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_4131433
_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         'C47 H70 B1 N6 Sc1'
_chemical_formula_sum            'C47 H70 B N6 Sc'
_chemical_formula_weight         774.88
_chemical_name_systematic
{MeC(NC6H3iPrCH(Me)CH2)CHC(Me)(NCH2CH2NMe}Sc{NHB(NDippCH)2}
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yab'
_space_group_name_H-M_alt        'P 1 21/a 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 122.244(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.8650(7)
_cell_length_b                   43.9807(9)
_cell_length_c                   11.0806(3)
_cell_measurement_reflns_used    41972
_cell_measurement_temperature    150
_cell_measurement_theta_max      76
_cell_measurement_theta_min      3
_cell_volume                     10248.8(6)
_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    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.990
_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  0.089
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       55
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            117743
_diffrn_reflns_theta_full        75.080
_diffrn_reflns_theta_max         76.613
_diffrn_reflns_theta_min         3.675
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.471
_exptl_absorpt_correction_T_max  0.56
_exptl_absorpt_correction_T_min  0.40
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlisPro, (Agilent, 2011)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.004
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3360
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.500
_exptl_crystal_size_min          0.400
_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         0.80
_refine_diff_density_min         -0.69
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0450
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1035
_refine_ls_number_reflns         17200
_refine_ls_number_restraints     1670
_refine_ls_R_factor_all          0.0852
_refine_ls_R_factor_gt           0.0781
_refine_ls_shift/su_max          0.0060473
_refine_ls_shift/su_mean         0.0001470
_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: 
 11.8 2.07 7.31 0.893 -2.31 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0773
_refine_ls_wR_factor_gt          0.0755
_refine_ls_wR_factor_ref         0.0746
_reflns_limit_h_max              26
_reflns_limit_h_min              -31
_reflns_limit_k_max              55
_reflns_limit_k_min              0
_reflns_limit_l_max              13
_reflns_limit_l_min              0
_reflns_number_gt                18457
_reflns_number_total             21320
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.69
_oxford_diffrn_Wilson_scale      0.35
_oxford_refine_ls_r_factor_ref   0.0742
_oxford_refine_ls_scale          1.688(2)
_oxford_reflns_number_all        21320
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            ja7b05405_si_003.cif
_cod_data_source_block           Compound_21
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_atom_sites_solution_primary' value 'Other' was changed to
'other' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        10248.8(3)
_cod_original_sg_symbol_H-M      'P 21/a '
_cod_original_formula_sum        'C47 H70 B1 N6 Sc1'
_cod_database_code               4131433