Supplementary Material (ESI) for Dalton Transactions
This journal is © The Royal Society of Chemistry 2003

data_global

_publ_contact_author_email       DJC@ST-AND.AC.UK

_publ_contact_author_name        'Prof David Cole-Hamilton'
_journal_name_full               'Dalton Trans.'

_journal_coden_Cambridge         0222
_journal_volume                  ?
_journal_year                    ?
_journal_page_first              ?
_publ_contact_author_address     
;
School of Chemistry
University of St. Andrews
St. Andrews
Fife
KY16 9ST
UNITED KINGDOM
;

_publ_section_title              
;
Limonene derived phosphines in the cobalt-catalysed
hydroformylation of alkenes
;

loop_
_publ_author_name
'David Cole-Hamilton'
'Douglas F. Foster'
'Michael J. Green'
'Anastasios Polas'
'Alexandra M. Z. Slawin'
;
P.J.Steynberg
;
'James D. E. T. Wilton-Ely'

data_1
_database_code_depnum_ccdc_archive 'CCDC 218353'
_chemical_name_common            -

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
-
;
_chemical_melting_point          -
_chemical_formula_moiety         'C62 H110 Co2 O6 P2'
_chemical_formula_sum            'C62 H110 Co2 O6 P2'
_chemical_formula_weight         1131.30

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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   P2(1)2(1)2(1)

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

_cell_length_a                   8.8894(3)
_cell_length_b                   12.6610(3)
_cell_length_c                   60.1359(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     6768.2(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    67
_cell_measurement_theta_min      12
_cell_measurement_theta_max      168

_exptl_crystal_description       red
_exptl_crystal_colour            plate
_exptl_crystal_size_max          .21
_exptl_crystal_size_mid          .11
_exptl_crystal_size_min          .01
_exptl_crystal_density_meas      -
_exptl_crystal_density_diffrn    1.110
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2456
_exptl_absorpt_coefficient_mu    0.580
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.856257
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   -

_exptl_special_details           
;
Many crystal tried - poor quality. Some  refinement isotropic
with distance constraints.
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 0.9
_diffrn_standards_number         -
_diffrn_standards_interval_count -
_diffrn_standards_interval_time  -
_diffrn_standards_decay_%        -
_diffrn_reflns_number            29519
_diffrn_reflns_av_R_equivalents  0.0763
_diffrn_reflns_av_sigmaI/netI    0.0950
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -61
_diffrn_reflns_limit_l_max       66
_diffrn_reflns_theta_min         1.64
_diffrn_reflns_theta_max         23.24
_reflns_number_total             9604
_reflns_number_gt                4474
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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^)+(0.2000P)^2^+0.0000P] 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    fixed
_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   0.10(5)
_refine_ls_number_reflns         9604
_refine_ls_number_parameters     241
_refine_ls_number_restraints     34
_refine_ls_R_factor_all          0.1989
_refine_ls_R_factor_gt           0.1046
_refine_ls_wR_factor_ref         0.3391
_refine_ls_wR_factor_gt          0.2785
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_restrained_S_all      0.992
_refine_ls_shift/su_max          0.296
_refine_ls_shift/su_mean         0.066

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
Co1 Co 0.44368(10) 1.41445(7) 0.175510(14) 0.0886(3) Uani 1 1 d . . .
Co2 Co 0.28531(11) 1.25880(7) 0.194149(15) 0.0932(3) Uani 1 1 d . . .
C61 C 0.6013(9) 1.3487(6) 0.18728(12) 0.122(3) Uiso 1 1 d . . .
O61 O 0.7013(7) 1.3155(5) 0.19763(10) 0.156(2) Uiso 1 1 d . . .
C62 C 0.3544(10) 1.4953(7) 0.19308(13) 0.126(3) Uiso 1 1 d . . .
O62 O 0.2836(9) 1.5562(6) 0.20405(12) 0.190(3) Uiso 1 1 d . . .
C63 C 0.3712(8) 1.3638(6) 0.15060(11) 0.105(2) Uiso 1 1 d . . .
O63 O 0.3228(7) 1.3363(5) 0.13451(9) 0.149(2) Uiso 1 1 d . . .
C64 C 0.3521(9) 1.2935(6) 0.22097(12) 0.107(2) Uiso 1 1 d . . .
O64 O 0.3990(7) 1.3204(5) 0.23824(9) 0.1401(19) Uiso 1 1 d . . .
C65 C 0.1414(11) 1.3277(8) 0.18464(15) 0.145(3) Uiso 1 1 d . . .
O65 O 0.0385(8) 1.3835(5) 0.17944(10) 0.161(2) Uiso 1 1 d . . .
C66 C 0.4027(10) 1.1766(7) 0.17946(14) 0.135(3) Uiso 1 1 d . . .
O66 O 0.4746(7) 1.1158(5) 0.16747(9) 0.1411(19) Uiso 1 1 d . . .
C1 C 0.5025(9) 1.6370(6) 0.13930(13) 0.115(3) Uani 1 1 d . . .
H1A H 0.5012 1.5990 0.1251 0.137 Uiso 1 1 calc R . .
P2 P 0.5776(2) 1.53797(16) 0.15938(3) 0.1082(7) Uani 1 1 d . . .
C3 C 0.6790(14) 1.6130(8) 0.1768(2) 0.256(5) Uani 1 1 d . . .
H3A H 0.6560 1.5888 0.1917 0.307 Uiso 1 1 calc R . .
H3B H 0.7838 1.5959 0.1741 0.307 Uiso 1 1 calc R . .
C4 C 0.66915(12) 1.72288(14) 0.17722(3) 0.207(5) Uani 1 1 d D . .
H4A H 0.5822 1.7288 0.1872 0.248 Uiso 1 1 calc R . .
C5 C 0.6093(12) 1.7913(8) 0.15827(16) 0.169(4) Uani 1 1 d . . .
H5A H 0.6779 1.8512 0.1565 0.203 Uiso 1 1 calc R . .
C6 C 0.4487(15) 1.8371(7) 0.1635(2) 0.205(5) Uani 1 1 d . . .
H6A H 0.4456 1.8643 0.1786 0.246 Uiso 1 1 calc R . .
H6B H 0.4252 1.8943 0.1534 0.246 Uiso 1 1 calc R . .
C7 C 0.3403(13) 1.7516(7) 0.1609(2) 0.191(5) Uani 1 1 d . . .
H7A H 0.3505 1.7063 0.1739 0.230 Uiso 1 1 calc R . .
H7B H 0.2409 1.7830 0.1618 0.230 Uiso 1 1 calc R . .
C8 C 0.3414(10) 1.6823(7) 0.14125(16) 0.142(3) Uani 1 1 d . . .
H8A H 0.3299 1.7297 0.1285 0.170 Uiso 1 1 calc R . .
C9 C 0.6106(12) 1.7263(6) 0.13532(14) 0.149(4) Uani 1 1 d . . .
H9A H 0.5773 1.7703 0.1231 0.179 Uiso 1 1 calc R . .
H9B H 0.7106 1.6998 0.1321 0.179 Uiso 1 1 calc R . .
C10 C 0.7822(2) 1.7768(2) 0.19184(4) 0.200 Uiso 1 1 d D . .
H10A H 0.8110 1.7301 0.2037 0.300 Uiso 1 1 calc R . .
H10B H 0.7387 1.8398 0.1980 0.300 Uiso 1 1 calc R . .
H10C H 0.8694 1.7950 0.1832 0.300 Uiso 1 1 calc R . .
C11 C 0.2109(14) 1.6052(10) 0.13968(19) 0.200 Uiso 1 1 d . . .
H11A H 0.1178 1.6429 0.1411 0.300 Uiso 1 1 calc R . .
H11B H 0.2188 1.5540 0.1514 0.300 Uiso 1 1 calc R . .
H11C H 0.2138 1.5700 0.1255 0.300 Uiso 1 1 calc R . .
C12 C 0.7388 1.4977 0.1486 0.200 Uiso 1 1 d D . .
H12A H 0.7928 1.5604 0.1439 0.240 Uiso 1 1 calc R . .
H12B H 0.7966 1.4665 0.1606 0.240 Uiso 1 1 calc R . .
C13 C 0.7433 1.4238 0.1301 0.200 Uiso 1 1 d D . .
H13A H 0.6783 1.4527 0.1187 0.240 Uiso 1 1 calc R . .
H13B H 0.6953 1.3596 0.1354 0.240 Uiso 1 1 calc R . .
C14 C 0.8805 1.3913 0.1190 0.200 Uiso 1 1 d D . .
H14A H 0.9304 1.4537 0.1133 0.240 Uiso 1 1 calc R . .
H14B H 0.9470 1.3595 0.1299 0.240 Uiso 1 1 calc R . .
C15 C 0.8594 1.3172 0.1009 0.200 Uiso 1 1 d D . .
H15A H 0.7900 1.3507 0.0907 0.240 Uiso 1 1 calc R . .
H15B H 0.8064 1.2572 0.1072 0.240 Uiso 1 1 calc R . .
C16 C 0.9794 1.2736 0.0874 0.200 Uiso 1 1 d D . .
H16A H 1.0343 1.3316 0.0807 0.240 Uiso 1 1 calc R . .
H16B H 1.0486 1.2364 0.0971 0.240 Uiso 1 1 calc R . .
C17 C 0.9330 1.2020 0.0699 0.200 Uiso 1 1 d D . .
H17A H 0.8740 1.2469 0.0602 0.240 Uiso 1 1 calc R . .
H17B H 0.8603 1.1568 0.0772 0.240 Uiso 1 1 calc R . .
C18 C 1.0070 1.1306 0.0545 0.200 Uiso 1 1 d D . .
H18A H 1.0724 1.1737 0.0453 0.240 Uiso 1 1 calc R . .
H18B H 1.0722 1.0858 0.0634 0.240 Uiso 1 1 calc R . .
C19 C 0.9257 1.0614 0.0395 0.200 Uiso 1 1 d D . .
H19A H 0.8567 1.0194 0.0484 0.240 Uiso 1 1 calc R . .
H19B H 0.8654 1.1051 0.0298 0.240 Uiso 1 1 calc R . .
C20 C 1.0126 0.9897 0.0258 0.200 Uiso 1 1 d D . .
H20A H 1.0822 1.0321 0.0171 0.240 Uiso 1 1 calc R . .
H20B H 1.0727 0.9463 0.0357 0.240 Uiso 1 1 calc R . .
C21 C 0.9367 0.9205 0.0108 0.200 Uiso 1 1 d D . .
H21A H 0.8723 0.9655 0.0018 0.240 Uiso 1 1 calc R . .
H21B H 0.8700 0.8782 0.0199 0.240 Uiso 1 1 calc R . .
C22 C 1.0053 0.8472 -0.0048 0.200 Uiso 1 1 d D . .
H22A H 1.0680 0.8017 0.0043 0.240 Uiso 1 1 calc R . .
H22B H 1.0740 0.8897 -0.0135 0.240 Uiso 1 1 calc R . .
C23 C 0.9336 0.7770 -0.0206 0.200 Uiso 1 1 d D . .
H23A H 0.8706 0.8212 -0.0299 0.240 Uiso 1 1 calc R . .
H23B H 0.8660 0.7325 -0.0121 0.240 Uiso 1 1 calc R . .
C24 C 1.0147 0.7073 -0.0355 0.200 Uiso 1 1 d D . .
H24A H 1.0850 0.7507 -0.0438 0.240 Uiso 1 1 calc R . .
H24B H 1.0744 0.6604 -0.0263 0.240 Uiso 1 1 calc R . .
C25 C 0.9363 0.6418 -0.0515 0.200 Uiso 1 1 d D . .
H25A H 0.8710 0.6875 -0.0602 0.240 Uiso 1 1 calc R . .
H25B H 0.8720 0.5939 -0.0433 0.240 Uiso 1 1 calc R . .
C26 C 1.0237 0.5793 -0.0671 0.200 Uiso 1 1 d D . .
H26A H 1.0850 0.6267 -0.0759 0.240 Uiso 1 1 calc R . .
H26B H 1.0914 0.5343 -0.0587 0.240 Uiso 1 1 calc R . .
C27 C 0.9363 0.5134 -0.0820 0.200 Uiso 1 1 d D . .
H27A H 0.8603 0.4749 -0.0737 0.240 Uiso 1 1 calc R . .
H27B H 0.8865 0.5566 -0.0931 0.240 Uiso 1 1 calc R . .
C28 C 1.0393 0.4403 -0.0926 0.200 Uiso 1 1 d D . .
H28A H 1.0776 0.3900 -0.0818 0.240 Uiso 1 1 calc R . .
H28B H 1.1237 0.4783 -0.0990 0.240 Uiso 1 1 calc R . .
C29 C 0.9530 0.3842 -0.1105 0.200 Uiso 1 1 d D . .
H29A H 1.0180 0.3350 -0.1179 0.300 Uiso 1 1 calc R . .
H29B H 0.9159 0.4348 -0.1210 0.300 Uiso 1 1 calc R . .
H29C H 0.8700 0.3469 -0.1039 0.300 Uiso 1 1 calc R . .
C31 C 0.1686(10) 1.0024(5) 0.21601(10) 0.126(3) Uani 1 1 d . . .
H31A H 0.1962 0.9593 0.2031 0.151 Uiso 1 1 calc R . .
P32 P 0.1257(3) 1.13661(16) 0.20518(3) 0.1111(7) Uani 1 1 d . . .
C33 C 0.0098(12) 1.1899(8) 0.22747(17) 0.190(4) Uani 1 1 d . . .
H33A H 0.0702 1.2384 0.2362 0.229 Uiso 1 1 calc R . .
H33B H -0.0720 1.2300 0.2209 0.229 Uiso 1 1 calc R . .
C34 C -0.05520(8) 1.1083(2) 0.2427(2) 0.222(6) Uani 1 1 d D . .
H34A H -0.0224 1.1387 0.2569 0.266 Uiso 1 1 calc R . .
C35 C -0.0118(16) 1.0082(7) 0.2463(2) 0.232(5) Uani 1 1 d . . .
H35A H -0.0927 0.9693 0.2537 0.279 Uiso 1 1 calc R . .
C36 C 0.1424(16) 1.0148(10) 0.26341(16) 0.211(6) Uani 1 1 d . . .
H36A H 0.1184 1.0625 0.2755 0.253 Uiso 1 1 calc R . .
H36B H 0.1576 0.9454 0.2698 0.253 Uiso 1 1 calc R . .
C37 C 0.2823(13) 1.0483(8) 0.25397(13) 0.156(4) Uani 1 1 d . . .
H37A H 0.2815 1.1241 0.2517 0.187 Uiso 1 1 calc R . .
H37B H 0.3645 1.0311 0.2639 0.187 Uiso 1 1 calc R . .
C38 C 0.3022(14) 0.9940(7) 0.23277(16) 0.165(4) Uani 1 1 d . . .
H38A H 0.3085 0.9189 0.2366 0.198 Uiso 1 1 calc R . .
C39 C 0.0350(15) 0.9514(7) 0.22617(15) 0.185(5) Uani 1 1 d . . .
H39A H -0.0470 0.9507 0.2155 0.222 Uiso 1 1 calc R . .
H39B H 0.0589 0.8788 0.2299 0.222 Uiso 1 1 calc R . .
C40 C -0.21700(11) 1.1417(3) 0.24350(18) 0.200 Uiso 1 1 d D . .
H40A H -0.2723 1.0940 0.2528 0.300 Uiso 1 1 calc R . .
H40B H -0.2585 1.1405 0.2288 0.300 Uiso 1 1 calc R . .
H40C H -0.2238 1.2119 0.2494 0.300 Uiso 1 1 calc R . .
C41 C 0.4562(14) 1.0229(10) 0.2246(2) 0.200 Uiso 1 1 d . . .
H41A H 0.5278 1.0132 0.2364 0.300 Uiso 1 1 calc R . .
H41B H 0.4568 1.0954 0.2200 0.300 Uiso 1 1 calc R . .
H41C H 0.4827 0.9785 0.2123 0.300 Uiso 1 1 calc R . .
C42 C -0.0080 1.1029 0.1819 0.200 Uiso 1 1 d D . .
H42A H -0.0818 1.0531 0.1875 0.240 Uiso 1 1 calc R . .
H42B H -0.0615 1.1666 0.1776 0.240 Uiso 1 1 calc R . .
C43 C 0.0617 1.0582 0.1622 0.200 Uiso 1 1 d D . .
H43A H 0.1262 1.0013 0.1673 0.240 Uiso 1 1 calc R . .
H43B H 0.1272 1.1123 0.1562 0.240 Uiso 1 1 calc R . .
C44 C -0.0257 1.0171 0.1438 0.200 Uiso 1 1 d D . .
H44A H -0.1051 0.9746 0.1503 0.240 Uiso 1 1 calc R . .
H44B H -0.0745 1.0774 0.1370 0.240 Uiso 1 1 calc R . .
C45 C 0.0364 0.9550 0.1257 0.200 Uiso 1 1 d D . .
H45A H 0.1068 0.9067 0.1327 0.240 Uiso 1 1 calc R . .
H45B H 0.0971 1.0040 0.1172 0.240 Uiso 1 1 calc R . .
C46 C -0.0435 0.8922 0.1094 0.200 Uiso 1 1 d D . .
H46A H -0.1211 0.8550 0.1176 0.240 Uiso 1 1 calc R . .
H46B H -0.0955 0.9425 0.0999 0.240 Uiso 1 1 calc R . .
C47 C 0.0217 0.8148 0.0945 0.200 Uiso 1 1 d D . .
H47A H 0.0918 0.8534 0.0852 0.240 Uiso 1 1 calc R . .
H47B H 0.0820 0.7686 0.1037 0.240 Uiso 1 1 calc R . .
C48 C -0.0614 0.7461 0.0796 0.200 Uiso 1 1 d D . .
H48A H -0.1257 0.7017 0.0886 0.240 Uiso 1 1 calc R . .
H48B H -0.1269 0.7904 0.0707 0.240 Uiso 1 1 calc R . .
C49 C 0.0200 0.6775 0.0645 0.200 Uiso 1 1 d D . .
H49A H 0.0876 0.6344 0.0733 0.240 Uiso 1 1 calc R . .
H49B H 0.0820 0.7218 0.0550 0.240 Uiso 1 1 calc R . .
C50 C -0.0653 0.6075 0.0501 0.200 Uiso 1 1 d D . .
H50A H -0.1338 0.6513 0.0416 0.240 Uiso 1 1 calc R . .
H50B H -0.1268 0.5636 0.0597 0.240 Uiso 1 1 calc R . .
C51 C 0.0104 0.5359 0.0341 0.200 Uiso 1 1 d D . .
H51A H 0.0740 0.5798 0.0248 0.240 Uiso 1 1 calc R . .
H51B H 0.0771 0.4912 0.0427 0.240 Uiso 1 1 calc R . .
C52 C -0.0724 0.4668 0.0193 0.200 Uiso 1 1 d D . .
H52A H -0.1372 0.5114 0.0103 0.240 Uiso 1 1 calc R . .
H52B H -0.1378 0.4237 0.0285 0.240 Uiso 1 1 calc R . .
C53 C 0.0048 0.3959 0.0042 0.200 Uiso 1 1 d D . .
H53A H 0.0711 0.4390 -0.0049 0.240 Uiso 1 1 calc R . .
H53B H 0.0688 0.3510 0.0132 0.240 Uiso 1 1 calc R . .
C54 C -0.0767 0.3273 -0.0109 0.200 Uiso 1 1 d D . .
H54A H -0.1466 0.3710 -0.0192 0.240 Uiso 1 1 calc R . .
H54B H -0.1365 0.2795 -0.0019 0.240 Uiso 1 1 calc R . .
C55 C 0.0055 0.2637 -0.0269 0.200 Uiso 1 1 d D . .
H55A H 0.0524 0.3109 -0.0375 0.240 Uiso 1 1 calc R . .
H55B H 0.0856 0.2274 -0.0190 0.240 Uiso 1 1 calc R . .
C56 C -0.0809 0.1858 -0.0391 0.200 Uiso 1 1 d D . .
H56A H -0.1551 0.2245 -0.0476 0.240 Uiso 1 1 calc R . .
H56B H -0.1362 0.1451 -0.0281 0.240 Uiso 1 1 calc R . .
C57 C -0.0125 0.1103 -0.0541 0.200 Uiso 1 1 d D . .
H57A H 0.0530 0.0660 -0.0452 0.240 Uiso 1 1 calc R . .
H57B H 0.0521 0.1503 -0.0640 0.240 Uiso 1 1 calc R . .
C58 C -0.1007 0.0400 -0.0680 0.200 Uiso 1 1 d D . .
H58A H -0.1520 0.0818 -0.0792 0.240 Uiso 1 1 calc R . .
H58B H -0.1770 0.0068 -0.0588 0.240 Uiso 1 1 calc R . .
C59 C -0.0122 -0.0448 -0.0795 0.200 Uiso 1 1 d D . .
H59A H -0.0788 -0.0875 -0.0882 0.300 Uiso 1 1 calc R . .
H59B H 0.0369 -0.0882 -0.0686 0.300 Uiso 1 1 calc R . .
H59C H 0.0620 -0.0130 -0.0889 0.300 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
Co1 0.0904(5) 0.0782(5) 0.0973(5) 0.0070(5) 0.0053(5) -0.0037(5)
Co2 0.0971(6) 0.0745(5) 0.1079(6) 0.0080(5) 0.0049(6) -0.0061(5)
C1 0.116(6) 0.092(5) 0.135(6) 0.017(4) -0.002(5) -0.012(4)
P2 0.0872(12) 0.1075(13) 0.1300(14) 0.0285(12) -0.0034(12) -0.0189(11)
C3 0.327(11) 0.168(7) 0.272(12) 0.058(8) -0.116(11) -0.168(7)
C4 0.198(10) 0.250(11) 0.172(7) -0.095(8) -0.052(8) 0.020(10)
C5 0.187(8) 0.146(6) 0.176(7) 0.052(6) -0.020(7) -0.079(6)
C6 0.245(12) 0.101(6) 0.267(12) 0.023(7) 0.035(11) -0.047(8)
C7 0.189(9) 0.105(6) 0.280(12) 0.034(8) 0.043(10) 0.022(7)
C8 0.133(7) 0.102(5) 0.190(8) 0.050(5) -0.017(6) -0.004(5)
C9 0.182(8) 0.110(5) 0.155(6) 0.054(5) -0.003(6) -0.037(6)
C31 0.222(9) 0.065(4) 0.091(4) 0.018(3) -0.033(5) -0.023(5)
P32 0.1204(15) 0.0953(13) 0.1177(14) 0.0172(12) 0.0034(13) -0.0245(12)
C33 0.195(8) 0.144(8) 0.233(9) 0.005(7) 0.125(7) -0.033(7)
C34 0.145(8) 0.286(15) 0.236(11) -0.012(12) 0.083(8) -0.025(11)
C35 0.291(10) 0.138(6) 0.268(10) 0.070(7) 0.079(9) -0.119(6)
C36 0.293(13) 0.197(10) 0.142(7) 0.009(7) -0.060(9) -0.092(10)
C37 0.213(10) 0.143(7) 0.111(5) 0.017(5) -0.039(7) -0.021(8)
C38 0.229(11) 0.096(5) 0.170(7) 0.034(5) -0.039(8) 0.011(7)
C39 0.323(14) 0.093(5) 0.139(6) 0.023(5) -0.025(9) -0.075(8)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 C62 1.671(8) . ?
Co1 C63 1.752(7) . ?
Co1 C61 1.776(8) . ?
Co1 P2 2.192(2) . ?
Co1 Co2 2.6687(12) . ?
Co2 C65 1.651(10) . ?
Co2 C66 1.718(9) . ?
Co2 C64 1.774(7) . ?
Co2 P32 2.201(2) . ?
C61 O61 1.164(10) . ?
C62 O62 1.195(11) . ?
C63 O63 1.115(8) . ?
C64 O64 1.170(9) . ?
C65 O65 1.197(11) . ?
C66 O66 1.233(10) . ?
C1 C9 1.503(11) . ?
C1 C8 1.547(12) . ?
C1 P2 1.865(8) . ?
P2 C12 1.654(2) . ?
P2 C3 1.677(11) . ?
C3 C4 1.394(10) . ?
C4 C10 1.4997(10) . ?
C4 C5 1.527(10) . ?
C5 C9 1.607(13) . ?
C5 C6 1.572(16) . ?
C6 C7 1.458(15) . ?
C7 C8 1.473(14) . ?
C8 C11 1.519(15) . ?
C12 C13 1.4498 . ?
C13 C14 1.4505 . ?
C14 C15 1.4500 . ?
C15 C16 1.4503 . ?
C16 C17 1.4501 . ?
C17 C18 1.4502 . ?
C18 C19 1.4501 . ?
C19 C20 1.4497 . ?
C20 C21 1.4300 . ?
C21 C22 1.4499 . ?
C22 C23 1.4500 . ?
C23 C24 1.4502 . ?
C24 C25 1.4497 . ?
C25 C26 1.4503 . ?
C26 C27 1.4500 . ?
C27 C28 1.4498 . ?
C28 C29 1.4999 . ?
C31 C39 1.484(14) . ?
C31 C38 1.561(13) . ?
C31 P32 1.859(7) . ?
P32 C33 1.821(10) . ?
P32 C42 1.885(2) . ?
C33 C34 1.496(12) . ?
C34 C35 1.342(11) . ?
C34 C40 1.4999(9) . ?
C35 C39 1.466(15) . ?
C35 C36 1.718(18) . ?
C36 C37 1.431(16) . ?
C37 C38 1.459(12) . ?
C38 C41 1.499(16) . ?
C42 C43 1.4501 . ?
C43 C44 1.4507 . ?
C44 C45 1.4502 . ?
C45 C46 1.4503 . ?
C46 C47 1.4502 . ?
C47 C48 1.4501 . ?
C48 C49 1.4501 . ?
C49 C50 1.4501 . ?
C50 C51 1.4829 . ?
C51 C52 1.4500 . ?
C52 C53 1.4501 . ?
C53 C54 1.4498 . ?
C54 C55 1.4501 . ?
C55 C56 1.4499 . ?
C56 C57 1.4501 . ?
C57 C58 1.4501 . ?
C58 C59 1.4999 . ?

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
C62 Co1 C63 126.1(4) . . ?
C62 Co1 C61 114.2(4) . . ?
C63 Co1 C61 117.3(4) . . ?
C62 Co1 P2 95.8(3) . . ?
C63 Co1 P2 94.7(2) . . ?
C61 Co1 P2 94.7(3) . . ?
C62 Co1 Co2 86.3(3) . . ?
C63 Co1 Co2 83.9(2) . . ?
C61 Co1 Co2 84.4(3) . . ?
P2 Co1 Co2 177.87(7) . . ?
C65 Co2 C66 127.8(4) . . ?
C65 Co2 C64 116.3(4) . . ?
C66 Co2 C64 114.5(4) . . ?
C65 Co2 P32 88.6(3) . . ?
C66 Co2 P32 96.9(3) . . ?
C64 Co2 P32 96.6(3) . . ?
C65 Co2 Co1 82.7(3) . . ?
C66 Co2 Co1 84.9(3) . . ?
C64 Co2 Co1 91.3(3) . . ?
P32 Co2 Co1 170.23(8) . . ?
O61 C61 Co1 170.0(7) . . ?
O62 C62 Co1 174.2(8) . . ?
O63 C63 Co1 176.7(7) . . ?
O64 C64 Co2 177.0(7) . . ?
O65 C65 Co2 173.9(8) . . ?
O66 C66 Co2 173.4(8) . . ?
C9 C1 C8 109.0(7) . . ?
C9 C1 P2 112.3(6) . . ?
C8 C1 P2 122.1(6) . . ?
C12 P2 C3 87.4(5) . . ?
C12 P2 C1 105.3(3) . . ?
C3 P2 C1 102.5(5) . . ?
C12 P2 Co1 115.12(11) . . ?
C3 P2 Co1 114.8(4) . . ?
C1 P2 Co1 124.9(3) . . ?
C4 C3 P2 122.8(8) . . ?
C3 C4 C10 115.0(5) . . ?
C3 C4 C5 125.1(6) . . ?
C10 C4 C5 114.4(4) . . ?
C4 C5 C9 110.4(7) . . ?
C4 C5 C6 112.1(8) . . ?
C9 C5 C6 111.6(9) . . ?
C7 C6 C5 107.7(8) . . ?
C8 C7 C6 121.5(10) . . ?
C7 C8 C1 106.7(8) . . ?
C7 C8 C11 115.3(9) . . ?
C1 C8 C11 117.6(8) . . ?
C1 C9 C5 104.1(7) . . ?
C13 C12 P2 121.57(7) . . ?
C12 C13 C14 124.0 . . ?
C15 C14 C13 114.9 . . ?
C14 C15 C16 124.9 . . ?
C17 C16 C15 115.8 . . ?
C16 C17 C18 136.4 . . ?
C19 C18 C17 123.1 . . ?
C20 C19 C18 117.8 . . ?
C21 C20 C19 119.5 . . ?
C20 C21 C22 127.0 . . ?
C21 C22 C23 129.1 . . ?
C22 C23 C24 124.1 . . ?
C25 C24 C23 121.3 . . ?
C24 C25 C26 118.9 . . ?
C27 C26 C25 115.2 . . ?
C28 C27 C26 107.5 . . ?
C27 C28 C29 107.2 . . ?
C39 C31 C38 108.2(7) . . ?
C39 C31 P32 112.2(6) . . ?
C38 C31 P32 116.4(5) . . ?
C33 P32 C31 101.4(4) . . ?
C33 P32 C42 105.9(4) . . ?
C31 P32 C42 100.5(2) . . ?
C33 P32 Co2 109.0(3) . . ?
C31 P32 Co2 128.0(3) . . ?
C42 P32 Co2 109.99(10) . . ?
C34 C33 P32 114.4(7) . . ?
C35 C34 C33 129.7(8) . . ?
C35 C34 C40 122.5(6) . . ?
C33 C34 C40 101.3(6) . . ?
C34 C35 C39 114.4(11) . . ?
C34 C35 C36 106.3(9) . . ?
C39 C35 C36 107.0(11) . . ?
C37 C36 C35 118.0(8) . . ?
C38 C37 C36 108.2(9) . . ?
C37 C38 C41 106.3(10) . . ?
C37 C38 C31 116.1(9) . . ?
C41 C38 C31 117.9(8) . . ?
C35 C39 C31 110.6(8) . . ?
C43 C42 P32 115.10(7) . . ?
C42 C43 C44 122.3 . . ?
C45 C44 C43 124.3 . . ?
C44 C45 C46 128.2 . . ?
C47 C46 C45 126.5 . . ?
C48 C47 C46 125.8 . . ?
C49 C48 C47 119.5 . . ?
C48 C49 C50 118.6 . . ?
C49 C50 C51 121.5 . . ?
C52 C51 C50 122.5 . . ?
C51 C52 C53 121.2 . . ?
C54 C53 C52 121.7 . . ?
C53 C54 C55 119.6 . . ?
C56 C55 C54 116.5 . . ?
C55 C56 C57 122.8 . . ?
C56 C57 C58 122.5 . . ?
C57 C58 C59 114.9 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C62 Co1 Co2 C65 60.9(4) . . . . ?
C63 Co1 Co2 C65 -66.0(4) . . . . ?
C61 Co1 Co2 C65 175.7(4) . . . . ?
P2 Co1 Co2 C65 -118(2) . . . . ?
C62 Co1 Co2 C66 -169.9(4) . . . . ?
C63 Co1 Co2 C66 63.2(4) . . . . ?
C61 Co1 Co2 C66 -55.1(4) . . . . ?
P2 Co1 Co2 C66 11(2) . . . . ?
C62 Co1 Co2 C64 -55.4(4) . . . . ?
C63 Co1 Co2 C64 177.6(4) . . . . ?
C61 Co1 Co2 C64 59.3(4) . . . . ?
P2 Co1 Co2 C64 125(2) . . . . ?
C62 Co1 Co2 P32 88.9(5) . . . . ?
C63 Co1 Co2 P32 -38.1(5) . . . . ?
C61 Co1 Co2 P32 -156.4(5) . . . . ?
P2 Co1 Co2 P32 -90(2) . . . . ?
C62 Co1 C61 O61 -9(4) . . . . ?
C63 Co1 C61 O61 -173(4) . . . . ?
P2 Co1 C61 O61 89(4) . . . . ?
Co2 Co1 C61 O61 -93(4) . . . . ?
C63 Co1 C62 O62 -28(8) . . . . ?
C61 Co1 C62 O62 170(8) . . . . ?
P2 Co1 C62 O62 72(8) . . . . ?
Co2 Co1 C62 O62 -108(8) . . . . ?
C62 Co1 C63 O63 47(13) . . . . ?
C61 Co1 C63 O63 -151(12) . . . . ?
P2 Co1 C63 O63 -53(13) . . . . ?
Co2 Co1 C63 O63 128(13) . . . . ?
C65 Co2 C64 O64 -74(14) . . . . ?
C66 Co2 C64 O64 93(14) . . . . ?
P32 Co2 C64 O64 -166(14) . . . . ?
Co1 Co2 C64 O64 8(14) . . . . ?
C66 Co2 C65 O65 -159(8) . . . . ?
C64 Co2 C65 O65 7(9) . . . . ?
P32 Co2 C65 O65 103(8) . . . . ?
Co1 Co2 C65 O65 -81(8) . . . . ?
C65 Co2 C66 O66 -28(7) . . . . ?
C64 Co2 C66 O66 166(7) . . . . ?
P32 Co2 C66 O66 65(7) . . . . ?
Co1 Co2 C66 O66 -105(7) . . . . ?
C9 C1 P2 C12 -57.1(6) . . . . ?
C8 C1 P2 C12 170.6(6) . . . . ?
C9 C1 P2 C3 33.6(8) . . . . ?
C8 C1 P2 C3 -98.7(8) . . . . ?
C9 C1 P2 Co1 166.3(5) . . . . ?
C8 C1 P2 Co1 34.0(8) . . . . ?
C62 Co1 P2 C12 153.5(3) . . . . ?
C63 Co1 P2 C12 -79.4(3) . . . . ?
C61 Co1 P2 C12 38.6(3) . . . . ?
Co2 Co1 P2 C12 -27(2) . . . . ?
C62 Co1 P2 C3 54.2(6) . . . . ?
C63 Co1 P2 C3 -178.7(5) . . . . ?
C61 Co1 P2 C3 -60.8(5) . . . . ?
Co2 Co1 P2 C3 -127(2) . . . . ?
C62 Co1 P2 C1 -73.6(4) . . . . ?
C63 Co1 P2 C1 53.5(4) . . . . ?
C61 Co1 P2 C1 171.5(4) . . . . ?
Co2 Co1 P2 C1 106(2) . . . . ?
C12 P2 C3 C4 118.0(10) . . . . ?
C1 P2 C3 C4 12.9(11) . . . . ?
Co1 P2 C3 C4 -125.5(8) . . . . ?
P2 C3 C4 C10 -172.6(7) . . . . ?
P2 C3 C4 C5 -20.4(13) . . . . ?
C3 C4 C5 C9 -18.8(11) . . . . ?
C10 C4 C5 C9 133.5(6) . . . . ?
C3 C4 C5 C6 106.3(10) . . . . ?
C10 C4 C5 C6 -101.4(7) . . . . ?
C4 C5 C6 C7 -75.2(11) . . . . ?
C9 C5 C6 C7 49.2(12) . . . . ?
C5 C6 C7 C8 -47.7(14) . . . . ?
C6 C7 C8 C1 54.1(12) . . . . ?
C6 C7 C8 C11 -173.3(10) . . . . ?
C9 C1 C8 C7 -63.2(9) . . . . ?
P2 C1 C8 C7 70.5(9) . . . . ?
C9 C1 C8 C11 165.5(8) . . . . ?
P2 C1 C8 C11 -60.9(11) . . . . ?
C8 C1 C9 C5 68.2(9) . . . . ?
P2 C1 C9 C5 -70.3(8) . . . . ?
C4 C5 C9 C1 63.4(9) . . . . ?
C6 C5 C9 C1 -61.9(9) . . . . ?
C3 P2 C12 C13 -179.0(4) . . . . ?
C1 P2 C12 C13 -76.8(3) . . . . ?
Co1 P2 C12 C13 64.73(12) . . . . ?
P2 C12 C13 C14 175.63(8) . . . . ?
C12 C13 C14 C15 -179.6 . . . . ?
C13 C14 C15 C16 -180.0 . . . . ?
C14 C15 C16 C17 -179.0 . . . . ?
C15 C16 C17 C18 -170.4 . . . . ?
C16 C17 C18 C19 175.0 . . . . ?
C17 C18 C19 C20 -176.8 . . . . ?
C18 C19 C20 C21 -179.7 . . . . ?
C19 C20 C21 C22 177.4 . . . . ?
C20 C21 C22 C23 -178.7 . . . . ?
C21 C22 C23 C24 179.5 . . . . ?
C22 C23 C24 C25 -177.7 . . . . ?
C23 C24 C25 C26 175.7 . . . . ?
C24 C25 C26 C27 177.9 . . . . ?
C25 C26 C27 C28 -167.5 . . . . ?
C26 C27 C28 C29 -171.4 . . . . ?
C39 C31 P32 C33 42.5(7) . . . . ?
C38 C31 P32 C33 -83.0(7) . . . . ?
C39 C31 P32 C42 -66.2(5) . . . . ?
C38 C31 P32 C42 168.3(6) . . . . ?
C39 C31 P32 Co2 167.9(4) . . . . ?
C38 C31 P32 Co2 42.4(7) . . . . ?
C65 Co2 P32 C33 -66.8(5) . . . . ?
C66 Co2 P32 C33 165.3(5) . . . . ?
C64 Co2 P32 C33 49.5(5) . . . . ?
Co1 Co2 P32 C33 -94.5(6) . . . . ?
C65 Co2 P32 C31 170.9(4) . . . . ?
C66 Co2 P32 C31 43.0(4) . . . . ?
C64 Co2 P32 C31 -72.8(4) . . . . ?
Co1 Co2 P32 C31 143.2(4) . . . . ?
C65 Co2 P32 C42 48.9(3) . . . . ?
C66 Co2 P32 C42 -79.1(3) . . . . ?
C64 Co2 P32 C42 165.2(3) . . . . ?
Co1 Co2 P32 C42 21.1(5) . . . . ?
C31 P32 C33 C34 -18.4(8) . . . . ?
C42 P32 C33 C34 86.1(7) . . . . ?
Co2 P32 C33 C34 -155.6(6) . . . . ?
P32 C33 C34 C35 19.9(15) . . . . ?
P32 C33 C34 C40 -131.4(7) . . . . ?
C33 C34 C35 C39 -39.8(17) . . . . ?
C40 C34 C35 C39 106.3(14) . . . . ?
C33 C34 C35 C36 78.0(14) . . . . ?
C40 C34 C35 C36 -135.9(11) . . . . ?
C34 C35 C36 C37 -74.6(14) . . . . ?
C39 C35 C36 C37 48.0(13) . . . . ?
C35 C36 C37 C38 -44.5(13) . . . . ?
C36 C37 C38 C41 -174.4(10) . . . . ?
C36 C37 C38 C31 52.3(11) . . . . ?
C39 C31 C38 C37 -62.8(10) . . . . ?
P32 C31 C38 C37 64.6(10) . . . . ?
C39 C31 C38 C41 169.4(9) . . . . ?
P32 C31 C38 C41 -63.2(10) . . . . ?
C34 C35 C39 C31 62.6(13) . . . . ?
C36 C35 C39 C31 -54.8(10) . . . . ?
C38 C31 C39 C35 63.8(10) . . . . ?
P32 C31 C39 C35 -66.0(10) . . . . ?
C33 P32 C42 C43 -179.8(3) . . . . ?
C31 P32 C42 C43 -74.6(3) . . . . ?
Co2 P32 C42 C43 62.56(11) . . . . ?
P32 C42 C43 C44 173.02(7) . . . . ?
C42 C43 C44 C45 -168.4 . . . . ?
C43 C44 C45 C46 165.6 . . . . ?
C44 C45 C46 C47 -166.6 . . . . ?
C45 C46 C47 C48 174.3 . . . . ?
C46 C47 C48 C49 175.8 . . . . ?
C47 C48 C49 C50 178.4 . . . . ?
C48 C49 C50 C51 179.4 . . . . ?
C49 C50 C51 C52 -178.6 . . . . ?
C50 C51 C52 C53 -178.6 . . . . ?
C51 C52 C53 C54 -179.4 . . . . ?
C52 C53 C54 C55 175.3 . . . . ?
C53 C54 C55 C56 171.2 . . . . ?
C54 C55 C56 C57 -174.4 . . . . ?
C55 C56 C57 C58 -173.5 . . . . ?
C56 C57 C58 C59 -169.9 . . . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        23.24
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         0.467
_refine_diff_density_min         -0.446
_refine_diff_density_rms         0.072