Generation of Cationic Two-Coordinate Group-13 Ligand Systems by Spontaneous Halide Ejection: Remarkably Nucleophile-Resistant (Dimethylamino)borylene Complexes
David A. Addy; Glesni A. Pierce; Dragoslav Vidovic; Dibyendu Mallick; Eluvathingal D. Jemmis; Jose M. Goicoechea; Simon Aldridge; Journal of the American Chemical Society 132 (2010) 4586–4588; doi:10.1021/ja101192e

data_4102223
_publ_contact_author             'Simon Aldridge'
_publ_contact_author_email       simon.aldridge@chem.ox.ac.uk
_publ_section_title
;
 Generation of Cationic Two-Coordinate Group-13 Ligand Systems by
 Spontaneous Halide Ejection: Remarkably Nucleophile-Resistant
 (Dimethylamino)borylene Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4586
_journal_page_last               4588
_journal_paper_doi               10.1021/ja101192e
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         'C12 H23 Fe1 O1 P2, C H2 Cl2, Cl'
_chemical_formula_sum            'C13 H25 Cl3 Fe O P2'
_chemical_formula_weight         421.49
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             08-02-19
_audit_creation_method           CRYSTALS_ver_12.85
_cell_angle_alpha                90
_cell_angle_beta                 124.6365(11)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   31.4550(6)
_cell_length_b                   7.9830(2)
_cell_length_c                   18.2228(4)
_cell_measurement_reflns_used    4446
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     3764.89(15)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997-2001).'
_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 0.990
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.073
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            23231
_diffrn_reflns_theta_full        26.354
_diffrn_reflns_theta_max         27.452
_diffrn_reflns_theta_min         5.108
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.390
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.88
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            clear_intense_yellow
_exptl_crystal_density_diffrn    1.487
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1744
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.48
_refine_diff_density_min         -1.31
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9520
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         4259
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0753
_refine_ls_R_factor_gt           0.0429
_refine_ls_shift/su_max          0.000749
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.02P)^2^ +11.51P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0894
_refine_ls_wR_factor_gt          0.0789
_refine_ls_wR_factor_ref         0.0894
_reflns_limit_h_max              32
_reflns_limit_h_min              -40
_reflns_limit_k_max              10
_reflns_limit_k_min              0
_reflns_limit_l_max              23
_reflns_limit_l_min              0
_reflns_number_gt                2982
_reflns_number_total             4259
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.17
_oxford_diffrn_Wilson_scale      133.60
_oxford_refine_ls_r_factor_ref   0.0753
_oxford_refine_ls_scale          0.08893(2)
_oxford_reflns_number_all        4259
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_cod_data_source_file            ja101192e_si_001_2.cif
_cod_data_source_block           CpFeCOPMe3_2_Cl
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      'C 1 2/c 1 '
_cod_original_formula_sum        'C13 H25 Cl3 Fe1 O1 P2'
_cod_database_code               4102223