CAAC Boranes. Synthesis and characterization of cyclic (alkyl) (amino) carbene borane complexes from BF₃ and BH₃.
Monot, Julien; Fensterbank, Louis; Malacria, Max; Lacôte, Emmanuel; Geib, Steven J.; Curran, Dennis P.; Beilstein journal of organic chemistry 6 (2010) 709–712; doi:10.3762/bjoc.6.82

data_4029783
_publ_section_title
;
 CAAC Boranes. Synthesis and characterization of cyclic (alkyl) (amino)
 carbene borane complexes from BF&#x2083; and BH&#x2083;.
;
_journal_name_full               'Beilstein journal of organic chemistry'
_journal_page_first              709
_journal_page_last               712
_journal_paper_doi               10.3762/bjoc.6.82
_journal_volume                  6
_journal_year                    2010
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C25 H33 B1 F3 N1'
_chemical_formula_sum            'C25 H33 B F3 N'
_chemical_formula_weight         415.35
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2b'
_symmetry_space_group_name_H-M   'P b c 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.3106(11)
_cell_length_b                   16.120(2)
_cell_length_c                   16.9678(18)
_cell_measurement_reflns_used    135
_cell_measurement_temperature    200
_cell_measurement_theta_max      22
_cell_measurement_theta_min      5
_cell_volume                     2273.1(5)
_computing_cell_refinement       'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_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      200
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.042
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            11847
_diffrn_reflns_theta_full        25.493
_diffrn_reflns_theta_max         29.991
_diffrn_reflns_theta_min         1.742
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.086
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.97
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.214
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.190
_refine_diff_density_max         0.38
_refine_diff_density_min         -0.34
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9218
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         3692
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0867
_refine_ls_R_factor_gt           0.0466
_refine_ls_shift/su_max          0.0054975
_refine_ls_shift/su_mean         0.4437670
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.06P)^2^ + 0.53P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1161
_refine_ls_wR_factor_gt          0.1007
_refine_ls_wR_factor_ref         0.1157
_reflns_limit_h_max              11
_reflns_limit_h_min              0
_reflns_limit_k_max              22
_reflns_limit_k_min              0
_reflns_limit_l_max              23
_reflns_limit_l_min              0
_reflns_number_gt                2509
_reflns_number_total             3695
_reflns_threshold_expression     I>2.0\s(I)
_oxford_refine_ls_r_factor_ref   0.0866
_oxford_reflns_number_all        3694
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_cod_data_source_file            1860-5397-6-82-S2.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/usr/data/users/saulius/automatic-downloads/retrospective/Beilstein/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 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        2273.2(5)
_cod_original_sg_symbol_H-M      'P b c 21 '
_cod_original_formula_sum        'C25 H33 B1 F3 N1'
_cod_database_code               4029783