Contrasting reactivity of anionic boron- and gallium-containing NHC analogues: E-C vs. E-M bond formation (E = B, Ga)
Andrey V. Protchenko; Liban M.A. Saleh; Dragoslav Vidovic; Deepack Dange; Cameron Jones; Philip Mountford; Simon Aldridge; Chem.Commun. 46 (2010) 8546–; doi:10.1039/c0cc02572k

data_7105684
_publ_section_title
;
 Contrasting reactivity of anionic boron- and gallium-containing NHC
 analogues: E-C vs. E-M bond formation (E = B, Ga)
;
_journal_name_full               Chem.Commun.
_journal_page_first              8546
_journal_paper_doi               10.1039/c0cc02572k
_journal_volume                  46
_journal_year                    2010
_chemical_formula_moiety         'C50 H70 B1 N5 Ti1'
_chemical_formula_sum            'C50 H70 B N5 Ti'
_chemical_formula_weight         799.85
_chemical_melting_point          ?
_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             10-07-08
_audit_creation_method           CRYSTALS_ver_14.03
_cell_angle_alpha                90
_cell_angle_beta                 106.8532(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   40.1529(3)
_cell_length_b                   10.87630(10)
_cell_length_c                   25.0464(2)
_cell_measurement_reflns_used    12410
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     10468.35(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    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.992
_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  0.031
_diffrn_reflns_limit_h_max       49
_diffrn_reflns_limit_h_min       -52
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            11929
_diffrn_reflns_theta_full        27.018
_diffrn_reflns_theta_max         27.569
_diffrn_reflns_theta_min         5.103
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.197
_exptl_absorpt_correction_T_max  0.97
_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            yellow
_exptl_crystal_density_diffrn    1.015
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3456
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.160
_platon_squeeze_details
;
The discrete Fourier transform of the void region were treated as
contributions to the A and B parts of the calculated structure factors.
;
_refine_diff_density_max         0.55
_refine_diff_density_min         -0.58
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9480
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     542
_refine_ls_number_reflns         11929
_refine_ls_number_restraints     162
_refine_ls_R_factor_all          0.0773
_refine_ls_R_factor_gt           0.0537
_refine_ls_shift/su_max          0.0086733
_refine_ls_shift/su_mean         0.0011106
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
Method= Modified Sheldrick
w=1/[\s^2^(F^2^) + ( 0.09P)^2^ +15.46P]
,where P=(max(Fo^2^,0) + 2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1627
_refine_ls_wR_factor_gt          0.1505
_refine_ls_wR_factor_ref         0.1627
_reflns_limit_h_max              49
_reflns_limit_h_min              -52
_reflns_limit_k_max              14
_reflns_limit_k_min              0
_reflns_limit_l_max              32
_reflns_limit_l_min              0
_reflns_number_gt                8768
_reflns_number_total             11929
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.40
_oxford_diffrn_Wilson_scale      40.83
_oxford_refine_ls_r_factor_ref   0.0773
_oxford_refine_ls_scale          0.15139(7)
_oxford_reflns_number_all        11929
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 124apdv09
_cod_data_source_file            C0CC02572K.TXT
_cod_data_source_block           124apdv09
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/adriana/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_enum 1555 2011-01-17 13:19:09Z saulius 

The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 
;
_cod_original_sg_symbol_H-M      'C 1 2/c 1 '
_cod_original_formula_sum        'C50 H70 B1 N5 Ti1'
_cod_database_code               7105684