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_4337893
_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, University of Oxford'
_chemical_formula_moiety         'C106.69 H68.46 B3 F53.23 P4 Rh1'
_chemical_formula_sum            'C106.69 H68.46 B3 F53.23 P4 Rh'
_chemical_formula_weight         2620.90
_chemical_melting_point          ?
_chemical_name_systematic        '[RhH(dpp3)(P(ArF)2BH3)(PH(ArF)2BH3)][BArF4]'
_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     other
_audit_creation_date             13-04-23
_audit_creation_method           CRYSTALS_ver_14.40
_cell_angle_alpha                79.5983(5)
_cell_angle_beta                 74.0583(6)
_cell_angle_gamma                64.6987(6)
_cell_formula_units_Z            2
_cell_length_a                   16.4783(2)
_cell_length_b                   18.4893(2)
_cell_length_c                   21.2720(3)
_cell_measurement_reflns_used    19295
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     5619.05(12)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_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 0.975
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.027
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            59262
_diffrn_reflns_theta_full        25.268
_diffrn_reflns_theta_max         27.465
_diffrn_reflns_theta_min         5.102
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.344
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.93
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.549
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2615.280
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.080
_refine_diff_density_max         1.33
_refine_diff_density_min         -1.14
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.8277
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1756
_refine_ls_number_reflns         24841
_refine_ls_number_restraints     2492
_refine_ls_R_factor_all          0.0859
_refine_ls_R_factor_gt           0.0629
_refine_ls_shift/su_max          0.0019604
_refine_ls_shift/su_mean         0.0000269
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.11P)^2^ +19.18P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1857
_refine_ls_wR_factor_gt          0.1623
_refine_ls_wR_factor_ref         0.1855
_reflns_limit_h_max              21
_reflns_limit_h_min              -20
_reflns_limit_k_max              23
_reflns_limit_k_min              -23
_reflns_limit_l_max              27
_reflns_limit_l_min              0
_reflns_number_gt                18981
_reflns_number_total             24847
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.32
_oxford_diffrn_Wilson_scale      14.17
_oxford_refine_ls_r_factor_ref   0.0859
_oxford_refine_ls_scale          0.3105(3)
_oxford_reflns_number_all        24845
_oxford_reflns_threshold_expression_ref I>0.0\s(I)
_oxford_structure_analysis_title Miguel_PB
_cod_data_source_file            ic500032f_si_002.cif
_cod_data_source_block           Compound14
_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/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 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 4337890--4337893.cif.
;
_cod_original_cell_volume        5619.05(13)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C106.69 H68.46 B3 F53.23 P4 Rh1'
_cod_database_code               4337893
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
RIDE C   ( 402,X'S) H   (4021,X'S) 
RIDE C   ( 403,X'S) H   (4031,X'S) 
RIDE C   ( 404,X'S) H   (4041,X'S) 
RIDE C   ( 405,X'S) H   (4051,X'S) 
RIDE C   (   1,X'S) H   (  12,X'S) H   (  11,X'S) 
RIDE C   (   2,X'S) H   (  22,X'S) H   (  21,X'S) 
RIDE C   (   3,X'S) H   (  31,X'S) H   (  32,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   (   9,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   (  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 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   ( 202,X'S) H   (2021,X'S) 
RIDE C   ( 203,X'S) H   (2031,X'S) 
RIDE C   ( 204,X'S) H   (2041,X'S) 
RIDE C   ( 205,X'S) H   (2051,X'S) 
RIDE C   ( 302,X'S) H   (3021,X'S) 
RIDE C   ( 303,X'S) H   (3031,X'S) 
RIDE C   ( 304,X'S) H   (3041,X'S) 
RIDE C   ( 305,X'S) H   (3051,X'S) 
RIDE P   (   4,X'S) H   (  41,X'S) 
RIDE B   (   1,X'S) H   (   1,X'S) H   (   3,X'S) H   (   2,X'S) 
RIDE B   (   2,X'S) H   (   4,X'S) H   (   6,X'S) H   (   5,X'S) 
RIDE RH  (   1,X'S) H   (   7,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
PLANAR 0.010000  C(406) C(401) C(402) C(403) C(404) C(405) F(62) F(63) 
SAME C(30) C(34) F(131) F(140) F(150) AND 
CONT C(30) C(34) F(140) F(150) F(131) AND 
CONT C(30) C(34) F(150) F(131) F(140) AND 
CONT C(30) C(34) F(130) F(141) F(151) AND 
CONT C(30) C(34) F(141) F(151) F(130) AND 
CONT C(30) C(34) F(151) F(130) F(141) 
DELU 0.015 C(30) C(34) F(131) F(140) F(150) AND 
CONT C(30) C(34) F(140) F(150) F(131) AND 
CONT C(30) C(34) F(150) F(131) F(140) AND 
CONT C(30) C(34) F(130) F(141) F(151) AND 
CONT C(30) C(34) F(141) F(151) F(130) AND 
CONT C(30) C(34) F(151) F(130) F(141) 
SIMU 0.015 C(30) C(34) F(131) F(140) F(150) AND 
CONT C(30) C(34) F(140) F(150) F(131) AND 
CONT C(30) C(34) F(150) F(131) F(140) AND 
CONT C(30) C(34) F(130) F(141) F(151) AND 
CONT C(30) C(34) F(141) F(151) F(130) AND 
CONT C(30) C(34) F(151) F(130) F(141) 
SAME C(54) C(58) F(280) F(290) F(301) AND 
CONT C(54) C(58) F(290) F(301) F(280) AND 
CONT C(54) C(58) F(301) F(280) F(290) AND 
CONT C(54) C(58) F(281) F(291) F(300) AND 
CONT C(54) C(58) F(291) F(300) F(281) AND 
CONT C(54) C(58) F(300) F(281) F(291) 
DELU 0.015 C(54) C(58) F(280) F(290) F(301) AND 
CONT C(54) C(58) F(290) F(301) F(280) AND 
CONT C(54) C(58) F(301) F(280) F(290) AND 
CONT C(54) C(58) F(281) F(291) F(300) AND 
CONT C(54) C(58) F(291) F(300) F(281) AND 
CONT C(54) C(58) F(300) F(281) F(291) 
SIMU 0.015 C(54) C(58) F(280) F(290) F(301) AND 
CONT C(54) C(58) F(290) F(301) F(280) AND 
CONT C(54) C(58) F(301) F(280) F(290) AND 
CONT C(54) C(58) F(281) F(291) F(300) AND 
CONT C(54) C(58) F(291) F(300) F(281) AND 
CONT C(54) C(58) F(300) F(281) F(291) 
SAME C(56) C(59) F(311) F(321) F(331) AND 
CONT C(56) C(59) F(321) F(331) F(311) AND 
CONT C(56) C(59) F(331) F(311) F(321) AND 
CONT C(56) C(59) F(310) F(320) F(330) AND 
CONT C(56) C(59) F(320) F(330) F(310) AND 
CONT C(56) C(59) F(330) F(310) F(320) 
DELU 0.015 C(56) C(59) F(311) F(321) F(331) AND 
CONT C(56) C(59) F(321) F(331) F(311) AND 
CONT C(56) C(59) F(331) F(311) F(321) AND 
CONT C(56) C(59) F(310) F(320) F(330) AND 
CONT C(56) C(59) F(320) F(330) F(310) AND 
CONT C(56) C(59) F(330) F(310) F(320) 
SIMU 0.015 C(56) C(59) F(311) F(321) F(331) AND 
CONT C(56) C(59) F(321) F(331) F(311) AND 
CONT C(56) C(59) F(331) F(311) F(321) AND 
CONT C(56) C(59) F(310) F(320) F(330) AND 
CONT C(56) C(59) F(320) F(330) F(310) AND 
CONT C(56) C(59) F(330) F(310) F(320) 
SAME C(127) C(131) F(520) F(530) F(541) AND 
CONT C(127) C(131) F(530) F(541) F(520) AND 
CONT C(127) C(131) F(541) F(520) F(530) AND 
CONT C(127) C(131) F(521) F(531) F(540) AND 
CONT C(127) C(131) F(531) F(540) F(521) AND 
CONT C(127) C(131) F(540) F(521) F(531) 
DELU 0.015 C(127) C(131) F(520) F(530) F(541) AND 
CONT C(127) C(131) F(530) F(541) F(520) AND 
CONT C(127) C(131) F(541) F(520) F(530) AND 
CONT C(127) C(131) F(521) F(531) F(540) AND 
CONT C(127) C(131) F(531) F(540) F(521) AND 
CONT C(127) C(131) F(540) F(521) F(531) 
SIMU 0.015 C(127) C(131) F(520) F(530) F(541) AND 
CONT C(127) C(131) F(530) F(541) F(520) AND 
CONT C(127) C(131) F(541) F(520) F(530) AND 
CONT C(127) C(131) F(521) F(531) F(540) AND 
CONT C(127) C(131) F(531) F(540) F(521) AND 
CONT C(127) C(131) F(540) F(521) F(531) 
SAME C(119) C(123) F(460) F(471) F(480) AND 
CONT C(119) C(123) F(471) F(480) F(460) AND 
CONT C(119) C(123) F(480) F(460) F(471) AND 
CONT C(119) C(123) F(461) F(470) F(481) AND 
CONT C(119) C(123) F(470) F(481) F(461) AND 
CONT C(119) C(123) F(481) F(461) F(470) 
DELU 0.015 C(119) C(123) F(460) F(471) F(480) AND 
CONT C(119) C(123) F(471) F(480) F(460) AND 
CONT C(119) C(123) F(480) F(460) F(471) AND 
CONT C(119) C(123) F(461) F(470) F(481) AND 
CONT C(119) C(123) F(470) F(481) F(461) AND 
CONT C(119) C(123) F(481) F(461) F(470) 
SIMU 0.015 C(119) C(123) F(460) F(471) F(480) AND 
CONT C(119) C(123) F(471) F(480) F(460) AND 
CONT C(119) C(123) F(480) F(460) F(471) AND 
CONT C(119) C(123) F(461) F(470) F(481) AND 
CONT C(119) C(123) F(470) F(481) F(461) AND 
CONT C(119) C(123) F(481) F(461) F(470) 
SAME C(121) C(124) F(491) F(500) F(511) AND 
CONT C(121) C(124) F(500) F(511) F(491) AND 
CONT C(121) C(124) F(511) F(491) F(500) AND 
CONT C(121) C(124) F(490) F(501) F(510) AND 
CONT C(121) C(124) F(501) F(510) F(490) AND 
CONT C(121) C(124) F(510) F(490) F(501) 
DELU 0.015 C(121) C(124) F(491) F(500) F(511) AND 
CONT C(121) C(124) F(500) F(511) F(491) AND 
CONT C(121) C(124) F(511) F(491) F(500) AND 
CONT C(121) C(124) F(490) F(501) F(510) AND 
CONT C(121) C(124) F(501) F(510) F(490) AND 
CONT C(121) C(124) F(510) F(490) F(501) 
SIMU 0.015 C(121) C(124) F(491) F(500) F(511) AND 
CONT C(121) C(124) F(500) F(511) F(491) AND 
CONT C(121) C(124) F(511) F(491) F(500) AND 
CONT C(121) C(124) F(490) F(501) F(510) AND 
CONT C(121) C(124) F(501) F(510) F(490) AND 
CONT C(121) C(124) F(510) F(490) F(501) 
SAME C(111) C(115) F(401) F(410) F(420) AND 
CONT C(111) C(115) F(410) F(420) F(401) AND 
CONT C(111) C(115) F(420) F(401) F(410) AND 
CONT C(111) C(115) F(400) F(411) F(421) AND 
CONT C(111) C(115) F(411) F(421) F(400) AND 
CONT C(111) C(115) F(421) F(400) F(411) 
DELU 0.015 C(111) C(115) F(401) F(410) F(420) AND 
CONT C(111) C(115) F(410) F(420) F(401) AND 
CONT C(111) C(115) F(420) F(401) F(410) AND 
CONT C(111) C(115) F(400) F(411) F(421) AND 
CONT C(111) C(115) F(411) F(421) F(400) AND 
CONT C(111) C(115) F(421) F(400) F(411) 
SIMU 0.015 C(111) C(115) F(401) F(410) F(420) AND 
CONT C(111) C(115) F(410) F(420) F(401) AND 
CONT C(111) C(115) F(420) F(401) F(410) AND 
CONT C(111) C(115) F(400) F(411) F(421) AND 
CONT C(111) C(115) F(411) F(421) F(400) AND 
CONT C(111) C(115) F(421) F(400) F(411) 
SAME C(103) C(107) F(340) F(350) F(361) AND 
CONT C(103) C(107) F(350) F(361) F(340) AND 
CONT C(103) C(107) F(361) F(340) F(350) AND 
CONT C(103) C(107) F(341) F(351) F(360) AND 
CONT C(103) C(107) F(351) F(360) F(341) AND 
CONT C(103) C(107) F(360) F(341) F(351) 
DELU 0.015 C(103) C(107) F(340) F(350) F(361) AND 
CONT C(103) C(107) F(350) F(361) F(340) AND 
CONT C(103) C(107) F(361) F(340) F(350) AND 
CONT C(103) C(107) F(341) F(351) F(360) AND 
CONT C(103) C(107) F(351) F(360) F(341) AND 
CONT C(103) C(107) F(360) F(341) F(351) 
SIMU 0.015 C(103) C(107) F(340) F(350) F(361) AND 
CONT C(103) C(107) F(350) F(361) F(340) AND 
CONT C(103) C(107) F(361) F(340) F(350) AND 
CONT C(103) C(107) F(341) F(351) F(360) AND 
CONT C(103) C(107) F(351) F(360) F(341) AND 
CONT C(103) C(107) F(360) F(341) F(351) 
SAME F(58) C(201) C(202) C(203) C(204) C(205) C(206) F(59) AND 
CONT F(59) C(206) C(205) C(204) C(203) C(202) C(201) F(58) AND 
CONT F(60) C(301) C(302) C(303) C(304) C(305) C(306) F(61) AND 
CONT F(61) C(306) C(305) C(304) C(303) C(302) C(301) F(60) AND 
CONT F(62) C(401) C(402) C(403) C(404) C(405) C(406) F(63) AND 
CONT F(63) C(406) C(405) C(404) C(403) C(402) C(401) F(62) 
SIMU 0.015 F(58) C(201) C(202) C(203) C(204) C(205) C(206) F(59) AND 
CONT F(59) C(206) C(205) C(204) C(203) C(202) C(201) F(58) AND 
CONT F(60) C(301) C(302) C(303) C(304) C(305) C(306) F(61) AND 
CONT F(61) C(306) C(305) C(304) C(303) C(302) C(301) F(60) AND 
CONT F(62) C(401) C(402) C(403) C(404) C(405) C(406) F(63) AND 
CONT F(63) C(406) C(405) C(404) C(403) C(402) C(401) F(62) 
DELU 0.015 F(58) C(201) C(202) C(203) C(204) C(205) C(206) F(59) AND 
CONT F(59) C(206) C(205) C(204) C(203) C(202) C(201) F(58) AND 
CONT F(60) C(301) C(302) C(303) C(304) C(305) C(306) F(61) AND 
CONT F(61) C(306) C(305) C(304) C(303) C(302) C(301) F(60) AND 
CONT F(62) C(401) C(402) C(403) C(404) C(405) C(406) F(63) AND 
CONT F(63) C(406) C(405) C(404) C(403) C(402) C(401) F(62) 
SAME C(201) C(202) C(203) C(204) C(205) C(206) AND 
CONT C(202) C(203) C(204) C(205) C(206) C(201) AND 
CONT C(203) C(204) C(205) C(206) C(201) C(202) AND 
CONT C(204) C(205) C(206) C(201) C(202) C(203) AND 
CONT C(205) C(206) C(201) C(202) C(203) C(204) AND 
CONT C(206) C(201) C(202) C(203) C(204) C(205) 
SAME C(301) C(302) C(303) C(304) C(305) C(306) AND 
CONT C(302) C(303) C(304) C(305) C(306) C(301) AND 
CONT C(303) C(304) C(305) C(306) C(301) C(302) AND 
CONT C(304) C(305) C(306) C(301) C(302) C(303) AND 
CONT C(305) C(306) C(301) C(302) C(303) C(304) AND 
CONT C(306) C(301) C(302) C(303) C(304) C(305) 
SAME C(401) C(402) C(403) C(404) C(405) C(406) AND 
CONT C(402) C(403) C(404) C(405) C(406) C(401) AND 
CONT C(403) C(404) C(405) C(406) C(401) C(402) AND 
CONT C(404) C(405) C(406) C(401) C(402) C(403) AND 
CONT C(405) C(406) C(401) C(402) C(403) C(404) AND 
CONT C(406) C(401) C(402) C(403) C(404) C(405) 
END                                                                             
;