Scandium complexes containing β-diketiminato ligands with pendant phosphanyl groups: competition between Sc/γ-C [4 + 2] cycloaddition and Sc/P frustrated Lewis pair reactions.
Yao, Tu; Xu, Pengfei; Xu, Xin; Dalton transactions (Cambridge, England : 2003) 48 (2019) 7743–7754; doi:10.1039/c9dt01035a

data_7049938
_publ_section_title
;
 Scandium complexes containing \b-diketiminato ligands with pendant
 phosphanyl groups: competition between Sc/\g-C [4 + 2] cycloaddition and
 Sc/P frustrated Lewis pair reactions.
;
_journal_issue                   22
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7743
_journal_page_last               7754
_journal_paper_doi               10.1039/c9dt01035a
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C55 H70 N3 O2 P Sc, C24 B F20, 2(C6 H6)'
_chemical_formula_sum            'C91 H82 B F20 N3 O2 P Sc'
_chemical_formula_weight         1716.34
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2019-03-07 deposited with the CCDC.    2019-05-01 downloaded from the CCDC.
;
_cell_angle_alpha                94.758(4)
_cell_angle_beta                 98.990(4)
_cell_angle_gamma                98.865(4)
_cell_formula_units_Z            2
_cell_length_a                   12.8116(7)
_cell_length_b                   17.3758(9)
_cell_length_c                   19.3172(8)
_cell_measurement_reflns_used    9927
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      26.6
_cell_measurement_theta_min      2.25
_cell_volume                     4171.4(4)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0807
_diffrn_reflns_av_unetI/netI     0.1238
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            40078
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.913
_diffrn_source                   'sealed tube'
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.203
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_description       block
_exptl_crystal_F_000             1772
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.850
_refine_diff_density_min         -0.863
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1050
_refine_ls_number_reflns         14688
_refine_ls_number_restraints     1982
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.1500
_refine_ls_R_factor_gt           0.0792
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0977P)^2^+3.7374P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1914
_refine_ls_wR_factor_ref         0.2520
_reflns_Friedel_coverage         0.968
_reflns_Friedel_fraction_full    0.973
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                7776
_reflns_number_total             14688
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01035a2.cif
_cod_data_source_block           g171227d
_cod_depositor_comments
'Adding full bibliography for 7049936--7049940.cif.'
_cod_database_code               7049938
_shelx_estimated_absorpt_t_min   0.106
_shelx_estimated_absorpt_t_max   0.159
_shelxl_version_number           2013-2
_shelx_res_checksum              9199