Circumventing redox chemistry: synthesis of transition metal boryl complexes from a boryl nucleophile by decarbonylation.
Frank, René; Howell, James; Tirfoin, Rémi; Dange, Deepak; Jones, Cameron; Mingos, D Michael P; Aldridge, Simon; Journal of the American Chemical Society 136 (2014) 15730–15741; doi:10.1021/ja508979x

data_4122859
_publ_section_title
;
 Circumventing redox chemistry: synthesis of transition metal boryl
 complexes from a boryl nucleophile by decarbonylation.
;
_journal_issue                   44
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15730
_journal_page_last               15741
_journal_paper_doi               10.1021/ja508979x
_journal_volume                  136
_journal_year                    2014
_chemical_formula_moiety         'C34.00 H41.00 B1 Fe1 N2 O3'
_chemical_formula_sum            'C34 H41 B Fe N2 O3'
_chemical_formula_weight         592.37
_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             13-08-05
_audit_creation_method           CRYSTALS_ver_14.40
_cell_angle_alpha                104.5077(5)
_cell_angle_beta                 93.2151(6)
_cell_angle_gamma                99.4456(6)
_cell_formula_units_Z            2
_cell_length_a                   10.58990(10)
_cell_length_b                   10.61490(10)
_cell_length_c                   14.9425(2)
_cell_measurement_reflns_used    6473
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     1595.76(3)
_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 0.990
_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  0.021
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            43676
_diffrn_reflns_theta_full        25.296
_diffrn_reflns_theta_max         27.496
_diffrn_reflns_theta_min         5.164
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.508
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_correction_T_min  0.89
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.233
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             628.000
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.37
_refine_diff_density_min         -0.40
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9136
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     407
_refine_ls_number_reflns         7258
_refine_ls_number_restraints     324
_refine_ls_R_factor_all          0.0498
_refine_ls_R_factor_gt           0.0393
_refine_ls_shift/su_max          0.0006380
_refine_ls_shift/su_mean         0.0000290
_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: 
 15.8 22.6 10.6 2.77 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0962
_refine_ls_wR_factor_gt          0.0842
_refine_ls_wR_factor_ref         0.0962
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              13
_reflns_limit_k_min              -13
_reflns_limit_l_max              19
_reflns_limit_l_min              0
_reflns_number_gt                6114
_reflns_number_total             7258
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0498
_oxford_refine_ls_scale          0.6144(8)
_oxford_reflns_number_all        7258
_oxford_reflns_threshold_expression_ref I>0.0\s(I)
_oxford_structure_analysis_title '084rfrt13 in P -1'
_cod_data_source_file            ja508979x_si_002.cif
_cod_data_source_block           13
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Other' changed to 'other'
according to
/home/saulius/struct/COD-crude-data--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 2827 2014-09-09 07:05:25Z andrius 

 Adding full bibliography for 4122854--4122863.cif.
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C34.00 H41.00 B1 Fe1 N2 O3'
_cod_database_code               4122859
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
EQUIV PART(1001,OCC) PART(1002,OCC) 
WEIGHT -1 PART(1002,OCC) 
RIDE C   (  41,X'S) H   ( 411,X'S) H   ( 413,X'S) H   ( 412,X'S) 
RIDE C   (  42,X'S) H   ( 421,X'S) H   ( 423,X'S) H   ( 422,X'S) 
RIDE C   (  43,X'S) H   ( 431,X'S) H   ( 433,X'S) H   ( 432,X'S) 
RIDE C   (  44,X'S) H   ( 441,X'S) H   ( 443,X'S) H   ( 442,X'S) 
RIDE C   (  45,X'S) H   ( 451,X'S) H   ( 453,X'S) H   ( 452,X'S) 
RIDE C   (  46,X'S) H   ( 461,X'S) H   ( 463,X'S) H   ( 462,X'S) 
RIDE C   (  47,X'S) H   ( 471,X'S) H   ( 473,X'S) H   ( 472,X'S) 
RIDE C   (  48,X'S) H   ( 481,X'S) H   ( 483,X'S) H   ( 482,X'S) 
RIDE C   (   8,X'S) H   (  81,X'S) H   (  82,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   (  15,X'S) H   ( 151,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) H   ( 163,X'S) H   ( 162,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) H   ( 173,X'S) H   ( 172,X'S) 
RIDE C   (  18,X'S) H   ( 181,X'S) 
RIDE C   (  19,X'S) H   ( 191,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) H   ( 243,X'S) H   ( 242,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) H   ( 253,X'S) H   ( 252,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) 
RIDE C   (  27,X'S) H   ( 271,X'S) 
RIDE C   (  28,X'S) H   ( 281,X'S) 
RIDE C   (  30,X'S) H   ( 301,X'S) H   ( 302,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   (  38,X'S) H   ( 381,X'S) 
RIDE C   (  39,X'S) H   ( 391,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
SAME  C(8)  C(7)  C(44)  C(43) AND 
CONT  C(8)  C(44)  C(43)  C(7) AND 
CONT  C(8)  C(43)  C(7)  C(44) AND 
CONT  C(8)  C(7)  C(42)  C(41) AND 
CONT  C(8)  C(42)  C(41)  C(7) AND 
CONT  C(8)  C(41)  C(7)  C(42) AND 
CONT  C(30)  C(29)  C(47)  C(48) AND 
CONT  C(30)  C(47)  C(48)  C(29) AND 
CONT  C(30)  C(48)  C(29)  C(47) AND 
CONT  C(30)  C(29)  C(46)  C(45) AND 
CONT  C(30)  C(46)  C(45)  C(29) AND 
CONT  C(30)  C(45)  C(29)  C(46) 
SIMU 0.01 C(8)  C(7)  C(44)  C(43) AND 
CONT  C(8)  C(44)  C(43)  C(7) AND 
CONT  C(8)  C(43)  C(7)  C(44) AND 
CONT  C(8)  C(7)  C(42)  C(41) AND 
CONT  C(8)  C(42)  C(41)  C(7) AND 
CONT  C(8)  C(41)  C(7)  C(42) AND 
CONT  C(30)  C(29)  C(47)  C(48) AND 
CONT  C(30)  C(47)  C(48)  C(29) AND 
CONT  C(30)  C(48)  C(29)  C(47) AND 
CONT  C(30)  C(29)  C(46)  C(45) AND 
CONT  C(30)  C(46)  C(45)  C(29) AND 
CONT  C(30)  C(45)  C(29)  C(46) 
DELU 0.01 C(8)  C(7)  C(44)  C(43) AND 
CONT  C(8)  C(44)  C(43)  C(7) AND 
CONT  C(8)  C(43)  C(7)  C(44) AND 
CONT  C(8)  C(7)  C(42)  C(41) AND 
CONT  C(8)  C(42)  C(41)  C(7) AND 
CONT  C(8)  C(41)  C(7)  C(42) AND 
CONT  C(30)  C(29)  C(47)  C(48) AND 
CONT  C(30)  C(47)  C(48)  C(29) AND 
CONT  C(30)  C(48)  C(29)  C(47) AND 
CONT  C(30)  C(29)  C(46)  C(45) AND 
CONT  C(30)  C(46)  C(45)  C(29) AND 
CONT  C(30)  C(45)  C(29)  C(46) 
END                                                                             
;