New Scandium Borylimido Chemistry: Synthesis, Bonding, and Reactivity.
Clough, Benjamin A.; Mellino, Simona; Clot, Eric; Mountford, Philip; Journal of the American Chemical Society 139 (2017) 11165–11183; doi:10.1021/jacs.7b05405

data_4131434
_publ_section_title
;
 New Scandium Borylimido Chemistry: Synthesis, Bonding, and Reactivity.
;
_journal_issue                   32
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11165
_journal_page_last               11183
_journal_paper_doi               10.1021/jacs.7b05405
_journal_volume                  139
_journal_year                    2017
_chemical_formula_moiety         'C56 H78 B1 N6 Sc1'
_chemical_formula_sum            'C56 H78 B N6 Sc'
_chemical_formula_weight         891.04
_chemical_name_systematic        (NacNacNMe2)Sc{N(B(NDippCH)2)C(Me)C(Ph)}
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 109.2232(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.59570(10)
_cell_length_b                   38.8679(3)
_cell_length_c                   12.42060(10)
_cell_measurement_reflns_used    38505
_cell_measurement_temperature    150
_cell_measurement_theta_max      76
_cell_measurement_theta_min      3
_cell_volume                     5285.85(8)
_computing_cell_refinement       'CrysAlisPro, (Agilent, 2011)'
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_data_reduction        'CrysAlisPro, (Agilent, 2011)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.021
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_k_min       -48
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            66893
_diffrn_reflns_theta_full        74.621
_diffrn_reflns_theta_max         76.144
_diffrn_reflns_theta_min         3.937
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.488
_exptl_absorpt_correction_T_max  0.55
_exptl_absorpt_correction_T_min  0.43
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlisPro, (Agilent, 2011)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.120
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1928
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.500
_exptl_crystal_size_min          0.400
_refine_diff_density_max         0.30
_refine_diff_density_min         -0.37
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0262
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     577
_refine_ls_number_reflns         10556
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0350
_refine_ls_R_factor_gt           0.0345
_refine_ls_shift/su_max          0.0030855
_refine_ls_shift/su_mean         0.0001547
_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: 
 -4.03 -19.6 -11.0 -7.83 -4.84 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0157
_refine_ls_wR_factor_gt          0.0157
_refine_ls_wR_factor_ref         0.0156
_reflns_limit_h_max              13
_reflns_limit_h_min              -14
_reflns_limit_k_max              48
_reflns_limit_k_min              0
_reflns_limit_l_max              15
_reflns_limit_l_min              0
_reflns_number_gt                10743
_reflns_number_total             11012
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.89
_oxford_diffrn_Wilson_scale      0.06
_oxford_refine_ls_r_factor_ref   0.0339
_oxford_refine_ls_scale          4.058(2)
_oxford_reflns_number_all        10970
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            ja7b05405_si_003.cif
_cod_data_source_block           Compound_27
_cod_original_cell_volume        5285.85(4)
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        'C56 H78 B1 N6 Sc1'
_cod_database_code               4131434