Effect of the Phosphine Steric and Electronic Profile on the Rh-Promoted Dehydrocoupling of Phosphine-Boranes.
Hooper, Thomas N.; Huertos, Miguel A.; Jurca, Titel; Pike, Sebastian D.; Weller, Andrew S.; Manners, Ian; Inorganic chemistry 53 (2014) 3716–; doi:10.1021/ic500032f

data_4337891
_publ_section_title
;
 Effect of the Phosphine Steric and Electronic Profile on the Rh-Promoted
 Dehydrocoupling of Phosphine-Boranes.
;
_journal_issue                   7
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3716
_journal_paper_doi               10.1021/ic500032f
_journal_volume                  53
_journal_year                    2014
_chemical_compound_source        'CRL, Universtity of Oxford'
_chemical_formula_moiety         'C96 H68 B3 F48 P4 Rh1'
_chemical_formula_sum            'C96 H68 B3 F48 P4 Rh'
_chemical_formula_weight         2392.74
_chemical_melting_point          ?
_chemical_name_systematic        RhH(dpp3)P(CF3)2BH2P(CF3)2BH3
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             13-03-27
_audit_creation_method           CRYSTALS_ver_14.40
_cell_angle_alpha                90
_cell_angle_beta                 109.424(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.0154(5)
_cell_length_b                   17.2614(3)
_cell_length_c                   28.0372(9)
_cell_measurement_reflns_used    14314
_cell_measurement_temperature    150
_cell_measurement_theta_max      77
_cell_measurement_theta_min      3
_cell_volume                     10504.6(5)
_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 0.988
_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       -28
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            21862
_diffrn_reflns_theta_full        74.390
_diffrn_reflns_theta_max         76.690
_diffrn_reflns_theta_min         3.057
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.066
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.80
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4784
_exptl_crystal_size_max          0.020
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.010
_platon_squeeze_details
;
;
_refine_diff_density_max         1.44
_refine_diff_density_min         -1.32
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9470
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1504
_refine_ls_number_reflns         20116
_refine_ls_number_restraints     1216
_refine_ls_R_factor_all          0.0961
_refine_ls_R_factor_gt           0.0650
_refine_ls_shift/su_max          0.0299076
_refine_ls_shift/su_mean         0.0004647
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.08P)^2^ +10.32P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1711
_refine_ls_wR_factor_gt          0.1596
_refine_ls_wR_factor_ref         0.1711
_reflns_limit_h_max              27
_reflns_limit_h_min              -28
_reflns_limit_k_max              21
_reflns_limit_k_min              0
_reflns_limit_l_max              35
_reflns_limit_l_min              0
_reflns_number_gt                14058
_reflns_number_total             21862
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.38
_oxford_diffrn_Wilson_scale      1.67
_oxford_refine_ls_r_factor_ref   0.0961
_oxford_refine_ls_scale          0.896(2)
_oxford_reflns_number_all        20116
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 062SDP13
_cod_data_source_file            ic500032f_si_003.cif
_cod_data_source_block           Compound17
_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.

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

 Adding full bibliography for 4337890--4337893.cif.
;
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_original_formula_sum        'C96 H68 B3 F48 P4 Rh1'
_cod_database_code               4337891
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
RIDE C   ( 102,X'S) H   (1021,X'S) 
RIDE C   ( 104,X'S) H   (1041,X'S) 
RIDE C   ( 106,X'S) H   (1061,X'S) 
RIDE C   ( 110,X'S) H   (1101,X'S) 
RIDE C   ( 112,X'S) H   (1121,X'S) 
RIDE C   ( 114,X'S) H   (1141,X'S) 
RIDE C   ( 118,X'S) H   (1181,X'S) 
RIDE C   ( 120,X'S) H   (1201,X'S) 
RIDE C   ( 122,X'S) H   (1221,X'S) 
RIDE C   ( 126,X'S) H   (1261,X'S) 
RIDE C   ( 128,X'S) H   (1281,X'S) 
RIDE C   ( 130,X'S) H   (1301,X'S) 
RIDE C   ( 301,X'S) H   (3011,X'S) H   (3012,X'S) H   (3013,X'S) 
RIDE C   ( 302,X'S) H   (3022,X'S) H   (3021,X'S) 
RIDE C   ( 303,X'S) H   (3032,X'S) H   (3031,X'S) 
RIDE C   ( 304,X'S) H   (3041,X'S) H   (3042,X'S) 
RIDE C   ( 305,X'S) H   (3051,X'S) H   (3052,X'S) H   (3053,X'S) 
RIDE C   (   1,X'S) H   (  11,X'S) H   (  12,X'S) 
RIDE C   (   2,X'S) H   (  21,X'S) H   (  22,X'S) 
RIDE C   (   3,X'S) H   (  31,X'S) H   (  32,X'S) 
RIDE C   (   4,X'S) H   (  41,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) 
RIDE C   (   7,X'S) H   (  71,X'S) 
RIDE C   (   8,X'S) H   (  81,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   (  20,X'S) H   ( 201,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) 
RIDE C   (  27,X'S) H   ( 271,X'S) 
RIDE C   (  29,X'S) H   ( 291,X'S) 
RIDE C   (  31,X'S) H   ( 311,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) 
RIDE C   (  37,X'S) H   ( 371,X'S) 
RIDE C   (  39,X'S) H   ( 391,X'S) 
RIDE C   (  41,X'S) H   ( 411,X'S) 
RIDE C   (  45,X'S) H   ( 451,X'S) 
RIDE C   (  47,X'S) H   ( 471,X'S) 
RIDE C   (  49,X'S) H   ( 491,X'S) 
RIDE C   (  53,X'S) H   ( 531,X'S) 
RIDE C   (  55,X'S) H   ( 551,X'S) 
RIDE C   (  57,X'S) H   ( 571,X'S) 
RIDE B   (   1,X'S) H   (   2,X'S) H   (   3,X'S) 
RIDE B   (   2,X'S) H   (   4,X'S) H   (   5,X'S) H   (   6,X'S) 
RIDE RH  (   1,X'S) H   (   1,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
SAME C(301) C(302) C(303) C(304) C(305) AND 
CONT C(305) C(304) C(303) C(302) C(301) 
SAME C(302) C(303) C(304) AND 
CONT C(304) C(303) C(302) 
SIMU 0.015 C(301) C(302) C(303) C(304) C(305) AND 
CONT C(305) C(304) C(303) C(302) C(301) 
DELU 0.015 C(301) C(302) C(303) C(304) C(305) AND 
CONT C(305) C(304) C(303) C(302) C(301) 
SAME C(105) C(108) F(1040) F(1051) F(1061) AND 
CONT C(105) C(108) F(1051) F(1061) F(1040) AND 
CONT C(105) C(108) F(1061) F(1040) F(1051) AND 
CONT C(105) C(108) F(1041) F(1050) F(1060) AND 
CONT C(105) C(108) F(1050) F(1060) F(1041) AND 
CONT C(105) C(108) F(1060) F(1041) F(1050) 
DELU 0.015 C(105) C(108) F(1040) F(1051) F(1061) AND 
CONT C(105) C(108) F(1051) F(1061) F(1040) AND 
CONT C(105) C(108) F(1061) F(1040) F(1051) AND 
CONT C(105) C(108) F(1041) F(1050) F(1060) AND 
CONT C(105) C(108) F(1050) F(1060) F(1041) AND 
CONT C(105) C(108) F(1060) F(1041) F(1050) 
SIMU 0.015 C(105) C(108) F(1040) F(1051) F(1061) AND 
CONT C(105) C(108) F(1051) F(1061) F(1040) AND 
CONT C(105) C(108) F(1061) F(1040) F(1051) AND 
CONT C(105) C(108) F(1041) F(1050) F(1060) AND 
CONT C(105) C(108) F(1050) F(1060) F(1041) AND 
CONT C(105) C(108) F(1060) F(1041) F(1050) 
SAME C(111) C(115) F(1070) F(1081) F(1090) AND 
CONT C(111) C(115) F(1081) F(1090) F(1070) AND 
CONT C(111) C(115) F(1090) F(1070) F(1081) AND 
CONT C(111) C(115) F(1071) F(1080) F(1091) AND 
CONT C(111) C(115) F(1080) F(1091) F(1071) AND 
CONT C(111) C(115) F(1091) F(1071) F(1080) 
DELU 0.015 C(111) C(115) F(1070) F(1081) F(1090) AND 
CONT C(111) C(115) F(1081) F(1090) F(1070) AND 
CONT C(111) C(115) F(1090) F(1070) F(1081) AND 
CONT C(111) C(115) F(1071) F(1080) F(1091) AND 
CONT C(111) C(115) F(1080) F(1091) F(1071) AND 
CONT C(111) C(115) F(1091) F(1071) F(1080) 
SIMU 0.015 C(111) C(115) F(1070) F(1081) F(1090) AND 
CONT C(111) C(115) F(1081) F(1090) F(1070) AND 
CONT C(111) C(115) F(1090) F(1070) F(1081) AND 
CONT C(111) C(115) F(1071) F(1080) F(1091) AND 
CONT C(111) C(115) F(1080) F(1091) F(1071) AND 
CONT C(111) C(115) F(1091) F(1071) F(1080) 
SAME C(113) C(116) F(1101) F(1110) F(1121) AND 
CONT C(113) C(116) F(1110) F(1121) F(1101) AND 
CONT C(113) C(116) F(1121) F(1101) F(1110) AND 
CONT C(113) C(116) F(1100) F(1111) F(1120) AND 
CONT C(113) C(116) F(1111) F(1120) F(1100) AND 
CONT C(113) C(116) F(1120) F(1100) F(1111) 
DELU 0.015 C(113) C(116) F(1101) F(1110) F(1121) AND 
CONT C(113) C(116) F(1110) F(1121) F(1101) AND 
CONT C(113) C(116) F(1121) F(1101) F(1110) AND 
CONT C(113) C(116) F(1100) F(1111) F(1120) AND 
CONT C(113) C(116) F(1111) F(1120) F(1100) AND 
CONT C(113) C(116) F(1120) F(1100) F(1111) 
SIMU 0.015 C(113) C(116) F(1101) F(1110) F(1121) AND 
CONT C(113) C(116) F(1110) F(1121) F(1101) AND 
CONT C(113) C(116) F(1121) F(1101) F(1110) AND 
CONT C(113) C(116) F(1100) F(1111) F(1120) AND 
CONT C(113) C(116) F(1111) F(1120) F(1100) AND 
CONT C(113) C(116) F(1120) F(1100) F(1111) 
SAME C(127) C(131) F(1191) F(1201) F(1210) AND 
CONT C(127) C(131) F(1201) F(1210) F(1191) AND 
CONT C(127) C(131) F(1210) F(1191) F(1201) AND 
CONT C(127) C(131) F(1190) F(1200) F(1211) AND 
CONT C(127) C(131) F(1200) F(1211) F(1190) AND 
CONT C(127) C(131) F(1211) F(1190) F(1200) 
DELU 0.015 C(127) C(131) F(1191) F(1201) F(1210) AND 
CONT C(127) C(131) F(1201) F(1210) F(1191) AND 
CONT C(127) C(131) F(1210) F(1191) F(1201) AND 
CONT C(127) C(131) F(1190) F(1200) F(1211) AND 
CONT C(127) C(131) F(1200) F(1211) F(1190) AND 
CONT C(127) C(131) F(1211) F(1190) F(1200) 
SIMU 0.015 C(127) C(131) F(1191) F(1201) F(1210) AND 
CONT C(127) C(131) F(1201) F(1210) F(1191) AND 
CONT C(127) C(131) F(1210) F(1191) F(1201) AND 
CONT C(127) C(131) F(1190) F(1200) F(1211) AND 
CONT C(127) C(131) F(1200) F(1211) F(1190) AND 
CONT C(127) C(131) F(1211) F(1190) F(1200) 
SAME C(38) C(42) F(500) F(510) F(521) AND 
CONT C(38) C(42) F(510) F(521) F(500) AND 
CONT C(38) C(42) F(521) F(500) F(510) AND 
CONT C(38) C(42) F(501) F(511) F(520) AND 
CONT C(38) C(42) F(511) F(520) F(501) AND 
CONT C(38) C(42) F(520) F(501) F(511) 
DELU 0.015 C(38) C(42) F(500) F(510) F(521) AND 
CONT C(38) C(42) F(510) F(521) F(500) AND 
CONT C(38) C(42) F(521) F(500) F(510) AND 
CONT C(38) C(42) F(501) F(511) F(520) AND 
CONT C(38) C(42) F(511) F(520) F(501) AND 
CONT C(38) C(42) F(520) F(501) F(511) 
SIMU 0.015 C(38) C(42) F(500) F(510) F(521) AND 
CONT C(38) C(42) F(510) F(521) F(500) AND 
CONT C(38) C(42) F(521) F(500) F(510) AND 
CONT C(38) C(42) F(501) F(511) F(520) AND 
CONT C(38) C(42) F(511) F(520) F(501) AND 
CONT C(38) C(42) F(520) F(501) F(511) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
DISTANCE 0.970000 , 0.005000 = C(305) TO H(3053) 
DISTANCE 0.970000 , 0.005000 = C(305) TO H(3051) 
DISTANCE 0.970000 , 0.005000 = C(305) TO H(3052) 
END                                                                             
;