# Supplementary Material (ESI) for Dalton Transactions
# This journal is (c) The Royal Society of Chemistry 2010

data_global
_journal_name_full               'Dalton Trans.'

_journal_coden_Cambridge         0222

_publ_contact_author_name        'Ulrich Fekl'
_publ_contact_author_email       ULRICH.FEKL@UTORONTO.CA

_publ_section_title              
;
Characterization of a Rhodium-Sparteine Complex,[((-)-sparteine)Rh(eta4-COD)]+:
Crystal Structure and DNMR/DFT Studies on COD-Rotation Dynamics
;
loop_
_publ_author_name
'Ulrich Fekl'
'Vincent T. Annibale'
'Antonio G. De Crisci'
'Gordon K. Hamer'
'Alan J Lough'

# Attachment 'sparteine_Rh_cod.cif'

data_k08228
_database_code_depnum_ccdc_archive 'CCDC 730876'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C23 H38 N2 Rh, B F4'
_chemical_formula_sum            'C23 H38 B F4 N2 Rh'
_chemical_formula_weight         532.27
_chemical_absolute_configuration rmad

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'
Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'C 2 2 21'
_symmetry_space_group_name_Hall  'C 2c 2'

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

_cell_length_a                   14.1899(3)
_cell_length_b                   14.3150(3)
_cell_length_c                   23.4356(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4760.44(17)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(1)
_cell_measurement_reflns_used    10906
_cell_measurement_theta_min      2.6
_cell_measurement_theta_max      27.5

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.485
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2208
_exptl_absorpt_coefficient_mu    0.761
# Absorption correction

_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.852
_exptl_absorpt_correction_T_max  0.922
_exptl_absorpt_process_details   
;
multi-scan from symmetry-related measurements
Sortav (Blessing 1995)
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f scans and \w scans with \k offsets'
_diffrn_detector_area_resol_mean 9
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            16475
_diffrn_reflns_av_R_equivalents  0.054
_diffrn_reflns_av_sigmaI/netI    0.055
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         2.67
_diffrn_reflns_theta_max         27.48
_reflns_number_total             5411
_reflns_number_gt                4658
_reflns_threshold_expression     I>2\s(I)

_computing_data_collection       'Collect (Nonius B.V., 1997-2002)'
_computing_cell_refinement       'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_data_reduction        Denzo-SMN
_computing_structure_solution    'SIR-92 (Altomare et al., 1994)'
_computing_structure_refinement  'SHELXTL V6.1 (Sheldrick, 2008)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXTL V6.1'

_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^)+(0.0516P)^2^+2.1416P] 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     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(3)
_refine_ls_number_reflns         5411
_refine_ls_number_parameters     292
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.0402
_refine_ls_wR_factor_ref         0.0987
_refine_ls_wR_factor_gt          0.0922
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_restrained_S_all      1.085
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Rh1 Rh 0.313839(19) 0.643209(19) 0.634711(13) 0.01939(9) Uani 1 1 d . . .
N1 N 0.1814(2) 0.6351(2) 0.58499(13) 0.0196(6) Uani 1 1 d . . .
N16 N 0.2245(2) 0.5931(2) 0.70741(15) 0.0218(7) Uani 1 1 d . . .
C2 C 0.1835(3) 0.6704(3) 0.52445(16) 0.0270(9) Uani 1 1 d . . .
H2A H 0.1291 0.6439 0.5035 0.032 Uiso 1 1 calc R . .
H2B H 0.2416 0.6476 0.5057 0.032 Uiso 1 1 calc R . .
C3 C 0.1802(4) 0.7765(3) 0.51986(19) 0.0359(10) Uani 1 1 d . . .
H3A H 0.1769 0.7945 0.4791 0.043 Uiso 1 1 calc R . .
H3B H 0.2389 0.8029 0.5359 0.043 Uiso 1 1 calc R . .
C4 C 0.0953(4) 0.8180(3) 0.5515(2) 0.0381(12) Uani 1 1 d . . .
H4A H 0.0995 0.8870 0.5518 0.046 Uiso 1 1 calc R . .
H4B H 0.0360 0.7999 0.5321 0.046 Uiso 1 1 calc R . .
C5 C 0.0960(3) 0.7809(3) 0.6120(2) 0.0328(10) Uani 1 1 d . . .
H5A H 0.0416 0.8062 0.6335 0.039 Uiso 1 1 calc R . .
H5B H 0.1546 0.8002 0.6316 0.039 Uiso 1 1 calc R . .
C6 C 0.0901(3) 0.6745(3) 0.6096(2) 0.0259(9) Uani 1 1 d . . .
H6A H 0.0390 0.6589 0.5819 0.031 Uiso 1 1 calc R . .
C7 C 0.0631(3) 0.6304(3) 0.6653(2) 0.0294(9) Uani 1 1 d . . .
H7A H 0.0019 0.6586 0.6774 0.035 Uiso 1 1 calc R . .
C8 C 0.0466(3) 0.5258(3) 0.6568(2) 0.0290(10) Uani 1 1 d . . .
H8A H -0.0009 0.5148 0.6266 0.035 Uiso 1 1 calc R . .
H8B H 0.0244 0.4965 0.6926 0.035 Uiso 1 1 calc R . .
C9 C 0.1434(3) 0.4852(3) 0.6390(2) 0.0242(8) Uani 1 1 d . . .
H9A H 0.1338 0.4171 0.6314 0.029 Uiso 1 1 calc R . .
C10 C 0.1721(3) 0.5299(3) 0.58273(18) 0.0247(9) Uani 1 1 d . . .
H10A H 0.2332 0.5030 0.5706 0.030 Uiso 1 1 calc R . .
H10B H 0.1247 0.5134 0.5534 0.030 Uiso 1 1 calc R . .
C11 C 0.2133(3) 0.4929(3) 0.68874(18) 0.0241(9) Uani 1 1 d . . .
H11A H 0.2760 0.4717 0.6741 0.029 Uiso 1 1 calc R . .
C12 C 0.1839(3) 0.4240(3) 0.73599(19) 0.0343(10) Uani 1 1 d . . .
H12A H 0.1164 0.4336 0.7450 0.041 Uiso 1 1 calc R . .
H12B H 0.1915 0.3593 0.7218 0.041 Uiso 1 1 calc R . .
C13 C 0.2422(3) 0.4361(4) 0.7907(2) 0.0425(13) Uani 1 1 d . . .
H13A H 0.2193 0.3926 0.8205 0.051 Uiso 1 1 calc R . .
H13B H 0.3092 0.4217 0.7830 0.051 Uiso 1 1 calc R . .
C14 C 0.2327(3) 0.5347(4) 0.8109(2) 0.0369(12) Uani 1 1 d . . .
H14A H 0.2684 0.5432 0.8469 0.044 Uiso 1 1 calc R . .
H14B H 0.1657 0.5492 0.8185 0.044 Uiso 1 1 calc R . .
C15 C 0.2709(3) 0.6001(3) 0.76541(18) 0.0286(10) Uani 1 1 d . . .
H15A H 0.2642 0.6651 0.7793 0.034 Uiso 1 1 calc R . .
H15B H 0.3391 0.5876 0.7608 0.034 Uiso 1 1 calc R . .
C17 C 0.1328(3) 0.6435(3) 0.71439(17) 0.0257(8) Uani 1 1 d . . .
H17A H 0.1460 0.7111 0.7187 0.031 Uiso 1 1 calc R . .
H17B H 0.1026 0.6219 0.7501 0.031 Uiso 1 1 calc R . .
C18 C 0.4011(3) 0.6133(3) 0.56203(19) 0.0255(9) Uani 1 1 d D . .
H18A H 0.364(3) 0.585(3) 0.5362(14) 0.031 Uiso 1 1 d D . .
C19 C 0.4007(3) 0.7085(3) 0.5703(2) 0.0286(10) Uani 1 1 d D . .
H19A H 0.362(3) 0.740(3) 0.5466(17) 0.034 Uiso 1 1 d D . .
C20 C 0.4823(3) 0.7636(3) 0.5949(2) 0.0360(12) Uani 1 1 d . . .
H20A H 0.4840 0.8261 0.5769 0.043 Uiso 1 1 calc R . .
H20B H 0.5420 0.7313 0.5855 0.043 Uiso 1 1 calc R . .
C21 C 0.4756(3) 0.7752(3) 0.6596(2) 0.0360(12) Uani 1 1 d . . .
H21A H 0.5399 0.7799 0.6757 0.043 Uiso 1 1 calc R . .
H21B H 0.4420 0.8341 0.6683 0.043 Uiso 1 1 calc R . .
C22 C 0.4247(3) 0.6951(3) 0.68745(19) 0.0278(10) Uani 1 1 d D . .
H22A H 0.412(3) 0.709(3) 0.7241(6) 0.033 Uiso 1 1 d D . .
C23 C 0.4430(3) 0.6016(3) 0.6759(2) 0.0273(10) Uani 1 1 d D . .
H23A H 0.425(3) 0.558(2) 0.7014(15) 0.033 Uiso 1 1 d D . .
C24 C 0.5200(3) 0.5673(3) 0.6358(2) 0.0312(9) Uani 1 1 d . . .
H24A H 0.5489 0.5098 0.6515 0.037 Uiso 1 1 calc R . .
H24B H 0.5699 0.6154 0.6325 0.037 Uiso 1 1 calc R . .
C25 C 0.4785(3) 0.5470(3) 0.5769(2) 0.0298(10) Uani 1 1 d . . .
H25A H 0.5290 0.5517 0.5478 0.036 Uiso 1 1 calc R . .
H25B H 0.4538 0.4823 0.5761 0.036 Uiso 1 1 calc R . .
F1 F 0.3644(2) 0.7977(2) 0.40780(17) 0.0623(10) Uani 1 1 d . . .
F2 F 0.3588(2) 0.7096(2) 0.32712(13) 0.0519(8) Uani 1 1 d . . .
F3 F 0.22362(18) 0.74394(19) 0.37388(14) 0.0462(7) Uani 1 1 d . . .
F4 F 0.32930(19) 0.64345(19) 0.41296(12) 0.0462(7) Uani 1 1 d . . .
B1 B 0.3187(4) 0.7252(3) 0.3801(2) 0.0311(11) 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
Rh1 0.01631(14) 0.01967(14) 0.02220(15) -0.00129(14) 0.00146(14) -0.00072(13)
N1 0.0166(14) 0.0222(15) 0.0201(16) -0.0019(14) 0.0006(14) 0.0056(16)
N16 0.0162(15) 0.0286(18) 0.0208(18) -0.0002(15) -0.0010(14) -0.0025(14)
C2 0.028(2) 0.031(2) 0.021(2) -0.0030(16) -0.005(2) 0.0082(19)
C3 0.042(3) 0.035(2) 0.031(2) 0.0104(19) 0.002(2) 0.009(2)
C4 0.040(3) 0.035(2) 0.039(3) 0.002(2) 0.003(2) 0.020(2)
C5 0.037(2) 0.027(2) 0.035(3) -0.0055(19) 0.003(2) 0.014(2)
C6 0.0179(19) 0.027(2) 0.032(2) -0.0074(18) -0.0013(18) 0.0047(16)
C7 0.0165(19) 0.032(2) 0.039(2) -0.008(2) 0.0025(19) 0.0000(18)
C8 0.0163(19) 0.032(2) 0.038(3) -0.0016(19) -0.0019(18) -0.0052(17)
C9 0.0225(18) 0.0205(18) 0.030(2) -0.0002(19) 0.0017(19) -0.0016(15)
C10 0.022(2) 0.025(2) 0.027(2) -0.0064(17) -0.0013(18) -0.0032(17)
C11 0.021(2) 0.0202(19) 0.031(2) 0.0003(17) 0.0023(17) 0.0009(16)
C12 0.032(2) 0.030(2) 0.041(3) 0.013(2) 0.003(2) 0.004(2)
C13 0.028(2) 0.060(3) 0.040(3) 0.022(3) 0.002(2) -0.005(2)
C14 0.021(2) 0.059(3) 0.031(3) 0.009(2) 0.0036(19) -0.001(2)
C15 0.022(2) 0.041(2) 0.023(2) 0.0011(19) -0.0021(18) -0.0011(19)
C17 0.0193(18) 0.031(2) 0.027(2) -0.002(2) 0.0040(16) 0.000(2)
C18 0.020(2) 0.033(2) 0.023(2) -0.0023(17) 0.0044(18) 0.0010(17)
C19 0.031(2) 0.032(2) 0.023(2) 0.0100(19) 0.0080(19) 0.004(2)
C20 0.034(3) 0.036(3) 0.038(3) 0.002(2) 0.014(2) -0.015(2)
C21 0.032(2) 0.028(2) 0.048(3) -0.015(2) 0.008(2) -0.017(2)
C22 0.029(2) 0.034(2) 0.020(2) -0.0027(19) -0.003(2) -0.010(2)
C23 0.015(2) 0.042(3) 0.026(2) 0.0098(18) -0.0006(18) 0.0016(19)
C24 0.0232(19) 0.037(2) 0.033(2) 0.005(2) 0.003(2) 0.0068(18)
C25 0.020(2) 0.036(2) 0.033(3) 0.000(2) 0.0041(19) -0.0013(19)
F1 0.0433(17) 0.0435(17) 0.100(3) -0.0245(19) 0.0025(19) -0.0088(14)
F2 0.0453(17) 0.073(2) 0.0372(17) 0.0075(16) 0.0084(14) 0.0000(17)
F3 0.0286(13) 0.0514(16) 0.059(2) 0.0075(15) -0.0052(14) -0.0018(12)
F4 0.0548(17) 0.0396(14) 0.0443(16) 0.0097(14) 0.0059(13) 0.0020(15)
B1 0.029(2) 0.026(2) 0.039(3) 0.003(2) -0.001(3) -0.008(2)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Rh1 C22 2.134(4) . ?
Rh1 C18 2.149(4) . ?
Rh1 C23 2.155(4) . ?
Rh1 C19 2.161(4) . ?
Rh1 N1 2.214(3) . ?
Rh1 N16 2.242(3) . ?
N1 C2 1.506(5) . ?
N1 C10 1.513(5) . ?
N1 C6 1.527(5) . ?
N16 C17 1.496(5) . ?
N16 C11 1.508(5) . ?
N16 C15 1.513(5) . ?
C2 C3 1.523(6) . ?
C3 C4 1.535(6) . ?
C4 C5 1.514(7) . ?
C5 C6 1.525(6) . ?
C6 C7 1.498(6) . ?
C7 C17 1.529(6) . ?
C7 C8 1.530(6) . ?
C8 C9 1.548(6) . ?
C9 C10 1.520(6) . ?
C9 C11 1.535(6) . ?
C11 C12 1.540(6) . ?
C12 C13 1.536(7) . ?
C13 C14 1.495(7) . ?
C14 C15 1.518(6) . ?
C18 C19 1.377(6) . ?
C18 C25 1.493(6) . ?
C19 C20 1.515(7) . ?
C20 C21 1.527(7) . ?
C21 C22 1.505(6) . ?
C22 C23 1.390(6) . ?
C23 C24 1.523(6) . ?
C24 C25 1.530(6) . ?
F1 B1 1.385(6) . ?
F2 B1 1.384(6) . ?
F3 B1 1.383(6) . ?
F4 B1 1.409(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C22 Rh1 C18 95.96(17) . . ?
C22 Rh1 C23 37.83(17) . . ?
C18 Rh1 C23 79.06(18) . . ?
C22 Rh1 C19 80.42(18) . . ?
C18 Rh1 C19 37.26(17) . . ?
C23 Rh1 C19 87.00(16) . . ?
C22 Rh1 N1 161.56(15) . . ?
C18 Rh1 N1 93.52(15) . . ?
C23 Rh1 N1 160.53(14) . . ?
C19 Rh1 N1 98.00(15) . . ?
C22 Rh1 N16 95.05(15) . . ?
C18 Rh1 N16 149.83(15) . . ?
C23 Rh1 N16 92.97(15) . . ?
C19 Rh1 N16 172.64(15) . . ?
N1 Rh1 N16 84.44(12) . . ?
C2 N1 C10 107.6(3) . . ?
C2 N1 C6 104.4(3) . . ?
C10 N1 C6 107.9(3) . . ?
C2 N1 Rh1 117.5(2) . . ?
C10 N1 Rh1 98.3(2) . . ?
C6 N1 Rh1 120.1(2) . . ?
C17 N16 C11 113.5(3) . . ?
C17 N16 C15 104.4(3) . . ?
C11 N16 C15 111.6(3) . . ?
C17 N16 Rh1 114.9(2) . . ?
C11 N16 Rh1 98.2(2) . . ?
C15 N16 Rh1 114.6(2) . . ?
N1 C2 C3 113.6(3) . . ?
C2 C3 C4 112.1(4) . . ?
C5 C4 C3 108.1(4) . . ?
C4 C5 C6 108.4(4) . . ?
C7 C6 C5 113.8(4) . . ?
C7 C6 N1 112.9(3) . . ?
C5 C6 N1 109.7(3) . . ?
C6 C7 C17 116.0(3) . . ?
C6 C7 C8 109.8(4) . . ?
C17 C7 C8 108.5(4) . . ?
C7 C8 C9 105.5(3) . . ?
C10 C9 C11 117.1(3) . . ?
C10 C9 C8 108.3(3) . . ?
C11 C9 C8 110.0(4) . . ?
N1 C10 C9 114.3(3) . . ?
N16 C11 C9 110.9(3) . . ?
N16 C11 C12 115.4(4) . . ?
C9 C11 C12 109.0(3) . . ?
C13 C12 C11 112.5(4) . . ?
C14 C13 C12 108.8(4) . . ?
C13 C14 C15 109.1(4) . . ?
N16 C15 C14 115.8(3) . . ?
N16 C17 C7 114.9(3) . . ?
C19 C18 C25 126.8(4) . . ?
C19 C18 Rh1 71.8(3) . . ?
C25 C18 Rh1 111.5(3) . . ?
C18 C19 C20 124.4(5) . . ?
C18 C19 Rh1 70.9(3) . . ?
C20 C19 Rh1 113.3(3) . . ?
C19 C20 C21 112.7(4) . . ?
C22 C21 C20 112.2(4) . . ?
C23 C22 C21 124.1(4) . . ?
C23 C22 Rh1 71.9(3) . . ?
C21 C22 Rh1 111.6(3) . . ?
C22 C23 C24 124.4(4) . . ?
C22 C23 Rh1 70.3(3) . . ?
C24 C23 Rh1 115.0(3) . . ?
C23 C24 C25 110.0(3) . . ?
C18 C25 C24 111.9(4) . . ?
F3 B1 F2 109.8(4) . . ?
F3 B1 F1 111.2(4) . . ?
F2 B1 F1 110.4(4) . . ?
F3 B1 F4 108.8(4) . . ?
F2 B1 F4 108.2(4) . . ?
F1 B1 F4 108.4(4) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         1.217
_refine_diff_density_min         -0.724
_refine_diff_density_rms         0.097

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.132 0.750 26 5 ' '
2 0.000 0.868 0.250 26 5 ' '
3 0.162 0.500 0.500 97 34 ' '
4 0.337 0.000 0.000 97 33 ' '
5 0.500 0.368 0.250 26 5 ' '
6 0.500 0.632 0.750 26 5 ' '
7 0.662 0.000 0.500 97 34 ' '
8 0.837 0.500 1.000 97 33 ' '
_platon_squeeze_details          
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_vrf_PLAT601_k08228              
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PROBLEM: Structure Contains Solvent Accessible VOIDS of . 96.00 A**3
RESPONSE: During the
refinement of the structure, electron density peaks were located
that were believed to be highly disordered
solvent molecules (possibly THF and/or diethylether). Attempts
made to model the solvent molecule were not successful.
The SQUEEZE option in PLATON (Spek, 2003) indicated there was a
solvent cavity of volume 96.0 \%A^3^ containing approximately 34
electrons. In the final cycles of refinement, this contribution to the
electron density was removed from the observed data. The
density, the F(000) value, the molecular weight and the formula are
given without taking into account the results obtained with the
SQUEEZE option PLATON (Spek, 2003). Similar treatments of disordered
solvent molecules were carried out by St\"ahler et al. (2001),
Cox et al. (2003), Mohamed et al. (2003) and Athimoolam et al. (2005).
References:

Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13

Athimoolam, S., Kumar, J., Ramakrishnan, V. & Rajaram, R.K. (2005).
Acta Cryst. E61, m2014-m2017.

Cox, J.P., Kumarasammy, Y., Nahar, L., Sarkar D.S. & Shoeb, M.
(2003). Acta Cryst. E59, o975-o977.

Mohamed, A.A., Krause Bauer, A.J., Bruce, E.A. & Bruce M.R.M.
(2003). Acta Cryst. C59, m84-m86.

St\"ahler, R., N\"ather, C. & Bensch, W. (2001). Acta Cryst.
C57, 26-27.

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# end Validation Reply Form