Group 3 and Lanthanide Boryl Compounds: Syntheses, Structures, and Bonding Analyses of Sc-B, Y-B, and Lu-B σ-Coordinated NHC Analogues
Liban M. A. Saleh; Krishna Hassomal Birjkumar; Andrey V. Protchenko; Andrew D. Schwarz; Simon Aldridge; Cameron Jones; Nikolas Kaltsoyannis; Philip Mountford; Journal of the American Chemical Society 133 (2011) 3836–3839; doi:10.1021/ja2007092

data_4105810
_publ_contact_author
;
 Prof P. Mountford           
 Chemistry Research Laboratory
 Mansfield Road
 Oxford
 OX1 3TA
 UK
;
_publ_contact_author_email       Philip.Mountford@chem.ox.ac.uk
_publ_contact_author_fax         '+44 1865 285141'
_publ_contact_author_phone       '+44 1865 285140'
_publ_section_title
;
 Group 3 and Lanthanide Boryl Compounds: Syntheses, Structures, and
 Bonding Analyses of Sc-B, Y-B, and Lu-B \s-Coordinated NHC Analogues
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3836
_journal_page_last               3839
_journal_paper_doi               10.1021/ja2007092
_journal_volume                  133
_journal_year                    2011
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C38 H66 B1 N2 O1 Sc1 Si2'
_chemical_formula_sum            'C38 H66 B N2 O Sc Si2'
_chemical_formula_weight         678.89
_chemical_name_systematic
;
Sc{BN2Ar2C2H2}(CH2SiMe3)2(THF)
;
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_space_group_name_H-M   'P 1 n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 102.091(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.4076(2)
_cell_length_b                   15.0050(2)
_cell_length_c                   12.8787(2)
_cell_measurement_reflns_used    14899
_cell_measurement_temperature    293
_cell_measurement_theta_max      30
_cell_measurement_theta_min      3
_cell_volume                     2155.56(6)
_computing_cell_refinement       'CrysAlis RED, (Oxford Diffraction, 2002)'
_computing_data_collection       'Gemini, (Oxford Diffraction, 2006)'
_computing_data_reduction        'CrysAlis RED, (Oxford Diffraction, 2002)'
_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      293
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.941
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction Gemini'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.038
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            37023
_diffrn_reflns_theta_full        28.331
_diffrn_reflns_theta_max         30.464
_diffrn_reflns_theta_min         3.161
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.254
_exptl_absorpt_correction_T_max  0.96
_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            colourless
_exptl_crystal_density_diffrn    1.046
_exptl_crystal_description       block
_exptl_crystal_F_000             740
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.45
_refine_diff_density_min         -0.44
_refine_ls_abs_structure_details 'Flack (1983), 5032 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.00(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.1107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     443
_refine_ls_number_reflns         7844
_refine_ls_number_restraints     111
_refine_ls_R_factor_all          0.0714
_refine_ls_R_factor_gt           0.0518
_refine_ls_shift/su_max          0.0012592
_refine_ls_shift/su_mean         0.0000655
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 11.1 -4.55 9.99 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0625
_refine_ls_wR_factor_gt          0.0531
_refine_ls_wR_factor_ref         0.0510
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              21
_reflns_limit_k_min              0
_reflns_limit_l_max              18
_reflns_limit_l_min              -18
_reflns_number_gt                8972
_reflns_number_total             11647
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.63
_oxford_diffrn_Wilson_scale      0.26
_oxford_refine_ls_r_factor_ref   0.0455
_oxford_refine_ls_scale          2.272(3)
_oxford_reflns_number_all        11627
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            ja2007092_si_002_1.cif
_cod_data_source_block           COMPOUND_2
_cod_original_cell_volume        2155.55(7)
_cod_original_sg_symbol_H-M      'P 1 n 1 '
_cod_original_formula_sum        'C38 H66 B1 N2 O1 Sc1 Si2'
_cod_database_code               4105810