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_4080503
_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         'C79 H63 B2 F24 N1 P2 Ru1'
_chemical_formula_sum            'C79 H63 B2 F24 N P2 Ru'
_chemical_formula_weight         1666.97
_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     other
_cell_angle_alpha                90
_cell_angle_beta                 94.1089(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.0982(2)
_cell_length_b                   16.8675(2)
_cell_length_c                   22.0476(3)
_cell_measurement_reflns_used    15854
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     7455.07(15)
_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 0.991
_diffrn_measured_fraction_theta_max 0.989
_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  0.032
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            29276
_diffrn_reflns_theta_full        25.210
_diffrn_reflns_theta_max         27.108
_diffrn_reflns_theta_min         5.103
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.358
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.67
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.485
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3376.000
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.64
_refine_diff_density_min         -1.50
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9100
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1123
_refine_ls_number_reflns         16296
_refine_ls_number_restraints     810
_refine_ls_R_factor_all          0.0722
_refine_ls_R_factor_gt           0.0536
_refine_ls_shift/su_max          0.0402752
_refine_ls_shift/su_mean         0.0002285
_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: 
 16.8 23.8 10.7 2.51 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1300
_refine_ls_wR_factor_gt          0.1129
_refine_ls_wR_factor_ref         0.1300
_reflns_limit_h_max              25
_reflns_limit_h_min              -25
_reflns_limit_k_max              21
_reflns_limit_k_min              0
_reflns_limit_l_max              28
_reflns_limit_l_min              0
_reflns_number_gt                12832
_reflns_number_total             16296
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.98
_oxford_diffrn_Wilson_scale      40.65
_oxford_refine_ls_r_factor_ref   0.0722
_oxford_refine_ls_scale          0.17543(6)
_oxford_reflns_number_all        16296
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_cod_data_source_file            om400040q_si_002.cif
_cod_data_source_block           4b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Other' changed to 'other'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_Hall     '-P 2yn '
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_original_formula_sum        'C79 H63 B2 F24 N1 P2 Ru1'
_cod_database_code               4080503
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S H(28, X'S), H(501, 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   (  10,X'S) H   ( 101,X'S) 
RIDE C   (  11,X'S) H   ( 111,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   (  16,X'S) H   ( 161,X'S) 
RIDE C   (  17,X'S) H   ( 171,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   (  22,X'S) H   ( 221,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) 
RIDE C   (  28,X'S) H   ( 281,X'S) 
RIDE C   (  30,X'S) H   ( 301,X'S) 
RIDE C   (  31,X'S) H   ( 311,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) 
RIDE C   (  37,X'S) H   ( 371,X'S) 
RIDE C   (  39,X'S) H   ( 391,X'S) 
RIDE C   (  40,X'S) H   ( 401,X'S) 
RIDE C   (  41,X'S) H   ( 411,X'S) 
RIDE C   (  42,X'S) H   ( 421,X'S) 
RIDE C   (  43,X'S) H   ( 431,X'S) 
RIDE C   (  45,X'S) H   ( 451,X'S) 
RIDE C   (  46,X'S) H   ( 461,X'S) 
RIDE C   (  47,X'S) H   ( 471,X'S) 
RIDE C   (  48,X'S) H   ( 481,X'S) 
RIDE C   (  49,X'S) H   ( 491,X'S) 
RIDE C   (  52,X'S) H   ( 521,X'S) 
RIDE C   (  53,X'S) H   ( 532,X'S) H   ( 531,X'S) H   ( 533,X'S) 
RIDE C   (  54,X'S) H   ( 543,X'S) H   ( 542,X'S) H   ( 541,X'S) 
RIDE C   (  55,X'S) H   ( 551,X'S) 
RIDE C   (  56,X'S) H   ( 562,X'S) H   ( 561,X'S) H   ( 563,X'S) 
RIDE C   (  57,X'S) H   ( 571,X'S) H   ( 573,X'S) H   ( 572,X'S) 
RIDE C   (  63,X'S) H   ( 631,X'S) 
RIDE C   (  65,X'S) H   ( 651,X'S) 
RIDE C   (  67,X'S) H   ( 671,X'S) 
RIDE C   (  74,X'S) H   ( 741,X'S) 
RIDE C   (  76,X'S) H   ( 761,X'S) 
RIDE C   (  78,X'S) H   ( 781,X'S) 
RIDE C   (  88,X'S) H   ( 881,X'S) 
RIDE C   (  90,X'S) H   ( 901,X'S) 
RIDE C   (  92,X'S) H   ( 921,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) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
REM FIRST CF3 
SAME C(200) F(201) F(202) F(203) AND 
CONT C(200) F(202) F(203) F(201) AND 
CONT C(200) F(203) F(201) F(202) AND 
CONT C(200) F(204) F(205) F(206) AND 
CONT C(200) F(205) F(206) F(204) AND 
CONT C(200) F(206) F(204) F(205) 
SIMU 0.01   C(200) F(201) F(202) F(203) AND 
CONT C(200) F(202) F(203) F(201) AND 
CONT C(200) F(203) F(201) F(202) AND 
CONT C(200) F(204) F(205) F(206) AND 
CONT C(200) F(205) F(206) F(204) AND 
CONT C(200) F(206) F(204) F(205) 
DELU 0.01   C(200) F(201) F(202) F(203) AND 
CONT C(200) F(202) F(203) F(201) AND 
CONT C(200) F(203) F(201) F(202) AND 
CONT C(200) F(204) F(205) F(206) AND 
CONT C(200) F(205) F(206) F(204) AND 
CONT C(200) F(206) F(204) F(205) 
REM SECOND CF3 
SAME C(210) F(211) F(212) F(213) AND 
CONT C(210) F(212) F(213) F(211) AND 
CONT C(210) F(213) F(211) F(212) AND 
CONT C(210) F(214) F(215) F(216) AND 
CONT C(210) F(215) F(216) F(214) AND 
CONT C(210) F(216) F(214) F(215) 
SIMU 0.01   C(210) F(211) F(212) F(213) AND 
CONT C(210) F(212) F(213) F(211) AND 
CONT C(210) F(213) F(211) F(212) AND 
CONT C(210) F(214) F(215) F(216) AND 
CONT C(210) F(215) F(216) F(214) AND 
CONT C(210) F(216) F(214) F(215) 
DELU 0.01   C(210) F(211) F(212) F(213) AND 
CONT C(210) F(212) F(213) F(211) AND 
CONT C(210) F(213) F(211) F(212) AND 
CONT C(210) F(214) F(215) F(216) AND 
CONT C(210) F(215) F(216) F(214) AND 
CONT C(210) F(216) F(214) F(215) 
REM THIRD CF3 
SAME C(220) F(221) F(222) F(223) AND 
CONT C(220) F(222) F(223) F(221) AND 
CONT C(220) F(223) F(221) F(222) AND 
CONT C(220) F(224) F(225) F(226) AND 
CONT C(220) F(225) F(226) F(224) AND 
CONT C(220) F(226) F(224) F(225) 
SIMU 0.01   C(220) F(221) F(222) F(223) AND 
CONT C(220) F(222) F(223) F(221) AND 
CONT C(220) F(223) F(221) F(222) AND 
CONT C(220) F(224) F(225) F(226) AND 
CONT C(220) F(225) F(226) F(224) AND 
CONT C(220) F(226) F(224) F(225) 
DELU 0.01   C(220) F(221) F(222) F(223) AND 
CONT C(220) F(222) F(223) F(221) AND 
CONT C(220) F(223) F(221) F(222) AND 
CONT C(220) F(224) F(225) F(226) AND 
CONT C(220) F(225) F(226) F(224) AND 
CONT C(220) F(226) F(224) F(225) 
REM FOURTH CF3 
SAME C(230) F(231) F(232) F(233) AND 
CONT C(230) F(232) F(233) F(231) AND 
CONT C(230) F(233) F(231) F(232) AND 
CONT C(230) F(234) F(235) F(236) AND 
CONT C(230) F(235) F(236) F(234) AND 
CONT C(230) F(236) F(234) F(235) 
SIMU 0.01   C(230) F(231) F(232) F(233) AND 
CONT C(230) F(232) F(233) F(231) AND 
CONT C(230) F(233) F(231) F(232) AND 
CONT C(230) F(234) F(235) F(236) AND 
CONT C(230) F(235) F(236) F(234) AND 
CONT C(230) F(236) F(234) F(235) 
DELU 0.01   C(230) F(231) F(232) F(233) AND 
CONT C(230) F(232) F(233) F(231) AND 
CONT C(230) F(233) F(231) F(232) AND 
CONT C(230) F(234) F(235) F(236) AND 
CONT C(230) F(235) F(236) F(234) AND 
CONT C(230) F(236) F(234) F(235) 
REM FIFTH CF3 
SAME C(240) F(241) F(242) F(243) AND 
CONT C(240) F(242) F(243) F(241) AND 
CONT C(240) F(243) F(241) F(242) AND 
CONT C(240) F(244) F(245) F(246) AND 
CONT C(240) F(245) F(246) F(244) AND 
CONT C(240) F(246) F(244) F(245) 
SIMU 0.01   C(240) F(241) F(242) F(243) AND 
CONT C(240) F(242) F(243) F(241) AND 
CONT C(240) F(243) F(241) F(242) AND 
CONT C(240) F(244) F(245) F(246) AND 
CONT C(240) F(245) F(246) F(244) AND 
CONT C(240) F(246) F(244) F(245) 
DELU 0.01   C(240) F(241) F(242) F(243) AND 
CONT C(240) F(242) F(243) F(241) AND 
CONT C(240) F(243) F(241) F(242) AND 
CONT C(240) F(244) F(245) F(246) AND 
CONT C(240) F(245) F(246) F(244) AND 
CONT C(240) F(246) F(244) F(245) 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;