Stereoselective intramolecular 1,3 C-H insertion in Rh(II) carbene reactions.
Shi, Weifeng; Zhang, Bo; Zhang, Jian; Liu, Binge; Zhang, Shiwei; Wang, Jianbo; Organic letters 7 (2005) 3103–3106; doi:10.1021/ol051130l

data_1506632
_publ_section_title
;
 Stereoselective intramolecular 1,3 C-H insertion in Rh(II) carbene
 reactions.
;
_journal_issue                   14
_journal_name_full               'Organic letters'
_journal_page_first              3103
_journal_page_last               3106
_journal_paper_doi               10.1021/ol051130l
_journal_volume                  7
_journal_year                    2005
_chemical_formula_sum            'C18 H24 O4 S'
_chemical_formula_weight         336.43
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   'hydrogen atoms are generated by HFIX'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                94.17(3)
_cell_angle_beta                 104.87(3)
_cell_angle_gamma                117.63(3)
_cell_formula_units_Z            2
_cell_length_a                   9.0592(18)
_cell_length_b                   9.6194(19)
_cell_length_c                   12.332(3)
_cell_measurement_reflns_used    7426
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.58
_cell_volume                     896.9(5)
_computing_cell_refinement       'Molecular Structure Corporation (1994)'
_computing_data_collection       'Molecular Structure Corporation (1994)'
_computing_data_reduction        'Sheldrick, G. M. (1997) SHELXS97, Program'
_computing_molecular_graphics    'Interactive Molecular Graphics XP, Virsion'
_computing_publication_material  'Sheldrick, G. M. (1997) SHELXL97, Program'
_computing_structure_refinement  'Sheldrick, G. M. (1997) SHELXL97, Program'
_computing_structure_solution    'Sheldrick, G. M. (1997) SHELXS97, Program'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean '100x100 microns'
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Rigaku RAXIS RAPID IP'
_diffrn_measurement_method       Oscillation
_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  0.0381
_diffrn_reflns_av_sigmaI/netI    0.0349
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            3984
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.58
_exptl_absorpt_coefficient_mu    0.197
_exptl_absorpt_correction_T_max  0.952
_exptl_absorpt_correction_T_min  0.906
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
                                  HIGASHI, T. (1995). Abscor-Empirical
                                  Absorption
                                  Correction based on Fourier Series
                                  Approximation.Rigaku Corporation,Tokyo,
                                  Japan.
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.246
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             360
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.354
_refine_diff_density_min         -0.362
_refine_diff_density_rms         0.045
_refine_ls_extinction_coef       0.185(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    'hydrogen coordinates ride on the coordinates'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         3984
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0652
_refine_ls_R_factor_gt           0.0459
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0818P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1275
_refine_ls_wR_factor_ref         0.1348
_reflns_number_gt                2809
_reflns_number_total             3984
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol051130lsi20050516_054138.cif
_cod_data_source_block           a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Empirical'
changed to 'empirical' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        896.9(3)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1506632