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_4085484
_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         'C83.40 H63 B1 F24.40 N1.00 O2 P2 Rh1 S1.00'
_chemical_formula_sum            'C83.4 H63 B F24.4 N O2 P2 Rh S'
_chemical_formula_weight         1782.50
_chemical_melting_point          ?
_chemical_name_systematic        'Compound 11'
_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     other
_audit_creation_date             14-04-29
_audit_creation_method           CRYSTALS_ver_14.40
_cell_angle_alpha                90
_cell_angle_beta                 90.2181(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.0601(2)
_cell_length_b                   24.9467(2)
_cell_length_c                   14.0763(2)
_cell_measurement_reflns_used    22082
_cell_measurement_temperature    150
_cell_measurement_theta_max      76
_cell_measurement_theta_min      4
_cell_volume                     7746.51(14)
_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    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_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  0.062
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8288
_diffrn_reflns_theta_full        75.025
_diffrn_reflns_theta_max         76.556
_diffrn_reflns_theta_min         3.543
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.384
_exptl_absorpt_correction_T_max  0.90
_exptl_absorpt_correction_T_min  0.66
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.528
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3608.000
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.030
_refine_diff_density_max         5.28
_refine_diff_density_min         -1.88
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9918
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     721
_refine_ls_number_reflns         7496
_refine_ls_number_restraints     971
_refine_ls_R_factor_all          0.0698
_refine_ls_R_factor_gt           0.0662
_refine_ls_shift/su_max          0.0348628
_refine_ls_shift/su_mean         0.0007580
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.11P)^2^ +44.48P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1809
_refine_ls_wR_factor_gt          0.1755
_refine_ls_wR_factor_ref         0.1808
_reflns_limit_h_max              27
_reflns_limit_h_min              -27
_reflns_limit_k_max              31
_reflns_limit_k_min              0
_reflns_limit_l_max              17
_reflns_limit_l_min              0
_reflns_number_gt                6936
_reflns_number_total             8288
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.26
_oxford_diffrn_Wilson_scale      0.49
_oxford_refine_ls_r_factor_ref   0.0698
_oxford_refine_ls_scale          1.599(13)
_oxford_reflns_number_all        7497
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title
'E:\Weller\116SDP14\116SDP14.cif_ At 11:27 on'
_cod_data_source_file            om500984y_si_001.cif
_cod_data_source_block           Compound116SDP14
_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.

'_atom_sites_solution_primary' value 'Other' changed to 'other'
according to
/usr/data/users/saulius/crontab/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 3008 2015-01-20 13:52:24Z robertas 

 Adding full bibliography for 4085478--4085487.cif.
;
_cod_original_sg_symbol_H-M      'C 2/m '
_cod_original_formula_sum        'C83.40 H63 B1 F24.40 N1.00 O2 P2 Rh1 S1.00'
_cod_database_code               4085484
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
RIDE C   (  62,X'S) H   ( 621,X'S) 
RIDE C   (  64,X'S) H   ( 641,X'S) 
RIDE C   (  66,X'S) H   ( 661,X'S) 
RIDE C   (  70,X'S) H   ( 701,X'S) 
RIDE C   (  72,X'S) H   ( 721,X'S) 
RIDE C   (  74,X'S) H   ( 741,X'S) 
RIDE C   (  20,X'S) H   ( 201,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) 
RIDE C   (  31,X'S) H   ( 354,X'S) 
RIDE C   (  32,X'S) H   ( 353,X'S) 
RIDE C   (  33,X'S) H   ( 352,X'S) 
RIDE C   (  34,X'S) H   ( 351,X'S) 
RIDE C   (  37,X'S) H   ( 371,X'S) H   ( 372,X'S) 
RIDE C   (  38,X'S) H   ( 381,X'S) H   ( 382,X'S) 
RIDE C   (  39,X'S) H   ( 393,X'S) H   ( 392,X'S) H   ( 391,X'S) 
RIDE C   (  41,X'S) H   ( 454,X'S) 
RIDE C   (  42,X'S) H   ( 453,X'S) 
RIDE C   (  43,X'S) H   ( 452,X'S) 
RIDE C   (  44,X'S) H   ( 451,X'S) 
RIDE C   (  47,X'S) H   ( 471,X'S) H   ( 472,X'S) 
RIDE C   (  48,X'S) H   ( 482,X'S) H   ( 481,X'S) 
RIDE C   (  49,X'S) H   ( 493,X'S) H   ( 492,X'S) H   ( 491,X'S) 
RIDE C   (   2,X'S) H   (  21,X'S) 
RIDE C   (   3,X'S) H   (  31,X'S) 
RIDE C   (   4,X'S) H   (  41,X'S) 
RIDE C   (   8,X'S) H   (  83,X'S) H   (  82,X'S) 
RIDE C   (   9,X'S) H   (  92,X'S) H   (  91,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   (  14,X'S) H   ( 141,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) 
RIDE C   (  18,X'S) H   ( 181,X'S) 
RIDE C   (  19,X'S) H   ( 191,X'S) 
RIDE C   ( 203,X'S) H   (2031,X'S) 
RIDE C   ( 202,X'S) H   (2021,X'S) 
RIDE C   ( 201,X'S) H   (2011,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
DELU 0.015 C(30) C(31) C(32) C(33) C(34) C(35) AND 
CONT C(31) C(32) C(33) C(34) C(35) C(30) AND 
CONT C(32) C(33) C(34) C(35) C(30) C(31) AND 
CONT C(33) C(34) C(35) C(30) C(31) C(32) AND 
CONT C(34) C(35) C(30) C(31) C(32) C(33) AND 
CONT C(35) C(30) C(31) C(32) C(33) C(34) 
SIMU 0.015 C(30) C(31) C(32) C(33) C(34) C(35) AND 
CONT C(31) C(32) C(33) C(34) C(35) C(30) AND 
CONT C(32) C(33) C(34) C(35) C(30) C(31) AND 
CONT C(33) C(34) C(35) C(30) C(31) C(32) AND 
CONT C(34) C(35) C(30) C(31) C(32) C(33) AND 
CONT C(35) C(30) C(31) C(32) C(33) C(34) 
PLANAR 0.010000 C(30) C(31) C(32) C(33) C(34) C(35) 
DELU 0.015 C(40) C(41) C(42) C(43) C(44) C(45) AND 
CONT C(41) C(42) C(43) C(44) C(45) C(40) AND 
CONT C(42) C(43) C(44) C(45) C(40) C(41) AND 
CONT C(43) C(44) C(45) C(40) C(41) C(42) AND 
CONT C(44) C(45) C(40) C(41) C(42) C(43) AND 
CONT C(45) C(40) C(41) C(42) C(43) C(44) 
SIMU 0.015 C(40) C(41) C(42) C(43) C(44) C(45) AND 
CONT C(41) C(42) C(43) C(44) C(45) C(40) AND 
CONT C(42) C(43) C(44) C(45) C(40) C(41) AND 
CONT C(43) C(44) C(45) C(40) C(41) C(42) AND 
CONT C(44) C(45) C(40) C(41) C(42) C(43) AND 
CONT C(45) C(40) C(41) C(42) C(43) C(44) 
PLANAR 0.010000 C(40) C(41) C(42) C(43) C(44) C(45) 
SAME N(2) C(36) C(35) C(30) RH(1) AND 
CONT N(3) C(46) C(45) C(40) RH(1) 
SAME N(2) C(36) O(2) C(37) C(38) AND 
CONT N(3) C(46) O(3) C(47) C(48) 
SIMU 0.015 N(2) C(36) O(2) C(37) C(38) AND 
CONT N(3) C(46) O(3) C(47) C(48) 
SAME RH(1) S(1) C(39) AND 
CONT RH(1) S(2) C(49) 
SAME C(63) C(67) F(101) F(110) F(121) AND 
CONT C(63) C(67) F(110) F(121) F(101) AND 
CONT C(63) C(67) F(121) F(101) F(110) AND 
CONT C(63) C(67) F(100) F(111) F(120) AND 
CONT C(63) C(67) F(111) F(120) F(100) AND 
CONT C(63) C(67) F(120) F(100) F(111) 
DELU 0.015 C(63) C(67) F(101) F(110) F(121) AND 
CONT C(63) C(67) F(110) F(121) F(101) AND 
CONT C(63) C(67) F(121) F(101) F(110) AND 
CONT C(63) C(67) F(100) F(111) F(120) AND 
CONT C(63) C(67) F(111) F(120) F(100) AND 
CONT C(63) C(67) F(120) F(100) F(111) 
SIMU 0.015 C(63) C(67) F(101) F(110) F(121) AND 
CONT C(63) C(67) F(110) F(121) F(101) AND 
CONT C(63) C(67) F(121) F(101) F(110) AND 
CONT C(63) C(67) F(100) F(111) F(120) AND 
CONT C(63) C(67) F(111) F(120) F(100) AND 
CONT C(63) C(67) F(120) F(100) F(111) 
SAME C(73) C(75) F(191) F(200) F(211) AND 
CONT C(73) C(75) F(200) F(211) F(191) AND 
CONT C(73) C(75) F(211) F(191) F(200) AND 
CONT C(73) C(75) F(190) F(201) F(210) AND 
CONT C(73) C(75) F(201) F(210) F(190) AND 
CONT C(73) C(75) F(210) F(190) F(201) 
DELU 0.015 C(73) C(75) F(191) F(200) F(211) AND 
CONT C(73) C(75) F(200) F(211) F(191) AND 
CONT C(73) C(75) F(211) F(191) F(200) AND 
CONT C(73) C(75) F(190) F(201) F(210) AND 
CONT C(73) C(75) F(201) F(210) F(190) AND 
CONT C(73) C(75) F(210) F(190) F(201) 
SIMU 0.015 C(73) C(75) F(191) F(200) F(211) AND 
CONT C(73) C(75) F(200) F(211) F(191) AND 
CONT C(73) C(75) F(211) F(191) F(200) AND 
CONT C(73) C(75) F(190) F(201) F(210) AND 
CONT C(73) C(75) F(201) F(210) F(190) AND 
CONT C(73) C(75) F(210) F(190) F(201) 
SIMU 0.015 F(300) C(201) C(202) C(203) 
DELU 0.015 F(300) C(201) C(202) C(203) 
PLANAR 0.010000 F(300) C(201) C(202) C(203) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;