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_4080504
_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         'C31 H12 B F24 N, C34 H62 B N P Ru'
_chemical_formula_sum            'C65 H74 B2 F24 N2 P Ru'
_chemical_formula_weight         1492.93
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 90.5439(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.79890(10)
_cell_length_b                   26.3879(2)
_cell_length_c                   20.09730(10)
_cell_measurement_reflns_used    15762
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     6787.28(8)
_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 0.993
_diffrn_measured_fraction_theta_max 0.992
_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  0.037
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            126616
_diffrn_reflns_theta_full        26.937
_diffrn_reflns_theta_max         27.487
_diffrn_reflns_theta_min         5.101
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.361
_exptl_absorpt_correction_T_max  0.96
_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    1.461
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3052
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.13
_refine_diff_density_min         -0.84
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9450
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     968
_refine_ls_number_reflns         15457
_refine_ls_number_restraints     648
_refine_ls_R_factor_all          0.0838
_refine_ls_R_factor_gt           0.0577
_refine_ls_shift/su_max          0.0085296
_refine_ls_shift/su_mean         0.0001548
_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: 
 11.6 16.7 7.65 1.87 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1556
_refine_ls_wR_factor_gt          0.1283
_refine_ls_wR_factor_ref         0.1556
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              34
_reflns_limit_k_min              0
_reflns_limit_l_max              26
_reflns_limit_l_min              0
_reflns_number_gt                11450
_reflns_number_total             15457
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.01
_oxford_diffrn_Wilson_scale      89.86
_oxford_refine_ls_r_factor_ref   0.0838
_oxford_refine_ls_scale          0.11661(4)
_oxford_reflns_number_all        15457
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_cod_data_source_file            om400040q_si_002.cif
_cod_data_source_block           6a
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        'C65 H74 B2 F24 N2 P1 Ru1'
_cod_database_code               4080504
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
EQUIV PART(4001,OCC) PART(4002,OCC) 
WEIGHT -1 PART(4002,OCC) 
EQUIV PART(3001,OCC) PART(3002,OCC) 
WEIGHT -1 PART(3002,OCC) 
EQUIV PART(1001,OCC) PART(1002,OCC) 
WEIGHT -1 PART(1002,OCC) 
EQUIV PART(2001,OCC) PART(2002,OCC) 
WEIGHT -1 PART(2002,OCC) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
SAME C(64) F(500) F(501) F(502) AND 
CONT C(64) F(501) F(502) F(500) AND 
CONT C(64) F(502) F(500) F(501) AND 
CONT C(64) F(503) F(504) F(505) AND 
CONT C(64) F(504) F(505) F(503) AND 
CONT C(64) F(505) F(503) F(504) 
SIMU 0.01 C(64) F(500) F(501) F(502) AND 
CONT C(64) F(501) F(502) F(500) AND 
CONT C(64) F(502) F(500) F(501) AND 
CONT C(64) F(503) F(504) F(505) AND 
CONT C(64) F(504) F(505) F(503) AND 
CONT C(64) F(505) F(503) F(504) 
DELU 0.01 C(64) F(500) F(501) F(502) AND 
CONT C(64) F(501) F(502) F(500) AND 
CONT C(64) F(502) F(500) F(501) AND 
CONT C(64) F(503) F(504) F(505) AND 
CONT C(64) F(504) F(505) F(503) AND 
CONT C(64) F(505) F(503) F(504) 
SAME C(88) F(510) F(511) F(512) AND 
CONT C(88) F(511) F(512) F(510) AND 
CONT C(88) F(512) F(510) F(511) AND 
CONT C(88) F(513) F(514) F(515) AND 
CONT C(88) F(514) F(515) F(513) AND 
CONT C(88) F(515) F(513) F(514) 
SIMU 0.01 C(88) F(510) F(511) F(512) AND 
CONT C(88) F(511) F(512) F(510) AND 
CONT C(88) F(512) F(510) F(511) AND 
CONT C(88) F(513) F(514) F(515) AND 
CONT C(88) F(514) F(515) F(513) AND 
CONT C(88) F(515) F(513) F(514) 
DELU 0.01 C(88) F(510) F(511) F(512) AND 
CONT C(88) F(511) F(512) F(510) AND 
CONT C(88) F(512) F(510) F(511) AND 
CONT C(88) F(513) F(514) F(515) AND 
CONT C(88) F(514) F(515) F(513) AND 
CONT C(88) F(515) F(513) F(514) 
SAME C(92) F(520) F(521) F(522) AND 
CONT C(92) F(521) F(522) F(520) AND 
CONT C(92) F(522) F(520) F(521) AND 
CONT C(92) F(523) F(524) F(525) AND 
CONT C(92) F(524) F(525) F(523) AND 
CONT C(92) F(525) F(523) F(524) 
SIMU 0.01 C(92) F(520) F(521) F(522) AND 
CONT C(92) F(521) F(522) F(520) AND 
CONT C(92) F(522) F(520) F(521) AND 
CONT C(92) F(523) F(524) F(525) AND 
CONT C(92) F(524) F(525) F(523) AND 
CONT C(92) F(525) F(523) F(524) 
DELU 0.01 C(92) F(520) F(521) F(522) AND 
CONT C(92) F(521) F(522) F(520) AND 
CONT C(92) F(522) F(520) F(521) AND 
CONT C(92) F(523) F(524) F(525) AND 
CONT C(92) F(524) F(525) F(523) AND 
CONT C(92) F(525) F(523) F(524) 
SAME C(74) F(530) F(531) F(532) AND 
CONT C(74) F(531) F(532) F(530) AND 
CONT C(74) F(532) F(530) F(531) AND 
CONT C(74) F(533) F(534) F(535) AND 
CONT C(74) F(534) F(535) F(533) AND 
CONT C(74) F(535) F(533) F(534) 
SIMU 0.01 C(74) F(530) F(531) F(532) AND 
CONT C(74) F(531) F(532) F(530) AND 
CONT C(74) F(532) F(530) F(531) AND 
CONT C(74) F(533) F(534) F(535) AND 
CONT C(74) F(534) F(535) F(533) AND 
CONT C(74) F(535) F(533) F(534) 
DELU 0.01 C(74) F(530) F(531) F(532) AND 
CONT C(74) F(531) F(532) F(530) AND 
CONT C(74) F(532) F(530) F(531) AND 
CONT C(74) F(533) F(534) F(535) AND 
CONT C(74) F(534) F(535) F(533) AND 
CONT C(74) F(535) F(533) F(534) 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
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