Scandium Carbene Complexes: Synthesis of Mixed Alkyl, Amido, and Phosphido Derivatives
Fustier, Marie; Le Goff, Xavier-Frédéric; Lutz, Martin; Slootweg, J. Chris; Mézailles, Nicolas; Organometallics 34 (2015) 63–; doi:10.1021/om500868a

data_4085111
_publ_section_title
;
 Scandium Carbene Complexes: Synthesis of Mixed Alkyl, Amido, and
 Phosphido Derivatives
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              63
_journal_paper_doi               10.1021/om500868a
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         '(C54 H49 O P4 S4 Sc), 1.5(C4H8O)'
_chemical_formula_sum            'C60 H61 O2.5 P4 S4 Sc'
_chemical_formula_weight         1119.17
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 99.380(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   27.085(1)
_cell_length_b                   21.739(1)
_cell_length_c                   19.163(1)
_cell_measurement_reflns_used    22655
_cell_measurement_temperature    150.0(1)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     11132.3(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      150.0(1)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Kappa APEX II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0602
_diffrn_reflns_av_sigmaI/netI    0.0674
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            62020
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         1.43
_exptl_absorpt_coefficient_mu    0.441
_exptl_absorpt_correction_T_max  0.9826
_exptl_absorpt_correction_T_min  0.8791
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Denzo/Scalepack (Otwinowski & Minor, 1996)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.336
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             4688
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.04
_platon_squeeze_details
;
 Three highly disordered C4H8O molecule was accounted for using the
 Platon SQUEEZE function.
;
_refine_diff_density_max         0.624
_refine_diff_density_min         -0.430
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1299
_refine_ls_number_reflns         20929
_refine_ls_number_restraints     186
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0862
_refine_ls_R_factor_gt           0.0628
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0641P)^2^+25.9285P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1509
_refine_ls_wR_factor_ref         0.1645
_reflns_number_gt                15574
_reflns_number_total             20929
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500868a_si_002.cif
_cod_data_source_block           mf162
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/home/saulius/struct/COD-crude-data--automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2935 2014-11-11 08:27:57Z andrius 

 Adding full bibliography for 4085110--4085113.cif.
;
_cod_original_sg_symbol_H-M      'P21/c     '
_cod_original_formula_sum        'C60 H61 O2.50 P4 S4 Sc'
_cod_database_code               4085111