Rh–POP Pincer Xantphos Complexes for C–S and C–H Activation. Implications for Carbothiolation Catalysis
Ren, Peng; Pike, Sebastian D.; Pernik, Indrek; Weller, Andrew S.; Willis, Michael C.; Organometallics 34 (2015) 711–; doi:10.1021/om500984y

data_4085480
_publ_section_title
;
 Rh--POP Pincer Xantphos Complexes for C--S and C--H Activation.
 Implications for Carbothiolation Catalysis
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              711
_journal_paper_doi               10.1021/om500984y
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C53 H42 O P2 Rh, C32 H12 B F24'
_chemical_formula_sum            'C85 H54 B F24 O P2 Rh'
_chemical_formula_weight         1722.96
_chemical_melting_point          ?
_chemical_name_common            'Compound 6'
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                92.0677(6)
_cell_angle_beta                 94.1593(6)
_cell_angle_gamma                104.8905(7)
_cell_formula_units_Z            2
_cell_length_a                   13.71570(20)
_cell_length_b                   14.87730(20)
_cell_length_c                   19.80160(29)
_cell_measurement_reflns_used    15839
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     3888.31(10)
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'Denzo/Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'ORTEP3 (Farrugia, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_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  0.0449
_diffrn_reflns_av_sigmaI/netI    0.0885
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            29731
_diffrn_reflns_theta_full        27.55
_diffrn_reflns_theta_max         27.55
_diffrn_reflns_theta_min         1.03
_exptl_absorpt_coefficient_mu    0.366
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.9375
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Denzo/Scalepack (Otwinowski & Minor 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.484
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1754
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.945
_refine_diff_density_min         -1.898
_refine_diff_density_rms         0.284
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1085
_refine_ls_number_reflns         17798
_refine_ls_number_restraints     342
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.1124
_refine_ls_R_factor_gt           0.0607
_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^)+(0.1365P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1561
_refine_ls_wR_factor_ref         0.2212
_reflns_number_gt                11944
_reflns_number_total             17798
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500984y_si_001.cif
_cod_data_source_block           035ip14
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

 Adding full bibliography for 4085478--4085487.cif.
;
_cod_original_cell_volume        3888.315(97)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C85 H54     B F24 O P2 Rh'
_cod_database_code               4085480