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_7105683
_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         'C45 H65 Ga1 N4 Ti1'
_chemical_formula_sum            'C45 H65 Ga N4 Ti'
_chemical_formula_weight         779.66
_chemical_melting_point          ?
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             10-02-11
_audit_creation_method           CRYSTALS_ver_12.86
_cell_angle_alpha                90
_cell_angle_beta                 105.2587(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.38040(10)
_cell_length_b                   16.7775(2)
_cell_length_c                   21.6398(2)
_cell_measurement_reflns_used    10117
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     4336.39(7)
_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 0.993
_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  0.085
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            67172
_diffrn_reflns_theta_full        26.933
_diffrn_reflns_theta_max         27.482
_diffrn_reflns_theta_min         5.101
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.839
_exptl_absorpt_correction_T_max  0.87
_exptl_absorpt_correction_T_min  0.82
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            dark_brown
_exptl_crystal_density_diffrn    1.194
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.78
_refine_diff_density_min         -0.86
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9483
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     579
_refine_ls_number_reflns         9855
_refine_ls_number_restraints     732
_refine_ls_R_factor_all          0.0826
_refine_ls_R_factor_gt           0.0447
_refine_ls_shift/su_max          0.007665
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
Method= Modified Sheldrick
w=1/[\s^2^(F^2^) + ( 0.05P)^2^ + 2.17P]
,where P=(max(Fo^2^,0) + 2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1078
_refine_ls_wR_factor_gt          0.0961
_refine_ls_wR_factor_ref         0.1077
_reflns_limit_h_max              15
_reflns_limit_h_min              -16
_reflns_limit_k_max              21
_reflns_limit_k_min              0
_reflns_limit_l_max              28
_reflns_limit_l_min              0
_reflns_number_gt                6572
_reflns_number_total             9856
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.90
_oxford_diffrn_Wilson_scale      49.02
_oxford_refine_ls_r_factor_ref   0.0825
_oxford_refine_ls_scale          0.14752(5)
_oxford_reflns_number_all        9856
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 015apdv10
_cod_data_source_file            C0CC02572K.TXT
_cod_data_source_block           1
_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      'P 1 21/n 1 '
_cod_original_formula_sum        'C45 H65 Ga1 N4 Ti1'
_cod_database_code               7105683