(Dimethylamino)borylene and Related Complexes of Electron-Rich Metal Fragments: Generation of Nucleophile-Resistant Cations by Spontaneous Halide Ejection
Addy, David A.; Phillips, Nicholas; Pierce, Glesni A.; Vidovic, Dragoslav; Krämer, Tobias; Mallick, Dibyendu; Jemmis, Eluvathingal D.; Reid, Gill; Aldridge, Simon; Organometallics 31 (2012) 1092–; doi:10.1021/om201144e

data_4068146
_publ_section_title
;
 (Dimethylamino)borylene and Related Complexes of Electron-Rich Metal
 Fragments: Generation of Nucleophile-Resistant Cations by Spontaneous
 Halide Ejection
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              1092
_journal_paper_doi               10.1021/om201144e
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C32 H12 B F24, C32 H31 Fe O P2, C6 H5 F'
_chemical_formula_sum            'C67 H45.5 B F24.5 Fe O P2'
_chemical_formula_weight         1460.65
_chemical_melting_point          ?
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_date             11-10-17
_audit_creation_method           CRYSTALS_ver_14.11
_cell_angle_alpha                100.2488(5)
_cell_angle_beta                 101.1516(5)
_cell_angle_gamma                95.9108(5)
_cell_formula_units_Z            2
_cell_length_a                   12.67910(10)
_cell_length_b                   13.8270(2)
_cell_length_c                   18.7636(2)
_cell_measurement_reflns_used    11665
_cell_measurement_temperature    150
_cell_measurement_theta_max      26
_cell_measurement_theta_min      5
_cell_volume                     3143.59(6)
_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 0.985
_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  0.030
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            39196
_diffrn_reflns_theta_full        25.713
_diffrn_reflns_theta_max         26.238
_diffrn_reflns_theta_min         5.088
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.408
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.94
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.543
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1474
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.080
_refine_diff_density_max         1.75
_refine_diff_density_min         -1.29
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9246
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     904
_refine_ls_number_reflns         12506
_refine_ls_number_restraints     690
_refine_ls_R_factor_all          0.0830
_refine_ls_R_factor_gt           0.0690
_refine_ls_shift/su_max          0.0215495
_refine_ls_shift/su_mean         0.0003294
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.08P)^2^ +11.04P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1822
_refine_ls_wR_factor_gt          0.1715
_refine_ls_wR_factor_ref         0.1822
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              16
_reflns_limit_k_min              -17
_reflns_limit_l_max              23
_reflns_limit_l_min              0
_reflns_number_gt                10166
_reflns_number_total             12506
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.21
_oxford_diffrn_Wilson_scale      5.69
_oxford_refine_ls_r_factor_ref   0.0830
_oxford_refine_ls_scale          0.4547(7)
_oxford_reflns_number_all        12506
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 074dadv09
_cod_data_source_file            om201144e_si_008.cif
_cod_data_source_block           global
_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.

'_symmetry_cell_setting' value
'Triclinic' changed to 'triclinic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C67 H45.50 B1 F24.50 Fe1 O1 P2'
_cod_database_code               4068146
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, FE(1,U'S) UNTIL F(95) 
CONT F(100,U[ISO]) UNTIL F(107) 
CONT F(110,U[ISO]) UNTIL F(117) 
CONT F(120,U[ISO]) UNTIL F(127) 
CONT C(95,U'S) UNTIL C(100) 
EQUIV PART(1001,OCC) PART(1002,OCC) 
EQUIV PART(1003,OCC) PART(1004,OCC) 
EQUIV PART(1005,OCC) PART(1006,OCC) 
WEIGHT -1 PART(1002,OCC) 
WEIGHT -1 PART(1004,OCC) 
WEIGHT -1 PART(1006,OCC) 
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   (  15,X'S) H   ( 151,X'S) H   ( 152,X'S) H   ( 153,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   (  22,X'S) H   ( 221,X'S) 
RIDE C   (  23,X'S) H   ( 233,X'S) H   ( 232,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   (  27,X'S) H   ( 271,X'S) 
RIDE C   (  28,X'S) H   ( 281,X'S) 
RIDE C   (  29,X'S) H   ( 291,X'S) 
RIDE C   (  32,X'S) H   ( 321,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   (  42,X'S) H   ( 421,X'S) 
RIDE C   (  44,X'S) H   ( 441,X'S) 
RIDE C   (  46,X'S) H   ( 461,X'S) 
RIDE C   (  49,X'S) H   ( 491,X'S) 
RIDE C   (  51,X'S) H   ( 511,X'S) 
RIDE C   (  53,X'S) H   ( 531,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   (  77,X'S) H   ( 771,X'S) 
RIDE C   (  79,X'S) H   ( 791,X'S) 
RIDE C   (  81,X'S) H   ( 811,X'S) 
RIDE C   (  95,X'S) H   ( 951,X'S) 
RIDE C   (  96,X'S) H   ( 961,X'S) 
RIDE C   (  97,X'S) H   ( 971,X'S) 
RIDE C   (  98,X'S) H   ( 981,X'S) 
RIDE C   (  99,X'S) H   ( 991,X'S) 
RIDE C   ( 100,X'S) H   (1001,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
PLANAR F(94) C(95) C(97) C(96) C(98) C(99) C(100) F(95) 
SAME F(94) C(95) C(96) C(97) C(98) C(99) C(100) AND 
CONT F(94) C(95) C(100) C(99) C(98) C(97) C(96) AND 
CONT F(95) C(99) C(100) C(95) C(96) C(97) C(98) AND 
CONT F(95) C(99) C(98) C(97) C(96) C(95) C(100) 
DELU 0.01 F(94) C(95) C(96) C(97) C(98) C(99) C(100) AND 
CONT F(94) C(95) C(100) C(99) C(98) C(97) C(96) AND 
CONT F(95) C(99) C(100) C(95) C(96) C(97) C(98) AND 
CONT F(95) C(99) C(98) C(97) C(96) C(95) C(100) 
SIMU 0.01 F(94) C(95) C(96) C(97) C(98) C(99) C(100) AND 
CONT F(94) C(95) C(100) C(99) C(98) C(97) C(96) AND 
CONT F(95) C(99) C(100) C(95) C(96) C(97) C(98) AND 
CONT F(95) C(99) C(98) C(97) C(96) C(95) C(100) 
SAME C(82) F(100) F(101) F(102) AND 
CONT C(82) F(102) F(100) F(101) AND 
CONT C(82) F(101) F(102) F(100) AND 
CONT C(68) F(110) F(111) F(112) AND 
CONT C(68) F(112) F(110) F(111) AND 
CONT C(68) F(111) F(112) F(110) AND 
CONT C(72) F(120) F(121) F(122) AND 
CONT C(72) F(122) F(120) F(121) AND 
CONT C(72) F(121) F(122) F(120) 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;