 0.121 Uiso 1 1 calc R U . . .
H51B H 0.0570 0.8854 0.6374 0.121 Uiso 1 1 calc R U . . .
C52 C 0.1910(16) 0.8028(9) 0.5910(12) 0.103(5) Uani 1 1 d D . . . .
H52A H 0.1429 0.7771 0.5438 0.124 Uiso 1 1 calc R U . . .
H52B H 0.1906 0.7582 0.6329 0.124 Uiso 1 1 calc R U . . .
C53 C 0.3298(18) 0.8308(14) 0.5802(9) 0.109(6) Uani 1 1 d . . . . .
H53A H 0.3897 0.7775 0.5851 0.131 Uiso 1 1 calc R U . . .
H53B H 0.3318 0.8593 0.5298 0.131 Uiso 1 1 calc R U . . .
C54 C 0.083(3) -0.0922(16) 0.3910(12) 0.156(6) Uani 1 1 d D U . . .
H54A H 0.1297 -0.1508 0.4022 0.187 Uiso 1 1 calc R U . . .
H54B H -0.0006 -0.0930 0.4133 0.187 Uiso 1 1 calc R U . . .
C55 C 0.060(3) -0.0732(12) 0.3068(12) 0.145(6) Uani 1 1 d D U . . .
H55A H -0.0116 -0.1115 0.2806 0.174 Uiso 1 1 calc R U . . .
H55B H 0.1410 -0.0820 0.2828 0.174 Uiso 1 1 calc R U . . .
C56 C 0.021(2) 0.0250(12) 0.3080(12) 0.132(5) Uani 1 1 d D U . . .
H56A H 0.0260 0.0548 0.2584 0.158 Uiso 1 1 calc R U . . .
H56B H -0.0685 0.0325 0.3222 0.158 Uiso 1 1 calc R U . . .
C57 C 0.125(2) 0.0621(13) 0.3689(11) 0.134(5) Uani 1 1 d D U . . .
H57A H 0.0875 0.1116 0.3976 0.161 Uiso 1 1 calc R U . . .
H57B H 0.2004 0.0867 0.3459 0.161 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 P2 2.280(2) . ?
Cu1 P1 2.287(2) . ?
Cu1 P3 2.289(2) . ?
Cu1 Br1 2.4137(12) . ?
P1 C4 1.829(8) . ?
P1 C1 1.836(8) . ?
P1 C10 1.835(8) . ?
P2 C22 1.821(8) . ?
P2 C16 1.826(8) . ?
P2 C2 1.847(8) . ?
P3 C34 1.827(8) . ?
P3 C28 1.828(8) . ?
P3 C3 1.840(8) . ?
Si1 C40 1.863(8) . ?
Si1 C3 1.887(8) . ?
Si1 C2 1.887(8) . ?
Si1 C1 1.903(9) . ?
O1 C49 1.400(12) . ?
O1 C46 1.415(17) . ?
O2 C50 1.401(19) . ?
O2 C53 1.44(2) . ?
O3 C54 1.47(3) . ?
O3 C57 1.450(13) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.385(12) . ?
C4 C9 1.393(12) . ?
C5 C6 1.384(15) . ?
C5 H5 0.9500 . ?
C6 C7 1.370(18) . ?
C6 H6 0.9500 . ?
C7 C8 1.391(17) . ?
C7 H7 0.9500 . ?
C8 C9 1.385(14) . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?
C10 C15 1.383(13) . ?
C10 C11 1.391(12) . ?
C11 C12 1.384(14) . ?
C11 H11 0.9500 . ?
C12 C13 1.346(17) . ?
C12 H12 0.9500 . ?
C13 C14 1.374(16) . ?
C13 H13 0.9500 . ?
C14 C15 1.395(14) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C16 C17 1.390(12) . ?
C16 C21 1.401(12) . ?
C17 C18 1.397(13) . ?
C17 H17 0.9500 . ?
C18 C19 1.395(14) . ?
C18 H18 0.9500 . ?
C19 C20 1.386(14) . ?
C19 H19 0.9500 . ?
C20 C21 1.381(13) . ?
C20 H20 0.9500 . ?
C21 H21 0.9500 . ?
C22 C23 1.393(13) . ?
C22 C27 1.392(12) . ?
C23 C24 1.403(14) . ?
C23 H23 0.9500 . ?
C24 C25 1.398(17) . ?
C24 H24 0.9500 . ?
C25 C26 1.379(16) . ?
C25 H25 0.9500 . ?
C26 C27 1.392(13) . ?
C26 H26 0.9500 . ?
C27 H27 0.9500 . ?
C28 C29 1.382(13) . ?
C28 C33 1.395(12) . ?
C29 C30 1.401(14) . ?
C29 H29 0.9500 . ?
C30 C31 1.373(17) . ?
C30 H30 0.9500 . ?
C31 C32 1.375(17) . ?
C31 H31 0.9500 . ?
C32 C33 1.369(14) . ?
C32 H32 0.9500 . ?
C33 H33 0.9500 . ?
C34 C39 1.377(12) . ?
C34 C35 1.397(12) . ?
C35 C36 1.385(13) . ?
C35 H35 0.9500 . ?
C36 C37 1.385(15) . ?
C36 H36 0.9500 . ?
C37 C38 1.366(15) . ?
C37 H37 0.9500 . ?
C38 C39 1.388(13) . ?
C38 H38 0.9500 . ?
C39 H39 0.9500 . ?
C40 C41 1.393(12) . ?
C40 C45 1.399(13) . ?
C41 C42 1.383(14) . ?
C41 H41 0.9500 . ?
C42 C43 1.346(17) . ?
C42 H42 0.9500 . ?
C43 C44 1.385(16) . ?
C43 H43 0.9500 . ?
C44 C45 1.370(14) . ?
C44 H44 0.9500 . ?
C45 H45 0.9500 . ?
C46 C47 1.46(2) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 C48 1.488(12) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 C49 1.490(13) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C50 C51 1.503(13) . ?
C50 H50A 0.9900 . ?
C50 H50B 0.9900 . ?
C51 C52 1.497(12) . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C52 C53 1.52(2) . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C54 C55 1.508(14) . ?
C54 H54A 0.9900 . ?
C54 H54B 0.9900 . ?
C55 C56 1.493(13) . ?
C55 H55A 0.9900 . ?
C55 H55B 0.9900 . ?
C56 C57 1.511(13) . ?
C56 H56A 0.9900 . ?
C56 H56B 0.9900 . ?
C57 H57A 0.9900 . ?
C57 H57B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
P2 Cu1 P1 98.85(8) . . ?
P2 Cu1 P3 101.38(8) . . ?
P1 Cu1 P3 101.46(8) . . ?
P2 Cu1 Br1 114.58(6) . . ?
P1 Cu1 Br1 120.54(7) . . ?
P3 Cu1 Br1 116.84(6) . . ?
C4 P1 C1 104.3(4) . . ?
C4 P1 C10 100.0(4) . . ?
C1 P1 C10 106.5(4) . . ?
C4 P1 Cu1 116.6(3) . . ?
C1 P1 Cu1 106.9(3) . . ?
C10 P1 Cu1 121.0(3) . . ?
C22 P2 C16 103.6(4) . . ?
C22 P2 C2 104.1(4) . . ?
C16 P2 C2 104.7(4) . . ?
C22 P2 Cu1 115.7(3) . . ?
C16 P2 Cu1 120.4(3) . . ?
C2 P2 Cu1 106.6(3) . . ?
C34 P3 C28 102.4(4) . . ?
C34 P3 C3 104.2(4) . . ?
C28 P3 C3 104.3(4) . . ?
C34 P3 Cu1 116.4(3) . . ?
C28 P3 Cu1 121.8(3) . . ?
C3 P3 Cu1 106.1(3) . . ?
C40 Si1 C3 108.1(4) . . ?
C40 Si1 C2 106.8(4) . . ?
C3 Si1 C2 109.3(4) . . ?
C40 Si1 C1 111.7(4) . . ?
C3 Si1 C1 110.5(4) . . ?
C2 Si1 C1 110.2(4) . . ?
C49 O1 C46 108.4(11) . . ?
C50 O2 C53 107.6(12) . . ?
C54 O3 C57 106.8(17) . . ?
P1 C1 Si1 111.7(4) . . ?
P1 C1 H1A 109.3 . . ?
Si1 C1 H1A 109.3 . . ?
P1 C1 H1B 109.3 . . ?
Si1 C1 H1B 109.3 . . ?
H1A C1 H1B 107.9 . . ?
P2 C2 Si1 113.4(4) . . ?
P2 C2 H2A 108.9 . . ?
Si1 C2 H2A 108.9 . . ?
P2 C2 H2B 108.9 . . ?
Si1 C2 H2B 108.9 . . ?
H2A C2 H2B 107.7 . . ?
P3 C3 Si1 113.3(4) . . ?
P3 C3 H3A 108.9 . . ?
Si1 C3 H3A 108.9 . . ?
P3 C3 H3B 108.9 . . ?
Si1 C3 H3B 108.9 . . ?
H3A C3 H3B 107.7 . . ?
C5 C4 C9 118.9(8) . . ?
C5 C4 P1 124.2(7) . . ?
C9 C4 P1 116.8(6) . . ?
C6 C5 C4 120.7(10) . . ?
C6 C5 H5 119.6 . . ?
C4 C5 H5 119.6 . . ?
C7 C6 C5 120.1(10) . . ?
C7 C6 H6 120.0 . . ?
C5 C6 H6 120.0 . . ?
C6 C7 C8 120.3(10) . . ?
C6 C7 H7 119.9 . . ?
C8 C7 H7 119.9 . . ?
C9 C8 C7 119.5(10) . . ?
C9 C8 H8 120.2 . . ?
C7 C8 H8 120.2 . . ?
C8 C9 C4 120.5(9) . . ?
C8 C9 H9 119.7 . . ?
C4 C9 H9 119.7 . . ?
C15 C10 C11 120.0(8) . . ?
C15 C10 P1 116.3(6) . . ?
C11 C10 P1 123.6(7) . . ?
C12 C11 C10 119.1(9) . . ?
C12 C11 H11 120.5 . . ?
C10 C11 H11 120.5 . . ?
C13 C12 C11 120.8(9) . . ?
C13 C12 H12 119.6 . . ?
C11 C12 H12 119.6 . . ?
C12 C13 C14 121.0(9) . . ?
C12 C13 H13 119.5 . . ?
C14 C13 H13 119.5 . . ?
C13 C14 C15 119.6(10) . . ?
C13 C14 H14 120.2 . . ?
C15 C14 H14 120.2 . . ?
C10 C15 C14 119.3(9) . . ?
C10 C15 H15 120.3 . . ?
C14 C15 H15 120.3 . . ?
C17 C16 C21 118.9(8) . . ?
C17 C16 P2 123.5(7) . . ?
C21 C16 P2 117.5(7) . . ?
C16 C17 C18 120.6(9) . . ?
C16 C17 H17 119.7 . . ?
C18 C17 H17 119.7 . . ?
C19 C18 C17 119.8(8) . . ?
C19 C18 H18 120.1 . . ?
C17 C18 H18 120.1 . . ?
C20 C19 C18 119.6(8) . . ?
C20 C19 H19 120.2 . . ?
C18 C19 H19 120.2 . . ?
C21 C20 C19 120.7(9) . . ?
C21 C20 H20 119.7 . . ?
C19 C20 H20 119.7 . . ?
C20 C21 C16 120.5(9) . . ?
C20 C21 H21 119.8 . . ?
C16 C21 H21 119.8 . . ?
C23 C22 C27 119.0(8) . . ?
C23 C22 P2 123.5(7) . . ?
C27 C22 P2 117.5(7) . . ?
C22 C23 C24 120.0(10) . . ?
C22 C23 H23 120.0 . . ?
C24 C23 H23 120.0 . . ?
C25 C24 C23 120.2(10) . . ?
C25 C24 H24 119.9 . . ?
C23 C24 H24 119.9 . . ?
C26 C25 C24 119.5(10) . . ?
C26 C25 H25 120.3 . . ?
C24 C25 H25 120.3 . . ?
C25 C26 C27 120.3(10) . . ?
C25 C26 H26 119.8 . . ?
C27 C26 H26 119.8 . . ?
C26 C27 C22 120.9(9) . . ?
C26 C27 H27 119.6 . . ?
C22 C27 H27 119.6 . . ?
C29 C28 C33 118.4(8) . . ?
C29 C28 P3 123.8(7) . . ?
C33 C28 P3 117.8(7) . . ?
C28 C29 C30 121.3(9) . . ?
C28 C29 H29 119.3 . . ?
C30 C29 H29 119.3 . . ?
C31 C30 C29 119.0(10) . . ?
C31 C30 H30 120.5 . . ?
C29 C30 H30 120.5 . . ?
C32 C31 C30 119.7(9) . . ?
C32 C31 H31 120.1 . . ?
C30 C31 H31 120.1 . . ?
C33 C32 C31 121.6(10) . . ?
C33 C32 H32 119.2 . . ?
C31 C32 H32 119.2 . . ?
C32 C33 C28 119.9(10) . . ?
C32 C33 H33 120.0 . . ?
C28 C33 H33 120.0 . . ?
C39 C34 C35 116.6(8) . . ?
C39 C34 P3 119.9(6) . . ?
C35 C34 P3 123.4(7) . . ?
C36 C35 C34 121.6(9) . . ?
C36 C35 H35 119.2 . . ?
C34 C35 H35 119.2 . . ?
C35 C36 C37 119.6(9) . . ?
C35 C36 H36 120.2 . . ?
C37 C36 H36 120.2 . . ?
C38 C37 C36 120.3(9) . . ?
C38 C37 H37 119.9 . . ?
C36 C37 H37 119.9 . . ?
C37 C38 C39 119.1(9) . . ?
C37 C38 H38 120.4 . . ?
C39 C38 H38 120.4 . . ?
C34 C39 C38 122.8(9) . . ?
C34 C39 H39 118.6 . . ?
C38 C39 H39 118.6 . . ?
C41 C40 C45 116.2(8) . . ?
C41 C40 Si1 123.2(7) . . ?
C45 C40 Si1 120.3(6) . . ?
C42 C41 C40 120.8(10) . . ?
C42 C41 H41 119.6 . . ?
C40 C41 H41 119.6 . . ?
C43 C42 C41 122.1(10) . . ?
C43 C42 H42 119.0 . . ?
C41 C42 H42 119.0 . . ?
C42 C43 C44 118.5(9) . . ?
C42 C43 H43 120.7 . . ?
C44 C43 H43 120.7 . . ?
C45 C44 C43 120.3(11) . . ?
C45 C44 H44 119.8 . . ?
C43 C44 H44 119.8 . . ?
C44 C45 C40 122.0(9) . . ?
C44 C45 H45 119.0 . . ?
C40 C45 H45 119.0 . . ?
O1 C46 C47 110.0(11) . . ?
O1 C46 H46A 109.7 . . ?
C47 C46 H46A 109.7 . . ?
O1 C46 H46B 109.7 . . ?
C47 C46 H46B 109.7 . . ?
H46A C46 H46B 108.2 . . ?
C46 C47 C48 103.0(11) . . ?
C46 C47 H47A 111.2 . . ?
C48 C47 H47A 111.2 . . ?
C46 C47 H47B 111.2 . . ?
C48 C47 H47B 111.2 . . ?
H47A C47 H47B 109.1 . . ?
C47 C48 C49 105.4(11) . . ?
C47 C48 H48A 110.7 . . ?
C49 C48 H48A 110.7 . . ?
C47 C48 H48B 110.7 . . ?
C49 C48 H48B 110.7 . . ?
H48A C48 H48B 108.8 . . ?
O1 C49 C48 107.8(12) . . ?
O1 C49 H49A 110.2 . . ?
C48 C49 H49A 110.2 . . ?
O1 C49 H49B 110.2 . . ?
C48 C49 H49B 110.2 . . ?
H49A C49 H49B 108.5 . . ?
O2 C50 C51 108.6(13) . . ?
O2 C50 H50A 110.0 . . ?
C51 C50 H50A 110.0 . . ?
O2 C50 H50B 110.0 . . ?
C51 C50 H50B 110.0 . . ?
H50A C50 H50B 108.3 . . ?
C50 C51 C52 100.4(13) . . ?
C50 C51 H51A 111.7 . . ?
C52 C51 H51A 111.7 . . ?
C50 C51 H51B 111.7 . . ?
C52 C51 H51B 111.7 . . ?
H51A C51 H51B 109.5 . . ?
C51 C52 C53 100.6(13) . . ?
C51 C52 H52A 111.6 . . ?
C53 C52 H52A 111.6 . . ?
C51 C52 H52B 111.6 . . ?
C53 C52 H52B 111.6 . . ?
H52A C52 H52B 109.4 . . ?
O2 C53 C52 104.0(11) . . ?
O2 C53 H53A 111.0 . . ?
C52 C53 H53A 111.0 . . ?
O2 C53 H53B 111.0 . . ?
C52 C53 H53B 111.0 . . ?
H53A C53 H53B 109.0 . . ?
C55 C54 O3 101.3(18) . . ?
C55 C54 H54A 111.5 . . ?
O3 C54 H54A 111.5 . . ?
C55 C54 H54B 111.5 . . ?
O3 C54 H54B 111.5 . . ?
H54A C54 H54B 109.3 . . ?
C54 C55 C56 99.8(17) . . ?
C54 C55 H55A 111.8 . . ?
C56 C55 H55A 111.8 . . ?
C54 C55 H55B 111.8 . . ?
C56 C55 H55B 111.8 . . ?
H55A C55 H55B 109.5 . . ?
C57 C56 C55 101.2(16) . . ?
C57 C56 H56A 111.5 . . ?
C55 C56 H56A 111.5 . . ?
C57 C56 H56B 111.5 . . ?
C55 C56 H56B 111.5 . . ?
H56A C56 H56B 109.4 . . ?
C56 C57 O3 106.1(16) . . ?
C56 C57 H57A 110.5 . . ?
O3 C57 H57A 110.5 . . ?
C56 C57 H57B 110.5 . . ?
O3 C57 H57B 110.5 . . ?
H57A C57 H57B 108.7 . . ?

_refine_diff_density_max         0.723
_refine_diff_density_min         -0.470
_refine_diff_density_rms         0.071

_shelxl_version_number           2014-3


####################################################################### 
# 
# 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_5prime-THF
_database_code_depnum_ccdc_archive 'CCDC 1481879'
_audit_update_record             
;
2016-06-21 deposited with the CCDC.
2016-07-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C46 H43 Cu I O4 P3 Si'
_chemical_formula_weight         971.24

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, 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                   19.0061(3)
_cell_length_b                   21.5469(5)
_cell_length_c                   21.4927(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     8801.8(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    284218
_cell_measurement_theta_min      2.37
_cell_measurement_theta_max      28.70

_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.466
_exptl_crystal_F_000             3936
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.14
_exptl_absorpt_coefficient_mu    1.376
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.668
_exptl_absorpt_correction_T_max  0.825
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_special_details           'crystal-to-detector distance 32 mm'
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method       
'two φ and six ω scans with 2° steps (458 frames)'
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            284218
_diffrn_reflns_av_unetI/netI     0.0228
_diffrn_reflns_av_R_equivalents  0.0156
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         2.371
_diffrn_reflns_theta_max         28.699
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             11344
_reflns_number_gt                8933
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  
'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)'

_refine_special_details          
;
 Structure solved by intrinsic phasing and subsequent difference Fourier
 synthesis. All non-hydrogen atoms were refined with anisotropic
 displacement parameters. The H atoms were introduced at calculated
 positions and were treated as riding atoms with an isotropic displacement
 parameter equal to 1.2 times that of the parent atom.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0493P)²+3.9672P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         11344
_refine_ls_number_parameters     505
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0487
_refine_ls_R_factor_gt           0.0349
_refine_ls_wR_factor_ref         0.0977
_refine_ls_wR_factor_gt          0.0927
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_restrained_S_all      1.061
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.37259(2) 0.22196(2) 0.61392(2) 0.03599(8) Uani 1 1 d . . . . .
I1 I 0.29237(2) 0.15087(2) 0.67680(2) 0.05191(7) Uani 1 1 d . . . . .
P1 P 0.43654(3) 0.29466(3) 0.66614(3) 0.03457(12) Uani 1 1 d . . . . .
P2 P 0.46354(3) 0.18256(3) 0.55735(3) 0.03792(13) Uani 1 1 d . . . . .
P3 P 0.33094(3) 0.28679(3) 0.53907(3) 0.03969(14) Uani 1 1 d . . . . .
Si1 Si 0.48019(3) 0.31565(3) 0.53911(3) 0.03338(13) Uani 1 1 d . . . . .
O1 O 0.48899(8) 0.32709(7) 0.61447(7) 0.0375(3) Uani 1 1 d . . . . .
O2 O 0.50004(9) 0.24317(7) 0.52357(7) 0.0403(4) Uani 1 1 d . . . . .
O3 O 0.39852(9) 0.33005(8) 0.51912(8) 0.0438(4) Uani 1 1 d . . . . .
O4 O 0.3496(3) 0.44141(16) 0.3855(2) 0.1460(15) Uani 1 1 d D . . . .
C1 C 0.38853(14) 0.36151(11) 0.69515(10) 0.0398(5) Uani 1 1 d . . . . .
C2 C 0.42208(17) 0.41741(12) 0.70698(13) 0.0560(7) Uani 1 1 d . . . . .
H2 H 0.4718 0.4205 0.7032 0.067 Uiso 1 1 calc R U . . .
C3 C 0.3827(2) 0.46877(14) 0.72429(15) 0.0745(10) Uani 1 1 d . . . . .
H3 H 0.4055 0.5071 0.7327 0.089 Uiso 1 1 calc R U . . .
C4 C 0.3103(2) 0.46430(15) 0.72931(15) 0.0719(10) Uani 1 1 d . . . . .
H4 H 0.2833 0.4999 0.7398 0.086 Uiso 1 1 calc R U . . .
C5 C 0.27705(19) 0.40821(16) 0.71909(14) 0.0640(8) Uani 1 1 d . . . . .
H5 H 0.2275 0.4048 0.7238 0.077 Uiso 1 1 calc R U . . .
C6 C 0.31652(15) 0.35724(13) 0.70193(12) 0.0492(6) Uani 1 1 d . . . . .
H6 H 0.2938 0.3187 0.6947 0.059 Uiso 1 1 calc R U . . .
C7 C 0.49742(13) 0.27458(10) 0.72774(10) 0.0389(5) Uani 1 1 d . . . . .
C8 C 0.46915(15) 0.24441(12) 0.77940(12) 0.0487(6) Uani 1 1 d . . . . .
H8 H 0.4196 0.2397 0.7832 0.058 Uiso 1 1 calc R U . . .
C9 C 0.51356(18) 0.22131(13) 0.82531(12) 0.0546(7) Uani 1 1 d . . . . .
H9 H 0.4943 0.2011 0.8607 0.066 Uiso 1 1 calc R U . . .
C10 C 0.58538(18) 0.22763(14) 0.81961(14) 0.0594(8) Uani 1 1 d . . . . .
H10 H 0.6156 0.2110 0.8506 0.071 Uiso 1 1 calc R U . . .
C11 C 0.61338(17) 0.25786(15) 0.76920(15) 0.0634(8) Uani 1 1 d . . . . .
H11 H 0.6629 0.2628 0.7659 0.076 Uiso 1 1 calc R U . . .
C12 C 0.56941(15) 0.28144(13) 0.72271(13) 0.0513(6) Uani 1 1 d . . . . .
H12 H 0.5890 0.3021 0.6877 0.062 Uiso 1 1 calc R U . . .
C13 C 0.53608(14) 0.14985(10) 0.60063(11) 0.0418(5) Uani 1 1 d . . . . .
C14 C 0.52632(18) 0.13563(12) 0.66306(13) 0.0536(7) Uani 1 1 d . . . . .
H14 H 0.4809 0.1397 0.6811 0.064 Uiso 1 1 calc R U . . .
C15 C 0.5818(2) 0.11577(14) 0.69883(15) 0.0711(10) Uani 1 1 d . . . . .
H15 H 0.5748 0.1070 0.7417 0.085 Uiso 1 1 calc R U . . .
C16 C 0.6470(2) 0.10852(15) 0.67310(18) 0.0755(11) Uani 1 1 d . . . . .
H16 H 0.6851 0.0951 0.6983 0.091 Uiso 1 1 calc R U . . .
C17 C 0.65788(17) 0.12051(14) 0.61094(18) 0.0671(8) Uani 1 1 d . . . . .
H17 H 0.7031 0.1144 0.5931 0.081 Uiso 1 1 calc R U . . .
C18 C 0.60245(15) 0.14165(13) 0.57421(14) 0.0536(6) Uani 1 1 d . . . . .
H18 H 0.6098 0.1504 0.5314 0.064 Uiso 1 1 calc R U . . .
C19 C 0.45324(13) 0.13079(11) 0.49158(11) 0.0418(5) Uani 1 1 d . . . . .
C20 C 0.46039(16) 0.14992(13) 0.43085(12) 0.0529(7) Uani 1 1 d . . . . .
H20 H 0.4741 0.1914 0.4222 0.063 Uiso 1 1 calc R U . . .
C21 C 0.44780(18) 0.10908(15) 0.38201(13) 0.0643(8) Uani 1 1 d . . . . .
H21 H 0.4530 0.1225 0.3402 0.077 Uiso 1 1 calc R U . . .
C22 C 0.42769(19) 0.04883(15) 0.39480(15) 0.0688(9) Uani 1 1 d . . . . .
H22 H 0.4193 0.0205 0.3617 0.083 Uiso 1 1 calc R U . . .
C23 C 0.4199(3) 0.03006(15) 0.45473(17) 0.0867(12) Uani 1 1 d . . . . .
H23 H 0.4056 -0.0113 0.4633 0.104 Uiso 1 1 calc R U . . .
C24 C 0.4327(2) 0.07039(14) 0.50334(15) 0.0782(11) Uani 1 1 d . . . . .
H24 H 0.4273 0.0566 0.5450 0.094 Uiso 1 1 calc R U . . .
C25 C 0.30537(12) 0.25320(13) 0.46541(11) 0.0438(5) Uani 1 1 d . . . . .
C26 C 0.28564(17) 0.19102(16) 0.46453(15) 0.0658(8) Uani 1 1 d . . . . .
H26 H 0.2869 0.1675 0.5019 0.079 Uiso 1 1 calc R U . . .
C27 C 0.2643(2) 0.16318(19) 0.40967(18) 0.0811(11) Uani 1 1 d . . . . .
H27 H 0.2505 0.1208 0.4093 0.097 Uiso 1 1 calc R U . . .
C28 C 0.26305(19) 0.1975(2) 0.35545(16) 0.0741(9) Uani 1 1 d . . . . .
H28 H 0.2475 0.1787 0.3179 0.089 Uiso 1 1 calc R U . . .
C29 C 0.28399(18) 0.25825(18) 0.35511(14) 0.0695(9) Uani 1 1 d . . . . .
H29 H 0.2837 0.2811 0.3173 0.083 Uiso 1 1 calc R U . . .
C30 C 0.30573(16) 0.28669(15) 0.41009(13) 0.0560(7) Uani 1 1 d . . . . .
H30 H 0.3207 0.3287 0.4098 0.067 Uiso 1 1 calc R U . . .
C31 C 0.26406(13) 0.34485(12) 0.55355(12) 0.0445(6) Uani 1 1 d . . . . .
C32 C 0.27248(16) 0.40766(13) 0.54085(14) 0.0556(7) Uani 1 1 d . . . . .
H32 H 0.3143 0.4221 0.5216 0.067 Uiso 1 1 calc R U . . .
C33 C 0.21986(18) 0.44877(15) 0.55632(17) 0.0682(8) Uani 1 1 d . . . . .
H33 H 0.2257 0.4917 0.5478 0.082 Uiso 1 1 calc R U . . .
C34 C 0.15853(17) 0.42813(16) 0.58418(15) 0.0664(8) Uani 1 1 d . . . . .
H34 H 0.1223 0.4568 0.5942 0.080 Uiso 1 1 calc R U . . .
C35 C 0.15011(16) 0.36678(16) 0.59720(15) 0.0621(8) Uani 1 1 d . . . . .
H35 H 0.1082 0.3527 0.6167 0.075 Uiso 1 1 calc R U . . .
C36 C 0.20253(14) 0.32485(14) 0.58212(13) 0.0525(6) Uani 1 1 d . . . . .
H36 H 0.1964 0.2821 0.5914 0.063 Uiso 1 1 calc R U . . .
C37 C 0.53720(13) 0.36721(11) 0.49409(10) 0.0380(5) Uani 1 1 d . . . . .
C38 C 0.51047(17) 0.41905(17) 0.46504(19) 0.0809(12) Uani 1 1 d . . . . .
H38 H 0.4618 0.4282 0.4687 0.097 Uiso 1 1 calc R U . . .
C39 C 0.55371(19) 0.4584(2) 0.4302(2) 0.0971(15) Uani 1 1 d . . . . .
H39 H 0.5348 0.4951 0.4123 0.117 Uiso 1 1 calc R U . . .
C40 C 0.62228(16) 0.44439(15) 0.42203(14) 0.0622(8) Uani 1 1 d . . . . .
H40 H 0.6513 0.4708 0.3977 0.075 Uiso 1 1 calc R U . . .
C41 C 0.64989(16) 0.39234(15) 0.44874(16) 0.0651(8) Uani 1 1 d . . . . .
H41 H 0.6981 0.3823 0.4426 0.078 Uiso 1 1 calc R U . . .
C42 C 0.60735(15) 0.35382(14) 0.48504(15) 0.0570(7) Uani 1 1 d . . . . .
H42 H 0.6271 0.3179 0.5038 0.068 Uiso 1 1 calc R U . . .
C43 C 0.3806(5) 0.4332(3) 0.3269(3) 0.150(3) Uani 1 1 d D . . . .
H43A H 0.3504 0.4053 0.3020 0.180 Uiso 1 1 calc R U . . .
H43B H 0.4265 0.4122 0.3326 0.180 Uiso 1 1 calc R U . . .
C44 C 0.3923(3) 0.4918(2) 0.2909(3) 0.143(2) Uani 1 1 d D . . . .
H44A H 0.3611 0.4947 0.2541 0.172 Uiso 1 1 calc R U . . .
H44B H 0.4419 0.4967 0.2778 0.172 Uiso 1 1 calc R U . . .
C45 C 0.3716(3) 0.53845(19) 0.3420(2) 0.1034(14) Uani 1 1 d D . . . .
H45A H 0.4142 0.5554 0.3622 0.124 Uiso 1 1 calc R U . . .
H45B H 0.3446 0.5733 0.3238 0.124 Uiso 1 1 calc R U . . .
C46 C 0.3271(3) 0.50399(19) 0.3889(3) 0.138(2) Uani 1 1 d D . . . .
H46A H 0.3346 0.5208 0.4313 0.165 Uiso 1 1 calc R U . . .
H46B H 0.2766 0.5075 0.3784 0.165 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 P3 2.2728(7) . ?
Cu1 P2 2.2777(7) . ?
Cu1 P1 2.2783(6) . ?
Cu1 I1 2.5491(3) . ?
P1 O1 1.6477(16) . ?
P1 C7 1.811(2) . ?
P1 C1 1.815(2) . ?
P2 O2 1.6474(16) . ?
P2 C13 1.806(3) . ?
P2 C19 1.811(2) . ?
P3 O3 1.6439(17) . ?
P3 C25 1.807(3) . ?
P3 C31 1.810(3) . ?
Si1 O3 1.6403(17) . ?
Si1 O2 1.6410(16) . ?
Si1 O1 1.6469(16) . ?
Si1 C37 1.829(2) . ?
O4 C46 1.416(4) . ?
O4 C43 1.401(7) . ?
C1 C6 1.380(4) . ?
C1 C2 1.386(4) . ?
C2 C3 1.387(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.384(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.381(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.380(4) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C12 1.380(4) . ?
C7 C8 1.394(3) . ?
C8 C9 1.391(4) . ?
C8 H8 0.9500 . ?
C9 C10 1.377(5) . ?
C9 H9 0.9500 . ?
C10 C11 1.372(4) . ?
C10 H10 0.9500 . ?
C11 C12 1.398(4) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 C14 1.389(4) . ?
C13 C18 1.394(4) . ?
C14 C15 1.373(5) . ?
C14 H14 0.9500 . ?
C15 C16 1.366(5) . ?
C15 H15 0.9500 . ?
C16 C17 1.376(5) . ?
C16 H16 0.9500 . ?
C17 C18 1.393(4) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 C20 1.375(4) . ?
C19 C24 1.382(4) . ?
C20 C21 1.391(4) . ?
C20 H20 0.9500 . ?
C21 C22 1.381(5) . ?
C21 H21 0.9500 . ?
C22 C23 1.358(5) . ?
C22 H22 0.9500 . ?
C23 C24 1.380(4) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 C30 1.391(4) . ?
C25 C26 1.391(4) . ?
C26 C27 1.384(5) . ?
C26 H26 0.9500 . ?
C27 C28 1.381(5) . ?
C27 H27 0.9500 . ?
C28 C29 1.368(5) . ?
C28 H28 0.9500 . ?
C29 C30 1.394(4) . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?
C31 C36 1.389(4) . ?
C31 C32 1.390(4) . ?
C32 C33 1.377(4) . ?
C32 H32 0.9500 . ?
C33 C34 1.384(5) . ?
C33 H33 0.9500 . ?
C34 C35 1.361(5) . ?
C34 H34 0.9500 . ?
C35 C36 1.383(4) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C37 C38 1.377(4) . ?
C37 C42 1.378(4) . ?
C38 C39 1.398(4) . ?
C38 H38 0.9500 . ?
C39 C40 1.349(5) . ?
C39 H39 0.9500 . ?
C40 C41 1.365(4) . ?
C40 H40 0.9500 . ?
C41 C42 1.397(4) . ?
C41 H41 0.9500 . ?
C42 H42 0.9500 . ?
C43 C44 1.499(4) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 C45 1.540(4) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C45 C46 1.511(4) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
P3 Cu1 P2 96.64(2) . . ?
P3 Cu1 P1 96.43(2) . . ?
P2 Cu1 P1 96.57(2) . . ?
P3 Cu1 I1 122.43(2) . . ?
P2 Cu1 I1 120.858(19) . . ?
P1 Cu1 I1 118.109(18) . . ?
O1 P1 C7 101.98(10) . . ?
O1 P1 C1 101.49(10) . . ?
C7 P1 C1 105.05(11) . . ?
O1 P1 Cu1 106.40(6) . . ?
C7 P1 Cu1 122.47(8) . . ?
C1 P1 Cu1 116.52(9) . . ?
O2 P2 C13 102.41(10) . . ?
O2 P2 C19 100.94(10) . . ?
C13 P2 C19 104.13(11) . . ?
O2 P2 Cu1 105.03(6) . . ?
C13 P2 Cu1 116.74(8) . . ?
C19 P2 Cu1 124.35(9) . . ?
O3 P3 C25 102.04(10) . . ?
O3 P3 C31 101.63(11) . . ?
C25 P3 C31 103.80(12) . . ?
O3 P3 Cu1 105.13(6) . . ?
C25 P3 Cu1 117.87(9) . . ?
C31 P3 Cu1 123.20(8) . . ?
O3 Si1 O2 110.14(9) . . ?
O3 Si1 O1 108.99(9) . . ?
O2 Si1 O1 108.62(9) . . ?
O3 Si1 C37 107.88(10) . . ?
O2 Si1 C37 109.53(10) . . ?
O1 Si1 C37 111.67(10) . . ?
Si1 O1 P1 122.54(10) . . ?
Si1 O2 P2 124.61(10) . . ?
Si1 O3 P3 124.31(10) . . ?
C46 O4 C43 107.1(5) . . ?
C6 C1 C2 119.7(2) . . ?
C6 C1 P1 118.83(19) . . ?
C2 C1 P1 121.4(2) . . ?
C3 C2 C1 119.6(3) . . ?
C3 C2 H2 120.2 . . ?
C1 C2 H2 120.2 . . ?
C4 C3 C2 120.1(3) . . ?
C4 C3 H3 119.9 . . ?
C2 C3 H3 119.9 . . ?
C5 C4 C3 120.2(3) . . ?
C5 C4 H4 119.9 . . ?
C3 C4 H4 119.9 . . ?
C6 C5 C4 119.4(3) . . ?
C6 C5 H5 120.3 . . ?
C4 C5 H5 120.3 . . ?
C1 C6 C5 121.0(3) . . ?
C1 C6 H6 119.5 . . ?
C5 C6 H6 119.5 . . ?
C12 C7 C8 119.6(2) . . ?
C12 C7 P1 123.41(19) . . ?
C8 C7 P1 116.58(19) . . ?
C9 C8 C7 119.9(3) . . ?
C9 C8 H8 120.1 . . ?
C7 C8 H8 120.1 . . ?
C10 C9 C8 120.2(3) . . ?
C10 C9 H9 119.9 . . ?
C8 C9 H9 119.9 . . ?
C11 C10 C9 120.1(3) . . ?
C11 C10 H10 119.9 . . ?
C9 C10 H10 119.9 . . ?
C10 C11 C12 120.4(3) . . ?
C10 C11 H11 119.8 . . ?
C12 C11 H11 119.8 . . ?
C7 C12 C11 119.8(3) . . ?
C7 C12 H12 120.1 . . ?
C11 C12 H12 120.1 . . ?
C14 C13 C18 119.1(3) . . ?
C14 C13 P2 118.8(2) . . ?
C18 C13 P2 122.0(2) . . ?
C15 C14 C13 120.5(3) . . ?
C15 C14 H14 119.8 . . ?
C13 C14 H14 119.8 . . ?
C16 C15 C14 120.4(3) . . ?
C16 C15 H15 119.8 . . ?
C14 C15 H15 119.8 . . ?
C15 C16 C17 120.5(3) . . ?
C15 C16 H16 119.7 . . ?
C17 C16 H16 119.7 . . ?
C16 C17 C18 119.8(3) . . ?
C16 C17 H17 120.1 . . ?
C18 C17 H17 120.1 . . ?
C17 C18 C13 119.7(3) . . ?
C17 C18 H18 120.2 . . ?
C13 C18 H18 120.2 . . ?
C20 C19 C24 118.9(2) . . ?
C20 C19 P2 123.06(19) . . ?
C24 C19 P2 117.9(2) . . ?
C19 C20 C21 120.7(3) . . ?
C19 C20 H20 119.7 . . ?
C21 C20 H20 119.7 . . ?
C22 C21 C20 119.5(3) . . ?
C22 C21 H21 120.3 . . ?
C20 C21 H21 120.3 . . ?
C23 C22 C21 119.9(3) . . ?
C23 C22 H22 120.0 . . ?
C21 C22 H22 120.0 . . ?
C22 C23 C24 120.8(3) . . ?
C22 C23 H23 119.6 . . ?
C24 C23 H23 119.6 . . ?
C23 C24 C19 120.3(3) . . ?
C23 C24 H24 119.9 . . ?
C19 C24 H24 119.9 . . ?
C30 C25 C26 119.3(3) . . ?
C30 C25 P3 122.7(2) . . ?
C26 C25 P3 118.0(2) . . ?
C27 C26 C25 120.5(3) . . ?
C27 C26 H26 119.7 . . ?
C25 C26 H26 119.7 . . ?
C28 C27 C26 119.5(3) . . ?
C28 C27 H27 120.3 . . ?
C26 C27 H27 120.3 . . ?
C29 C28 C27 120.8(3) . . ?
C29 C28 H28 119.6 . . ?
C27 C28 H28 119.6 . . ?
C28 C29 C30 120.2(3) . . ?
C28 C29 H29 119.9 . . ?
C30 C29 H29 119.9 . . ?
C25 C30 C29 119.7(3) . . ?
C25 C30 H30 120.2 . . ?
C29 C30 H30 120.2 . . ?
C36 C31 C32 119.1(3) . . ?
C36 C31 P3 116.9(2) . . ?
C32 C31 P3 123.9(2) . . ?
C33 C32 C31 119.7(3) . . ?
C33 C32 H32 120.1 . . ?
C31 C32 H32 120.1 . . ?
C32 C33 C34 120.6(3) . . ?
C32 C33 H33 119.7 . . ?
C34 C33 H33 119.7 . . ?
C35 C34 C33 120.0(3) . . ?
C35 C34 H34 120.0 . . ?
C33 C34 H34 120.0 . . ?
C34 C35 C36 120.1(3) . . ?
C34 C35 H35 119.9 . . ?
C36 C35 H35 119.9 . . ?
C35 C36 C31 120.5(3) . . ?
C35 C36 H36 119.8 . . ?
C31 C36 H36 119.8 . . ?
C38 C37 C42 117.6(2) . . ?
C38 C37 Si1 120.9(2) . . ?
C42 C37 Si1 121.38(19) . . ?
C37 C38 C39 121.2(3) . . ?
C37 C38 H38 119.4 . . ?
C39 C38 H38 119.4 . . ?
C40 C39 C38 120.2(3) . . ?
C40 C39 H39 119.9 . . ?
C38 C39 H39 119.9 . . ?
C39 C40 C41 120.0(3) . . ?
C39 C40 H40 120.0 . . ?
C41 C40 H40 120.0 . . ?
C40 C41 C42 120.0(3) . . ?
C40 C41 H41 120.0 . . ?
C42 C41 H41 120.0 . . ?
C37 C42 C41 121.0(3) . . ?
C37 C42 H42 119.5 . . ?
C41 C42 H42 119.5 . . ?
O4 C43 C44 114.8(5) . . ?
O4 C43 H43A 108.6 . . ?
C44 C43 H43A 108.6 . . ?
O4 C43 H43B 108.6 . . ?
C44 C43 H43B 108.6 . . ?
H43A C43 H43B 107.5 . . ?
C43 C44 C45 98.2(4) . . ?
C43 C44 H44A 112.1 . . ?
C45 C44 H44A 112.1 . . ?
C43 C44 H44B 112.1 . . ?
C45 C44 H44B 112.1 . . ?
H44A C44 H44B 109.8 . . ?
C46 C45 C44 107.4(4) . . ?
C46 C45 H45A 110.2 . . ?
C44 C45 H45A 110.2 . . ?
C46 C45 H45B 110.2 . . ?
C44 C45 H45B 110.2 . . ?
H45A C45 H45B 108.5 . . ?
O4 C46 C45 105.3(4) . . ?
O4 C46 H46A 110.7 . . ?
C45 C46 H46A 110.7 . . ?
O4 C46 H46B 110.7 . . ?
C45 C46 H46B 110.7 . . ?
H46A C46 H46B 108.8 . . ?

_refine_diff_density_max         1.017
_refine_diff_density_min         -0.736
_refine_diff_density_rms         0.062

_shelxl_version_number           2014-3


####################################################################### 
# 
# 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_6-CH3CN
_database_code_depnum_ccdc_archive 'CCDC 1481880'
_audit_update_record             
;
2016-06-21 deposited with the CCDC.
2016-07-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C32 H32 Cu2 I2 N4 O P2'
_chemical_formula_weight         931.43

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'
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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   22.3076(10)
_cell_length_b                   8.4153(3)
_cell_length_c                   21.1830(10)
_cell_angle_alpha                90
_cell_angle_beta                 118.621(2)
_cell_angle_gamma                90
_cell_volume                     3490.7(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    60399
_cell_measurement_theta_min      2.63
_cell_measurement_theta_max      30.51

_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.772
_exptl_crystal_F_000             1816
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_exptl_absorpt_coefficient_mu    3.110
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.541
_exptl_absorpt_correction_T_max  0.627
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_special_details           'crystal-to-detector distance 30 mm'
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method       
'two φ and five ω scans with 2° steps (478 frames)'
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            60399
_diffrn_reflns_av_unetI/netI     0.0470
_diffrn_reflns_av_R_equivalents  0.0454
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         2.634
_diffrn_reflns_theta_max         30.506
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.985
_reflns_number_total             5263
_reflns_number_gt                4550
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  
'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)'

_refine_special_details          
;
 Structure solved by intrinsic phasing. All non-hydrogen atoms were refined
 with anisotropic displacement parameters. The H atoms were introduced at
 calculated positions and were treated as riding atoms with an isotropic
 displacement parameter equal to 1.2 times that of the parent atom (1.5
 for CH₃, with optimized geometry). 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0466P)²+0.7212P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5263
_refine_ls_number_parameters     197
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0321
_refine_ls_wR_factor_ref         0.0859
_refine_ls_wR_factor_gt          0.0832
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_restrained_S_all      1.064
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.43809(2) 0.65291(3) 0.68560(2) 0.03097(8) Uani 1 1 d . . . . .
I1 I 0.55596(2) 0.73299(2) 0.68774(2) 0.03329(6) Uani 1 1 d . . . . .
P1 P 0.43459(3) 0.39067(7) 0.68404(3) 0.02542(11) Uani 1 1 d . . . . .
O1 O 0.5000 0.2991(3) 0.7500 0.0287(4) Uani 1 2 d S T P . .
N1 N 0.36643(10) 0.7911(2) 0.61376(11) 0.0343(4) Uani 1 1 d . . . . .
N2 N 0.19447(18) 0.7482(4) 0.5840(2) 0.0730(9) Uani 1 1 d . . . . .
C1 C 0.43203(11) 0.2901(3) 0.60685(11) 0.0272(4) Uani 1 1 d . . . . .
C2 C 0.45117(11) 0.1317(3) 0.60853(12) 0.0305(4) Uani 1 1 d . . . . .
H2 H 0.4680 0.0724 0.6519 0.037 Uiso 1 1 calc R U . . .
C3 C 0.44548(12) 0.0605(3) 0.54643(12) 0.0347(5) Uani 1 1 d . . . . .
H3 H 0.4586 -0.0473 0.5475 0.042 Uiso 1 1 calc R U . . .
C4 C 0.42080(13) 0.1467(3) 0.48335(13) 0.0389(5) Uani 1 1 d . . . . .
H4 H 0.4163 0.0973 0.4409 0.047 Uiso 1 1 calc R U . . .
C5 C 0.40263(14) 0.3050(3) 0.48163(13) 0.0415(6) Uani 1 1 d . . . . .
H5 H 0.3862 0.3642 0.4383 0.050 Uiso 1 1 calc R U . . .
C6 C 0.40848(12) 0.3763(3) 0.54312(12) 0.0352(5) Uani 1 1 d . . . . .
H6 H 0.3964 0.4849 0.5420 0.042 Uiso 1 1 calc R U . . .
C7 C 0.36395(11) 0.3003(3) 0.69073(11) 0.0280(4) Uani 1 1 d . . . . .
C8 C 0.36404(12) 0.1415(3) 0.70939(12) 0.0338(5) Uani 1 1 d . . . . .
H8 H 0.4023 0.0762 0.7194 0.041 Uiso 1 1 calc R U . . .
C9 C 0.30807(13) 0.0776(3) 0.71344(13) 0.0396(5) Uani 1 1 d . . . . .
H9 H 0.3082 -0.0307 0.7261 0.047 Uiso 1 1 calc R U . . .
C10 C 0.25224(13) 0.1737(4) 0.69876(14) 0.0430(6) Uani 1 1 d . . . . .
H10 H 0.2142 0.1310 0.7017 0.052 Uiso 1 1 calc R U . . .
C11 C 0.25170(12) 0.3313(3) 0.67984(14) 0.0411(6) Uani 1 1 d . . . . .
H11 H 0.2132 0.3961 0.6695 0.049 Uiso 1 1 calc R U . . .
C12 C 0.30736(11) 0.3953(3) 0.67597(12) 0.0343(5) Uani 1 1 d . . . . .
H12 H 0.3069 0.5037 0.6633 0.041 Uiso 1 1 calc R U . . .
C13 C 0.32690(12) 0.8782(3) 0.57521(12) 0.0346(5) Uani 1 1 d . . . . .
C14 C 0.27690(13) 0.9920(3) 0.52676(14) 0.0424(6) Uani 1 1 d . . . . .
H14A H 0.2549 1.0450 0.5515 0.064 Uiso 1 1 calc R U . . .
H14B H 0.2423 0.9362 0.4843 0.064 Uiso 1 1 calc R U . . .
H14C H 0.2998 1.0713 0.5119 0.064 Uiso 1 1 calc R U . . .
C15 C 0.15236(15) 0.7731(3) 0.59796(16) 0.0441(6) Uani 1 1 d . . . . .
C16 C 0.09910(17) 0.8047(4) 0.61648(19) 0.0561(7) Uani 1 1 d . . . . .
H16A H 0.0565 0.8292 0.5727 0.084 Uiso 1 1 calc R U . . .
H16B H 0.1122 0.8954 0.6494 0.084 Uiso 1 1 calc R U . . .
H16C H 0.0924 0.7110 0.6398 0.084 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N1 1.973(2) . ?
Cu1 P1 2.2079(6) . ?
Cu1 I1 2.6937(3) . ?
Cu1 I1 2.7074(3) 2_656 ?
Cu1 Cu1 2.8024(5) 2_656 ?
I1 Cu1 2.7073(3) 2_656 ?
P1 O1 1.6498(12) . ?
P1 C7 1.815(2) . ?
P1 C1 1.818(2) . ?
O1 P1 1.6498(12) 2_656 ?
N1 C13 1.136(3) . ?
N2 C15 1.131(4) . ?
C1 C6 1.394(3) . ?
C1 C2 1.395(3) . ?
C2 C3 1.395(3) . ?
C2 H2 0.9500 . ?
C3 C4 1.382(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.388(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.382(3) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C8 1.393(3) . ?
C7 C12 1.398(3) . ?
C8 C9 1.399(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.389(4) . ?
C9 H9 0.9500 . ?
C10 C11 1.384(4) . ?
C10 H10 0.9500 . ?
C11 C12 1.391(3) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 C14 1.455(3) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.443(4) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 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
N1 Cu1 P1 124.59(6) . . ?
N1 Cu1 I1 106.81(6) . . ?
P1 Cu1 I1 106.114(18) . . ?
N1 Cu1 I1 104.75(6) . 2_656 ?
P1 Cu1 I1 104.369(17) . 2_656 ?
I1 Cu1 I1 109.697(10) . 2_656 ?
O1 P1 C7 100.77(9) . . ?
O1 P1 C1 100.28(8) . . ?
C7 P1 C1 102.75(10) . . ?
O1 P1 Cu1 116.33(7) . . ?
C7 P1 Cu1 116.33(8) . . ?
C1 P1 Cu1 117.66(8) . . ?
P1 O1 P1 124.31(14) . 2_656 ?
C13 N1 Cu1 175.8(2) . . ?
C6 C1 C2 119.4(2) . . ?
C6 C1 P1 117.64(17) . . ?
C2 C1 P1 122.99(16) . . ?
C3 C2 C1 119.9(2) . . ?
C3 C2 H2 120.1 . . ?
C1 C2 H2 120.1 . . ?
C4 C3 C2 120.0(2) . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
C3 C4 C5 120.3(2) . . ?
C3 C4 H4 119.8 . . ?
C5 C4 H4 119.8 . . ?
C6 C5 C4 119.8(2) . . ?
C6 C5 H5 120.1 . . ?
C4 C5 H5 120.1 . . ?
C5 C6 C1 120.5(2) . . ?
C5 C6 H6 119.7 . . ?
C1 C6 H6 119.7 . . ?
C8 C7 C12 119.4(2) . . ?
C8 C7 P1 122.74(17) . . ?
C12 C7 P1 117.88(18) . . ?
C7 C8 C9 120.4(2) . . ?
C7 C8 H8 119.8 . . ?
C9 C8 H8 119.8 . . ?
C10 C9 C8 119.6(2) . . ?
C10 C9 H9 120.2 . . ?
C8 C9 H9 120.2 . . ?
C11 C10 C9 120.3(2) . . ?
C11 C10 H10 119.8 . . ?
C9 C10 H10 119.8 . . ?
C10 C11 C12 120.2(2) . . ?
C10 C11 H11 119.9 . . ?
C12 C11 H11 119.9 . . ?
C11 C12 C7 120.1(2) . . ?
C11 C12 H12 119.9 . . ?
C7 C12 H12 119.9 . . ?
N1 C13 C14 179.0(3) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N2 C15 C16 179.4(4) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?

_refine_diff_density_max         1.082
_refine_diff_density_min         -0.995
_refine_diff_density_rms         0.144

_shelxl_version_number           2014-3


####################################################################### 
# 
# 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_7
_database_code_depnum_ccdc_archive 'CCDC 1481881'
_audit_update_record             
;
2016-06-21 deposited with the CCDC.
2016-07-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C54 H45 Cl Cu O6 P3 Si3'
_chemical_formula_weight         1066.07

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      cubic
_space_group_IT_number           205
_space_group_name_H-M_alt        'P a -3'
_space_group_name_Hall           '-P 2ac 2ab 3'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'
'-z, -x, -y'
'-z-1/2, x-1/2, y'
'z-1/2, x, -y-1/2'
'z, -x-1/2, y-1/2'
'-y, -z, -x'
'y, -z-1/2, x-1/2'
'-y-1/2, z-1/2, x'
'y-1/2, z, -x-1/2'

_cell_length_a                   22.2970(4)
_cell_length_b                   22.2970(4)
_cell_length_c                   22.2970(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     11085.1(6)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    119259
_cell_measurement_theta_min      3.17
_cell_measurement_theta_max      25.68

_exptl_crystal_description       irregular
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.278
_exptl_crystal_F_000             4400
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.17
_exptl_absorpt_coefficient_mu    0.640
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.745
_exptl_absorpt_correction_T_max  0.897
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_special_details           'crystal-to-detector distance 35 mm'
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method       
'two φ and one ω scans with 2° steps (190 frames)'
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            119259
_diffrn_reflns_av_unetI/netI     0.0358
_diffrn_reflns_av_R_equivalents  0.0267
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.165
_diffrn_reflns_theta_max         25.675
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             3506
_reflns_number_gt                2617
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  
'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)'

_refine_special_details          
;
 Structure solved by intrinsic phasing and subsequent difference Fourier
 synthesis. All non-hydrogen atoms were refined with anisotropic
 displacement parameters. The H atoms were introduced at calculated
 positions and were treated as riding atoms with an isotropic displacement
 parameter equal to 1.2 times that of the parent atom. Some voids in the
 lattice indicate the presence of unresolved solvent molecules, but,
 the residual electronic density in these voids being quite low, the SQUEEZE
 software did not improve the data. The solvent may have at least partially 
 left the lattice, as suggested by the partly opaque aspect of all crystals.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0626P)²+6.1654P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3506
_refine_ls_number_parameters     205
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0680
_refine_ls_R_factor_gt           0.0469
_refine_ls_wR_factor_ref         0.1297
_refine_ls_wR_factor_gt          0.1234
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_restrained_S_all      1.099
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.74005(2) 0.74005(2) 0.74005(2) 0.0388(2) Uani 1 3 d S T P . .
Cl1 Cl 0.79966(4) 0.79966(4) 0.79966(4) 0.0513(4) Uani 1 3 d S T P . .
P1 P 0.71782(4) 0.65960(4) 0.79717(3) 0.0393(2) Uani 1 1 d . . . . .
Si1 Si 0.64003(4) 0.59603(4) 0.70498(4) 0.0402(2) Uani 1 1 d . . . . .
O1 O 0.67501(10) 0.60859(9) 0.76773(9) 0.0448(5) Uani 1 1 d . . . . .
O2 O 0.68914(9) 0.59357(9) 0.65045(9) 0.0421(5) Uani 1 1 d . . . . .
C1 C 0.60095(14) 0.52464(14) 0.71657(14) 0.0447(8) Uani 1 1 d . . . . .
C2 C 0.63112(17) 0.47605(16) 0.74256(18) 0.0615(10) Uani 1 1 d . . . . .
H2 H 0.6723 0.4802 0.7526 0.074 Uiso 1 1 calc R U . . .
C3 C 0.60242(19) 0.42189(17) 0.7540(2) 0.0693(11) Uani 1 1 d . . . . .
H3 H 0.6242 0.3891 0.7703 0.083 Uiso 1 1 calc R U . . .
C4 C 0.54293(19) 0.41629(17) 0.74182(19) 0.0682(11) Uani 1 1 d . . . . .
H4 H 0.5230 0.3795 0.7501 0.082 Uiso 1 1 calc R U . . .
C5 C 0.51208(18) 0.46252(17) 0.7181(2) 0.0699(11) Uani 1 1 d . . . . .
H5 H 0.4705 0.4582 0.7101 0.084 Uiso 1 1 calc R U . . .
C6 C 0.54055(16) 0.51638(16) 0.70523(17) 0.0591(9) Uani 1 1 d . . . . .
H6 H 0.5180 0.5483 0.6882 0.071 Uiso 1 1 calc R U . . .
C7 C 0.78309(14) 0.61476(13) 0.81638(14) 0.0417(7) Uani 1 1 d . . . . .
C8 C 0.79889(16) 0.56514(14) 0.78220(16) 0.0516(8) Uani 1 1 d . . . . .
H8 H 0.7744 0.5533 0.7494 0.062 Uiso 1 1 calc R U . . .
C9 C 0.85014(16) 0.53302(16) 0.79582(18) 0.0606(10) Uani 1 1 d . . . . .
H9 H 0.8609 0.4991 0.7723 0.073 Uiso 1 1 calc R U . . .
C10 C 0.88580(17) 0.55012(17) 0.84366(19) 0.0641(10) Uani 1 1 d . . . . .
H10 H 0.9202 0.5272 0.8540 0.077 Uiso 1 1 calc R U . . .
C11 C 0.87113(16) 0.60059(17) 0.87626(17) 0.0584(9) Uani 1 1 d . . . . .
H11 H 0.8964 0.6135 0.9081 0.070 Uiso 1 1 calc R U . . .
C12 C 0.81994(15) 0.63227(15) 0.86276(15) 0.0496(8) Uani 1 1 d . . . . .
H12 H 0.8099 0.6667 0.8857 0.060 Uiso 1 1 calc R U . . .
C13 C 0.68242(14) 0.66884(14) 0.87008(13) 0.0420(7) Uani 1 1 d . . . . .
C14 C 0.65820(19) 0.61991(17) 0.89956(16) 0.0671(11) Uani 1 1 d . . . . .
H14 H 0.6594 0.5814 0.8814 0.081 Uiso 1 1 calc R U . . .
C15 C 0.6321(2) 0.6270(2) 0.95572(19) 0.0859(14) Uani 1 1 d . . . . .
H15 H 0.6157 0.5932 0.9760 0.103 Uiso 1 1 calc R U . . .
C16 C 0.62986(19) 0.68265(19) 0.98196(17) 0.0697(11) Uani 1 1 d . . . . .
H16 H 0.6116 0.6874 1.0202 0.084 Uiso 1 1 calc R U . . .
C17 C 0.65393(16) 0.73150(17) 0.95326(15) 0.0544(9) Uani 1 1 d . . . . .
H17 H 0.6527 0.7699 0.9718 0.065 Uiso 1 1 calc R U . . .
C18 C 0.68023(15) 0.72469(15) 0.89672(14) 0.0473(8) Uani 1 1 d . . . . .
H18 H 0.6966 0.7585 0.8766 0.057 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 P1 2.2550(8) . ?
Cu1 P1 2.2550(8) 9 ?
Cu1 P1 2.2550(8) 5 ?
Cu1 Cl1 2.3022(15) . ?
P1 O1 1.623(2) . ?
P1 C7 1.817(3) . ?
P1 C13 1.819(3) . ?
Si1 O1 1.626(2) . ?
Si1 O2 1.634(2) 9 ?
Si1 O2 1.637(2) . ?
Si1 C1 1.833(3) . ?
O2 Si1 1.634(2) 5 ?
C1 C6 1.383(5) . ?
C1 C2 1.401(5) . ?
C2 C3 1.390(5) . ?
C2 H2 0.9500 . ?
C3 C4 1.360(6) . ?
C3 H3 0.9500 . ?
C4 C5 1.347(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.388(5) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C12 1.377(5) . ?
C7 C8 1.389(4) . ?
C8 C9 1.382(5) . ?
C8 H8 0.9500 . ?
C9 C10 1.384(5) . ?
C9 H9 0.9500 . ?
C10 C11 1.379(5) . ?
C10 H10 0.9500 . ?
C11 C12 1.376(5) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 C18 1.381(5) . ?
C13 C14 1.384(5) . ?
C14 C15 1.390(5) . ?
C14 H14 0.9500 . ?
C15 C16 1.373(6) . ?
C15 H15 0.9500 . ?
C16 C17 1.373(5) . ?
C16 H16 0.9500 . ?
C17 C18 1.399(5) . ?
C17 H17 0.9500 . ?
C18 H18 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
P1 Cu1 P1 113.48(2) . 9 ?
P1 Cu1 P1 113.49(2) . 5 ?
P1 Cu1 P1 113.48(2) 9 5 ?
P1 Cu1 Cl1 105.08(3) . . ?
P1 Cu1 Cl1 105.08(3) 9 . ?
P1 Cu1 Cl1 105.08(3) 5 . ?
O1 P1 C7 100.41(13) . . ?
O1 P1 C13 100.70(13) . . ?
C7 P1 C13 101.49(14) . . ?
O1 P1 Cu1 117.27(8) . . ?
C7 P1 Cu1 113.25(10) . . ?
C13 P1 Cu1 120.67(11) . . ?
O1 Si1 O2 111.23(11) . 9 ?
O1 Si1 O2 108.90(12) . . ?
O2 Si1 O2 106.75(14) 9 . ?
O1 Si1 C1 104.85(13) . . ?
O2 Si1 C1 111.96(13) 9 . ?
O2 Si1 C1 113.18(13) . . ?
P1 O1 Si1 138.64(14) . . ?
Si1 O2 Si1 132.44(14) 5 . ?
C6 C1 C2 116.1(3) . . ?
C6 C1 Si1 123.6(3) . . ?
C2 C1 Si1 120.1(3) . . ?
C3 C2 C1 121.8(4) . . ?
C3 C2 H2 119.1 . . ?
C1 C2 H2 119.1 . . ?
C4 C3 C2 119.5(4) . . ?
C4 C3 H3 120.3 . . ?
C2 C3 H3 120.3 . . ?
C5 C4 C3 120.4(4) . . ?
C5 C4 H4 119.8 . . ?
C3 C4 H4 119.8 . . ?
C4 C5 C6 120.6(4) . . ?
C4 C5 H5 119.7 . . ?
C6 C5 H5 119.7 . . ?
C1 C6 C5 121.5(3) . . ?
C1 C6 H6 119.2 . . ?
C5 C6 H6 119.2 . . ?
C12 C7 C8 119.1(3) . . ?
C12 C7 P1 119.9(2) . . ?
C8 C7 P1 120.8(2) . . ?
C9 C8 C7 120.1(3) . . ?
C9 C8 H8 119.9 . . ?
C7 C8 H8 119.9 . . ?
C8 C9 C10 120.1(3) . . ?
C8 C9 H9 120.0 . . ?
C10 C9 H9 120.0 . . ?
C11 C10 C9 119.7(3) . . ?
C11 C10 H10 120.2 . . ?
C9 C10 H10 120.2 . . ?
C12 C11 C10 120.0(3) . . ?
C12 C11 H11 120.0 . . ?
C10 C11 H11 120.0 . . ?
C11 C12 C7 120.9(3) . . ?
C11 C12 H12 119.5 . . ?
C7 C12 H12 119.5 . . ?
C18 C13 C14 119.5(3) . . ?
C18 C13 P1 120.1(2) . . ?
C14 C13 P1 120.3(3) . . ?
C13 C14 C15 120.2(4) . . ?
C13 C14 H14 119.9 . . ?
C15 C14 H14 119.9 . . ?
C16 C15 C14 120.1(4) . . ?
C16 C15 H15 120.0 . . ?
C14 C15 H15 120.0 . . ?
C17 C16 C15 120.3(3) . . ?
C17 C16 H16 119.9 . . ?
C15 C16 H16 119.9 . . ?
C16 C17 C18 119.9(3) . . ?
C16 C17 H17 120.1 . . ?
C18 C17 H17 120.1 . . ?
C13 C18 C17 120.0(3) . . ?
C13 C18 H18 120.0 . . ?
C17 C18 H18 120.0 . . ?

_refine_diff_density_max         0.316
_refine_diff_density_min         -0.368
_refine_diff_density_rms         0.065

_shelxl_version_number           2014-3



