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_4085483
_publ_section_title
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 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_compound_source        'S10, CRL, University of Oxford'
_chemical_formula_moiety         'C78 H51 B1 F24 N1 O3 P2 Rh1 S1'
_chemical_formula_sum            'C78 H51 B F24 N O3 P2 Rh S'
_chemical_formula_weight         1713.95
_chemical_melting_point          ?
_chemical_name_systematic        'Compound 10''
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             14-04-30
_audit_creation_method           CRYSTALS_ver_14.40
_cell_angle_alpha                90
_cell_angle_beta                 91.0396(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.9983(2)
_cell_length_b                   24.7598(2)
_cell_length_c                   14.20600(10)
_cell_measurement_reflns_used    15641
_cell_measurement_temperature    150
_cell_measurement_theta_max      74
_cell_measurement_theta_min      4
_cell_volume                     7736.36(11)
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.000
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7974
_diffrn_reflns_theta_full        71.445
_diffrn_reflns_theta_max         74.422
_diffrn_reflns_theta_min         3.570
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.369
_exptl_absorpt_correction_T_max  0.60
_exptl_absorpt_correction_T_min  0.42
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.471
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3448
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.150
_platon_squeeze_details
;
The discrete Fourier transform of the void region were treated as 
contributions to the A and B parts of the calculated structure factors.
;
_refine_diff_density_max         1.07
_refine_diff_density_min         -0.68
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0278
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     613
_refine_ls_number_reflns         7253
_refine_ls_number_restraints     698
_refine_ls_R_factor_all          0.0388
_refine_ls_R_factor_gt           0.0374
_refine_ls_shift/su_max          0.0305563
_refine_ls_shift/su_mean         0.0004189
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.04P)^2^ +21.86P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0944
_refine_ls_wR_factor_gt          0.0936
_refine_ls_wR_factor_ref         0.0944
_reflns_limit_h_max              27
_reflns_limit_h_min              -27
_reflns_limit_k_max              30
_reflns_limit_k_min              0
_reflns_limit_l_max              17
_reflns_limit_l_min              0
_reflns_number_gt                6930
_reflns_number_total             7974
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.83
_oxford_diffrn_Wilson_scale      0.42
_oxford_refine_ls_r_factor_ref   0.0388
_oxford_refine_ls_scale          1.802(9)
_oxford_reflns_number_all        7253
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title
'E:\Weller\121SDP14\Solve\121SDP1 At 9:32 on '
_cod_data_source_file            om500984y_si_001.cif
_cod_data_source_block           Compound121SDP14
_cod_depositor_comments
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The following automatic conversions were performed:

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

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

 Adding full bibliography for 4085478--4085487.cif.
;
_cod_original_sg_symbol_H-M      'C 1 2/m 1 '
_cod_original_formula_sum        'C78 H51 B1 F24 N1 O3 P2 Rh1 S1'
_cod_database_code               4085483
_iucr_refine_instruction_details_restraints
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NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
SAME C(33) C(37) F(160) F(170) F(180) AND 
CONT C(33) C(37) F(170) F(180) F(160) AND 
CONT C(33) C(37) F(180) F(160) F(170) AND 
CONT C(33) C(37) F(161) F(171) F(181) AND 
CONT C(33) C(37) F(171) F(181) F(161) AND 
CONT C(33) C(37) F(181) F(161) F(171) 
DELU 0.015 C(33) C(37) F(160) F(170) F(180) AND 
CONT C(33) C(37) F(170) F(180) F(160) AND 
CONT C(33) C(37) F(180) F(160) F(170) AND 
CONT C(33) C(37) F(161) F(171) F(181) AND 
CONT C(33) C(37) F(171) F(181) F(161) AND 
CONT C(33) C(37) F(181) F(161) F(171) 
SIMU 0.015 C(33) C(37) F(160) F(170) F(180) AND 
CONT C(33) C(37) F(170) F(180) F(160) AND 
CONT C(33) C(37) F(180) F(160) F(170) AND 
CONT C(33) C(37) F(161) F(171) F(181) AND 
CONT C(33) C(37) F(171) F(181) F(161) AND 
CONT C(33) C(37) F(181) F(161) F(171) 
SAME C(35) C(38) F(191) F(200) F(210) AND 
CONT C(35) C(38) F(200) F(210) F(191) AND 
CONT C(35) C(38) F(210) F(191) F(200) AND 
CONT C(35) C(38) F(190) F(201) F(211) AND 
CONT C(35) C(38) F(201) F(211) F(190) AND 
CONT C(35) C(38) F(211) F(190) F(201) 
DELU 0.01 C(35) C(38) F(191) F(200) F(210) AND 
CONT C(35) C(38) F(200) F(210) F(191) AND 
CONT C(35) C(38) F(210) F(191) F(200) AND 
CONT C(35) C(38) F(190) F(201) F(211) AND 
CONT C(35) C(38) F(201) F(211) F(190) AND 
CONT C(35) C(38) F(211) F(190) F(201) 
SIMU 0.01 C(35) C(38) F(191) F(200) F(210) AND 
CONT C(35) C(38) F(200) F(210) F(191) AND 
CONT C(35) C(38) F(210) F(191) F(200) AND 
CONT C(35) C(38) F(190) F(201) F(211) AND 
CONT C(35) C(38) F(201) F(211) F(190) AND 
CONT C(35) C(38) F(211) F(190) F(201) 
SAME C(43) C(46) F(101) F(110) F(120) AND 
CONT C(43) C(46) F(110) F(120) F(101) AND 
CONT C(43) C(46) F(120) F(101) F(110) AND 
CONT C(43) C(46) F(100) F(111) F(121) AND 
CONT C(43) C(46) F(111) F(121) F(100) AND 
CONT C(43) C(46) F(121) F(100) F(111) 
DELU 0.015 C(43) C(46) F(101) F(110) F(120) AND 
CONT C(43) C(46) F(110) F(120) F(101) AND 
CONT C(43) C(46) F(120) F(101) F(110) AND 
CONT C(43) C(46) F(100) F(111) F(121) AND 
CONT C(43) C(46) F(111) F(121) F(100) AND 
CONT C(43) C(46) F(121) F(100) F(111) 
SIMU 0.015 C(43) C(46) F(101) F(110) F(120) AND 
CONT C(43) C(46) F(110) F(120) F(101) AND 
CONT C(43) C(46) F(120) F(101) F(110) AND 
CONT C(43) C(46) F(100) F(111) F(121) AND 
CONT C(43) C(46) F(111) F(121) F(100) AND 
CONT C(43) C(46) F(121) F(100) F(111) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
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