#------------------------------------------------------------------------------
#$Date: 2008-01-14 00:15:36 +0200 (Mon, 14 Jan 2008) $
#$Revision: 14 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/7000009.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7000009
_journal_name_full               'Dalton Trans.'
_journal_year                    2005
_publ_section_title
;
Thione complexes of Rh(I): a first comparison with the bonding and catalytic
activity of related carbene and imine compounds.
;
loop_
_publ_author_name
'A.Neveling'
'H.G.Raubenheimer'
'S.Cronje'
'G.R.Julius'
'C.Esterhuysen'
_chemical_formula_sum            'C30 H35 Cl N2 O P Rh S'
_chemical_formula_weight         640.99
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/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                   9.04670(10)
_cell_length_b                   10.58750(10)
_cell_length_c                   30.4334(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.147(1)
_cell_angle_gamma                90.00
_cell_volume                     2907.34(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    7915
_cell_measurement_theta_max      28.7
_cell_measurement_theta_min      1.02
_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.464
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1320
_exptl_absorpt_coefficient_mu    0.832
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       '\f and \w scans to fill Ewald sphere'
_diffrn_reflns_number            12308
_diffrn_reflns_av_R_equivalents  0.0223
_diffrn_reflns_av_sigmaI/netI    0.0329
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_theta_min         3.32
_diffrn_reflns_theta_max         27.00
_reflns_number_total             6329
_reflns_number_gt                5053
_reflns_threshold_expression     >2sigma(I)
_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^)+(0.0305P)^2^+0.8904P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     heavy
_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         6329
_refine_ls_number_parameters     340
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0271
_refine_ls_wR_factor_ref         0.0663
_refine_ls_wR_factor_gt          0.0620
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.035
_refine_ls_shift/su_max          0.004
_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 0.307016(17) 0.926122(15) 0.601524(5) 0.02312(6) Uani 1 1 d . . .
Cl1 Cl 0.44174(7) 0.83313(6) 0.662922(18) 0.03925(15) Uani 1 1 d . . .
S1 S 0.22484(7) 1.09230(5) 0.647904(19) 0.03464(14) Uani 1 1 d . . .
P1 P 0.38199(6) 0.76861(5) 0.557925(17) 0.02212(12) Uani 1 1 d . . .
O1 O 0.1520(2) 1.07106(17) 0.52934(6) 0.0492(5) Uani 1 1 d . . .
N11 N 0.13744(18) 0.94410(16) 0.71545(6) 0.0260(4) Uani 1 1 d . . .
N12 N 0.31544(19) 1.07418(17) 0.73592(6) 0.0302(4) Uani 1 1 d . . .
C1 C 0.2115(2) 1.0105(2) 0.55642(7) 0.0306(5) Uani 1 1 d . . .
C11 C 0.2294(2) 1.0325(2) 0.70063(7) 0.0268(5) Uani 1 1 d . . .
C12 C 0.1648(2) 0.9316(2) 0.76100(7) 0.0281(5) Uani 1 1 d . . .
C13 C 0.2758(2) 1.0119(2) 0.77350(7) 0.0303(5) Uani 1 1 d . . .
C14 C 0.0279(2) 0.8752(2) 0.68579(7) 0.0336(5) Uani 1 1 d . . .
H14 H 0.0601 0.8849 0.6552 0.040 Uiso 1 1 calc R . .
C15 C 0.0786(3) 0.8496(3) 0.78974(8) 0.0407(6) Uani 1 1 d . . .
H15A H 0.1021 0.7608 0.7844 0.061 Uiso 1 1 calc R . .
H15B H -0.0276 0.8638 0.7830 0.061 Uiso 1 1 calc R . .
H15C H 0.1048 0.8703 0.8207 0.061 Uiso 1 1 calc R . .
C16 C 0.3462(3) 1.0371(3) 0.81856(8) 0.0456(6) Uani 1 1 d . . .
H16A H 0.2964 0.9869 0.8402 0.068 Uiso 1 1 calc R . .
H16B H 0.3372 1.1271 0.8255 0.068 Uiso 1 1 calc R . .
H16C H 0.4513 1.0138 0.8196 0.068 Uiso 1 1 calc R . .
C17 C 0.4360(3) 1.1697(2) 0.73676(9) 0.0419(6) Uani 1 1 d . . .
H17 H 0.4733 1.1754 0.7684 0.050 Uiso 1 1 calc R . .
C18 C 0.0261(3) 0.7350(2) 0.69542(9) 0.0460(6) Uani 1 1 d . . .
H18A H 0.1280 0.7047 0.7012 0.069 Uiso 1 1 calc R . .
H18B H -0.0212 0.6901 0.6700 0.069 Uiso 1 1 calc R . .
H18C H -0.0296 0.7196 0.7213 0.069 Uiso 1 1 calc R . .
C19 C -0.1222(3) 0.9392(3) 0.68654(9) 0.0515(7) Uani 1 1 d . . .
H19A H -0.1519 0.9418 0.7169 0.077 Uiso 1 1 calc R . .
H19B H -0.1958 0.8917 0.6680 0.077 Uiso 1 1 calc R . .
H19C H -0.1155 1.0255 0.6752 0.077 Uiso 1 1 calc R . .
C21 C 0.5801(2) 0.7356(2) 0.56621(7) 0.0264(5) Uani 1 1 d . . .
C22 C 0.6770(2) 0.8378(2) 0.56816(8) 0.0361(5) Uani 1 1 d . . .
H22 H 0.6390 0.9214 0.5665 0.043 Uiso 1 1 calc R . .
C23 C 0.8288(3) 0.8180(3) 0.57254(8) 0.0470(7) Uani 1 1 d . . .
H23 H 0.8946 0.8880 0.5731 0.056 Uiso 1 1 calc R . .
C24 C 0.8844(3) 0.6973(3) 0.57604(8) 0.0488(7) Uani 1 1 d . . .
H24 H 0.9885 0.6841 0.5794 0.059 Uiso 1 1 calc R . .
C25 C 0.7898(3) 0.5955(3) 0.57471(8) 0.0432(6) Uani 1 1 d . . .
H25 H 0.8288 0.5123 0.5772 0.052 Uiso 1 1 calc R . .
C26 C 0.6375(2) 0.6137(2) 0.56966(7) 0.0321(5) Uani 1 1 d . . .
H26 H 0.5725 0.5431 0.5686 0.039 Uiso 1 1 calc R . .
C31 C 0.3530(2) 0.78535(19) 0.49799(7) 0.0243(4) Uani 1 1 d . . .
C32 C 0.4679(2) 0.7709(2) 0.47042(7) 0.0332(5) Uani 1 1 d . . .
H32 H 0.5654 0.7541 0.4827 0.040 Uiso 1 1 calc R . .
C33 C 0.4411(3) 0.7810(3) 0.42502(8) 0.0432(6) Uani 1 1 d . . .
H33 H 0.5202 0.7704 0.4065 0.052 Uiso 1 1 calc R . .
C34 C 0.3004(3) 0.8063(2) 0.40681(8) 0.0411(6) Uani 1 1 d . . .
H34 H 0.2826 0.8136 0.3758 0.049 Uiso 1 1 calc R . .
C35 C 0.1857(3) 0.8210(2) 0.43374(8) 0.0371(6) Uani 1 1 d . . .
H35 H 0.0886 0.8383 0.4212 0.045 Uiso 1 1 calc R . .
C36 C 0.2110(2) 0.8109(2) 0.47900(7) 0.0306(5) Uani 1 1 d . . .
H36 H 0.1312 0.8214 0.4973 0.037 Uiso 1 1 calc R . .
C41 C 0.2935(2) 0.6164(2) 0.56771(7) 0.0260(5) Uani 1 1 d . . .
C42 C 0.2475(3) 0.5344(2) 0.53354(8) 0.0407(6) Uani 1 1 d . . .
H42 H 0.2624 0.5568 0.5040 0.049 Uiso 1 1 calc R . .
C43 C 0.1803(3) 0.4206(2) 0.54239(10) 0.0499(7) Uani 1 1 d . . .
H43 H 0.1489 0.3658 0.5188 0.060 Uiso 1 1 calc R . .
C44 C 0.1589(3) 0.3869(2) 0.58460(10) 0.0478(7) Uani 1 1 d . . .
H44 H 0.1136 0.3083 0.5904 0.057 Uiso 1 1 calc R . .
C45 C 0.2029(3) 0.4665(3) 0.61904(9) 0.0466(7) Uani 1 1 d . . .
H45 H 0.1878 0.4425 0.6485 0.056 Uiso 1 1 calc R . .
C46 C 0.2690(3) 0.5814(2) 0.61065(8) 0.0365(5) Uani 1 1 d . . .
H46 H 0.2977 0.6366 0.6344 0.044 Uiso 1 1 calc R . .
C110 C 0.5652(3) 1.1275(3) 0.71365(12) 0.0607(9) Uani 1 1 d . . .
H11D H 0.5970 1.0441 0.7246 0.091 Uiso 1 1 calc R . .
H11E H 0.6466 1.1879 0.7190 0.091 Uiso 1 1 calc R . .
H11F H 0.5379 1.1223 0.6819 0.091 Uiso 1 1 calc R . .
C111 C 0.3801(3) 1.2987(2) 0.72544(11) 0.0538(7) Uani 1 1 d . . .
H11G H 0.3500 1.3028 0.6939 0.081 Uiso 1 1 calc R . .
H11H H 0.4587 1.3606 0.7326 0.081 Uiso 1 1 calc R . .
H11I H 0.2947 1.3176 0.7424 0.081 Uiso 1 1 calc R . .