Supplementary Material (ESI) for Chemical Communications
This journal is © The Royal Society of Chemistry 2002
data_global

_journal_coden_Cambridge      182

loop_
_publ_author_name
'Danopoulos, Andreas'
'Gelbrich, Thomas'
'Hursthouse, Michael B.'
'Tooze, R. P.'
'Winston, Scott'

_publ_requested_journal               ' ChemComm'


_publ_contact_author_name     	'Dr Andreas Danopoulos'  
_publ_contact_author_address 
;
Chemistry
University of Southampton
Highfield
Southampton
Hants
SO17 1BJ
UNITED KINGDOM
;


_publ_contact_author_email            'ad1@soton.ac.uk'


_publ_section_title
;
Synthesis and Structural Characterisation of Stable Pyridine- and Phosphine-
functionalised N-heterocyclic Carbenes
;

_publ_section_references
;
WinGX L.J. Farrugia, J. Appl. Cryst., 1999, 32, 837-838.
ORTEP3 for Windows - L. J. Farrugia, J. Appl. Crystallogr. 1997, 30, 565.
PLATON/PLUTON - (a) A. L. Spek, Acta Crystallogr., Sect A 1990, 46, C34. (b) 
PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The 
Netherlands, A. L. Spek, 1998. 
SHELX97 [Includes SHELXS97, SHELXL97, CIFTAB (and SHELXA?) ] - Programs for 
Crystal Structure Analysis (Release 97-2). G. M. Sheldrick, Institüt für 
Anorganische Chemie der Universität, Tammanstrasse 4, D-3400 Göttingen, Germany, 
1998. 
;

data_COMPOUND-I-pyridinecarbene

_database_code_CSD	176893


_audit_creation_method            SHELXL
_chemical_name_systematic
;
[1-(2-pyridyl-6-trimethylsilyl)]-3-[(2,6-diisopropyl)phenyl]-imidazol-2-ylidene
;
_chemical_name_common             01SW061
_chemical_formula_moiety          ?
_chemical_formula_structural      ?
_chemical_formula_analytical      ?
_chemical_formula_sum             'C23 H31 N3 Si'
_chemical_formula_weight          377.6
_chemical_melting_point           ?
_chemical_compound_source         ?

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'
'Si'  'Si'   0.0817   0.0704
'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/n

loop_
_symmetry_equiv_pos_as_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                    22.1736(5)
_cell_length_b                    10.6162(2)
_cell_length_c                    22.1766(6)
_cell_angle_alpha                 90.00
_cell_angle_beta                  99.1950(10)
_cell_angle_gamma                 90.00
_cell_volume                      5153.3(2)
_cell_formula_units_Z             8
_cell_measurement_temperature     150(2)
_cell_measurement_reflns_used     50084
_cell_measurement_theta_min       2.91
_cell_measurement_theta_max       27.48

_exptl_crystal_description        Plate
_exptl_crystal_colour             Yellow
_exptl_crystal_size_max           0.15
_exptl_crystal_size_mid           0.15
_exptl_crystal_size_min           0.03
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     0.973
_exptl_crystal_density_method     ?
_exptl_crystal_F_000              1632
_exptl_absorpt_coefficient_mu     0.101
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.95813
_exptl_absorpt_correction_T_max   1.05349

_exptl_special_details
;
SORTAV; Blessing, 1997
;

_diffrn_ambient_temperature       150(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'Nonius FR591 rotating anode'
_diffrn_radiation_monochromator   graphite
_diffrn_measurement_device        'Nonius KappaCCD Area Detector'
_diffrn_measurement_method        'Phi and Omega scans to fill Ewald Sphere'
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             44430
_diffrn_reflns_av_R_equivalents   0.1776
_diffrn_reflns_av_sigmaI/netI     0.1916
_diffrn_reflns_limit_h_min        -24
_diffrn_reflns_limit_h_max        28
_diffrn_reflns_limit_k_min        -13
_diffrn_reflns_limit_k_max        13
_diffrn_reflns_limit_l_min        -28
_diffrn_reflns_limit_l_max        28
_diffrn_reflns_theta_min          2.93
_diffrn_reflns_theta_max          25.00
_reflns_number_total              9033
_reflns_number_observed           3482
_reflns_observed_criterion        >2sigma(I)

_computing_data_collection        'Collect (Nonius BV, 1997-2000)'
_computing_cell_refinement        'Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction         'Denzo a. Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement   'SHELXL-93 (Sheldrick, 1993)'
_computing_molecular_graphics     'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material   'PLATON (Spek, 1990)'

_refine_special_details
;
Refinement on F^2^ for ALL reflections except for 1851 with very negative F^2^
or flagged by the user for potential systematic errors.  Weighted R-factors
wR and all goodnesses 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 observed criterion
of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+10.0000P] 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     ?
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          7182
_refine_ls_number_parameters      503
_refine_ls_number_restraints      18
_refine_ls_R_factor_all           0.2662
_refine_ls_R_factor_obs           0.1042
_refine_ls_wR_factor_all          0.3041
_refine_ls_wR_factor_obs          0.1792
_refine_ls_goodness_of_fit_all    1.296
_refine_ls_goodness_of_fit_obs    1.720
_refine_ls_restrained_S_all       1.897
_refine_ls_restrained_S_obs       1.715
_refine_ls_shift/esd_max          0.002
_refine_ls_shift/esd_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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
C1 C 0.4370(3) 0.6406(6) 0.1453(3) 0.031(2) Uani 1 d . .
C2 C 0.4211(3) 0.8531(6) 0.1363(3) 0.034(2) Uani 1 d . .
H2 H 0.4001(3) 0.9314(6) 0.1307(3) 0.040 Uiso 1 calc R .
C3 C 0.4804(3) 0.8363(5) 0.1457(3) 0.033(2) Uani 1 d . .
H3 H 0.5108(3) 0.9000(5) 0.1482(3) 0.039 Uiso 1 calc R .
C4 C 0.5491(3) 0.6506(6) 0.1619(3) 0.027(2) Uani 1 d . .
C5 C 0.3291(4) 0.6151(8) 0.2794(4) 0.087(3) Uani 1 d . .
H5A H 0.3513(22) 0.6328(19) 0.3204(8) 0.130 Uiso 1 calc R .
H5B H 0.3485(23) 0.5441(16) 0.2616(14) 0.130 Uiso 1 calc R .
H5C H 0.2866(4) 0.5937(32) 0.2820(21) 0.130 Uiso 1 calc R .
C6 C 0.6132(3) 0.4737(6) 0.1868(3) 0.043(2) Uani 1 d . .
H6 H 0.6192(3) 0.3875(6) 0.1976(3) 0.051 Uiso 1 calc R .
C7 C 0.5554(3) 0.5228(6) 0.1762(3) 0.035(2) Uani 1 d . .
H7 H 0.5207(3) 0.4716(6) 0.1786(3) 0.042 Uiso 1 calc R .
C8 C 0.6625(3) 0.5485(6) 0.1817(3) 0.041(2) Uani 1 d . .
H8 H 0.7026(3) 0.5144(6) 0.1890(3) 0.049 Uiso 1 calc R .
C9 C 0.6534(3) 0.6751(6) 0.1657(3) 0.038(2) Uani 1 d . .
C10 C 0.7279(3) 0.7741(8) 0.0717(3) 0.064(2) Uani 1 d . .
H10A H 0.7396(20) 0.6882(13) 0.0622(6) 0.096 Uiso 1 calc R .
H10B H 0.7601(15) 0.8328(32) 0.0645(6) 0.096 Uiso 1 calc R .
H10C H 0.6896(7) 0.7967(41) 0.0454(3) 0.096 Uiso 1 calc R .
C11 C 0.7882(3) 0.7307(7) 0.2031(3) 0.060(2) Uani 1 d . .
H11A H 0.7979(12) 0.6441(17) 0.1927(14) 0.090 Uiso 1 calc R .
H11B H 0.7819(7) 0.7339(40) 0.2459(4) 0.090 Uiso 1 calc R .
H11C H 0.8220(5) 0.7865(27) 0.1975(15) 0.090 Uiso 1 calc R .
C12 C 0.6975(3) 0.9455(6) 0.1713(4) 0.058(2) Uani 1 d . .
H12A H 0.7308(9) 1.0023(8) 0.1650(19) 0.088 Uiso 1 calc R .
H12B H 0.6913(19) 0.9498(10) 0.2140(6) 0.088 Uiso 1 calc R .
H12C H 0.6599(11) 0.9709(15) 0.1446(14) 0.088 Uiso 1 calc R .
C13 C 0.3302(3) 0.7093(5) 0.1252(3) 0.029(2) Uani 1 d . .
C14 C 0.2995(3) 0.7054(6) 0.1754(3) 0.036(2) Uani 1 d . .
C15 C 0.2376(3) 0.6784(6) 0.1636(4) 0.047(2) Uani 1 d . .
H15 H 0.2150(3) 0.6735(6) 0.1965(4) 0.056 Uiso 1 calc R .
C16 C 0.2079(3) 0.6581(6) 0.1035(4) 0.048(2) Uani 1 d . .
H16 H 0.1654(3) 0.6401(6) 0.0959(4) 0.057 Uiso 1 calc R .
C17 C 0.2400(3) 0.6642(6) 0.0566(4) 0.045(2) Uani 1 d . .
H17 H 0.2193(3) 0.6489(6) 0.0164(4) 0.055 Uiso 1 calc R .
C18 C 0.3021(3) 0.6919(6) 0.0651(3) 0.035(2) Uani 1 d . .
C19 C 0.3364(3) 0.7042(7) 0.0119(3) 0.048(2) Uani 1 d . .
H19 H 0.3809(3) 0.7128(7) 0.0285(3) 0.057 Uiso 1 calc R .
C20 C 0.3283(4) 0.5911(9) -0.0284(4) 0.085(3) Uani 1 d . .
H20A H 0.3498(21) 0.5194(15) -0.0070(10) 0.127 Uiso 1 calc R .
H20B H 0.3451(22) 0.6082(19) -0.0658(11) 0.127 Uiso 1 calc R .
H20C H 0.2847(4) 0.5715(32) -0.0388(21) 0.127 Uiso 1 calc R .
C21 C 0.3156(4) 0.8248(8) -0.0252(4) 0.081(3) Uani 1 d . .
H21A H 0.3392(18) 0.8339(28) -0.0588(15) 0.122 Uiso 1 calc R .
H21B H 0.3223(23) 0.8986(10) 0.0016(7) 0.122 Uiso 1 calc R .
H21C H 0.2720(7) 0.8182(23) -0.0420(21) 0.122 Uiso 1 calc R .
C22 C 0.3306(3) 0.7296(7) 0.2396(3) 0.047(2) Uani 1 d . .
H22 H 0.3744(3) 0.7492(7) 0.2379(3) 0.057 Uiso 1 calc R .
C23 C 0.3033(4) 0.8439(8) 0.2686(4) 0.087(3) Uani 1 d . .
H23A H 0.3002(24) 0.9153(18) 0.2403(11) 0.131 Uiso 1 calc R .
H23B H 0.3298(15) 0.8668(35) 0.3068(14) 0.131 Uiso 1 calc R .
H23C H 0.2626(12) 0.8223(19) 0.2773(25) 0.131 Uiso 1 calc R .
C24 C 0.7108(3) 0.6664(5) 0.8943(3) 0.031(2) Uani 1 d . .
H24 H 0.7411(3) 0.6026(5) 0.9025(3) 0.038 Uiso 1 calc R .
C25 C 0.6672(3) 0.8636(5) 0.8839(3) 0.030(2) Uani 1 d . .
C26 C 0.6516(3) 0.6494(5) 0.8744(3) 0.033(2) Uani 1 d . .
H26 H 0.6310(3) 0.5713(5) 0.8663(3) 0.040 Uiso 1 calc R .
C28 C 0.7761(3) 0.8536(5) 0.9247(3) 0.027(2) Uani 1 d . .
C29 C 0.7845(3) 0.9822(5) 0.9215(3) 0.036(2) Uani 1 d . .
H29 H 0.7521(3) 1.0355(5) 0.9036(3) 0.043 Uiso 1 calc R .
C30 C 0.8398(3) 1.0303(6) 0.9446(3) 0.045(2) Uani 1 d . .
H30 H 0.8470(3) 1.1184(6) 0.9429(3) 0.054 Uiso 1 calc R .
C31 C 0.8857(3) 0.9502(6) 0.9708(3) 0.045(2) Uani 1 d . .
H31 H 0.9247(3) 0.9832(6) 0.9872(3) 0.054 Uiso 1 calc R .
C32 C 0.8751(3) 0.8226(6) 0.9730(3) 0.034(2) Uani 1 d . .
C33 C 1.0075(3) 0.7712(7) 1.0310(3) 0.055(2) Uani 1 d U .
H33A H 1.0044(4) 0.8399(27) 1.0598(15) 0.083 Uiso 1 calc R .
H33B H 1.0229(9) 0.8042(35) 0.9951(4) 0.083 Uiso 1 calc R .
H33C H 1.0356(6) 0.7068(12) 1.0507(17) 0.083 Uiso 1 calc R .
C34 C 0.9342(4) 0.5818(8) 0.9464(5) 0.110(4) Uani 1 d U .
H34A H 0.9607(25) 0.5120(31) 0.9630(9) 0.165 Uiso 1 calc R .
H34B H 0.9506(28) 0.6208(18) 0.9124(14) 0.165 Uiso 1 calc R .
H34C H 0.8930(6) 0.5498(47) 0.9318(22) 0.165 Uiso 1 calc R .
C35 C 0.9014(4) 0.6326(9) 1.0710(5) 0.109(4) Uani 1 d U .
H35A H 0.9013(29) 0.6966(20) 1.1029(13) 0.164 Uiso 1 calc R .
H35B H 0.9273(19) 0.5618(42) 1.0874(20) 0.164 Uiso 1 calc R .
H35C H 0.8596(12) 0.6027(58) 1.0576(8) 0.164 Uiso 1 calc R .
C36 C 0.5620(3) 0.7924(6) 0.8524(3) 0.030(2) Uani 1 d . .
C37 C 0.5373(3) 0.8161(6) 0.7919(3) 0.036(2) Uani 1 d . .
C38 C 0.5272(3) 0.7914(5) 0.8991(3) 0.031(2) Uani 1 d . .
C39 C 0.4749(3) 0.8409(6) 0.7785(4) 0.046(2) Uani 1 d . .
H39 H 0.4564(3) 0.8566(6) 0.7376(4) 0.055 Uiso 1 calc R .
C40 C 0.4403(3) 0.8425(6) 0.8245(4) 0.050(2) Uani 1 d . .
H40 H 0.3979(3) 0.8612(6) 0.8149(4) 0.060 Uiso 1 calc R .
C41 C 0.4656(3) 0.8175(6) 0.8845(4) 0.042(2) Uani 1 d . .
H41 H 0.4407(3) 0.8183(6) 0.9155(4) 0.050 Uiso 1 calc R .
C42 C 0.5752(3) 0.8130(8) 0.7415(3) 0.061(2) Uani 1 d . .
H42 H 0.6191(3) 0.8161(8) 0.7611(3) 0.073 Uiso 1 calc R .
C43 C 0.5636(4) 0.9275(8) 0.6980(4) 0.091(3) Uani 1 d . .
H43A H 0.5953(15) 0.9308(32) 0.6719(18) 0.136 Uiso 1 calc R .
H43B H 0.5648(26) 1.0051(9) 0.7221(4) 0.136 Uiso 1 calc R .
H43C H 0.5235(12) 0.9191(28) 0.6725(18) 0.136 Uiso 1 calc R .
C44 C 0.5658(5) 0.6914(8) 0.7067(4) 0.099(3) Uani 1 d . .
H44A H 0.5855(24) 0.6966(23) 0.6702(15) 0.148 Uiso 1 calc R .
H44B H 0.5220(5) 0.6763(30) 0.6944(25) 0.148 Uiso 1 calc R .
H44C H 0.5838(25) 0.6220(11) 0.7326(10) 0.148 Uiso 1 calc R .
C45 C 0.5560(3) 0.7603(6) 0.9643(3) 0.043(2) Uani 1 d . .
H45 H 0.6002(3) 0.7427(6) 0.9635(3) 0.051 Uiso 1 calc R .
C46 C 0.5290(4) 0.6404(7) 0.9890(4) 0.082(3) Uani 1 d . .
H46A H 0.5528(16) 0.6181(30) 1.0286(12) 0.123 Uiso 1 calc R .
H46B H 0.5305(23) 0.5710(15) 0.9601(12) 0.123 Uiso 1 calc R .
H46C H 0.4865(9) 0.6561(18) 0.9938(24) 0.123 Uiso 1 calc R .
C47 C 0.5536(4) 0.8693(7) 1.0072(4) 0.067(2) Uani 1 d . .
H47A H 0.5766(18) 0.8482(18) 1.0474(7) 0.101 Uiso 1 calc R .
H47B H 0.5110(4) 0.8866(29) 1.0111(17) 0.101 Uiso 1 calc R .
H47C H 0.5715(20) 0.9439(13) 0.9911(11) 0.101 Uiso 1 calc R .
Si1 Si 0.71733(8) 0.7828(2) 0.15277(9) 0.0407(5) Uani 1 d . .
Si2 Si 0.93092(9) 0.7004(2) 1.00697(10) 0.0522(6) Uani 1 d . .
N1 N 0.5955(2) 0.7259(4) 0.1561(2) 0.0324(13) Uani 1 d . .
N2 N 0.4904(2) 0.7070(4) 0.1510(2) 0.0298(12) Uani 1 d . .
N3 N 0.3948(2) 0.7346(4) 0.1362(2) 0.0296(12) Uani 1 d . .
N4 N 0.8201(2) 0.7751(4) 0.9482(2) 0.0322(13) Uani 1 d . .
N5 N 0.7200(2) 0.7956(4) 0.9007(2) 0.0277(12) Uani 1 d . .
N6 N 0.6261(2) 0.7694(5) 0.8677(2) 0.0308(13) Uani 1 d . .

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
C1 0.034(4) 0.029(4) 0.030(4) -0.001(3) 0.006(3) 0.001(3)
C2 0.041(5) 0.020(4) 0.041(4) 0.001(3) 0.009(3) 0.003(3)
C3 0.026(4) 0.023(4) 0.047(5) -0.004(3) -0.001(3) -0.002(3)
C4 0.023(4) 0.026(4) 0.032(4) -0.003(3) 0.000(3) 0.001(3)
C5 0.106(8) 0.094(7) 0.054(6) 0.023(5) -0.002(5) -0.003(6)
C6 0.042(5) 0.031(4) 0.052(5) -0.001(4) -0.003(4) 0.003(4)
C7 0.029(4) 0.033(4) 0.041(5) -0.001(3) -0.001(3) -0.002(3)
C8 0.030(4) 0.033(4) 0.057(5) -0.007(4) -0.004(4) 0.001(3)
C9 0.033(4) 0.033(4) 0.046(5) -0.007(3) -0.005(3) 0.007(3)
C10 0.048(5) 0.086(6) 0.057(5) -0.020(5) 0.009(4) -0.016(4)
C11 0.041(4) 0.055(5) 0.078(6) -0.001(5) -0.009(4) -0.004(4)
C12 0.060(5) 0.042(4) 0.071(6) 0.004(4) 0.006(4) -0.007(4)
C13 0.028(4) 0.020(3) 0.040(4) 0.000(3) 0.006(3) 0.003(3)
C14 0.038(4) 0.033(4) 0.038(4) 0.009(4) 0.009(4) 0.005(3)
C15 0.041(5) 0.038(4) 0.061(6) 0.010(4) 0.011(4) 0.004(4)
C16 0.031(4) 0.028(4) 0.082(7) 0.005(4) 0.006(5) -0.002(3)
C17 0.045(5) 0.033(4) 0.055(5) -0.003(4) -0.004(4) 0.003(4)
C18 0.033(4) 0.033(4) 0.038(4) -0.006(4) -0.003(3) 0.004(3)
C19 0.036(4) 0.062(5) 0.043(5) -0.013(4) 0.001(4) -0.002(4)
C20 0.090(7) 0.099(7) 0.069(7) -0.020(6) 0.023(6) 0.002(6)
C21 0.058(6) 0.090(7) 0.099(7) 0.033(6) 0.026(5) 0.008(5)
C22 0.047(5) 0.054(5) 0.041(5) 0.002(4) 0.006(4) 0.000(4)
C23 0.077(6) 0.099(7) 0.081(7) -0.034(6) -0.003(5) 0.017(5)
C24 0.039(4) 0.020(4) 0.033(4) -0.001(3) -0.001(3) 0.006(3)
C25 0.028(4) 0.025(3) 0.035(4) 0.002(3) -0.002(3) -0.001(3)
C26 0.038(4) 0.017(3) 0.042(4) -0.005(3) 0.002(3) 0.000(3)
C28 0.025(4) 0.023(4) 0.033(4) -0.001(3) 0.001(3) 0.005(3)
C29 0.030(4) 0.022(4) 0.052(5) 0.005(3) -0.004(3) 0.005(3)
C30 0.039(5) 0.021(4) 0.069(5) 0.005(4) -0.008(4) -0.001(3)
C31 0.030(4) 0.036(4) 0.065(5) -0.005(4) -0.006(4) -0.005(3)
C32 0.026(4) 0.040(4) 0.036(4) -0.005(3) 0.001(3) -0.007(3)
C33 0.044(4) 0.052(5) 0.064(5) 0.000(4) -0.009(4) 0.000(4)
C34 0.077(7) 0.060(6) 0.166(10) -0.056(6) -0.063(7) 0.032(5)
C35 0.041(5) 0.131(8) 0.152(10) 0.094(8) 0.002(6) 0.005(5)
C36 0.020(4) 0.030(4) 0.038(4) 0.005(3) -0.003(3) -0.003(3)
C37 0.033(4) 0.030(4) 0.044(5) -0.007(3) 0.001(4) -0.003(3)
C38 0.027(4) 0.026(4) 0.040(4) 0.002(3) 0.000(3) 0.001(3)
C39 0.041(5) 0.045(5) 0.049(5) -0.005(4) -0.007(4) -0.001(4)
C40 0.030(4) 0.025(4) 0.090(7) 0.001(4) -0.002(5) 0.007(3)
C41 0.031(4) 0.038(4) 0.058(5) 0.002(4) 0.010(4) 0.005(3)
C42 0.052(5) 0.091(7) 0.039(5) 0.005(5) 0.003(4) 0.008(5)
C43 0.118(8) 0.086(7) 0.070(7) 0.024(6) 0.022(6) 0.008(6)
C44 0.152(10) 0.083(7) 0.073(7) -0.028(6) 0.051(7) 0.014(6)
C45 0.041(4) 0.048(5) 0.040(5) 0.001(4) 0.009(4) -0.003(3)
C46 0.115(8) 0.056(5) 0.074(7) 0.012(5) 0.011(6) -0.025(5)
C47 0.084(6) 0.054(5) 0.060(6) 0.003(5) -0.001(5) 0.010(5)
Si1 0.0304(11) 0.0429(11) 0.0473(13) 0.0003(11) 0.0021(9) -0.0002(9)
Si2 0.0359(12) 0.0385(12) 0.074(2) 0.0060(12) -0.0152(11) 0.0001(10)
N1 0.035(3) 0.028(3) 0.033(3) -0.006(3) 0.002(3) -0.001(3)
N2 0.029(3) 0.022(3) 0.038(3) 0.000(3) 0.002(2) -0.004(3)
N3 0.031(3) 0.019(3) 0.040(3) -0.001(3) 0.008(3) 0.001(3)
N4 0.031(3) 0.028(3) 0.039(3) 0.000(3) 0.006(3) 0.001(3)
N5 0.024(3) 0.022(3) 0.037(3) 0.002(3) 0.000(2) 0.003(2)
N6 0.029(3) 0.030(3) 0.033(3) 0.000(3) 0.003(3) 0.000(3)

_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
C1 N2 1.366(7) . ?
C1 N3 1.360(7) . ?
C2 C3 1.311(7) . ?
C2 N3 1.387(7) . ?
C3 N2 1.392(7) . ?
C4 N1 1.326(7) . ?
C4 C7 1.396(8) . ?
C4 N2 1.417(7) . ?
C5 C22 1.506(10) . ?
C6 C7 1.369(8) . ?
C6 C8 1.370(8) . ?
C8 C9 1.396(8) . ?
C9 N1 1.377(7) . ?
C9 Si1 1.877(7) . ?
C10 Si1 1.853(7) . ?
C11 Si1 1.861(6) . ?
C12 Si1 1.845(7) . ?
C13 C18 1.390(8) . ?
C13 C14 1.395(8) . ?
C13 N3 1.439(7) . ?
C14 C15 1.385(8) . ?
C14 C22 1.502(9) . ?
C15 C16 1.405(9) . ?
C16 C17 1.352(9) . ?
C17 C18 1.392(8) . ?
C18 C19 1.508(9) . ?
C19 C20 1.489(10) . ?
C19 C21 1.553(10) . ?
C22 C23 1.542(10) . ?
C24 C26 1.328(8) . ?
C24 N5 1.390(7) . ?
C25 N6 1.361(7) . ?
C25 N5 1.376(7) . ?
C26 N6 1.392(7) . ?
C28 N4 1.325(7) . ?
C28 C29 1.381(8) . ?
C28 N5 1.413(7) . ?
C29 C30 1.352(8) . ?
C30 C31 1.381(8) . ?
C31 C32 1.378(8) . ?
C32 N4 1.352(7) . ?
C32 Si2 1.867(6) . ?
C33 Si2 1.856(6) . ?
C34 Si2 1.850(9) . ?
C35 Si2 1.806(9) . ?
C36 C38 1.387(8) . ?
C36 C37 1.390(8) . ?
C36 N6 1.429(7) . ?
C37 C39 1.393(8) . ?
C37 C42 1.501(9) . ?
C38 C41 1.380(8) . ?
C38 C45 1.520(9) . ?
C39 C40 1.371(9) . ?
C40 C41 1.385(9) . ?
C42 C44 1.502(10) . ?
C42 C43 1.548(10) . ?
C45 C47 1.504(9) . ?
C45 C46 1.544(9) . ?

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 C1 N3 101.6(5) . . ?
C3 C2 N3 106.7(5) . . ?
C2 C3 N2 106.9(5) . . ?
N1 C4 C7 123.8(6) . . ?
N1 C4 N2 115.8(5) . . ?
C7 C4 N2 120.3(6) . . ?
C7 C6 C8 120.2(6) . . ?
C6 C7 C4 117.8(6) . . ?
C6 C8 C9 119.7(6) . . ?
N1 C9 C8 120.6(6) . . ?
N1 C9 Si1 116.5(4) . . ?
C8 C9 Si1 122.9(5) . . ?
C18 C13 C14 124.0(6) . . ?
C18 C13 N3 118.0(6) . . ?
C14 C13 N3 118.0(6) . . ?
C15 C14 C13 116.8(6) . . ?
C15 C14 C22 120.3(6) . . ?
C13 C14 C22 122.9(6) . . ?
C14 C15 C16 120.7(7) . . ?
C17 C16 C15 119.8(7) . . ?
C16 C17 C18 122.5(7) . . ?
C17 C18 C13 116.1(6) . . ?
C17 C18 C19 121.7(6) . . ?
C13 C18 C19 122.2(6) . . ?
C20 C19 C18 111.8(6) . . ?
C20 C19 C21 110.5(6) . . ?
C18 C19 C21 109.9(6) . . ?
C14 C22 C5 111.5(6) . . ?
C14 C22 C23 112.3(6) . . ?
C5 C22 C23 110.1(7) . . ?
C26 C24 N5 106.8(5) . . ?
N6 C25 N5 101.0(5) . . ?
C24 C26 N6 105.9(5) . . ?
N4 C28 C29 123.0(6) . . ?
N4 C28 N5 115.0(5) . . ?
C29 C28 N5 122.0(5) . . ?
C30 C29 C28 118.4(6) . . ?
C29 C30 C31 119.3(6) . . ?
C32 C31 C30 120.1(6) . . ?
N4 C32 C31 120.0(6) . . ?
N4 C32 Si2 113.7(4) . . ?
C31 C32 Si2 126.3(5) . . ?
C38 C36 C37 122.9(5) . . ?
C38 C36 N6 118.3(5) . . ?
C37 C36 N6 118.8(6) . . ?
C36 C37 C39 117.6(6) . . ?
C36 C37 C42 122.3(6) . . ?
C39 C37 C42 120.1(7) . . ?
C41 C38 C36 118.0(6) . . ?
C41 C38 C45 121.2(6) . . ?
C36 C38 C45 120.8(5) . . ?
C40 C39 C37 120.0(7) . . ?
C39 C40 C41 121.5(6) . . ?
C38 C41 C40 119.9(7) . . ?
C44 C42 C37 110.7(7) . . ?
C44 C42 C43 111.0(7) . . ?
C37 C42 C43 112.9(7) . . ?
C47 C45 C38 112.5(6) . . ?
C47 C45 C46 110.7(6) . . ?
C38 C45 C46 112.8(6) . . ?
C12 Si1 C10 109.5(4) . . ?
C12 Si1 C11 110.7(3) . . ?
C10 Si1 C11 110.0(3) . . ?
C12 Si1 C9 108.9(3) . . ?
C10 Si1 C9 109.5(3) . . ?
C11 Si1 C9 108.2(3) . . ?
C35 Si2 C34 111.2(5) . . ?
C35 Si2 C33 111.4(4) . . ?
C34 Si2 C33 110.1(4) . . ?
C35 Si2 C32 107.1(3) . . ?
C34 Si2 C32 106.3(3) . . ?
C33 Si2 C32 110.6(3) . . ?
C4 N1 C9 118.0(5) . . ?
C1 N2 C3 112.2(5) . . ?
C1 N2 C4 123.8(5) . . ?
C3 N2 C4 124.0(5) . . ?
C1 N3 C2 112.7(5) . . ?
C1 N3 C13 122.1(5) . . ?
C2 N3 C13 125.1(5) . . ?
C28 N4 C32 119.0(5) . . ?
C25 N5 C24 112.6(5) . . ?
C25 N5 C28 122.2(5) . . ?
C24 N5 C28 125.1(5) . . ?
C25 N6 C26 113.6(5) . . ?
C25 N6 C36 122.4(5) . . ?
C26 N6 C36 123.6(5) . . ?

_refine_diff_density_max    0.852
_refine_diff_density_min   -0.363
_refine_diff_density_rms    0.074

#===END

data_COMPOUND-II-phosphinecarbene

_database_code_CSD	176894


_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
1-[b-(diphenylphosphino)ethyl]-3-[(2,6-diisopropyl)phenyl]-imidazol-2-ylidene
;
_chemical_name_common             01SW077
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum             'C29 H33 N2 P'
_chemical_formula_weight          440.54

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'
'N'  'N'   0.0061   0.0033
'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

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                    16.1180(13)
_cell_length_b                    11.4876(8)
_cell_length_c                    14.2506(8)
_cell_angle_alpha                 90.00
_cell_angle_beta                  108.920(2)
_cell_angle_gamma                 90.00
_cell_volume                      2496.0(3)
_cell_formula_units_Z             4
_cell_measurement_temperature     150(2)
_cell_measurement_reflns_used     18529
_cell_measurement_theta_min       2.91
_cell_measurement_theta_max       25.35

_exptl_crystal_description        Plate
_exptl_crystal_colour             Clear
_exptl_crystal_size_max           0.04
_exptl_crystal_size_mid           0.03
_exptl_crystal_size_min           0.01
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.172
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              944
_exptl_absorpt_coefficient_mu     0.129
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.9949
_exptl_absorpt_correction_T_max   0.9987
_exptl_absorpt_process_details    ?

_exptl_special_details
;
SORTAV, Blessing 1997
;

_diffrn_ambient_temperature       150(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'Nonius FR591 rotating anode'
_diffrn_radiation_monochromator   graphite
_diffrn_measurement_device_type   'Nonius KappaCCD Area Detector'
_diffrn_measurement_method        'Phi and Omega scans to fill Ewald Sphere'
_diffrn_detector_area_resol_mean  ?
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             8197
_diffrn_reflns_av_R_equivalents   0.0669
_diffrn_reflns_av_sigmaI/netI     0.1066
_diffrn_reflns_limit_h_min        -19
_diffrn_reflns_limit_h_max        19
_diffrn_reflns_limit_k_min        -13
_diffrn_reflns_limit_k_max        13
_diffrn_reflns_limit_l_min        -17
_diffrn_reflns_limit_l_max        17
_diffrn_reflns_theta_min          2.92
_diffrn_reflns_theta_max          25.37
_reflns_number_total              4505
_reflns_number_gt                 2636
_reflns_threshold_expression      >2sigma(I)

_computing_data_collection        'Collect (Nonius BV, 1997-2000)'
_computing_cell_refinement        'Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction         'Denzo a. Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution     'DirDiff-99.2 (1999)'
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material   'PLATON (Spek, 1990)'

_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^)+(0.0468P)^2^+1.2064P] 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     mixed
_refine_ls_extinction_method      SHELXL
_refine_ls_extinction_coef        0.0073(10)
_refine_ls_extinction_expression
'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^'
_refine_ls_number_reflns          4505
_refine_ls_number_parameters      294
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.1183
_refine_ls_R_factor_gt            0.0567
_refine_ls_wR_factor_ref          0.1434
_refine_ls_wR_factor_gt           0.1144
_refine_ls_goodness_of_fit_ref    0.968
_refine_ls_restrained_S_all       0.968
_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
C1 C 0.4710(2) 0.0249(2) 0.2188(2) 0.0315(7) Uani 1 1 d . . .
C2 C 0.5402(2) 0.1977(2) 0.2822(2) 0.0324(7) Uani 1 1 d . . .
H2 H 0.5853 0.2508 0.3152 0.039 Uiso 1 1 calc R . .
C3 C 0.4555(2) 0.2223(2) 0.2369(2) 0.0330(7) Uani 1 1 d . . .
H3 H 0.4284 0.2965 0.2315 0.040 Uiso 1 1 calc R . .
C4 C 0.63167(19) 0.0196(2) 0.3047(2) 0.0270(7) Uani 1 1 d . . .
C5 C 0.6639(2) -0.0192(2) 0.4025(2) 0.0291(7) Uani 1 1 d . . .
C6 C 0.7465(2) -0.0696(2) 0.4342(2) 0.0343(7) Uani 1 1 d . . .
H6 H 0.7705 -0.0950 0.5010 0.041 Uiso 1 1 calc R . .
C7 C 0.7944(2) -0.0836(3) 0.3705(2) 0.0377(8) Uani 1 1 d . . .
H7 H 0.8509 -0.1184 0.3936 0.045 Uiso 1 1 calc R . .
C8 C 0.7603(2) -0.0472(3) 0.2736(2) 0.0368(8) Uani 1 1 d . . .
H8 H 0.7935 -0.0582 0.2301 0.044 Uiso 1 1 calc R . .
C9 C 0.6780(2) 0.0057(2) 0.2377(2) 0.0313(7) Uani 1 1 d . . .
C10 C 0.6400(2) 0.0395(3) 0.1294(2) 0.0364(8) Uani 1 1 d . . .
H10 H 0.5909 0.0956 0.1226 0.044 Uiso 1 1 calc R . .
C11 C 0.6022(2) -0.0680(3) 0.0671(2) 0.0445(9) Uani 1 1 d . . .
H11A H 0.6489 -0.1253 0.0744 0.067 Uiso 1 1 calc R . .
H11B H 0.5772 -0.0456 -0.0028 0.067 Uiso 1 1 calc R . .
H11C H 0.5562 -0.1021 0.0897 0.067 Uiso 1 1 calc R . .
C12 C 0.6055(2) -0.1256(3) 0.5209(2) 0.0421(8) Uani 1 1 d . . .
H12A H 0.5753 -0.1818 0.4694 0.063 Uiso 1 1 calc R . .
H12B H 0.5727 -0.1164 0.5675 0.063 Uiso 1 1 calc R . .
H12C H 0.6647 -0.1538 0.5564 0.063 Uiso 1 1 calc R . .
C13 C 0.7067(2) 0.0981(3) 0.0912(2) 0.0502(9) Uani 1 1 d . . .
H13A H 0.7339 0.1631 0.1349 0.075 Uiso 1 1 calc R . .
H13B H 0.6775 0.1274 0.0240 0.075 Uiso 1 1 calc R . .
H13C H 0.7520 0.0417 0.0899 0.075 Uiso 1 1 calc R . .
C14 C 0.6112(2) -0.0087(2) 0.4730(2) 0.0337(7) Uani 1 1 d . . .
H14 H 0.5503 0.0155 0.4335 0.040 Uiso 1 1 calc R . .
C15 C 0.6498(2) 0.0857(3) 0.5507(2) 0.0481(9) Uani 1 1 d . . .
H15A H 0.7095 0.0637 0.5910 0.072 Uiso 1 1 calc R . .
H15B H 0.6133 0.0940 0.5935 0.072 Uiso 1 1 calc R . .
H15C H 0.6514 0.1598 0.5173 0.072 Uiso 1 1 calc R . .
C16 C 0.32193(19) 0.1066(3) 0.1442(2) 0.0318(7) Uani 1 1 d . . .
H16A H 0.3119 0.0319 0.1075 0.038 Uiso 1 1 calc R . .
H16B H 0.3043 0.1703 0.0949 0.038 Uiso 1 1 calc R . .
C17 C 0.2650(2) 0.1106(3) 0.2102(2) 0.0319(7) Uani 1 1 d . . .
H17A H 0.2742 0.1854 0.2465 0.038 Uiso 1 1 calc R . .
H17B H 0.2822 0.0469 0.2596 0.038 Uiso 1 1 calc R . .
C19 C 0.1026(2) 0.1801(3) 0.2952(2) 0.0389(8) Uani 1 1 d . . .
H19 H 0.1340 0.2474 0.2872 0.047 Uiso 1 1 calc R . .
C20 C 0.0598(2) 0.1807(3) 0.3657(2) 0.0453(9) Uani 1 1 d . . .
H20 H 0.0622 0.2479 0.4053 0.054 Uiso 1 1 calc R . .
C21 C 0.0141(2) 0.0839(3) 0.3780(2) 0.0456(9) Uani 1 1 d . . .
H21 H -0.0160 0.0847 0.4254 0.055 Uiso 1 1 calc R . .
C22 C 0.0550(2) -0.0148(3) 0.2513(2) 0.0371(8) Uani 1 1 d . . .
H22 H 0.0533 -0.0831 0.2132 0.045 Uiso 1 1 calc R . .
C23 C 0.1003(2) 0.0823(3) 0.2358(2) 0.0329(7) Uani 1 1 d . . .
C24 C 0.1459(2) -0.0535(2) 0.0907(2) 0.0320(7) Uani 1 1 d . . .
C25 C 0.1924(2) -0.1471(3) 0.1472(2) 0.0394(8) Uani 1 1 d . . .
H25 H 0.2253 -0.1352 0.2150 0.047 Uiso 1 1 calc R . .
C26 C 0.1910(2) -0.2553(3) 0.1060(2) 0.0410(8) Uani 1 1 d . . .
H26 H 0.2227 -0.3176 0.1453 0.049 Uiso 1 1 calc R . .
C27 C 0.1433(2) -0.2739(3) 0.0069(2) 0.0410(8) Uani 1 1 d . . .
H27 H 0.1428 -0.3487 -0.0217 0.049 Uiso 1 1 calc R . .
C28 C 0.0970(2) -0.1842(3) -0.0495(2) 0.0401(8) Uani 1 1 d . . .
H28 H 0.0639 -0.1970 -0.1172 0.048 Uiso 1 1 calc R . .
C29 C 0.0984(2) -0.0749(3) -0.0082(2) 0.0367(8) Uani 1 1 d . . .
H29 H 0.0662 -0.0133 -0.0482 0.044 Uiso 1 1 calc R . .
C30 C 0.0119(2) -0.0137(3) 0.3217(2) 0.0427(8) Uani 1 1 d . . .
H30 H -0.0191 -0.0808 0.3308 0.051 Uiso 1 1 calc R . .
N1 N 0.41511(16) 0.11786(19) 0.19966(16) 0.0287(6) Uani 1 1 d . . .
N2 N 0.54868(16) 0.07880(19) 0.27112(16) 0.0272(6) Uani 1 1 d . . .
P1 P 0.14820(5) 0.09517(7) 0.13636(6) 0.0323(2) Uani 1 1 d . . .

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
C1 0.036(2) 0.0326(17) 0.0245(16) -0.0017(13) 0.0079(14) 0.0043(14)
C2 0.042(2) 0.0242(16) 0.0309(17) -0.0028(12) 0.0125(15) -0.0023(14)
C3 0.044(2) 0.0246(17) 0.0305(16) -0.0004(13) 0.0128(15) 0.0019(14)
C4 0.0289(18) 0.0244(15) 0.0253(15) -0.0013(12) 0.0057(14) 0.0000(12)
C5 0.0315(19) 0.0264(16) 0.0287(16) -0.0021(12) 0.0087(14) -0.0023(13)
C6 0.035(2) 0.0360(18) 0.0284(16) 0.0024(13) 0.0062(15) 0.0015(14)
C7 0.034(2) 0.0343(18) 0.0425(19) 0.0008(14) 0.0094(15) 0.0047(14)
C8 0.039(2) 0.0375(18) 0.0383(18) -0.0008(14) 0.0194(16) 0.0012(15)
C9 0.036(2) 0.0280(16) 0.0308(16) -0.0012(12) 0.0113(14) 0.0007(14)
C10 0.047(2) 0.0341(17) 0.0309(17) 0.0036(13) 0.0164(16) 0.0050(15)
C11 0.053(2) 0.051(2) 0.0286(17) -0.0026(15) 0.0118(16) -0.0024(17)
C12 0.051(2) 0.044(2) 0.0342(18) 0.0025(14) 0.0179(16) -0.0011(16)
C13 0.068(3) 0.046(2) 0.0419(19) 0.0066(16) 0.0237(18) -0.0059(18)
C14 0.039(2) 0.0354(17) 0.0273(16) 0.0012(13) 0.0118(14) 0.0030(14)
C15 0.068(3) 0.042(2) 0.0376(19) -0.0024(15) 0.0226(18) 0.0010(18)
C16 0.0285(18) 0.0398(18) 0.0244(15) 0.0015(13) 0.0049(13) 0.0040(14)
C17 0.0359(19) 0.0352(17) 0.0262(15) 0.0007(13) 0.0121(14) 0.0010(14)
C19 0.041(2) 0.0399(19) 0.0357(18) 0.0013(14) 0.0120(16) 0.0061(15)
C20 0.049(2) 0.050(2) 0.0365(19) -0.0006(15) 0.0128(17) 0.0146(17)
C21 0.039(2) 0.063(2) 0.0387(19) 0.0084(17) 0.0177(16) 0.0134(18)
C22 0.0330(19) 0.0416(19) 0.0350(18) 0.0027(14) 0.0087(15) 0.0038(15)
C23 0.0281(18) 0.0388(18) 0.0302(16) 0.0051(14) 0.0075(14) 0.0082(14)
C24 0.0301(19) 0.0382(18) 0.0267(16) 0.0019(13) 0.0077(14) 0.0006(14)
C25 0.040(2) 0.0414(19) 0.0316(17) 0.0021(14) 0.0049(15) 0.0023(15)
C26 0.041(2) 0.0343(19) 0.044(2) 0.0049(15) 0.0086(16) 0.0027(15)
C27 0.042(2) 0.0336(18) 0.046(2) -0.0068(15) 0.0124(17) 0.0005(15)
C28 0.037(2) 0.046(2) 0.0329(18) -0.0061(15) 0.0057(15) 0.0008(15)
C29 0.035(2) 0.0416(19) 0.0312(17) -0.0009(14) 0.0073(14) 0.0018(14)
C30 0.037(2) 0.050(2) 0.043(2) 0.0084(16) 0.0157(17) 0.0037(16)
N1 0.0335(16) 0.0323(14) 0.0213(12) -0.0006(10) 0.0102(11) 0.0026(11)
N2 0.0298(15) 0.0284(14) 0.0226(12) -0.0006(10) 0.0075(11) 0.0006(11)
P1 0.0336(5) 0.0347(5) 0.0274(4) 0.0016(3) 0.0084(3) 0.0027(4)

_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
C1 N1 1.367(4) . ?
C1 N2 1.378(4) . ?
C2 C3 1.337(4) . ?
C2 N2 1.386(3) . ?
C3 N1 1.386(4) . ?
C4 C5 1.393(4) . ?
C4 C9 1.400(4) . ?
C4 N2 1.437(4) . ?
C5 C6 1.387(4) . ?
C5 C14 1.517(4) . ?
C6 C7 1.378(4) . ?
C7 C8 1.377(4) . ?
C8 C9 1.396(4) . ?
C9 C10 1.515(4) . ?
C10 C13 1.512(4) . ?
C10 C11 1.528(4) . ?
C12 C14 1.522(4) . ?
C14 C15 1.530(4) . ?
C16 N1 1.459(4) . ?
C16 C17 1.513(4) . ?
C17 P1 1.843(3) . ?
C19 C20 1.389(4) . ?
C19 C23 1.400(4) . ?
C20 C21 1.377(5) . ?
C21 C30 1.372(4) . ?
C22 C23 1.389(4) . ?
C22 C30 1.392(4) . ?
C23 P1 1.827(3) . ?
C24 C29 1.390(4) . ?
C24 C25 1.405(4) . ?
C24 P1 1.824(3) . ?
C25 C26 1.372(4) . ?
C26 C27 1.387(4) . ?
C27 C28 1.370(4) . ?
C28 C29 1.383(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 N2 100.5(2) . . ?
C3 C2 N2 106.1(3) . . ?
C2 C3 N1 106.3(3) . . ?
C5 C4 C9 122.5(3) . . ?
C5 C4 N2 119.3(2) . . ?
C9 C4 N2 118.2(2) . . ?
C6 C5 C4 117.8(3) . . ?
C6 C5 C14 120.1(3) . . ?
C4 C5 C14 122.0(3) . . ?
C7 C6 C5 121.2(3) . . ?
C6 C7 C8 119.9(3) . . ?
C7 C8 C9 121.5(3) . . ?
C8 C9 C4 117.0(3) . . ?
C8 C9 C10 120.5(3) . . ?
C4 C9 C10 122.4(3) . . ?
C13 C10 C9 112.4(3) . . ?
C13 C10 C11 110.3(3) . . ?
C9 C10 C11 109.8(2) . . ?
C5 C14 C12 110.8(2) . . ?
C5 C14 C15 110.6(3) . . ?
C12 C14 C15 111.8(2) . . ?
N1 C16 C17 112.7(2) . . ?
C16 C17 P1 110.82(19) . . ?
C20 C19 C23 121.2(3) . . ?
C21 C20 C19 120.0(3) . . ?
C20 C21 C30 119.9(3) . . ?
C23 C22 C30 121.2(3) . . ?
C22 C23 C19 117.4(3) . . ?
C22 C23 P1 124.4(2) . . ?
C19 C23 P1 118.0(2) . . ?
C29 C24 C25 117.5(3) . . ?
C29 C24 P1 117.9(2) . . ?
C25 C24 P1 124.5(2) . . ?
C26 C25 C24 121.1(3) . . ?
C25 C26 C27 120.1(3) . . ?
C28 C27 C26 119.9(3) . . ?
C27 C28 C29 120.2(3) . . ?
C24 C29 C28 121.3(3) . . ?
C21 C30 C22 120.3(3) . . ?
C1 N1 C3 113.7(3) . . ?
C1 N1 C16 122.4(2) . . ?
C3 N1 C16 123.9(2) . . ?
C1 N2 C2 113.4(2) . . ?
C1 N2 C4 123.5(2) . . ?
C2 N2 C4 123.0(2) . . ?
C23 P1 C24 103.65(14) . . ?
C23 P1 C17 100.11(13) . . ?
C24 P1 C17 101.10(14) . . ?

_diffrn_measured_fraction_theta_max    0.984
_diffrn_reflns_theta_full              25.37
_diffrn_measured_fraction_theta_full   0.984
_refine_diff_density_max    0.279
_refine_diff_density_min   -0.323
_refine_diff_density_rms    0.055

#===END