Stereospecific Syntheses and Structures of Planar Chiral Bidentate η5:κS-Indenyl-Sulfanyl and-Sulfinyl Complexes of Rhodium(III)
Baker, Robert W.; Radzey, Hanna; Lucas, Nigel T.; Turner, Peter; Organometallics 31 (2012) 5622–; doi:10.1021/om300581r

data_4078952
_publ_section_title
;
 Stereospecific Syntheses and Structures of Planar Chiral Bidentate
 \h5:\kS-Indenyl-Sulfanyl and-Sulfinyl Complexes of Rhodium(III)
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              5622
_journal_paper_doi               10.1021/om300581r
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C21 H17 Cl2 O Rh S, C D Cl3'
_chemical_formula_sum            'C22 H17 Cl5 D O Rh S'
_chemical_formula_weight         611.59
_chemical_name_systematic
;
(pR*,R~S~*)-Dichloro[(1,2,3,3a,7a-\h)-1-[2-(methylsulfinyl-\kS)-1-naphthyl]-
2-methyl-1H-inden-1-yl]rhodium
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_code                rwb10rm1_face
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.306(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.3101(9)
_cell_length_b                   10.2161(7)
_cell_length_c                   18.6589(13)
_cell_measurement_reflns_used    9472
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      33.359
_cell_measurement_theta_min      2.591
_cell_volume                     2346.0(3)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2003)'
_computing_data_collection       'Bruker APEX 2'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2003)'
_computing_molecular_graphics
;
OLEX2: a complete structure solution, refinement and analysis program. 
Dolomanov et al., J. Appl. Cryst. (2009). 42, 339-341
;
_computing_publication_material
;
OLEX2: a complete structure solution, refinement and analysis program. 
Dolomanov et al., J. Appl. Cryst. (2009). 42, 339-341
ORTEP3 for Windows - L. J. Farrugia, J. Appl. Crystallogr. 1997, 30, 565.
ORTEP-III - M. N. Burnett and C. K. Johnson, Report ORNL-6895. Oak Ridge 
National Laboratory, Oak Ridge, Tennessee, 1996.
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution
;
"A short history of SHELX". Sheldrick, G.M. (2008). Acta Cryst. A64,
112-122.
;
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker FR591 X8 APEX II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0233
_diffrn_reflns_av_sigmaI/netI    0.0145
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            64525
_diffrn_reflns_theta_full        33.39
_diffrn_reflns_theta_max         33.39
_diffrn_reflns_theta_min         1.96
_diffrn_source_current           80.0
_diffrn_source_power             4.0
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.400
_exptl_absorpt_correction_T_max  0.91889
_exptl_absorpt_correction_T_min  0.73451
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
 SADABS-2008/1 (Bruker,2008) was used to apply a Gaussian absorption correction
 using indexed crystal faces, followed by a multiscan absorption correction.
 wR2(int) was 0.0520 before and 0.0352 after correction.
 The Ratio of minimum to maximum transmission is 0.799.
 A Lambda/2 correction factor = 0.0015 was applied to the data.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.732
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.333
_exptl_crystal_size_mid          0.115
_exptl_crystal_size_min          0.101
_refine_diff_density_max         0.993
_refine_diff_density_min         -0.897
_refine_diff_density_rms         0.182
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.349
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         9046
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.349
_refine_ls_R_factor_all          0.0266
_refine_ls_R_factor_gt           0.0205
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
calc w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+0.7000P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0610
_refine_ls_wR_factor_ref         0.0816
_reflns_number_gt                8149
_reflns_number_total             9046
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300581r_si_001.cif
_cod_data_source_block           rac-8
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from
2011-04-26.

'_exptl_absorpt_correction_type' value 'Gaussian'
changed to 'gaussian' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_database_code               4078952