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_4085481
_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_compound_source        'S10, CRL,University of Oxford'
_chemical_formula_moiety         'C32 H12 B1 F24, C54 H44 Cl2 O1 P2 Rh1'
_chemical_formula_sum            'C86 H56 B Cl2 F24 O P2 Rh'
_chemical_formula_weight         1807.91
_chemical_melting_point          ?
_chemical_name_systematic        'Compound 7'
_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             14-04-29
_audit_creation_method           CRYSTALS_ver_14.40
_cell_angle_alpha                107.4533(17)
_cell_angle_beta                 99.9664(17)
_cell_angle_gamma                97.8760(19)
_cell_formula_units_Z            2
_cell_length_a                   12.7495(3)
_cell_length_b                   18.6412(4)
_cell_length_c                   19.2796(3)
_cell_measurement_reflns_used    18884
_cell_measurement_temperature    150
_cell_measurement_theta_max      75
_cell_measurement_theta_min      4
_cell_volume                     4217.25(16)
_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 0.995
_diffrn_measured_fraction_theta_max 0.966
_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  0.019
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            31819
_diffrn_reflns_theta_full        68.366
_diffrn_reflns_theta_max         75.127
_diffrn_reflns_theta_min         2.893
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.443
_exptl_absorpt_correction_T_max  0.71
_exptl_absorpt_correction_T_min  0.53
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1820
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_refine_diff_density_max         2.70
_refine_diff_density_min         -1.51
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9953
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1194
_refine_ls_number_reflns         16743
_refine_ls_number_restraints     980
_refine_ls_R_factor_all          0.0748
_refine_ls_R_factor_gt           0.0718
_refine_ls_shift/su_max          0.0244884
_refine_ls_shift/su_mean         0.0006627
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.13P)^2^ +10.95P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2072
_refine_ls_wR_factor_gt          0.2038
_refine_ls_wR_factor_ref         0.2072
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              22
_reflns_limit_k_min              -23
_reflns_limit_l_max              23
_reflns_limit_l_min              0
_reflns_number_gt                15550
_reflns_number_total             16811
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.46
_oxford_diffrn_Wilson_scale      0.13
_oxford_refine_ls_r_factor_ref   0.0748
_oxford_refine_ls_scale          2.84(3)
_oxford_reflns_number_all        16743
_oxford_reflns_threshold_expression_ref I>0.0\s(I)
_oxford_structure_analysis_title
'E:\Weller\118SDP14\Solve\118SDP1 At 10:28 on'
_cod_data_source_file            om500984y_si_001.cif
_cod_data_source_block           Compound118SDP14
_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_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C86 H56 B1 Cl2 F24.00 O1 P2 Rh1'
_cod_database_code               4085481
_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
SAME C(63) C(67) F(131) F(140) F(150) AND 
CONT C(63) C(67) F(140) F(150) F(131) AND 
CONT C(63) C(67) F(150) F(131) F(140) AND 
CONT C(63) C(67) F(130) F(141) F(151) AND 
CONT C(63) C(67) F(141) F(151) F(130) AND 
CONT C(63) C(67) F(151) F(130) F(141) 
DELU 0.015 C(63) C(67) F(131) F(140) F(150) AND 
CONT C(63) C(67) F(140) F(150) F(131) AND 
CONT C(63) C(67) F(150) F(131) F(140) AND 
CONT C(63) C(67) F(130) F(141) F(151) AND 
CONT C(63) C(67) F(141) F(151) F(130) AND 
CONT C(63) C(67) F(151) F(130) F(141) 
SIMU 0.015 C(63) C(67) F(131) F(140) F(150) AND 
CONT C(63) C(67) F(140) F(150) F(131) AND 
CONT C(63) C(67) F(150) F(131) F(140) AND 
CONT C(63) C(67) F(130) F(141) F(151) AND 
CONT C(63) C(67) F(141) F(151) F(130) AND 
CONT C(63) C(67) F(151) F(130) F(141) 
SAME C(89) C(92) F(221) F(230) F(240) AND 
CONT C(89) C(92) F(230) F(240) F(221) AND 
CONT C(89) C(92) F(240) F(221) F(230) AND 
CONT C(89) C(92) F(220) F(231) F(241) AND 
CONT C(89) C(92) F(231) F(241) F(220) AND 
CONT C(89) C(92) F(241) F(220) F(231) 
DELU 0.015 C(89) C(92) F(221) F(230) F(240) AND 
CONT C(89) C(92) F(230) F(240) F(221) AND 
CONT C(89) C(92) F(240) F(221) F(230) AND 
CONT C(89) C(92) F(220) F(231) F(241) AND 
CONT C(89) C(92) F(231) F(241) F(220) AND 
CONT C(89) C(92) F(241) F(220) F(231) 
SIMU 0.01 C(89) C(92) F(221) F(230) F(240) AND 
CONT C(89) C(92) F(230) F(240) F(221) AND 
CONT C(89) C(92) F(240) F(221) F(230) AND 
CONT C(89) C(92) F(220) F(231) F(241) AND 
CONT C(89) C(92) F(231) F(241) F(220) AND 
CONT C(89) C(92) F(241) F(220) F(231) 
SAME C(87) C(91) F(251) F(261) F(270) AND 
CONT C(87) C(91) F(261) F(270) F(251) AND 
CONT C(87) C(91) F(270) F(251) F(261) AND 
CONT C(87) C(91) F(250) F(260) F(271) AND 
CONT C(87) C(91) F(260) F(271) F(250) AND 
CONT C(87) C(91) F(271) F(250) F(260) 
DELU 0.015 C(87) C(91) F(251) F(261) F(270) AND 
CONT C(87) C(91) F(261) F(270) F(251) AND 
CONT C(87) C(91) F(270) F(251) F(261) AND 
CONT C(87) C(91) F(250) F(260) F(271) AND 
CONT C(87) C(91) F(260) F(271) F(250) AND 
CONT C(87) C(91) F(271) F(250) F(260) 
SIMU 0.015 C(87) C(91) F(251) F(261) F(270) AND 
CONT C(87) C(91) F(261) F(270) F(251) AND 
CONT C(87) C(91) F(270) F(251) F(261) AND 
CONT C(87) C(91) F(250) F(260) F(271) AND 
CONT C(87) C(91) F(260) F(271) F(250) AND 
CONT C(87) C(91) F(271) F(250) F(260) 
SAME C(81) C(84) F(281) F(291) F(301) AND 
CONT C(81) C(84) F(291) F(301) F(281) AND 
CONT C(81) C(84) F(301) F(281) F(291) AND 
CONT C(81) C(84) F(280) F(290) F(300) AND 
CONT C(81) C(84) F(290) F(300) F(280) AND 
CONT C(81) C(84) F(300) F(280) F(290) 
DELU 0.015 C(81) C(84) F(281) F(291) F(301) AND 
CONT C(81) C(84) F(291) F(301) F(281) AND 
CONT C(81) C(84) F(301) F(281) F(291) AND 
CONT C(81) C(84) F(280) F(290) F(300) AND 
CONT C(81) C(84) F(290) F(300) F(280) AND 
CONT C(81) C(84) F(300) F(280) F(290) 
SIMU 0.015 C(81) C(84) F(281) F(291) F(301) AND 
CONT C(81) C(84) F(291) F(301) F(281) AND 
CONT C(81) C(84) F(301) F(281) F(291) AND 
CONT C(81) C(84) F(280) F(290) F(300) AND 
CONT C(81) C(84) F(290) F(300) F(280) AND 
CONT C(81) C(84) F(300) F(280) F(290) 
SAME CL(200) C(201) CL(202) AND 
CONT CL(202) C(201) CL(200) AND 
CONT CL(300) C(301) CL(302) AND 
CONT CL(302) C(301) CL(300) 
SIMU 0.015 CL(200) C(201) CL(202) AND 
CONT CL(202) C(201) CL(200) AND 
CONT CL(300) C(301) CL(302) AND 
CONT CL(302) C(301) CL(300) 
DELU 0.015 CL(200) C(201) CL(202) AND 
CONT CL(202) C(201) CL(200) AND 
CONT CL(300) C(301) CL(302) AND 
CONT CL(302) C(301) CL(300) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
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