Trinuclear scandium methylidyne complexes stabilized by pentamethylcyclopentadienyl ligands.
Deng, Peng; Shi, Xianghui; Gong, Xun; Cheng, Jianhua; Chemical communications (Cambridge, England) 57 (2021) 6436–6439; doi:10.1039/d1cc01645h

data_7128445
_publ_section_title
;
 Trinuclear scandium methylidyne complexes stabilized by
 pentamethylcyclopentadienyl ligands.
;
_journal_issue                   52
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              6436
_journal_page_last               6439
_journal_paper_doi               10.1039/d1cc01645h
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C39 H64 N O3 Sc3'
_chemical_formula_sum            'C39 H64 N O3 Sc3'
_chemical_formula_weight         729.79
_chemical_name_common            '[(Cp*)Sc(OMe)]3(CHCNtBu)'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   iterative
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-09-28 deposited with the CCDC.	2021-05-31 downloaded from the CCDC.
;
_cell_angle_alpha                63.681(2)
_cell_angle_beta                 77.428(2)
_cell_angle_gamma                76.109(2)
_cell_formula_units_Z            4
_cell_length_a                   12.1700(6)
_cell_length_b                   19.2637(9)
_cell_length_c                   19.9851(10)
_cell_measurement_reflns_used    9979
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      29.92
_cell_measurement_theta_min      2.41
_cell_volume                     4043.3(3)
_computing_data_collection       'Bruker D8 Venture diffractometer'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SUPERFLIP (Palatinus & Chapuis,2007)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0604
_diffrn_reflns_av_unetI/netI     0.0351
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            111818
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.941
_exptl_absorpt_coefficient_mu    0.523
_exptl_absorpt_correction_T_max  0.954
_exptl_absorpt_correction_T_min  0.929
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
'Sheldrick, G. M. SADABS, Version 2.10; Bruker AXS, Inc.: Madison, WI 2003.'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.199
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1568
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: benzene'
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.426
_refine_diff_density_min         -0.363
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     840
_refine_ls_number_reflns         14160
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0569
_refine_ls_R_factor_gt           0.0419
_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^)+(0.0456P)^2^+4.4439P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1038
_refine_ls_wR_factor_ref         0.1135
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11468
_reflns_number_total             14160
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc01645h2.cif
_cod_data_source_block           Deng07-2020
_cod_depositor_comments
;
Adding full bibliography for 7128441--7128448.cif.

2024-10-08
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C78 H128 N2 O6 Sc6'
_cod_original_formula_weight         1459.58
_cod_original_formula_moiety         'C78 H128 N2 O6 Sc6'
_cod_original_formula_units_Z            2
_cod_database_code               7128445
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.930
_shelx_estimated_absorpt_t_max   0.954
_shelx_res_checksum              746