#------------------------------------------------------------------------------
#$Date: 2016-03-24 17:08:07 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179678 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/00/7000009.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
loop_
_publ_author_name
'Neveling, Arno'
'Julius, Gerrit R.'
'Cronje, Stephanie'
'Esterhuysen, Catharine'
'Raubenheimer, Helgard G.'
_publ_section_title
;
 Thione complexes of Rh(I): a first comparison with the bonding and
 catalytic activity of related carbene and imine compounds.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              181
_journal_page_last               192
_journal_paper_doi               10.1039/b414040k
_journal_year                    2005
_chemical_formula_sum            'C30 H35 Cl N2 O P Rh S'
_chemical_formula_weight         640.99
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.147(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.04670(10)
_cell_length_b                   10.58750(10)
_cell_length_c                   30.4334(3)
_cell_measurement_reflns_used    7915
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.7
_cell_measurement_theta_min      1.02
_cell_volume                     2907.34(5)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEP-III for Windows (Farrugia,1997)'
_computing_publication_material  'X-Seed (Barbour, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'φ and ω scans to fill Ewald sphere'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0223
_diffrn_reflns_av_sigmaI/netI    0.0329
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            12308
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         3.32
_exptl_absorpt_coefficient_mu    0.832
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.464
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.838
_refine_diff_density_min         -0.553
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     340
_refine_ls_number_reflns         6329
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0271
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0305P)²+0.8904P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0620
_refine_ls_wR_factor_ref         0.0663
_reflns_number_gt                5053
_reflns_number_total             6329
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b414040k.txt
_cod_data_source_block           19
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7000009
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'
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 . .
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'
Cl Cl 0.1484 0.1585 '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'
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'
Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
C1 Rh1 P1 93.79(7) . . ?
C1 Rh1 Cl1 174.81(7) . . ?
P1 Rh1 Cl1 89.84(2) . . ?
C1 Rh1 S1 86.16(7) . . ?
P1 Rh1 S1 179.38(2) . . ?
Cl1 Rh1 S1 90.25(2) . . ?
C11 S1 Rh1 106.86(7) . . ?
C21 P1 C31 102.96(9) . . ?
C21 P1 C41 104.18(10) . . ?
C31 P1 C41 102.36(10) . . ?
C21 P1 Rh1 113.12(7) . . ?
C31 P1 Rh1 118.98(7) . . ?
C41 P1 Rh1 113.53(7) . . ?
C11 N11 C12 109.14(18) . . ?
C11 N11 C14 122.55(18) . . ?
C12 N11 C14 128.31(18) . . ?
C11 N12 C13 109.31(18) . . ?
C11 N12 C17 127.9(2) . . ?
C13 N12 C17 122.78(19) . . ?
O1 C1 Rh1 175.6(2) . . ?
N11 C11 N12 107.06(18) . . ?
N11 C11 S1 126.26(17) . . ?
N12 C11 S1 126.37(17) . . ?
C13 C12 N11 107.14(19) . . ?
C13 C12 C15 127.7(2) . . ?
N11 C12 C15 125.1(2) . . ?
C12 C13 N12 107.34(18) . . ?
C12 C13 C16 129.1(2) . . ?
N12 C13 C16 123.6(2) . . ?
N11 C14 C18 112.38(19) . . ?
N11 C14 C19 109.24(19) . . ?
C18 C14 C19 114.4(2) . . ?
N11 C14 H14 106.8 . . ?
C18 C14 H14 106.8 . . ?
C19 C14 H14 106.8 . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C13 C16 H16A 109.5 . . ?
C13 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C13 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C110 C17 N12 113.0(2) . . ?
C110 C17 C111 115.8(2) . . ?
N12 C17 C111 112.6(2) . . ?
C110 C17 H17 104.7 . . ?
N12 C17 H17 104.7 . . ?
C111 C17 H17 104.7 . . ?
C14 C18 H18A 109.5 . . ?
C14 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C14 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C14 C19 H19A 109.5 . . ?
C14 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C14 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C22 C21 C26 119.2(2) . . ?
C22 C21 P1 117.78(17) . . ?
C26 C21 P1 123.01(17) . . ?
C23 C22 C21 120.2(2) . . ?
C23 C22 H22 119.9 . . ?
C21 C22 H22 119.9 . . ?
C24 C23 C22 120.2(3) . . ?
C24 C23 H23 119.9 . . ?
C22 C23 H23 119.9 . . ?
C23 C24 C25 120.2(2) . . ?
C23 C24 H24 119.9 . . ?
C25 C24 H24 119.9 . . ?
C24 C25 C26 120.4(2) . . ?
C24 C25 H25 119.8 . . ?
C26 C25 H25 119.8 . . ?
C25 C26 C21 119.9(2) . . ?
C25 C26 H26 120.1 . . ?
C21 C26 H26 120.1 . . ?
C32 C31 C36 118.46(19) . . ?
C32 C31 P1 122.05(16) . . ?
C36 C31 P1 119.47(16) . . ?
C33 C32 C31 120.5(2) . . ?
C33 C32 H32 119.8 . . ?
C31 C32 H32 119.8 . . ?
C34 C33 C32 120.3(2) . . ?
C34 C33 H33 119.8 . . ?
C32 C33 H33 119.8 . . ?
C33 C34 C35 119.8(2) . . ?
C33 C34 H34 120.1 . . ?
C35 C34 H34 120.1 . . ?
C34 C35 C36 120.4(2) . . ?
C34 C35 H35 119.8 . . ?
C36 C35 H35 119.8 . . ?
C35 C36 C31 120.6(2) . . ?
C35 C36 H36 119.7 . . ?
C31 C36 H36 119.7 . . ?
C46 C41 C42 118.4(2) . . ?
C46 C41 P1 119.18(17) . . ?
C42 C41 P1 122.44(17) . . ?
C43 C42 C41 120.5(2) . . ?
C43 C42 H42 119.7 . . ?
C41 C42 H42 119.7 . . ?
C44 C43 C42 120.4(3) . . ?
C44 C43 H43 119.8 . . ?
C42 C43 H43 119.8 . . ?
C43 C44 C45 120.3(2) . . ?
C43 C44 H44 119.9 . . ?
C45 C44 H44 119.9 . . ?
C44 C45 C46 120.0(2) . . ?
C44 C45 H45 120.0 . . ?
C46 C45 H45 120.0 . . ?
C45 C46 C41 120.4(2) . . ?
C45 C46 H46 119.8 . . ?
C41 C46 H46 119.8 . . ?
C17 C110 H11D 109.5 . . ?
C17 C110 H11E 109.5 . . ?
H11D C110 H11E 109.5 . . ?
C17 C110 H11F 109.5 . . ?
H11D C110 H11F 109.5 . . ?
H11E C110 H11F 109.5 . . ?
C17 C111 H11G 109.5 . . ?
C17 C111 H11H 109.5 . . ?
H11G C111 H11H 109.5 . . ?
C17 C111 H11I 109.5 . . ?
H11G C111 H11I 109.5 . . ?
H11H C111 H11I 109.5 . . ?
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 C1 1.805(2) . ?
Rh1 P1 2.2654(5) . ?
Rh1 Cl1 2.3700(6) . ?
Rh1 S1 2.4067(6) . ?
S1 C11 1.723(2) . ?
P1 C21 1.826(2) . ?
P1 C31 1.832(2) . ?
P1 C41 1.833(2) . ?
O1 C1 1.147(3) . ?
N11 C11 1.352(3) . ?
N11 C12 1.397(3) . ?
N11 C14 1.483(3) . ?
N12 C11 1.354(3) . ?
N12 C13 1.389(3) . ?
N12 C17 1.487(3) . ?
C12 C13 1.350(3) . ?
C12 C15 1.492(3) . ?
C13 C16 1.494(3) . ?
C14 C18 1.512(3) . ?
C14 C19 1.519(3) . ?
C14 H14 1.0000 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C110 1.477(4) . ?
C17 C111 1.488(4) . ?
C17 H17 1.0000 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C21 C22 1.391(3) . ?
C21 C26 1.392(3) . ?
C22 C23 1.387(3) . ?
C22 H22 0.9500 . ?
C23 C24 1.374(4) . ?
C23 H23 0.9500 . ?
C24 C25 1.375(4) . ?
C24 H24 0.9500 . ?
C25 C26 1.389(3) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C31 C32 1.391(3) . ?
C31 C36 1.396(3) . ?
C32 C33 1.389(3) . ?
C32 H32 0.9500 . ?
C33 C34 1.377(3) . ?
C33 H33 0.9500 . ?
C34 C35 1.377(3) . ?
C34 H34 0.9500 . ?
C35 C36 1.384(3) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C41 C46 1.391(3) . ?
C41 C42 1.395(3) . ?
C42 C43 1.384(3) . ?
C42 H42 0.9500 . ?
C43 C44 1.361(4) . ?
C43 H43 0.9500 . ?
C44 C45 1.381(4) . ?
C44 H44 0.9500 . ?
C45 C46 1.388(3) . ?
C45 H45 0.9500 . ?
C46 H46 0.9500 . ?
C110 H11D 0.9800 . ?
C110 H11E 0.9800 . ?
C110 H11F 0.9800 . ?
C111 H11G 0.9800 . ?
C111 H11H 0.9800 . ?
C111 H11I 0.9800 . ?
