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_4135023
_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
'C48 H64 Al N P3 Sc, 0.25(C7 H8), 0.25(C5 H12)'
_chemical_formula_sum            'C51 H69 Al N P3 Sc'
_chemical_formula_weight         860.92
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-09-03
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 97.6830(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.6374(7)
_cell_length_b                   17.6783(7)
_cell_length_c                   33.7373(14)
_cell_measurement_reflns_used    9708
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.472
_cell_measurement_theta_min      2.604
_cell_volume                     9833.8(7)
_computing_cell_refinement       'SAINT V8.38A (2016)'
_computing_data_collection       'Bruker APEX3 v2018.7-2'
_computing_data_reduction        'SAINT V8.38A (2016)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 2012)'
_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 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'CMOS area detector'
_diffrn_measurement_device_type  'Bruker D8QUEST'
_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  0.0721
_diffrn_reflns_av_unetI/netI     0.0362
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            283447
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.569
_diffrn_reflns_theta_min         2.605
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.298
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6996
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2014/5'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.163
_exptl_crystal_description       bar
_exptl_crystal_F_000             3688
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.453
_refine_diff_density_min         -0.447
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1260
_refine_ls_number_reflns         22702
_refine_ls_number_restraints     498
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0736
_refine_ls_R_factor_gt           0.0530
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0327P)^2^+12.9037P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1074
_refine_ls_wR_factor_ref         0.1153
_reflns_number_gt                18269
_reflns_number_total             22702
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c02742_si_009.cif
_cod_data_source_block           9543
_cod_database_code               4135023
_shelx_shelxl_version_number     2018/3