Potential Carbon‒Fluorine Reductive Elimination from Pincer-Supported Rh(III) and Dominating Side Reactions: Theoretical and Experimental Examination
Timpa, Samuel D.; Zhou, Jia; Bhuvanesh, Nattamai; Ozerov, Oleg V.; Organometallics 33 (2014) 6210–; doi:10.1021/om5008902

data_4084427
_publ_section_title
;
 Potential Carbon--Fluorine Reductive Elimination from Pincer-Supported
 Rh(III) and Dominating Side Reactions: Theoretical and Experimental
 Examination
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              6210
_journal_paper_doi               10.1021/om5008902
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C32 H59 O3 P2 Rh'
_chemical_formula_sum            'C32 H59 O3 P2 Rh'
_chemical_formula_weight         656.64
_chemical_name_common            (POCOP)Rh(CHCH2)(OtBu)
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.306(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.411(7)
_cell_length_b                   16.436(9)
_cell_length_c                   17.215(10)
_cell_measurement_reflns_used    5134
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      23.27
_cell_measurement_theta_min      2.38
_cell_volume                     3497(3)
_computing_cell_refinement
; 
  APEX-II(BRUKER-NONIUS, 2003) 
;
_computing_data_collection       'APEX-II (BRUKER-NONIUS, 2003)'
_computing_data_reduction        APEX-II
_computing_molecular_graphics    Olex2
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'APEX II'
_diffrn_measurement_method       'omega scans'
_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  0.0679
_diffrn_reflns_av_sigmaI/netI    0.0615
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            29115
_diffrn_reflns_theta_full        24.14
_diffrn_reflns_theta_max         24.14
_diffrn_reflns_theta_min         1.94
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.608
_exptl_absorpt_correction_T_max  0.9702
_exptl_absorpt_correction_T_min  0.7119
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; (Sheldrick, 2006)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.247
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1400
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.397
_refine_diff_density_min         -0.404
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.897
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     359
_refine_ls_number_reflns         5538
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      0.900
_refine_ls_R_factor_all          0.0398
_refine_ls_R_factor_gt           0.0291
_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^)+(0.0116P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0511
_refine_ls_wR_factor_ref         0.0532
_reflns_number_gt                4373
_reflns_number_total             5538
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5008902_si_003.cif
_cod_data_source_block           13
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/home/saulius/struct/COD-crude-data--automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 4084426--4084428.cif.
;
_cod_original_sg_symbol_Hall     '-P 2ybn'
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4084427