Aminoborane σ Complexes: Significance of Hydride Co-ligands in Dynamic Processes and Dehydrogenative Borylene Formation
Addy, David A.; Bates, Joshua I.; Kelly, Michael J.; Riddlestone, Ian M.; Aldridge, Simon; Organometallics 32 (2013) 1583–; doi:10.1021/om400040q

data_4080502
_publ_section_title
;
 Aminoborane \s Complexes: Significance of Hydride Co-ligands in Dynamic
 Processes and Dehydrogenative Borylene Formation
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1583
_journal_paper_doi               10.1021/om400040q
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C32 H12 B F24, C34 H46 B N P Ru'
_chemical_formula_sum            'C66 H58 B2 F24 N P Ru'
_chemical_formula_weight         1474.81
_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
_cell_angle_alpha                91.1751(9)
_cell_angle_beta                 90.1685(10)
_cell_angle_gamma                90.5343(8)
_cell_formula_units_Z            2
_cell_length_a                   12.8893(2)
_cell_length_b                   13.6791(3)
_cell_length_c                   18.9851(4)
_cell_measurement_reflns_used    13085
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     3346.47(11)
_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    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.987
_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  0.040
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            46883
_diffrn_reflns_theta_full        25.007
_diffrn_reflns_theta_max         27.480
_diffrn_reflns_theta_min         5.111
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.365
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.91
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.464
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1492
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.060
_refine_diff_density_max         1.61
_refine_diff_density_min         -1.65
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9332
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1027
_refine_ls_number_reflns         15158
_refine_ls_number_restraints     972
_refine_ls_R_factor_all          0.1126
_refine_ls_R_factor_gt           0.0702
_refine_ls_shift/su_max          0.0091801
_refine_ls_shift/su_mean         0.0001413
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 10.4 11.8 3.33 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1767
_refine_ls_wR_factor_gt          0.1313
_refine_ls_wR_factor_ref         0.1767
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              17
_reflns_limit_k_min              -17
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                10252
_reflns_number_total             15158
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.06
_oxford_diffrn_Wilson_scale      28.90
_oxford_refine_ls_r_factor_ref   0.1126
_oxford_refine_ls_scale          0.21994(13)
_oxford_reflns_number_all        15158
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_cod_data_source_file            om400040q_si_002.cif
_cod_data_source_block           3b
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C66 H58 B2 F24 N1 P1 Ru1'
_cod_database_code               4080502
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S H(11, X'S), H(17, X'S), H(311, 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   (  10,X'S) H   ( 101,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   (  16,X'S) H   ( 161,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   (  26,X'S) H   ( 261,X'S) 
RIDE C   (  27,X'S) H   ( 271,X'S) H   ( 272,X'S) H   ( 273,X'S) 
RIDE C   (  28,X'S) H   ( 281,X'S) 
RIDE C   (  29,X'S) H   ( 291,X'S) H   ( 292,X'S) H   ( 293,X'S) 
RIDE C   (  30,X'S) H   ( 301,X'S) H   ( 302,X'S) H   ( 303,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) H   ( 342,X'S) H   ( 343,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) H   ( 352,X'S) H   ( 353,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) 
RIDE C   (  37,X'S) H   ( 371,X'S) H   ( 372,X'S) H   ( 373,X'S) 
RIDE C   (  38,X'S) H   ( 381,X'S) H   ( 382,X'S) H   ( 383,X'S) 
RIDE C   (  44,X'S) H   ( 441,X'S) 
RIDE C   (  46,X'S) H   ( 461,X'S) 
RIDE C   (  48,X'S) H   ( 481,X'S) 
RIDE C   (  55,X'S) H   ( 551,X'S) 
RIDE C   (  57,X'S) H   ( 571,X'S) 
RIDE C   (  59,X'S) H   ( 591,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   (  84,X'S) H   ( 841,X'S) 
RIDE C   (  86,X'S) H   ( 861,X'S) 
RIDE C   (  88,X'S) H   ( 881,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
SAME C(79) F(300) F(301) F(302) AND 
CONT C(79) F(301) F(302) F(300) AND 
CONT C(79) F(302) F(300) F(301) AND 
CONT C(79) F(303) F(304) F(305) AND 
CONT C(79) F(304) F(305) F(303) AND 
CONT C(79) F(305) F(303) F(304) 
SIMU 0.01 C(79) F(300) F(301) F(302) AND 
CONT C(79) F(301) F(302) F(300) AND 
CONT C(79) F(302) F(300) F(301) AND 
CONT C(79) F(303) F(304) F(305) AND 
CONT C(79) F(304) F(305) F(303) AND 
CONT C(79) F(305) F(303) F(304) 
DELU 0.01 C(79) F(300) F(301) F(302) AND 
CONT C(79) F(301) F(302) F(300) AND 
CONT C(79) F(302) F(300) F(301) AND 
CONT C(79) F(303) F(304) F(305) AND 
CONT C(79) F(304) F(305) F(303) AND 
CONT C(79) F(305) F(303) F(304) 
SAME C(75) F(320) F(321) F(322) AND 
CONT C(75) F(321) F(322) F(320) AND 
CONT C(75) F(322) F(320) F(321) AND 
CONT C(75) F(323) F(324) F(325) AND 
CONT C(75) F(324) F(325) F(323) AND 
CONT C(75) F(325) F(323) F(324) 
SIMU 0.01 C(75) F(320) F(321) F(322) AND 
CONT C(75) F(321) F(322) F(320) AND 
CONT C(75) F(322) F(320) F(321) AND 
CONT C(75) F(323) F(324) F(325) AND 
CONT C(75) F(324) F(325) F(323) AND 
CONT C(75) F(325) F(323) F(324) 
DELU 0.01 C(75) F(320) F(321) F(322) AND 
CONT C(75) F(321) F(322) F(320) AND 
CONT C(75) F(322) F(320) F(321) AND 
CONT C(75) F(323) F(324) F(325) AND 
CONT C(75) F(324) F(325) F(323) AND 
CONT C(75) F(325) F(323) F(324) 
SAME C(65) F(330) F(331) F(332) AND 
CONT C(65) F(331) F(332) F(330) AND 
CONT C(65) F(332) F(330) F(331) AND 
CONT C(65) F(333) F(334) F(335) AND 
CONT C(65) F(334) F(335) F(333) AND 
CONT C(65) F(335) F(333) F(334) 
SIMU 0.01 C(65) F(330) F(331) F(332) AND 
CONT C(65) F(331) F(332) F(330) AND 
CONT C(65) F(332) F(330) F(331) AND 
CONT C(65) F(333) F(334) F(335) AND 
CONT C(65) F(334) F(335) F(333) AND 
CONT C(65) F(335) F(333) F(334) 
DELU 0.01 C(65) F(330) F(331) F(332) AND 
CONT C(65) F(331) F(332) F(330) AND 
CONT C(65) F(332) F(330) F(331) AND 
CONT C(65) F(333) F(334) F(335) AND 
CONT C(65) F(334) F(335) F(333) AND 
CONT C(65) F(335) F(333) F(334) 
SAME C(89) F(340) F(341) F(342) AND 
CONT C(89) F(341) F(342) F(340) AND 
CONT C(89) F(342) F(340) F(341) AND 
CONT C(89) F(343) F(344) F(345) AND 
CONT C(89) F(344) F(345) F(343) AND 
CONT C(89) F(345) F(343) F(344) 
SIMU 0.01 C(89) F(340) F(341) F(342) AND 
CONT C(89) F(341) F(342) F(340) AND 
CONT C(89) F(342) F(340) F(341) AND 
CONT C(89) F(343) F(344) F(345) AND 
CONT C(89) F(344) F(345) F(343) AND 
CONT C(89) F(345) F(343) F(344) 
DELU 0.01 C(89) F(340) F(341) F(342) AND 
CONT C(89) F(341) F(342) F(340) AND 
CONT C(89) F(342) F(340) F(341) AND 
CONT C(89) F(343) F(344) F(345) AND 
CONT C(89) F(344) F(345) F(343) AND 
CONT C(89) F(345) F(343) F(344) 
SAME C(60) F(350) F(351) F(352) AND 
CONT C(60) F(351) F(352) F(350) AND 
CONT C(60) F(352) F(350) F(351) AND 
CONT C(60) F(353) F(354) F(355) AND 
CONT C(60) F(354) F(355) F(353) AND 
CONT C(60) F(355) F(353) F(354) 
SIMU 0.01 C(60) F(350) F(351) F(352) AND 
CONT C(60) F(351) F(352) F(350) AND 
CONT C(60) F(352) F(350) F(351) AND 
CONT C(60) F(353) F(354) F(355) AND 
CONT C(60) F(354) F(355) F(353) AND 
CONT C(60) F(355) F(353) F(354) 
DELU 0.01 C(60) F(350) F(351) F(352) AND 
CONT C(60) F(351) F(352) F(350) AND 
CONT C(60) F(352) F(350) F(351) AND 
CONT C(60) F(353) F(354) F(355) AND 
CONT C(60) F(354) F(355) F(353) AND 
CONT C(60) F(355) F(353) F(354) 
SAME C(49) F(360) F(361) F(362) AND 
CONT C(49) F(361) F(362) F(360) AND 
CONT C(49) F(362) F(360) F(361) AND 
CONT C(49) F(363) F(364) F(365) AND 
CONT C(49) F(364) F(365) F(363) AND 
CONT C(49) F(365) F(363) F(364) 
SIMU 0.01 C(49) F(360) F(361) F(362) AND 
CONT C(49) F(361) F(362) F(360) AND 
CONT C(49) F(362) F(360) F(361) AND 
CONT C(49) F(363) F(364) F(365) AND 
CONT C(49) F(364) F(365) F(363) AND 
CONT C(49) F(365) F(363) F(364) 
DELU 0.01 C(49) F(360) F(361) F(362) AND 
CONT C(49) F(361) F(362) F(360) AND 
CONT C(49) F(362) F(360) F(361) AND 
CONT C(49) F(363) F(364) F(365) AND 
CONT C(49) F(364) F(365) F(363) AND 
CONT C(49) F(365) F(363) F(364) 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;