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_4131430
_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         'C45 H71.00 B2 N9 Sc1'
_chemical_formula_sum            'C45 H71 B2 N9 Sc'
_chemical_formula_weight         804.70
_chemical_name_systematic        (NacNacNMe2)Sc{NHB(NiPr)2C6H4}2
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                83.7821(15)
_cell_angle_beta                 77.6045(17)
_cell_angle_gamma                80.4089(15)
_cell_formula_units_Z            4
_cell_length_a                   14.2099(3)
_cell_length_b                   18.1022(3)
_cell_length_c                   24.3590(5)
_cell_measurement_reflns_used    24965
_cell_measurement_temperature    150
_cell_measurement_theta_max      76
_cell_measurement_theta_min      4
_cell_volume                     6017.1(2)
_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 0.997
_diffrn_measured_fraction_theta_max 0.989
_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  0.047
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            24925
_diffrn_reflns_theta_full        74.025
_diffrn_reflns_theta_max         76.315
_diffrn_reflns_theta_min         3.765
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.278
_exptl_absorpt_correction_T_max  0.68
_exptl_absorpt_correction_T_min  0.58
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlisPro, (Agilent, 2011)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    0.888
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1739.983
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.300
_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.

PLATON
PLATON, A Multipurpose Crystallographic Tool, A. L. Spek. Utrecht, 
the Netherlands, 1998.; A. Spek, J. Appl. Cryst. (2003), 36, 7-13.

SQUEEZE
A. Spek, J. Appl. Cryst. (2003), 36, 7-13; 
P. van der Sluis & A. L. Spek, Acta Cryst. (1990). A46, 194-201.

MCE
J. Rohlicek & M. Husak, J. Appl. Cryst. (2007), 40, 600-601.
;
_refine_diff_density_max         0.55
_refine_diff_density_min         -0.37
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0956
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1043
_refine_ls_number_reflns         18025
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0789
_refine_ls_R_factor_gt           0.0655
_refine_ls_shift/su_max          0.0293583
_refine_ls_shift/su_mean         0.0008209
_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: 
 14.7 3.12 12.6 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0977
_refine_ls_wR_factor_gt          0.0784
_refine_ls_wR_factor_ref         0.0756
_reflns_limit_h_max              17
_reflns_limit_h_min              -17
_reflns_limit_k_max              22
_reflns_limit_k_min              -22
_reflns_limit_l_max              30
_reflns_limit_l_min              0
_reflns_number_gt                19538
_reflns_number_total             24925
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   3.51
_oxford_diffrn_Wilson_scale      0.09
_oxford_refine_ls_r_factor_ref   0.0626
_oxford_refine_ls_scale          3.365(4)
_oxford_reflns_number_all        24925
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            ja7b05405_si_003.cif
_cod_data_source_block           Compound_16
_cod_original_cell_volume        6017.13(12)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C45 H71.00 B2 N9 Sc1'
_cod_database_code               4131430