Tebbe-like and Phosphonioalkylidene and -alkylidyne Complexes of Scandium.
Zatsepin, Pavel; Lee, Eunji; Gu, Jun; Gau, Michael R.; Carroll, Patrick J.; Baik, Mu-Hyun; Mindiola, Daniel J.; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.0c02742

data_4135025
_publ_section_title
;
 Tebbe-like and Phosphonioalkylidene and -alkylidyne Complexes of
 Scandium.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c02742
_journal_year                    2020
_chemical_formula_moiety         'C37 H60 N3 P2 Sc Si, 3(C7 H8)'
_chemical_formula_sum            'C58 H84 N3 P2 Sc Si'
_chemical_formula_weight         958.27
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-02-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                64.146(6)
_cell_angle_beta                 84.121(5)
_cell_angle_gamma                66.561(5)
_cell_formula_units_Z            2
_cell_length_a                   13.215(2)
_cell_length_b                   15.972(3)
_cell_length_c                   16.231(3)
_cell_measurement_reflns_used    9941
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.48
_cell_measurement_theta_min      2.55
_cell_volume                     2818.1(9)
_computing_cell_refinement       'Bruker SAINT v8.38A'
_computing_data_collection       'Bruker APEX2 v2014.11-0'
_computing_data_reduction        'Bruker SAINT v8.38A'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'CCD area detector'
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0683
_diffrn_reflns_av_unetI/netI     0.0602
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            73135
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.511
_diffrn_reflns_theta_min         1.399
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.246
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7079
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2016/2'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.129
_exptl_crystal_description       block
_exptl_crystal_F_000             1036
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.891
_refine_diff_density_min         -0.555
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     598
_refine_ls_number_reflns         12930
_refine_ls_number_restraints     162
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0981
_refine_ls_R_factor_gt           0.0579
_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^)+(0.0779P)^2^+2.2896P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1452
_refine_ls_wR_factor_ref         0.1652
_reflns_number_gt                8745
_reflns_number_total             12930
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c02742_si_007.cif
_cod_data_source_block           9427
_cod_database_code               4135025
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.983
_shelx_estimated_absorpt_t_min   0.957