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_4085487
_publ_section_title
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 Rh--POP Pincer Xantphos Complexes for C--S and C--H Activation.
 Implications for Carbothiolation Catalysis
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_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, Uni Oxford'
_chemical_formula_moiety         'C86 H59 B1 Cl1 F24 O2 P2 Rh1 S1'
_chemical_formula_sum            'C86 H59 B Cl F24 O2 P2 Rh S'
_chemical_formula_weight         1823.55
_chemical_melting_point          ?
_chemical_name_systematic        'Compound 14?'
_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   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2014-06-25
_audit_creation_method           CRYSTALS_ver_14.43
_cell_angle_alpha                105.052(2)
_cell_angle_beta                 109.735(2)
_cell_angle_gamma                109.714(3)
_cell_formula_units_Z            2
_cell_length_a                   16.0282(4)
_cell_length_b                   17.0414(5)
_cell_length_c                   17.8413(5)
_cell_measurement_reflns_used    17113
_cell_measurement_temperature    150
_cell_measurement_theta_max      75
_cell_measurement_theta_min      3
_cell_volume                     3915.6(3)
_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 0.964
_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  0.048
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            28185
_diffrn_reflns_theta_full        67.752
_diffrn_reflns_theta_max         75.280
_diffrn_reflns_theta_min         3.038
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.659
_exptl_absorpt_correction_T_max  0.86
_exptl_absorpt_correction_T_min  0.75
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.547
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1840
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.040
_refine_diff_density_max         1.44
_refine_diff_density_min         -0.85
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1091
_refine_ls_number_reflns         15534
_refine_ls_number_restraints     228
_refine_ls_R_factor_all          0.0446
_refine_ls_R_factor_gt           0.0413
_refine_ls_shift/su_max          0.0145718
_refine_ls_shift/su_mean         0.0001354
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.06P)^2^ + 3.14P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1097
_refine_ls_wR_factor_gt          0.1061
_refine_ls_wR_factor_ref         0.1097
_reflns_limit_h_max              18
_reflns_limit_h_min              -19
_reflns_limit_k_max              20
_reflns_limit_k_min              -21
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                14152
_reflns_number_total             15600
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.75
_oxford_diffrn_Wilson_scale      0.29
_oxford_refine_ls_r_factor_ref   0.0445
_oxford_refine_ls_scale          1.887(7)
_oxford_reflns_number_all        15535
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 132SDP14
_cod_data_source_file            om500984y_si_001.cif
_cod_data_source_block           132SDP14
_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      'P -1 '
_cod_original_formula_sum        'C86 H59 B1 Cl1 F24 O2 P2 Rh1 S1'
_cod_database_code               4085487
_iucr_refine_instructions_details_constraints
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BLOCK SCALE X'S, U'S 
EQUIV PART(1001,OCC) PART(1002,OCC) 
WEIGHT -1 PART(1002,OCC) 
RIDE C   (   2,X'S) H   (  21,X'S) 
RIDE C   (   4,X'S) H   (  41,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) 
RIDE C   (   8,X'S) H   (  81,X'S) H   (  82,X'S) H   (  83,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) H   (  92,X'S) H   (  93,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) H   ( 172,X'S) H   ( 173,X'S) 
RIDE C   (  18,X'S) H   ( 181,X'S) H   ( 182,X'S) H   ( 183,X'S) 
RIDE C   (  20,X'S) H   ( 201,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) 
RIDE C   (  27,X'S) H   ( 271,X'S) 
RIDE C   (  28,X'S) H   ( 281,X'S) 
RIDE C   (  29,X'S) H   ( 291,X'S) 
RIDE C   (  30,X'S) H   ( 301,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) 
RIDE C   (  38,X'S) H   ( 381,X'S) 
RIDE C   (  39,X'S) H   ( 391,X'S) 
RIDE C   (  40,X'S) H   ( 401,X'S) 
RIDE C   (  41,X'S) H   ( 411,X'S) 
RIDE C   (  42,X'S) H   ( 421,X'S) 
RIDE C   (  44,X'S) H   ( 441,X'S) 
RIDE C   (  45,X'S) H   ( 451,X'S) 
RIDE C   (  46,X'S) H   ( 461,X'S) 
RIDE C   (  47,X'S) H   ( 471,X'S) 
RIDE C   (  48,X'S) H   ( 481,X'S) 
RIDE C   (  52,X'S) H   ( 521,X'S) 
RIDE C   (  54,X'S) H   ( 541,X'S) 
RIDE C   (  56,X'S) H   ( 561,X'S) 
RIDE C   (  60,X'S) H   ( 601,X'S) 
RIDE C   (  62,X'S) H   ( 621,X'S) 
RIDE C   (  64,X'S) H   ( 641,X'S) 
RIDE C   (  68,X'S) H   ( 681,X'S) 
RIDE C   (  70,X'S) H   ( 701,X'S) 
RIDE C   (  72,X'S) H   ( 721,X'S) 
RIDE C   (  76,X'S) H   ( 761,X'S) 
RIDE C   (  78,X'S) H   ( 781,X'S) 
RIDE C   (  80,X'S) H   ( 801,X'S) 
RIDE C   ( 101,X'S) H   (1011,X'S) 
RIDE C   ( 102,X'S) H   (1021,X'S) 
RIDE C   ( 104,X'S) H   (1041,X'S) 
RIDE C   ( 105,X'S) H   (1051,X'S) 
RIDE C   ( 106,X'S) H   (1061,X'S) 
END                                                                             
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_iucr_refine_instructions_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
SAME C(79) C(82) F(311) F(321) F(330) AND 
CONT C(79) C(82) F(321) F(330) F(311) AND 
CONT C(79) C(82) F(330) F(311) F(321) AND 
CONT C(79) C(82) F(310) F(320) F(331) AND 
CONT C(79) C(82) F(320) F(331) F(310) AND 
CONT C(79) C(82) F(331) F(310) F(320) 
DELU 0.015 C(79) C(82) F(311) F(321) F(330) AND 
CONT C(79) C(82) F(321) F(330) F(311) AND 
CONT C(79) C(82) F(330) F(311) F(321) AND 
CONT C(79) C(82) F(310) F(320) F(331) AND 
CONT C(79) C(82) F(320) F(331) F(310) AND 
CONT C(79) C(82) F(331) F(310) F(320) 
SIMU 0.015 C(79) C(82) F(311) F(321) F(330) AND 
CONT C(79) C(82) F(321) F(330) F(311) AND 
CONT C(79) C(82) F(330) F(311) F(321) AND 
CONT C(79) C(82) F(310) F(320) F(331) AND 
CONT C(79) C(82) F(320) F(331) F(310) AND 
CONT C(79) C(82) F(331) F(310) F(320) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
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