# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2013

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
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#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
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#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
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data_bg237
#TrackingRef '2013_bousrez_dalton trans.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C26 H22 Zr, 1/2(C4 H8 O)'
_chemical_formula_sum            'C28 H26 O0.50 Zr'
_chemical_formula_weight         461.71

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'
Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P-1 '
_symmetry_space_group_name_Hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   13.136(1)
_cell_length_b                   13.406(1)
_cell_length_c                   13.761(1)
_cell_angle_alpha                115.669(1)
_cell_angle_beta                 95.441(1)
_cell_angle_gamma                95.918(1)
_cell_volume                     2146.1(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    150.0(1)
_cell_measurement_reflns_used    309
_cell_measurement_theta_min      0.998
_cell_measurement_theta_max      30.034

_exptl_crystal_description       Block
_exptl_crystal_colour            Orange
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.429
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             952
_exptl_absorpt_coefficient_mu    0.526
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8170
_exptl_absorpt_correction_T_max  0.9492
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1996)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150.0(1)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            23820
_diffrn_reflns_av_R_equivalents  0.0348
_diffrn_reflns_av_sigmaI/netI    0.0371
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.00
_diffrn_reflns_theta_max         30.03
_reflns_number_total             12382
_reflns_number_gt                10938
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_cell_refinement       'DENZO (Otwinowski & Minor, 1997) & COLLECT'
_computing_data_reduction        'DENZO & COLLECT'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  'PLATON (Spek, 2009)'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+3.0712P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         12382
_refine_ls_number_parameters     532
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0448
_refine_ls_R_factor_gt           0.0375
_refine_ls_wR_factor_ref         0.0841
_refine_ls_wR_factor_gt          0.0789
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_restrained_S_all      1.082
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zr1 Zr 0.166945(14) 0.732926(15) 0.438048(15) 0.01785(5) Uani 1 1 d . . .
C1 C 0.25334(17) 0.53404(18) 0.16884(17) 0.0264(4) Uani 1 1 d . . .
H1 H 0.1831 0.5402 0.1780 0.032 Uiso 1 1 calc R . .
C2 C 0.27535(19) 0.4495(2) 0.07382(18) 0.0304(5) Uani 1 1 d . . .
H2 H 0.2204 0.3990 0.0191 0.036 Uiso 1 1 calc R . .
C3 C 0.3771(2) 0.4387(2) 0.05866(19) 0.0320(5) Uani 1 1 d . . .
H3 H 0.3922 0.3812 -0.0064 0.038 Uiso 1 1 calc R . .
C4 C 0.45664(18) 0.51253(19) 0.13916(19) 0.0303(5) Uani 1 1 d . . .
H4 H 0.5266 0.5054 0.1293 0.036 Uiso 1 1 calc R . .
C5 C 0.43485(16) 0.59702(18) 0.23423(18) 0.0258(4) Uani 1 1 d . . .
H5 H 0.4904 0.6468 0.2887 0.031 Uiso 1 1 calc R . .
C6 C 0.33231(15) 0.61038(16) 0.25147(15) 0.0206(4) Uani 1 1 d . . .
C7 C 0.30569(15) 0.69701(16) 0.35250(16) 0.0203(4) Uani 1 1 d . . .
C8 C 0.37814(15) 0.78336(17) 0.42625(16) 0.0214(4) Uani 1 1 d . . .
H8 H 0.4449 0.7899 0.4064 0.026 Uiso 1 1 calc R . .
C9 C 0.36287(16) 0.86774(17) 0.53413(16) 0.0230(4) Uani 1 1 d . . .
H9 H 0.4208 0.9236 0.5770 0.028 Uiso 1 1 calc R . .
C10 C 0.27411(16) 0.87365(16) 0.57841(16) 0.0217(4) Uani 1 1 d . . .
C11 C 0.26993(17) 0.95626(17) 0.69088(17) 0.0241(4) Uani 1 1 d . . .
C12 C 0.35743(17) 1.02836(18) 0.76335(17) 0.0268(4) Uani 1 1 d . . .
H12 H 0.4231 1.0250 0.7396 0.032 Uiso 1 1 calc R . .
C13 C 0.35012(19) 1.10456(19) 0.86912(18) 0.0316(5) Uani 1 1 d . . .
H13 H 0.4106 1.1521 0.9168 0.038 Uiso 1 1 calc R . .
C14 C 0.2551(2) 1.1116(2) 0.90554(19) 0.0349(5) Uani 1 1 d . . .
H14 H 0.2501 1.1644 0.9776 0.042 Uiso 1 1 calc R . .
C15 C 0.1678(2) 1.0412(2) 0.8363(2) 0.0402(6) Uani 1 1 d . . .
H15 H 0.1024 1.0452 0.8608 0.048 Uiso 1 1 calc R . .
C16 C 0.17553(19) 0.9642(2) 0.73051(19) 0.0339(5) Uani 1 1 d . . .
H16 H 0.1149 0.9158 0.6840 0.041 Uiso 1 1 calc R . .
C17 C 0.0466(2) 0.5952(3) 0.4667(4) 0.0641(11) Uani 1 1 d . . .
H17 H -0.0258 0.5929 0.4511 0.077 Uiso 1 1 calc R . .
C18 C 0.1065(3) 0.6579(2) 0.5642(3) 0.0515(8) Uani 1 1 d . . .
H18 H 0.0834 0.7079 0.6284 0.062 Uiso 1 1 calc R . .
C19 C 0.2069(3) 0.6377(3) 0.5557(3) 0.0578(10) Uani 1 1 d . . .
H19 H 0.2650 0.6705 0.6122 0.069 Uiso 1 1 calc R . .
C20 C 0.2064(3) 0.5601(3) 0.4485(4) 0.0690(13) Uani 1 1 d . . .
H20 H 0.2645 0.5294 0.4181 0.083 Uiso 1 1 calc R . .
C21 C 0.1066(4) 0.5358(2) 0.3943(3) 0.0720(14) Uani 1 1 d . . .
H21 H 0.0838 0.4860 0.3194 0.086 Uiso 1 1 calc R . .
C22 C 0.12441(19) 0.7924(3) 0.2918(2) 0.0389(6) Uani 1 1 d . . .
H22 H 0.1692 0.7798 0.2388 0.047 Uiso 1 1 calc R . .
C23 C 0.13249(19) 0.8887(2) 0.3907(2) 0.0391(6) Uani 1 1 d . . .
H23 H 0.1843 0.9531 0.4167 0.047 Uiso 1 1 calc R . .
C24 C 0.0517(2) 0.8746(2) 0.4450(2) 0.0357(5) Uani 1 1 d . . .
H24 H 0.0392 0.9274 0.5140 0.043 Uiso 1 1 calc R . .
C25 C -0.00698(17) 0.7694(2) 0.3801(2) 0.0321(5) Uani 1 1 d . . .
H25 H -0.0670 0.7384 0.3972 0.039 Uiso 1 1 calc R . .
C26 C 0.03711(19) 0.7167(2) 0.2851(2) 0.0349(5) Uani 1 1 d . . .
H26 H 0.0130 0.6439 0.2272 0.042 Uiso 1 1 calc R . .
Zr2 Zr 0.307422(14) 0.189057(15) 0.309097(15) 0.01739(5) Uani 1 1 d . . .
C27 C 0.36725(18) -0.05766(19) 0.05851(18) 0.0281(4) Uani 1 1 d . . .
H27 H 0.3663 0.0157 0.0650 0.034 Uiso 1 1 calc R . .
C28 C 0.37364(19) -0.1443(2) -0.04266(19) 0.0332(5) Uani 1 1 d . . .
H28 H 0.3772 -0.1296 -0.1040 0.040 Uiso 1 1 calc R . .
C29 C 0.37479(18) -0.2523(2) -0.0540(2) 0.0334(5) Uani 1 1 d . . .
H29 H 0.3796 -0.3117 -0.1227 0.040 Uiso 1 1 calc R . .
C30 C 0.36877(19) -0.27244(18) 0.0363(2) 0.0332(5) Uani 1 1 d . . .
H30 H 0.3690 -0.3462 0.0291 0.040 Uiso 1 1 calc R . .
C31 C 0.36235(18) -0.18576(18) 0.13709(19) 0.0287(4) Uani 1 1 d . . .
H31 H 0.3580 -0.2012 0.1978 0.034 Uiso 1 1 calc R . .
C32 C 0.36220(15) -0.07544(16) 0.15105(17) 0.0224(4) Uani 1 1 d . . .
C33 C 0.35299(15) 0.01819(16) 0.25591(16) 0.0209(4) Uani 1 1 d . . .
C34 C 0.37008(16) 0.01166(17) 0.35186(17) 0.0237(4) Uani 1 1 d . . .
H34 H 0.3944 -0.0534 0.3499 0.028 Uiso 1 1 calc R . .
C35 C 0.35403(16) 0.09696(17) 0.45807(17) 0.0228(4) Uani 1 1 d . . .
H35 H 0.3696 0.0832 0.5196 0.027 Uiso 1 1 calc R . .
C36 C 0.31871(15) 0.19379(17) 0.47542(16) 0.0212(4) Uani 1 1 d . . .
C37 C 0.29407(15) 0.27065(17) 0.58238(16) 0.0217(4) Uani 1 1 d . . .
C38 C 0.28546(18) 0.2408(2) 0.66755(17) 0.0279(4) Uani 1 1 d . . .
H38 H 0.2972 0.1684 0.6576 0.034 Uiso 1 1 calc R . .
C39 C 0.26009(19) 0.3151(2) 0.76614(18) 0.0333(5) Uani 1 1 d . . .
H39 H 0.2556 0.2931 0.8228 0.040 Uiso 1 1 calc R . .
C40 C 0.2414(2) 0.4202(2) 0.78299(18) 0.0348(5) Uani 1 1 d . . .
H40 H 0.2244 0.4707 0.8508 0.042 Uiso 1 1 calc R . .
C41 C 0.2476(2) 0.4513(2) 0.69955(19) 0.0358(5) Uani 1 1 d . . .
H41 H 0.2344 0.5233 0.7098 0.043 Uiso 1 1 calc R . .
C42 C 0.27330(19) 0.37715(18) 0.60101(18) 0.0298(5) Uani 1 1 d . . .
H42 H 0.2769 0.3995 0.5445 0.036 Uiso 1 1 calc R . .
C43 C 0.15357(18) 0.2211(2) 0.2096(2) 0.0348(5) Uani 1 1 d . . .
H43 H 0.1642 0.2720 0.1790 0.042 Uiso 1 1 calc R . .
C44 C 0.13333(17) 0.2482(2) 0.3158(2) 0.0329(5) Uani 1 1 d . . .
H44 H 0.1290 0.3210 0.3702 0.040 Uiso 1 1 calc R . .
C45 C 0.12065(16) 0.1490(2) 0.32794(19) 0.0292(4) Uani 1 1 d . . .
H45 H 0.1052 0.1425 0.3912 0.035 Uiso 1 1 calc R . .
C46 C 0.13496(17) 0.06097(19) 0.22914(19) 0.0300(5) Uani 1 1 d . . .
H46 H 0.1315 -0.0155 0.2142 0.036 Uiso 1 1 calc R . .
C47 C 0.15521(18) 0.1056(2) 0.15677(19) 0.0335(5) Uani 1 1 d . . .
H47 H 0.1679 0.0646 0.0842 0.040 Uiso 1 1 calc R . .
C48 C 0.48535(17) 0.30393(19) 0.39459(19) 0.0290(4) Uani 1 1 d . . .
H48 H 0.5177 0.3041 0.4594 0.035 Uiso 1 1 calc R . .
C49 C 0.42121(18) 0.37972(18) 0.38910(19) 0.0296(4) Uani 1 1 d . . .
H49 H 0.4028 0.4400 0.4497 0.036 Uiso 1 1 calc R . .
C50 C 0.38914(17) 0.35103(19) 0.2790(2) 0.0295(5) Uani 1 1 d . . .
H50 H 0.3456 0.3886 0.2519 0.035 Uiso 1 1 calc R . .
C51 C 0.43282(18) 0.2567(2) 0.21558(19) 0.0304(5) Uani 1 1 d . . .
H51 H 0.4234 0.2189 0.1381 0.036 Uiso 1 1 calc R . .
C52 C 0.49315(17) 0.22781(19) 0.2872(2) 0.0300(5) Uani 1 1 d . . .
H52 H 0.5320 0.1678 0.2666 0.036 Uiso 1 1 calc R . .
O1 O 0.0319(2) 0.5923(2) 0.8695(2) 0.0742(8) Uani 1 1 d . . .
C53 C 0.0849(3) 0.6832(4) 0.8554(3) 0.0648(10) Uani 1 1 d . . .
H53A H 0.0503 0.6869 0.7902 0.078 Uiso 1 1 calc R . .
H53B H 0.1577 0.6735 0.8465 0.078 Uiso 1 1 calc R . .
C54 C 0.0805(2) 0.7906(3) 0.9596(3) 0.0530(8) Uani 1 1 d . . .
H54A H 0.1501 0.8242 1.0036 0.064 Uiso 1 1 calc R . .
H54B H 0.0513 0.8469 0.9416 0.064 Uiso 1 1 calc R . .
C55 C 0.0102(3) 0.7492(3) 1.0190(2) 0.0480(7) Uani 1 1 d . . .
H55A H 0.0299 0.7928 1.0990 0.058 Uiso 1 1 calc R . .
H55B H -0.0631 0.7529 0.9982 0.058 Uiso 1 1 calc R . .
C56 C 0.0275(3) 0.6311(3) 0.9812(3) 0.0594(9) Uani 1 1 d . . .
H56A H 0.0932 0.6275 1.0204 0.071 Uiso 1 1 calc R . .
H56B H -0.0302 0.5861 0.9931 0.071 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Zr1 0.01613(8) 0.01713(8) 0.02126(9) 0.00937(7) 0.00370(6) 0.00250(6)
C1 0.0222(10) 0.0298(10) 0.0248(10) 0.0100(8) 0.0036(8) 0.0042(8)
C2 0.0309(11) 0.0307(11) 0.0239(10) 0.0076(9) 0.0035(8) 0.0034(9)
C3 0.0395(13) 0.0307(11) 0.0263(10) 0.0109(9) 0.0129(9) 0.0094(10)
C4 0.0267(11) 0.0319(11) 0.0354(12) 0.0154(9) 0.0130(9) 0.0089(9)
C5 0.0209(9) 0.0278(10) 0.0284(10) 0.0118(8) 0.0058(8) 0.0043(8)
C6 0.0218(9) 0.0221(9) 0.0196(9) 0.0108(7) 0.0042(7) 0.0028(7)
C7 0.0196(9) 0.0230(9) 0.0213(9) 0.0123(7) 0.0037(7) 0.0043(7)
C8 0.0174(8) 0.0250(9) 0.0239(9) 0.0125(8) 0.0034(7) 0.0047(7)
C9 0.0214(9) 0.0227(9) 0.0226(9) 0.0089(7) -0.0006(7) 0.0024(7)
C10 0.0218(9) 0.0200(9) 0.0230(9) 0.0095(7) 0.0013(7) 0.0037(7)
C11 0.0263(10) 0.0214(9) 0.0234(9) 0.0086(8) 0.0036(8) 0.0055(8)
C12 0.0246(10) 0.0266(10) 0.0262(10) 0.0092(8) 0.0023(8) 0.0050(8)
C13 0.0334(12) 0.0285(11) 0.0250(10) 0.0065(9) -0.0011(9) 0.0025(9)
C14 0.0390(13) 0.0304(11) 0.0276(11) 0.0053(9) 0.0068(9) 0.0072(10)
C15 0.0319(13) 0.0440(14) 0.0345(13) 0.0069(11) 0.0128(10) 0.0053(11)
C16 0.0256(11) 0.0345(12) 0.0320(11) 0.0065(9) 0.0060(9) 0.0018(9)
C17 0.0351(15) 0.077(2) 0.110(3) 0.078(2) -0.0038(17) -0.0136(15)
C18 0.082(2) 0.0372(14) 0.0554(17) 0.0309(13) 0.0434(17) 0.0173(15)
C19 0.0519(18) 0.064(2) 0.075(2) 0.0595(19) -0.0228(16) -0.0185(15)
C20 0.086(3) 0.059(2) 0.124(3) 0.076(2) 0.078(3) 0.055(2)
C21 0.144(4) 0.0237(13) 0.0390(16) 0.0164(12) -0.002(2) -0.0217(18)
C22 0.0269(11) 0.0677(18) 0.0454(14) 0.0428(14) 0.0121(10) 0.0195(12)
C23 0.0263(11) 0.0373(13) 0.0637(17) 0.0364(13) -0.0089(11) -0.0019(9)
C24 0.0359(13) 0.0306(11) 0.0402(13) 0.0145(10) 0.0005(10) 0.0157(10)
C25 0.0172(9) 0.0387(12) 0.0456(13) 0.0233(11) 0.0041(9) 0.0059(9)
C26 0.0319(12) 0.0372(12) 0.0308(11) 0.0130(10) -0.0069(9) 0.0066(10)
Zr2 0.01720(9) 0.01700(8) 0.01968(9) 0.00934(7) 0.00387(6) 0.00378(6)
C27 0.0308(11) 0.0260(10) 0.0301(11) 0.0130(9) 0.0096(9) 0.0084(8)
C28 0.0359(12) 0.0328(12) 0.0302(11) 0.0113(9) 0.0128(9) 0.0081(10)
C29 0.0278(11) 0.0277(11) 0.0353(12) 0.0049(9) 0.0101(9) 0.0026(9)
C30 0.0341(12) 0.0188(9) 0.0417(13) 0.0079(9) 0.0105(10) 0.0046(8)
C31 0.0311(11) 0.0211(9) 0.0348(11) 0.0123(9) 0.0092(9) 0.0052(8)
C32 0.0193(9) 0.0202(9) 0.0288(10) 0.0105(8) 0.0077(7) 0.0061(7)
C33 0.0181(8) 0.0197(8) 0.0265(9) 0.0109(7) 0.0069(7) 0.0037(7)
C34 0.0212(9) 0.0205(9) 0.0321(10) 0.0137(8) 0.0057(8) 0.0044(7)
C35 0.0232(9) 0.0236(9) 0.0243(9) 0.0139(8) 0.0037(7) 0.0011(7)
C36 0.0198(9) 0.0226(9) 0.0218(9) 0.0113(7) 0.0024(7) 0.0001(7)
C37 0.0191(9) 0.0239(9) 0.0203(9) 0.0097(7) 0.0002(7) -0.0009(7)
C38 0.0295(11) 0.0331(11) 0.0252(10) 0.0166(9) 0.0032(8) 0.0062(9)
C39 0.0355(12) 0.0443(13) 0.0215(10) 0.0166(10) 0.0039(9) 0.0052(10)
C40 0.0355(12) 0.0372(12) 0.0211(10) 0.0048(9) 0.0038(9) 0.0005(10)
C41 0.0459(14) 0.0268(11) 0.0305(12) 0.0081(9) 0.0094(10) 0.0070(10)
C42 0.0398(13) 0.0253(10) 0.0245(10) 0.0110(8) 0.0072(9) 0.0048(9)
C43 0.0259(11) 0.0405(13) 0.0481(14) 0.0308(11) -0.0022(10) 0.0045(9)
C44 0.0201(10) 0.0282(11) 0.0441(13) 0.0096(10) 0.0033(9) 0.0090(8)
C45 0.0189(9) 0.0380(12) 0.0315(11) 0.0163(9) 0.0059(8) 0.0027(8)
C46 0.0227(10) 0.0234(10) 0.0383(12) 0.0111(9) -0.0028(9) -0.0007(8)
C47 0.0250(11) 0.0429(13) 0.0264(11) 0.0112(10) -0.0021(8) 0.0047(9)
C48 0.0221(10) 0.0333(11) 0.0343(11) 0.0209(9) -0.0020(8) -0.0042(8)
C49 0.0280(11) 0.0210(9) 0.0364(12) 0.0102(9) 0.0080(9) -0.0012(8)
C50 0.0248(10) 0.0286(10) 0.0447(13) 0.0260(10) 0.0039(9) 0.0018(8)
C51 0.0321(11) 0.0329(11) 0.0298(11) 0.0175(9) 0.0102(9) -0.0007(9)
C52 0.0221(10) 0.0286(10) 0.0480(13) 0.0228(10) 0.0141(9) 0.0071(8)
O1 0.098(2) 0.0445(13) 0.0530(14) -0.0009(11) 0.0006(14) 0.0098(14)
C53 0.0420(17) 0.098(3) 0.0464(18) 0.0230(19) 0.0092(14) 0.0165(18)
C54 0.0365(15) 0.0454(16) 0.067(2) 0.0193(15) -0.0058(14) 0.0029(12)
C55 0.0515(17) 0.0489(16) 0.0384(14) 0.0151(12) -0.0021(12) 0.0147(14)
C56 0.068(2) 0.0461(17) 0.0563(19) 0.0193(15) -0.0078(16) 0.0095(16)

_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
Zr1 C7 2.2442(19) . ?
Zr1 C10 2.248(2) . ?
Zr1 C21 2.465(3) . ?
Zr1 C20 2.486(3) . ?
Zr1 C17 2.492(3) . ?
Zr1 C26 2.496(2) . ?
Zr1 C22 2.502(2) . ?
Zr1 C18 2.503(2) . ?
Zr1 C19 2.509(3) . ?
Zr1 C23 2.512(2) . ?
Zr1 C25 2.514(2) . ?
Zr1 C24 2.523(2) . ?
C1 C2 1.390(3) . ?
C1 C6 1.402(3) . ?
C1 H1 0.9500 . ?
C2 C3 1.385(3) . ?
C2 H2 0.9500 . ?
C3 C4 1.384(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.389(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.406(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.477(3) . ?
C7 C8 1.359(3) . ?
C8 C9 1.474(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.360(3) . ?
C9 H9 0.9500 . ?
C10 C11 1.473(3) . ?
C11 C16 1.397(3) . ?
C11 C12 1.403(3) . ?
C12 C13 1.389(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.385(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.380(4) . ?
C14 H14 0.9500 . ?
C15 C16 1.394(3) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C17 C18 1.346(5) . ?
C17 C21 1.356(6) . ?
C17 H17 0.9500 . ?
C18 C19 1.379(5) . ?
C18 H18 0.9500 . ?
C19 C20 1.387(5) . ?
C19 H19 0.9500 . ?
C20 C21 1.378(6) . ?
C20 H20 0.9500 . ?
C21 H21 0.9500 . ?
C22 C23 1.397(4) . ?
C22 C26 1.418(4) . ?
C22 H22 0.9500 . ?
C23 C24 1.397(4) . ?
C23 H23 0.9500 . ?
C24 C25 1.391(3) . ?
C24 H24 0.9500 . ?
C25 C26 1.403(3) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
Zr2 C33 2.2482(19) . ?
Zr2 C36 2.2522(19) . ?
Zr2 C44 2.493(2) . ?
Zr2 C51 2.509(2) . ?
Zr2 C43 2.511(2) . ?
Zr2 C52 2.515(2) . ?
Zr2 C45 2.519(2) . ?
Zr2 C47 2.521(2) . ?
Zr2 C46 2.526(2) . ?
Zr2 C48 2.527(2) . ?
Zr2 C50 2.534(2) . ?
Zr2 C49 2.538(2) . ?
C27 C28 1.391(3) . ?
C27 C32 1.399(3) . ?
C27 H27 0.9500 . ?
C28 C29 1.390(3) . ?
C28 H28 0.9500 . ?
C29 C30 1.388(4) . ?
C29 H29 0.9500 . ?
C30 C31 1.388(3) . ?
C30 H30 0.9500 . ?
C31 C32 1.407(3) . ?
C31 H31 0.9500 . ?
C32 C33 1.472(3) . ?
C33 C34 1.360(3) . ?
C34 C35 1.466(3) . ?
C34 H34 0.9500 . ?
C35 C36 1.354(3) . ?
C35 H35 0.9500 . ?
C36 C37 1.476(3) . ?
C37 C42 1.398(3) . ?
C37 C38 1.403(3) . ?
C38 C39 1.388(3) . ?
C38 H38 0.9500 . ?
C39 C40 1.379(4) . ?
C39 H39 0.9500 . ?
C40 C41 1.387(3) . ?
C40 H40 0.9500 . ?
C41 C42 1.389(3) . ?
C41 H41 0.9500 . ?
C42 H42 0.9500 . ?
C43 C47 1.400(4) . ?
C43 C44 1.405(4) . ?
C43 H43 0.9500 . ?
C44 C45 1.405(3) . ?
C44 H44 0.9500 . ?
C45 C46 1.407(3) . ?
C45 H45 0.9500 . ?
C46 C47 1.398(3) . ?
C46 H46 0.9500 . ?
C47 H47 0.9500 . ?
C48 C52 1.407(3) . ?
C48 C49 1.407(3) . ?
C48 H48 0.9500 . ?
C49 C50 1.401(3) . ?
C49 H49 0.9500 . ?
C50 C51 1.407(3) . ?
C50 H50 0.9500 . ?
C51 C52 1.413(3) . ?
C51 H51 0.9500 . ?
C52 H52 0.9500 . ?
O1 C56 1.403(4) . ?
O1 C53 1.436(5) . ?
C53 C54 1.542(5) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C54 C55 1.503(5) . ?
C54 H54A 0.9900 . ?
C54 H54B 0.9900 . ?
C55 C56 1.487(4) . ?
C55 H55A 0.9900 . ?
C55 H55B 0.9900 . ?
C56 H56A 0.9900 . ?
C56 H56B 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
C7 Zr1 C10 86.74(7) . . ?
C7 Zr1 C21 94.82(13) . . ?
C10 Zr1 C21 133.28(10) . . ?
C7 Zr1 C20 77.23(8) . . ?
C10 Zr1 C20 104.72(13) . . ?
C21 Zr1 C20 32.31(14) . . ?
C7 Zr1 C17 126.05(11) . . ?
C10 Zr1 C17 121.33(11) . . ?
C21 Zr1 C17 31.74(13) . . ?
C20 Zr1 C17 52.75(12) . . ?
C7 Zr1 C26 99.73(8) . . ?
C10 Zr1 C26 135.74(8) . . ?
C21 Zr1 C26 90.09(12) . . ?
C20 Zr1 C26 119.45(14) . . ?
C17 Zr1 C26 89.90(10) . . ?
C7 Zr1 C22 79.11(7) . . ?
C10 Zr1 C22 108.97(9) . . ?
C21 Zr1 C22 117.19(11) . . ?
C20 Zr1 C22 137.20(13) . . ?
C17 Zr1 C22 122.86(10) . . ?
C26 Zr1 C22 32.97(9) . . ?
C7 Zr1 C18 127.20(9) . . ?
C10 Zr1 C18 90.26(10) . . ?
C21 Zr1 C18 52.50(11) . . ?
C20 Zr1 C18 52.78(10) . . ?
C17 Zr1 C18 31.26(11) . . ?
C26 Zr1 C18 117.70(11) . . ?
C22 Zr1 C18 149.17(11) . . ?
C7 Zr1 C19 96.16(11) . . ?
C10 Zr1 C19 80.07(9) . . ?
C21 Zr1 C19 53.30(11) . . ?
C20 Zr1 C19 32.24(12) . . ?
C17 Zr1 C19 52.63(10) . . ?
C26 Zr1 C19 141.20(9) . . ?
C22 Zr1 C19 169.34(12) . . ?
C18 Zr1 C19 31.94(11) . . ?
C7 Zr1 C23 94.96(8) . . ?
C10 Zr1 C23 82.02(8) . . ?
C21 Zr1 C23 143.83(12) . . ?
C20 Zr1 C23 169.17(12) . . ?
C17 Zr1 C23 130.95(10) . . ?
C26 Zr1 C23 53.92(8) . . ?
C22 Zr1 C23 32.36(9) . . ?
C18 Zr1 C23 136.73(10) . . ?
C19 Zr1 C23 158.29(12) . . ?
C7 Zr1 C25 130.99(8) . . ?
C10 Zr1 C25 118.47(8) . . ?
C21 Zr1 C25 95.19(14) . . ?
C20 Zr1 C25 127.06(12) . . ?
C17 Zr1 C25 78.19(10) . . ?
C26 Zr1 C25 32.54(8) . . ?
C22 Zr1 C25 53.85(8) . . ?
C18 Zr1 C25 96.01(10) . . ?
C19 Zr1 C25 127.46(10) . . ?
C23 Zr1 C25 53.28(8) . . ?
C7 Zr1 C24 127.08(8) . . ?
C10 Zr1 C24 87.44(8) . . ?
C21 Zr1 C24 125.46(15) . . ?
C20 Zr1 C24 154.03(10) . . ?
C17 Zr1 C24 101.30(11) . . ?
C26 Zr1 C24 53.80(8) . . ?
C22 Zr1 C24 53.71(9) . . ?
C18 Zr1 C24 105.37(10) . . ?
C19 Zr1 C24 134.24(12) . . ?
C23 Zr1 C24 32.21(9) . . ?
C25 Zr1 C24 32.06(8) . . ?
C2 C1 C6 121.6(2) . . ?
C2 C1 H1 119.2 . . ?
C6 C1 H1 119.2 . . ?
C3 C2 C1 120.3(2) . . ?
C3 C2 H2 119.9 . . ?
C1 C2 H2 119.9 . . ?
C4 C3 C2 119.4(2) . . ?
C4 C3 H3 120.3 . . ?
C2 C3 H3 120.3 . . ?
C3 C4 C5 120.4(2) . . ?
C3 C4 H4 119.8 . . ?
C5 C4 H4 119.8 . . ?
C4 C5 C6 121.4(2) . . ?
C4 C5 H5 119.3 . . ?
C6 C5 H5 119.3 . . ?
C1 C6 C5 116.93(19) . . ?
C1 C6 C7 119.90(18) . . ?
C5 C6 C7 123.13(18) . . ?
C8 C7 C6 121.57(18) . . ?
C8 C7 Zr1 100.29(13) . . ?
C6 C7 Zr1 138.07(14) . . ?
C7 C8 C9 126.15(19) . . ?
C7 C8 Zr1 51.44(11) . . ?
C9 C8 Zr1 74.80(11) . . ?
C7 C8 H8 116.9 . . ?
C9 C8 H8 116.9 . . ?
Zr1 C8 H8 167.9 . . ?
C10 C9 C8 126.50(19) . . ?
C10 C9 Zr1 51.66(11) . . ?
C8 C9 Zr1 74.94(11) . . ?
C10 C9 H9 116.8 . . ?
C8 C9 H9 116.8 . . ?
Zr1 C9 H9 167.9 . . ?
C9 C10 C11 121.87(19) . . ?
C9 C10 Zr1 100.02(13) . . ?
C11 C10 Zr1 138.10(15) . . ?
C16 C11 C12 116.8(2) . . ?
C16 C11 C10 119.9(2) . . ?
C12 C11 C10 123.33(19) . . ?
C13 C12 C11 121.4(2) . . ?
C13 C12 H12 119.3 . . ?
C11 C12 H12 119.3 . . ?
C14 C13 C12 120.4(2) . . ?
C14 C13 H13 119.8 . . ?
C12 C13 H13 119.8 . . ?
C15 C14 C13 119.5(2) . . ?
C15 C14 H14 120.3 . . ?
C13 C14 H14 120.3 . . ?
C14 C15 C16 120.0(2) . . ?
C14 C15 H15 120.0 . . ?
C16 C15 H15 120.0 . . ?
C15 C16 C11 121.9(2) . . ?
C15 C16 H16 119.1 . . ?
C11 C16 H16 119.1 . . ?
C18 C17 C21 108.9(3) . . ?
C18 C17 Zr1 74.83(16) . . ?
C21 C17 Zr1 73.03(17) . . ?
C18 C17 H17 125.6 . . ?
C21 C17 H17 125.6 . . ?
Zr1 C17 H17 118.4 . . ?
C17 C18 C19 108.9(3) . . ?
C17 C18 Zr1 73.91(16) . . ?
C19 C18 Zr1 74.25(15) . . ?
C17 C18 H18 125.6 . . ?
C19 C18 H18 125.6 . . ?
Zr1 C18 H18 118.1 . . ?
C18 C19 C20 106.6(3) . . ?
C18 C19 Zr1 73.81(16) . . ?
C20 C19 Zr1 72.96(16) . . ?
C18 C19 H19 126.7 . . ?
C20 C19 H19 126.7 . . ?
Zr1 C19 H19 118.6 . . ?
C21 C20 C19 107.6(3) . . ?
C21 C20 Zr1 73.02(16) . . ?
C19 C20 Zr1 74.79(16) . . ?
C21 C20 H20 126.2 . . ?
C19 C20 H20 126.2 . . ?
Zr1 C20 H20 118.0 . . ?
C17 C21 C20 108.0(3) . . ?
C17 C21 Zr1 75.23(17) . . ?
C20 C21 Zr1 74.66(17) . . ?
C17 C21 H21 126.0 . . ?
C20 C21 H21 126.0 . . ?
Zr1 C21 H21 116.2 . . ?
C23 C22 C26 107.5(2) . . ?
C23 C22 Zr1 74.18(14) . . ?
C26 C22 Zr1 73.26(13) . . ?
C23 C22 H22 126.3 . . ?
C26 C22 H22 126.3 . . ?
Zr1 C22 H22 118.3 . . ?
C24 C23 C22 108.7(2) . . ?
C24 C23 Zr1 74.36(13) . . ?
C22 C23 Zr1 73.46(14) . . ?
C24 C23 H23 125.7 . . ?
C22 C23 H23 125.7 . . ?
Zr1 C23 H23 118.4 . . ?
C25 C24 C23 107.9(2) . . ?
C25 C24 Zr1 73.58(13) . . ?
C23 C24 Zr1 73.43(14) . . ?
C25 C24 H24 126.1 . . ?
C23 C24 H24 126.1 . . ?
Zr1 C24 H24 118.8 . . ?
C24 C25 C26 108.7(2) . . ?
C24 C25 Zr1 74.36(13) . . ?
C26 C25 Zr1 73.04(13) . . ?
C24 C25 H25 125.6 . . ?
C26 C25 H25 125.6 . . ?
Zr1 C25 H25 118.8 . . ?
C25 C26 C22 107.2(2) . . ?
C25 C26 Zr1 74.43(13) . . ?
C22 C26 Zr1 73.77(13) . . ?
C25 C26 H26 126.4 . . ?
C22 C26 H26 126.4 . . ?
Zr1 C26 H26 117.5 . . ?
C33 Zr2 C36 84.67(7) . . ?
C33 Zr2 C44 130.79(7) . . ?
C36 Zr2 C44 93.74(8) . . ?
C33 Zr2 C51 96.28(7) . . ?
C36 Zr2 C51 133.24(8) . . ?
C44 Zr2 C51 118.42(8) . . ?
C33 Zr2 C43 121.86(8) . . ?
C36 Zr2 C43 126.06(8) . . ?
C44 Zr2 C43 32.60(8) . . ?
C51 Zr2 C43 92.89(8) . . ?
C33 Zr2 C52 78.92(7) . . ?
C36 Zr2 C52 103.79(8) . . ?
C44 Zr2 C52 147.29(8) . . ?
C51 Zr2 C52 32.66(8) . . ?
C43 Zr2 C52 125.55(8) . . ?
C33 Zr2 C45 100.91(7) . . ?
C36 Zr2 C45 77.02(7) . . ?
C44 Zr2 C45 32.56(8) . . ?
C51 Zr2 C45 146.70(8) . . ?
C43 Zr2 C45 53.83(8) . . ?
C52 Zr2 C45 179.14(8) . . ?
C33 Zr2 C47 89.56(8) . . ?
C36 Zr2 C47 128.11(8) . . ?
C44 Zr2 C47 53.73(8) . . ?
C51 Zr2 C47 98.65(8) . . ?
C43 Zr2 C47 32.32(8) . . ?
C52 Zr2 C47 125.55(8) . . ?
C45 Zr2 C47 53.59(8) . . ?
C33 Zr2 C46 77.57(7) . . ?
C36 Zr2 C46 96.89(7) . . ?
C44 Zr2 C46 53.72(8) . . ?
C51 Zr2 C46 129.12(8) . . ?
C43 Zr2 C46 53.52(8) . . ?
C52 Zr2 C46 146.89(8) . . ?
C45 Zr2 C46 32.39(7) . . ?
C47 Zr2 C46 32.15(8) . . ?
C33 Zr2 C48 97.91(7) . . ?
C36 Zr2 C48 79.73(7) . . ?
C44 Zr2 C48 130.29(8) . . ?
C51 Zr2 C48 53.74(8) . . ?
C43 Zr2 C48 131.83(8) . . ?
C52 Zr2 C48 32.40(8) . . ?
C45 Zr2 C48 148.39(8) . . ?
C47 Zr2 C48 151.90(8) . . ?
C46 Zr2 C48 174.65(7) . . ?
C33 Zr2 C50 128.32(7) . . ?
C36 Zr2 C50 122.43(7) . . ?
C44 Zr2 C50 93.56(8) . . ?
C51 Zr2 C50 32.39(8) . . ?
C43 Zr2 C50 79.49(8) . . ?
C52 Zr2 C50 53.73(7) . . ?
C45 Zr2 C50 126.11(8) . . ?
C47 Zr2 C50 101.10(8) . . ?
C46 Zr2 C50 131.69(8) . . ?
C48 Zr2 C50 53.45(7) . . ?
C33 Zr2 C49 129.47(7) . . ?
C36 Zr2 C49 90.50(7) . . ?
C44 Zr2 C49 99.69(8) . . ?
C51 Zr2 C49 53.46(8) . . ?
C43 Zr2 C49 101.29(8) . . ?
C52 Zr2 C49 53.54(7) . . ?
C45 Zr2 C49 126.88(8) . . ?
C47 Zr2 C49 129.82(8) . . ?
C46 Zr2 C49 152.67(8) . . ?
C48 Zr2 C49 32.25(7) . . ?
C50 Zr2 C49 32.07(7) . . ?
C28 C27 C32 121.9(2) . . ?
C28 C27 H27 119.0 . . ?
C32 C27 H27 119.0 . . ?
C29 C28 C27 120.0(2) . . ?
C29 C28 H28 120.0 . . ?
C27 C28 H28 120.0 . . ?
C30 C29 C28 119.2(2) . . ?
C30 C29 H29 120.4 . . ?
C28 C29 H29 120.4 . . ?
C31 C30 C29 120.6(2) . . ?
C31 C30 H30 119.7 . . ?
C29 C30 H30 119.7 . . ?
C30 C31 C32 121.3(2) . . ?
C30 C31 H31 119.3 . . ?
C32 C31 H31 119.3 . . ?
C27 C32 C31 116.95(19) . . ?
C27 C32 C33 120.07(18) . . ?
C31 C32 C33 122.94(19) . . ?
C34 C33 C32 121.95(18) . . ?
C34 C33 Zr2 102.27(13) . . ?
C32 C33 Zr2 135.73(14) . . ?
C33 C34 C35 125.26(18) . . ?
C33 C34 H34 117.4 . . ?
C35 C34 H34 117.4 . . ?
C36 C35 C34 125.16(19) . . ?
C36 C35 H35 117.4 . . ?
C34 C35 H35 117.4 . . ?
C35 C36 C37 122.36(18) . . ?
C35 C36 Zr2 102.36(14) . . ?
C37 C36 Zr2 135.24(14) . . ?
C42 C37 C38 116.72(19) . . ?
C42 C37 C36 120.09(18) . . ?
C38 C37 C36 123.13(19) . . ?
C39 C38 C37 121.2(2) . . ?
C39 C38 H38 119.4 . . ?
C37 C38 H38 119.4 . . ?
C40 C39 C38 121.0(2) . . ?
C40 C39 H39 119.5 . . ?
C38 C39 H39 119.5 . . ?
C39 C40 C41 119.1(2) . . ?
C39 C40 H40 120.5 . . ?
C41 C40 H40 120.5 . . ?
C40 C41 C42 120.0(2) . . ?
C40 C41 H41 120.0 . . ?
C42 C41 H41 120.0 . . ?
C41 C42 C37 122.1(2) . . ?
C41 C42 H42 119.0 . . ?
C37 C42 H42 119.0 . . ?
C47 C43 C44 107.8(2) . . ?
C47 C43 Zr2 74.22(13) . . ?
C44 C43 Zr2 72.99(13) . . ?
C47 C43 H43 126.1 . . ?
C44 C43 H43 126.1 . . ?
Zr2 C43 H43 118.6 . . ?
C43 C44 C45 108.2(2) . . ?
C43 C44 Zr2 74.41(13) . . ?
C45 C44 Zr2 74.72(13) . . ?
C43 C44 H44 125.9 . . ?
C45 C44 H44 125.9 . . ?
Zr2 C44 H44 117.0 . . ?
C44 C45 C46 107.5(2) . . ?
C44 C45 Zr2 72.72(13) . . ?
C46 C45 Zr2 74.08(13) . . ?
C44 C45 H45 126.3 . . ?
C46 C45 H45 126.3 . . ?
Zr2 C45 H45 118.9 . . ?
C47 C46 C45 108.2(2) . . ?
C47 C46 Zr2 73.73(13) . . ?
C45 C46 Zr2 73.53(12) . . ?
C47 C46 H46 125.9 . . ?
C45 C46 H46 125.9 . . ?
Zr2 C46 H46 118.7 . . ?
C46 C47 C43 108.3(2) . . ?
C46 C47 Zr2 74.11(13) . . ?
C43 C47 Zr2 73.47(13) . . ?
C46 C47 H47 125.9 . . ?
C43 C47 H47 125.9 . . ?
Zr2 C47 H47 118.5 . . ?
C52 C48 C49 108.0(2) . . ?
C52 C48 Zr2 73.34(12) . . ?
C49 C48 Zr2 74.32(12) . . ?
C52 C48 H48 126.0 . . ?
C49 C48 H48 126.0 . . ?
Zr2 C48 H48 118.3 . . ?
C50 C49 C48 108.3(2) . . ?
C50 C49 Zr2 73.82(12) . . ?
C48 C49 Zr2 73.43(12) . . ?
C50 C49 H49 125.8 . . ?
C48 C49 H49 125.8 . . ?
Zr2 C49 H49 118.8 . . ?
C49 C50 C51 107.9(2) . . ?
C49 C50 Zr2 74.11(12) . . ?
C51 C50 Zr2 72.82(12) . . ?
C49 C50 H50 126.0 . . ?
C51 C50 H50 126.0 . . ?
Zr2 C50 H50 118.9 . . ?
C50 C51 C52 108.1(2) . . ?
C50 C51 Zr2 74.80(12) . . ?
C52 C51 Zr2 73.91(12) . . ?
C50 C51 H51 126.0 . . ?
C52 C51 H51 126.0 . . ?
Zr2 C51 H51 117.3 . . ?
C48 C52 C51 107.7(2) . . ?
C48 C52 Zr2 74.26(12) . . ?
C51 C52 Zr2 73.44(13) . . ?
C48 C52 H52 126.2 . . ?
C51 C52 H52 126.2 . . ?
Zr2 C52 H52 118.1 . . ?
C56 O1 C53 107.5(3) . . ?
O1 C53 C54 105.9(3) . . ?
O1 C53 H53A 110.5 . . ?
C54 C53 H53A 110.5 . . ?
O1 C53 H53B 110.5 . . ?
C54 C53 H53B 110.5 . . ?
H53A C53 H53B 108.7 . . ?
C55 C54 C53 103.1(3) . . ?
C55 C54 H54A 111.1 . . ?
C53 C54 H54A 111.1 . . ?
C55 C54 H54B 111.1 . . ?
C53 C54 H54B 111.1 . . ?
H54A C54 H54B 109.1 . . ?
C56 C55 C54 102.4(3) . . ?
C56 C55 H55A 111.3 . . ?
C54 C55 H55A 111.3 . . ?
C56 C55 H55B 111.3 . . ?
C54 C55 H55B 111.3 . . ?
H55A C55 H55B 109.2 . . ?
O1 C56 C55 104.5(3) . . ?
O1 C56 H56A 110.9 . . ?
C55 C56 H56A 110.9 . . ?
O1 C56 H56B 110.9 . . ?
C55 C56 H56B 110.9 . . ?
H56A C56 H56B 108.9 . . ?

_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        30.03
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         0.568
_refine_diff_density_min         -0.613
_refine_diff_density_rms         0.075
_database_code_depnum_ccdc_archive 'CCDC 926967'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_fj373
#TrackingRef '2013_bousrez_dalton trans.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H17 P'
_chemical_formula_sum            'C22 H17 P'
_chemical_formula_weight         312.33

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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P21/c
_symmetry_space_group_name_Hall  '-P 2ybc'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   5.884(1)
_cell_length_b                   8.898(1)
_cell_length_c                   30.968(1)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.658(2)
_cell_angle_gamma                90.00
_cell_volume                     1610.4(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    150.0(1)
_cell_measurement_reflns_used    3413
_cell_measurement_theta_min      0.998
_cell_measurement_theta_max      30.034

_exptl_crystal_description       Block
_exptl_crystal_colour            Yellow
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             656
_exptl_absorpt_coefficient_mu    0.167
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9515
_exptl_absorpt_correction_T_max  0.9753
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1996)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150.0(1)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8866
_diffrn_reflns_av_R_equivalents  0.0329
_diffrn_reflns_av_sigmaI/netI    0.0343
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_theta_min         4.03
_diffrn_reflns_theta_max         28.70
_reflns_number_total             4031
_reflns_number_gt                3582
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_cell_refinement       'DENZO (Otwinowski & Minor, 1997) & COLLECT'
_computing_data_reduction        'DENZO & COLLECT'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  'PLATON (Spek, 2009)'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0483P)^2^+0.8203P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4031
_refine_ls_number_parameters     208
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0522
_refine_ls_R_factor_gt           0.0462
_refine_ls_wR_factor_ref         0.1199
_refine_ls_wR_factor_gt          0.1149
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_restrained_S_all      1.055
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.77845(6) -0.43321(5) -0.148807(12) 0.02933(12) Uani 1 1 d . . .
C1 C 0.6229(3) -0.38646(19) -0.20008(5) 0.0326(3) Uani 1 1 d . . .
H1 H 0.6739 -0.3167 -0.2201 0.039 Uiso 1 1 calc R . .
C2 C 0.4223(2) -0.46349(17) -0.20684(5) 0.0285(3) Uani 1 1 d . . .
C3 C 0.3742(2) -0.54752(17) -0.16820(5) 0.0286(3) Uani 1 1 d . . .
H3 H 0.2408 -0.6074 -0.1678 0.034 Uiso 1 1 calc R . .
C4 C 0.5329(2) -0.53404(16) -0.13303(5) 0.0270(3) Uani 1 1 d . . .
C5 C 0.2644(3) -0.46298(17) -0.24777(5) 0.0301(3) Uani 1 1 d . . .
C6 C 0.3050(3) -0.3707(2) -0.28257(5) 0.0380(4) Uani 1 1 d . . .
H6 H 0.4389 -0.3102 -0.2803 0.046 Uiso 1 1 calc R . .
C7 C 0.1538(3) -0.3661(2) -0.32025(5) 0.0417(4) Uani 1 1 d . . .
H7 H 0.1844 -0.3026 -0.3436 0.050 Uiso 1 1 calc R . .
C8 C -0.0426(3) -0.4538(2) -0.32412(5) 0.0415(4) Uani 1 1 d . . .
H8 H -0.1470 -0.4500 -0.3499 0.050 Uiso 1 1 calc R . .
C9 C -0.0849(3) -0.5464(2) -0.29031(6) 0.0451(4) Uani 1 1 d . . .
H9 H -0.2187 -0.6070 -0.2929 0.054 Uiso 1 1 calc R . .
C10 C 0.0673(3) -0.5516(2) -0.25235(5) 0.0384(4) Uani 1 1 d . . .
H10 H 0.0366 -0.6164 -0.2293 0.046 Uiso 1 1 calc R . .
C11 C 0.5227(2) -0.59648(16) -0.08940(5) 0.0272(3) Uani 1 1 d . . .
C12 C 0.3221(3) -0.66366(17) -0.07768(5) 0.0312(3) Uani 1 1 d . . .
H12 H 0.1908 -0.6715 -0.0985 0.037 Uiso 1 1 calc R . .
C13 C 0.3149(3) -0.71849(18) -0.03598(5) 0.0359(3) Uani 1 1 d . . .
H13 H 0.1790 -0.7648 -0.0287 0.043 Uiso 1 1 calc R . .
C14 C 0.5028(3) -0.70683(18) -0.00472(5) 0.0363(3) Uani 1 1 d . . .
H14 H 0.4959 -0.7441 0.0238 0.044 Uiso 1 1 calc R . .
C15 C 0.7013(3) -0.63983(18) -0.01577(5) 0.0348(3) Uani 1 1 d . . .
H15 H 0.8309 -0.6307 0.0054 0.042 Uiso 1 1 calc R . .
C16 C 0.7111(3) -0.58626(17) -0.05752(5) 0.0307(3) Uani 1 1 d . . .
H16 H 0.8486 -0.5417 -0.0646 0.037 Uiso 1 1 calc R . .
C17 C 0.7893(2) -0.26105(16) -0.11641(5) 0.0272(3) Uani 1 1 d . . .
C18 C 0.9901(3) -0.22704(18) -0.08997(5) 0.0325(3) Uani 1 1 d . . .
H18 H 1.1195 -0.2909 -0.0899 0.039 Uiso 1 1 calc R . .
C19 C 1.0022(3) -0.09981(19) -0.06368(5) 0.0376(4) Uani 1 1 d . . .
H19 H 1.1394 -0.0772 -0.0455 0.045 Uiso 1 1 calc R . .
C20 C 0.8143(3) -0.00626(19) -0.06402(6) 0.0396(4) Uani 1 1 d . . .
H20 H 0.8223 0.0806 -0.0461 0.048 Uiso 1 1 calc R . .
C21 C 0.6139(3) -0.03924(19) -0.09060(6) 0.0390(4) Uani 1 1 d . . .
H21 H 0.4852 0.0253 -0.0908 0.047 Uiso 1 1 calc R . .
C22 C 0.6008(3) -0.16545(18) -0.11673(5) 0.0331(3) Uani 1 1 d . . .
H22 H 0.4635 -0.1873 -0.1349 0.040 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
P1 0.0254(2) 0.0331(2) 0.0301(2) -0.00404(14) 0.00588(14) -0.00096(14)
C1 0.0323(7) 0.0378(8) 0.0286(7) -0.0012(6) 0.0075(6) -0.0034(6)
C2 0.0286(7) 0.0315(7) 0.0261(6) -0.0043(5) 0.0057(5) 0.0020(5)
C3 0.0264(7) 0.0291(7) 0.0307(7) -0.0025(6) 0.0049(5) -0.0007(5)
C4 0.0274(7) 0.0248(7) 0.0294(7) -0.0029(5) 0.0057(5) 0.0012(5)
C5 0.0304(7) 0.0336(7) 0.0268(7) -0.0063(6) 0.0052(5) 0.0035(6)
C6 0.0425(9) 0.0359(8) 0.0350(8) -0.0003(6) 0.0021(7) -0.0018(7)
C7 0.0560(11) 0.0380(9) 0.0306(8) 0.0025(6) 0.0028(7) 0.0021(8)
C8 0.0463(10) 0.0479(10) 0.0290(8) -0.0067(7) -0.0018(7) 0.0056(8)
C9 0.0378(9) 0.0623(12) 0.0343(8) -0.0064(8) 0.0008(7) -0.0084(8)
C10 0.0348(8) 0.0520(10) 0.0286(7) -0.0023(7) 0.0047(6) -0.0061(7)
C11 0.0298(7) 0.0229(6) 0.0291(7) -0.0024(5) 0.0048(5) 0.0028(5)
C12 0.0302(7) 0.0305(7) 0.0334(7) -0.0014(6) 0.0052(6) 0.0004(6)
C13 0.0385(8) 0.0313(8) 0.0398(8) 0.0014(6) 0.0129(6) -0.0001(6)
C14 0.0449(9) 0.0323(8) 0.0326(8) 0.0036(6) 0.0084(6) 0.0068(7)
C15 0.0389(8) 0.0316(8) 0.0329(7) 0.0010(6) -0.0000(6) 0.0056(6)
C16 0.0316(7) 0.0274(7) 0.0331(7) 0.0000(6) 0.0033(6) 0.0020(6)
C17 0.0281(7) 0.0277(7) 0.0264(6) 0.0005(5) 0.0055(5) -0.0027(5)
C18 0.0302(7) 0.0321(8) 0.0345(7) 0.0029(6) 0.0013(6) -0.0012(6)
C19 0.0401(9) 0.0363(8) 0.0347(8) 0.0002(6) -0.0030(6) -0.0082(7)
C20 0.0543(10) 0.0275(7) 0.0378(8) -0.0042(6) 0.0081(7) -0.0045(7)
C21 0.0404(9) 0.0313(8) 0.0463(9) 0.0010(7) 0.0092(7) 0.0054(6)
C22 0.0298(7) 0.0343(8) 0.0348(8) 0.0022(6) 0.0021(6) 0.0007(6)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1 C1 1.7873(16) . ?
P1 C4 1.8150(15) . ?
P1 C17 1.8283(15) . ?
C1 C2 1.360(2) . ?
C1 H1 0.9500 . ?
C2 C3 1.466(2) . ?
C2 C5 1.482(2) . ?
C3 C4 1.355(2) . ?
C3 H3 0.9500 . ?
C4 C11 1.469(2) . ?
C5 C10 1.396(2) . ?
C5 C6 1.397(2) . ?
C6 C7 1.384(2) . ?
C6 H6 0.9500 . ?
C7 C8 1.388(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.377(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.393(2) . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
C11 C16 1.399(2) . ?
C11 C12 1.408(2) . ?
C12 C13 1.386(2) . ?
C12 H12 0.9500 . ?
C13 C14 1.386(2) . ?
C13 H13 0.9500 . ?
C14 C15 1.389(2) . ?
C14 H14 0.9500 . ?
C15 C16 1.385(2) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C17 C18 1.391(2) . ?
C17 C22 1.397(2) . ?
C18 C19 1.392(2) . ?
C18 H18 0.9500 . ?
C19 C20 1.383(3) . ?
C19 H19 0.9500 . ?
C20 C21 1.389(2) . ?
C20 H20 0.9500 . ?
C21 C22 1.381(2) . ?
C21 H21 0.9500 . ?
C22 H22 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
C1 P1 C4 90.72(7) . . ?
C1 P1 C17 105.91(7) . . ?
C4 P1 C17 104.16(6) . . ?
C2 C1 P1 111.43(12) . . ?
C2 C1 H1 124.3 . . ?
P1 C1 H1 124.3 . . ?
C1 C2 C3 112.18(13) . . ?
C1 C2 C5 125.23(14) . . ?
C3 C2 C5 122.58(13) . . ?
C4 C3 C2 115.50(13) . . ?
C4 C3 H3 122.2 . . ?
C2 C3 H3 122.2 . . ?
C3 C4 C11 127.44(13) . . ?
C3 C4 P1 108.86(11) . . ?
C11 C4 P1 123.60(11) . . ?
C10 C5 C6 117.92(14) . . ?
C10 C5 C2 121.07(14) . . ?
C6 C5 C2 120.99(14) . . ?
C7 C6 C5 121.14(16) . . ?
C7 C6 H6 119.4 . . ?
C5 C6 H6 119.4 . . ?
C6 C7 C8 120.23(16) . . ?
C6 C7 H7 119.9 . . ?
C8 C7 H7 119.9 . . ?
C9 C8 C7 119.52(16) . . ?
C9 C8 H8 120.2 . . ?
C7 C8 H8 120.2 . . ?
C8 C9 C10 120.42(17) . . ?
C8 C9 H9 119.8 . . ?
C10 C9 H9 119.8 . . ?
C9 C10 C5 120.76(16) . . ?
C9 C10 H10 119.6 . . ?
C5 C10 H10 119.6 . . ?
C16 C11 C12 117.70(14) . . ?
C16 C11 C4 120.73(13) . . ?
C12 C11 C4 121.53(13) . . ?
C13 C12 C11 120.46(14) . . ?
C13 C12 H12 119.8 . . ?
C11 C12 H12 119.8 . . ?
C12 C13 C14 121.08(15) . . ?
C12 C13 H13 119.5 . . ?
C14 C13 H13 119.5 . . ?
C13 C14 C15 119.03(15) . . ?
C13 C14 H14 120.5 . . ?
C15 C14 H14 120.5 . . ?
C16 C15 C14 120.33(15) . . ?
C16 C15 H15 119.8 . . ?
C14 C15 H15 119.8 . . ?
C15 C16 C11 121.38(15) . . ?
C15 C16 H16 119.3 . . ?
C11 C16 H16 119.3 . . ?
C18 C17 C22 119.43(14) . . ?
C18 C17 P1 118.60(11) . . ?
C22 C17 P1 121.95(11) . . ?
C17 C18 C19 120.27(15) . . ?
C17 C18 H18 119.9 . . ?
C19 C18 H18 119.9 . . ?
C20 C19 C18 119.89(15) . . ?
C20 C19 H19 120.1 . . ?
C18 C19 H19 120.1 . . ?
C19 C20 C21 120.03(15) . . ?
C19 C20 H20 120.0 . . ?
C21 C20 H20 120.0 . . ?
C22 C21 C20 120.32(15) . . ?
C22 C21 H21 119.8 . . ?
C20 C21 H21 119.8 . . ?
C21 C22 C17 120.05(15) . . ?
C21 C22 H22 120.0 . . ?
C17 C22 H22 120.0 . . ?

_diffrn_measured_fraction_theta_max 0.972
_diffrn_reflns_theta_full        28.70
_diffrn_measured_fraction_theta_full 0.972
_refine_diff_density_max         0.362
_refine_diff_density_min         -0.306
_refine_diff_density_rms         0.047
_database_code_depnum_ccdc_archive 'CCDC 926968'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_fj_triphenylphosphol
#TrackingRef '2013_bousrez_dalton trans.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H17 P'
_chemical_formula_sum            'C22 H17 P'
_chemical_formula_weight         312.33

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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P21 '
_symmetry_space_group_name_Hall  'P 2yb'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   12.079(1)
_cell_length_b                   5.832(1)
_cell_length_c                   12.562(1)
_cell_angle_alpha                90.00
_cell_angle_beta                 115.528(1)
_cell_angle_gamma                90.00
_cell_volume                     798.54(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    150.0(1)
_cell_measurement_reflns_used    2080
_cell_measurement_theta_min      0.998
_cell_measurement_theta_max      30.034

_exptl_crystal_description       Block
_exptl_crystal_colour            Yellow
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.299
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             328
_exptl_absorpt_coefficient_mu    0.169
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9638
_exptl_absorpt_correction_T_max  0.9833
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1996)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150.0(1)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5707
_diffrn_reflns_av_R_equivalents  0.0256
_diffrn_reflns_av_sigmaI/netI    0.0378
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.10
_diffrn_reflns_theta_max         30.03
_reflns_number_total             3917
_reflns_number_gt                3796
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_cell_refinement       'DENZO (Otwinowski & Minor, 1997) & COLLECT'
_computing_data_reduction        'DENZO & COLLECT'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  'PLATON (Spek, 2009)'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.

Flack's parameter was refined to 0.17(8).
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.3882P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.17(8)
_refine_ls_number_reflns         3917
_refine_ls_number_parameters     209
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0359
_refine_ls_wR_factor_ref         0.0806
_refine_ls_wR_factor_gt          0.0788
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_restrained_S_all      1.064
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.62735(3) 0.76527(7) 0.91318(3) 0.01881(9) Uani 1 1 d . . .
C1 C 0.52610(14) 0.5623(3) 0.80446(14) 0.0193(3) Uani 1 1 d . . .
C2 C 0.51908(14) 0.3691(3) 0.86151(14) 0.0215(3) Uani 1 1 d . . .
H2 H 0.4654 0.2464 0.8220 0.026 Uiso 1 1 calc R . .
C3 C 0.59845(14) 0.3627(3) 0.98591(14) 0.0205(3) Uani 1 1 d . . .
H3 H 0.6005 0.2357 1.0340 0.025 Uiso 1 1 calc R . .
C4 C 0.67025(14) 0.5509(3) 1.02986(14) 0.0191(3) Uani 1 1 d . . .
C5 C 0.45363(14) 0.6142(3) 0.67891(15) 0.0211(3) Uani 1 1 d . . .
C6 C 0.46895(15) 0.8194(3) 0.62900(14) 0.0245(4) Uani 1 1 d . . .
H6 H 0.5269 0.9291 0.6774 0.029 Uiso 1 1 calc R . .
C7 C 0.40050(17) 0.8649(4) 0.50959(16) 0.0299(4) Uani 1 1 d . . .
H7 H 0.4127 1.0041 0.4768 0.036 Uiso 1 1 calc R . .
C8 C 0.31413(17) 0.7065(4) 0.43807(16) 0.0321(4) Uani 1 1 d . . .
H8 H 0.2670 0.7376 0.3566 0.039 Uiso 1 1 calc R . .
C9 C 0.29746(18) 0.5031(4) 0.48664(16) 0.0334(4) Uani 1 1 d . . .
H9 H 0.2387 0.3947 0.4381 0.040 Uiso 1 1 calc R . .
C10 C 0.36597(16) 0.4571(3) 0.60534(15) 0.0272(4) Uani 1 1 d . . .
H10 H 0.3535 0.3173 0.6375 0.033 Uiso 1 1 calc R . .
C11 C 0.75077(14) 0.5924(3) 1.15461(14) 0.0203(3) Uani 1 1 d . . .
C12 C 0.75902(15) 0.4329(3) 1.24196(15) 0.0242(3) Uani 1 1 d . . .
H12 H 0.7136 0.2942 1.2192 0.029 Uiso 1 1 calc R . .
C13 C 0.83213(16) 0.4745(4) 1.36041(16) 0.0290(4) Uani 1 1 d . . .
H13 H 0.8355 0.3654 1.4179 0.035 Uiso 1 1 calc R . .
C14 C 0.90061(17) 0.6752(4) 1.39550(16) 0.0314(4) Uani 1 1 d . . .
H14 H 0.9514 0.7031 1.4766 0.038 Uiso 1 1 calc R . .
C15 C 0.89389(17) 0.8342(3) 1.31083(16) 0.0302(4) Uani 1 1 d . . .
H15 H 0.9405 0.9715 1.3343 0.036 Uiso 1 1 calc R . .
C16 C 0.81964(14) 0.7948(3) 1.19192(14) 0.0245(3) Uani 1 1 d . . .
H16 H 0.8155 0.9064 1.1352 0.029 Uiso 1 1 calc R . .
C17 C 0.76013(12) 0.7899(3) 0.87907(13) 0.0198(3) Uani 1 1 d . . .
C18 C 0.79232(15) 0.6151(3) 0.82219(16) 0.0253(3) Uani 1 1 d . . .
H18 H 0.7457 0.4775 0.8013 0.030 Uiso 1 1 calc R . .
C19 C 0.89211(17) 0.6406(4) 0.79583(18) 0.0308(4) Uani 1 1 d . . .
H19 H 0.9131 0.5214 0.7563 0.037 Uiso 1 1 calc R . .
C20 C 0.96118(16) 0.8405(4) 0.82720(16) 0.0308(4) Uani 1 1 d . . .
H20 H 1.0295 0.8577 0.8092 0.037 Uiso 1 1 calc R . .
C21 C 0.93088(16) 1.0149(4) 0.88470(16) 0.0292(4) Uani 1 1 d . . .
H21 H 0.9789 1.1507 0.9070 0.035 Uiso 1 1 calc R . .
C22 C 0.82980(16) 0.9903(3) 0.90966(15) 0.0254(3) Uani 1 1 d . . .
H22 H 0.8082 1.1110 0.9479 0.030 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
P1 0.02144(16) 0.01604(18) 0.02046(17) -0.00004(17) 0.01046(13) -0.00078(16)
C1 0.0199(7) 0.0182(8) 0.0214(7) -0.0036(6) 0.0103(6) -0.0018(5)
C2 0.0234(7) 0.0182(8) 0.0255(7) -0.0020(7) 0.0128(6) -0.0015(6)
C3 0.0251(7) 0.0163(7) 0.0242(7) 0.0013(6) 0.0146(6) 0.0005(6)
C4 0.0224(7) 0.0174(8) 0.0210(7) 0.0008(6) 0.0127(6) 0.0026(5)
C5 0.0224(7) 0.0203(8) 0.0235(8) -0.0006(6) 0.0126(6) 0.0006(6)
C6 0.0271(7) 0.0227(10) 0.0243(8) 0.0021(7) 0.0118(6) -0.0004(6)
C7 0.0351(9) 0.0300(10) 0.0269(8) 0.0059(8) 0.0156(7) 0.0039(8)
C8 0.0356(9) 0.0369(12) 0.0221(8) 0.0043(7) 0.0107(7) 0.0048(7)
C9 0.0334(9) 0.0333(11) 0.0258(9) -0.0019(8) 0.0056(7) -0.0035(8)
C10 0.0301(8) 0.0235(9) 0.0259(8) -0.0008(7) 0.0102(7) -0.0050(7)
C11 0.0198(7) 0.0206(8) 0.0221(8) 0.0002(6) 0.0105(6) 0.0025(6)
C12 0.0250(8) 0.0225(9) 0.0260(8) 0.0039(7) 0.0119(6) 0.0017(6)
C13 0.0289(8) 0.0321(10) 0.0257(8) 0.0081(8) 0.0115(7) 0.0035(7)
C14 0.0287(8) 0.0402(11) 0.0224(8) 0.0004(8) 0.0084(7) 0.0009(8)
C15 0.0317(8) 0.0313(11) 0.0261(8) -0.0040(7) 0.0112(7) -0.0074(7)
C16 0.0289(7) 0.0227(9) 0.0230(7) 0.0001(7) 0.0123(6) -0.0035(7)
C17 0.0203(6) 0.0194(8) 0.0198(6) 0.0010(7) 0.0087(5) -0.0013(6)
C18 0.0258(8) 0.0218(8) 0.0307(9) -0.0024(7) 0.0146(7) -0.0028(6)
C19 0.0294(9) 0.0332(11) 0.0361(10) -0.0025(8) 0.0202(8) -0.0005(7)
C20 0.0242(8) 0.0396(11) 0.0320(9) 0.0043(8) 0.0153(7) -0.0018(7)
C21 0.0263(8) 0.0302(10) 0.0300(9) 0.0027(8) 0.0112(7) -0.0086(7)
C22 0.0281(8) 0.0222(9) 0.0270(8) -0.0008(7) 0.0130(7) -0.0047(6)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1 C1 1.8229(17) . ?
P1 C4 1.8237(17) . ?
P1 C17 1.8355(15) . ?
C1 C2 1.357(2) . ?
C1 C5 1.468(2) . ?
C2 C3 1.439(2) . ?
C2 H2 0.9500 . ?
C3 C4 1.359(2) . ?
C3 H3 0.9500 . ?
C4 C11 1.465(2) . ?
C5 C6 1.400(2) . ?
C5 C10 1.404(2) . ?
C6 C7 1.391(2) . ?
C6 H6 0.9500 . ?
C7 C8 1.393(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.388(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.384(3) . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
C11 C16 1.403(2) . ?
C11 C12 1.409(2) . ?
C12 C13 1.386(2) . ?
C12 H12 0.9500 . ?
C13 C14 1.391(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.387(3) . ?
C14 H14 0.9500 . ?
C15 C16 1.391(2) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C17 C18 1.393(2) . ?
C17 C22 1.394(2) . ?
C18 C19 1.389(2) . ?
C18 H18 0.9500 . ?
C19 C20 1.388(3) . ?
C19 H19 0.9500 . ?
C20 C21 1.385(3) . ?
C20 H20 0.9500 . ?
C21 C22 1.393(2) . ?
C21 H21 0.9500 . ?
C22 H22 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
C1 P1 C4 91.34(8) . . ?
C1 P1 C17 104.33(7) . . ?
C4 P1 C17 105.49(7) . . ?
C2 C1 C5 126.47(15) . . ?
C2 C1 P1 108.53(12) . . ?
C5 C1 P1 124.60(12) . . ?
C1 C2 C3 115.52(15) . . ?
C1 C2 H2 122.2 . . ?
C3 C2 H2 122.2 . . ?
C4 C3 C2 115.47(15) . . ?
C4 C3 H3 122.3 . . ?
C2 C3 H3 122.3 . . ?
C3 C4 C11 125.52(15) . . ?
C3 C4 P1 108.45(12) . . ?
C11 C4 P1 125.04(13) . . ?
C6 C5 C10 118.08(16) . . ?
C6 C5 C1 121.65(15) . . ?
C10 C5 C1 120.27(15) . . ?
C7 C6 C5 120.96(17) . . ?
C7 C6 H6 119.5 . . ?
C5 C6 H6 119.5 . . ?
C6 C7 C8 120.04(18) . . ?
C6 C7 H7 120.0 . . ?
C8 C7 H7 120.0 . . ?
C9 C8 C7 119.57(17) . . ?
C9 C8 H8 120.2 . . ?
C7 C8 H8 120.2 . . ?
C10 C9 C8 120.43(18) . . ?
C10 C9 H9 119.8 . . ?
C8 C9 H9 119.8 . . ?
C9 C10 C5 120.92(18) . . ?
C9 C10 H10 119.5 . . ?
C5 C10 H10 119.5 . . ?
C16 C11 C12 117.54(15) . . ?
C16 C11 C4 121.39(15) . . ?
C12 C11 C4 121.04(16) . . ?
C13 C12 C11 121.30(17) . . ?
C13 C12 H12 119.3 . . ?
C11 C12 H12 119.3 . . ?
C12 C13 C14 120.28(17) . . ?
C12 C13 H13 119.9 . . ?
C14 C13 H13 119.9 . . ?
C15 C14 C13 119.30(17) . . ?
C15 C14 H14 120.4 . . ?
C13 C14 H14 120.4 . . ?
C14 C15 C16 120.73(18) . . ?
C14 C15 H15 119.6 . . ?
C16 C15 H15 119.6 . . ?
C15 C16 C11 120.85(16) . . ?
C15 C16 H16 119.6 . . ?
C11 C16 H16 119.6 . . ?
C18 C17 C22 119.09(14) . . ?
C18 C17 P1 121.84(13) . . ?
C22 C17 P1 119.06(13) . . ?
C19 C18 C17 120.43(17) . . ?
C19 C18 H18 119.8 . . ?
C17 C18 H18 119.8 . . ?
C20 C19 C18 119.98(18) . . ?
C20 C19 H19 120.0 . . ?
C18 C19 H19 120.0 . . ?
C21 C20 C19 120.21(16) . . ?
C21 C20 H20 119.9 . . ?
C19 C20 H20 119.9 . . ?
C20 C21 C22 119.75(17) . . ?
C20 C21 H21 120.1 . . ?
C22 C21 H21 120.1 . . ?
C21 C22 C17 120.53(17) . . ?
C21 C22 H22 119.7 . . ?
C17 C22 H22 119.7 . . ?

_diffrn_measured_fraction_theta_max 0.976
_diffrn_reflns_theta_full        30.03
_diffrn_measured_fraction_theta_full 0.976
_refine_diff_density_max         0.219
_refine_diff_density_min         -0.188
_refine_diff_density_rms         0.041

#===EN



_database_code_depnum_ccdc_archive 'CCDC 926969'