#------------------------------------------------------------------------------
#$Date: 2021-07-05 19:15:28 +0300 (Mon, 05 Jul 2021) $
#$Revision: 267011 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/84/7128447.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7128447
loop_
_publ_author_name
'Deng, Peng'
'Shi, Xianghui'
'Gong, Xun'
'Cheng, Jianhua'
_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         'C34  H55  Sc3'
_chemical_formula_sum            'C34 H55 Sc3'
_chemical_formula_weight         598.66
_chemical_name_common            '[(Cp*)ScMe]3(CH)'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   direct
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   19.1878(9)
_cell_length_b                   19.1878(9)
_cell_length_c                   15.6298(14)
_cell_measurement_reflns_used    9958
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      30.45
_cell_measurement_theta_min      2.78
_cell_volume                     4983.5(6)
_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    'SIR-92 (Altomare et al., 1994)'
_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  0.0660
_diffrn_reflns_av_unetI/netI     0.0183
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            52107
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        24.983
_diffrn_reflns_theta_max         24.983
_diffrn_reflns_theta_min         2.123
_exptl_absorpt_coefficient_mu    0.615
_exptl_absorpt_correction_T_max  0.935
_exptl_absorpt_correction_T_min  0.909
_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    1.197
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1932
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: benzene'
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.110
_refine_diff_density_max         0.471
_refine_diff_density_min         -0.422
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     126
_refine_ls_number_reflns         1941
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0410
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0551P)²+22.9996P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1118
_refine_ls_wR_factor_ref         0.1176
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1732
_reflns_number_total             1941
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1cc01645h2.cif
_cod_data_source_block           Deng02-2020
_cod_depositor_comments
'Adding full bibliography for 7128441--7128448.cif.'
_cod_database_code               7128447
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;

The symmetry employed for this shelxl refinement is uniquely defined

by the following loop, which should always be used as a source of

symmetry information in preference to the above space-group names.

They are only intended as comments.

;
_shelx_estimated_absorpt_t_min   0.903
_shelx_estimated_absorpt_t_max   0.935
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.000000 0.000000 0.2200(3) 0.0209(9) Uani 1 3 d S T P . .
C2 C 0.03453(18) 0.12098(18) 0.38421(18) 0.0266(6) Uani 1 1 d . . . . .
C10 C 0.20122(15) 0.21060(15) 0.24434(17) 0.0254(6) Uani 1 1 d . . . . .
C11 C 0.23681(15) 0.19672(16) 0.31662(17) 0.0263(6) Uani 1 1 d . . . . .
C12 C 0.25259(15) 0.13388(16) 0.29589(18) 0.0282(6) Uani 1 1 d . . . . .
C13 C 0.19462(16) 0.15663(16) 0.17889(17) 0.0272(6) Uani 1 1 d . . . . .
C14 C 0.22647(16) 0.10902(16) 0.21077(18) 0.0288(6) Uani 1 1 d . . . . .
C15 C 0.23579(19) 0.04675(19) 0.1613(2) 0.0411(8) Uani 1 1 d . . . . .
H15A H 0.212652 0.040884 0.104013 0.062 Uiso 1 1 calc R U . . .
H15B H 0.293039 0.063818 0.156267 0.062 Uiso 1 1 calc R U . . .
H15C H 0.207720 -0.004949 0.191316 0.062 Uiso 1 1 calc R U . . .
C16 C 0.29553(18) 0.1043(2) 0.3533(2) 0.0439(8) Uani 1 1 d . . . . .
H16A H 0.306390 0.131746 0.408706 0.066 Uiso 1 1 calc R U . . .
H16B H 0.261666 0.046156 0.361825 0.066 Uiso 1 1 calc R U . . .
H16C H 0.346460 0.115854 0.326708 0.066 Uiso 1 1 calc R U . . .
C17 C 0.25797(19) 0.24325(19) 0.3994(2) 0.0383(7) Uani 1 1 d . . . . .
H17A H 0.281898 0.221437 0.438942 0.057 Uiso 1 1 calc R U . . .
H17B H 0.296601 0.300035 0.388059 0.057 Uiso 1 1 calc R U . . .
H17C H 0.209152 0.238520 0.424972 0.057 Uiso 1 1 calc R U . . .
C18 C 0.17791(19) 0.27483(18) 0.2376(2) 0.0362(7) Uani 1 1 d . . . . .
H18A H 0.154449 0.272040 0.181162 0.054 Uiso 1 1 calc R U . . .
H18B H 0.138362 0.266210 0.282076 0.054 Uiso 1 1 calc R U . . .
H18C H 0.225807 0.327920 0.245295 0.054 Uiso 1 1 calc R U . . .
C19 C 0.1619(2) 0.1524(2) 0.09010(18) 0.0393(7) Uani 1 1 d . . . . .
H19A H 0.164005 0.109862 0.057520 0.059 Uiso 1 1 calc R U . . .
H19B H 0.105999 0.140452 0.093966 0.059 Uiso 1 1 calc R U . . .
H19C H 0.194402 0.204146 0.061144 0.059 Uiso 1 1 calc R U . . .
Sc1 Sc 0.10417(3) 0.07355(3) 0.29486(3) 0.01930(19) Uani 1 1 d . . . . .
H1 H 0.000000 0.000000 0.158(4) 0.051(18) Uiso 1 3 d S . P . .
H2A H -0.006(3) 0.103(2) 0.424(3) 0.058(11) Uiso 1 1 d . . . . .
H2B H 0.041(3) 0.173(3) 0.374(3) 0.082(15) Uiso 1 1 d . . . . .
H2C H 0.079(3) 0.134(3) 0.416(3) 0.069(13) Uiso 1 1 d . . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sc Sc 0.2519 0.3716 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Sc1 C1 Sc1 92.69(13) 2 3 ?
Sc1 C1 Sc1 92.69(13) 2 . ?
Sc1 C1 Sc1 92.69(13) 3 . ?
Sc1 C1 H1 123.34(10) 2 . ?
Sc1 C1 H1 123.34(10) 3 . ?
Sc1 C1 H1 123.34(10) . . ?
Sc1 C2 Sc1 80.22(9) 2 . ?
Sc1 C2 H2A 82(2) 2 . ?
Sc1 C2 H2A 141(2) . . ?
Sc1 C2 H2B 106(3) 2 . ?
Sc1 C2 H2B 120(3) . . ?
H2A C2 H2B 99(4) . . ?
Sc1 C2 H2C 151(3) 2 . ?
Sc1 C2 H2C 78(3) . . ?
H2A C2 H2C 104(4) . . ?
H2B C2 H2C 101(4) . . ?
C11 C10 C13 108.4(2) . . ?
C11 C10 C18 125.3(3) . . ?
C13 C10 C18 126.3(3) . . ?
C11 C10 Sc1 73.85(14) . . ?
C13 C10 Sc1 73.04(14) . . ?
C18 C10 Sc1 121.16(18) . . ?
C10 C11 C12 107.8(2) . . ?
C10 C11 C17 125.9(3) . . ?
C12 C11 C17 126.2(3) . . ?
C10 C11 Sc1 73.01(14) . . ?
C12 C11 Sc1 73.30(15) . . ?
C17 C11 Sc1 121.71(18) . . ?
C14 C12 C11 108.1(2) . . ?
C14 C12 C16 126.9(3) . . ?
C11 C12 C16 124.9(3) . . ?
C14 C12 Sc1 72.94(15) . . ?
C11 C12 Sc1 73.45(15) . . ?
C16 C12 Sc1 122.96(19) . . ?
C10 C13 C14 107.9(2) . . ?
C10 C13 C19 125.9(3) . . ?
C14 C13 C19 126.1(3) . . ?
C10 C13 Sc1 73.63(14) . . ?
C14 C13 Sc1 73.50(15) . . ?
C19 C13 Sc1 120.15(18) . . ?
C12 C14 C13 107.8(2) . . ?
C12 C14 C15 125.9(3) . . ?
C13 C14 C15 126.1(3) . . ?
C12 C14 Sc1 73.78(15) . . ?
C13 C14 Sc1 73.06(15) . . ?
C15 C14 Sc1 121.85(18) . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C12 C16 H16A 109.5 . . ?
C12 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C12 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C11 C17 H17A 109.5 . . ?
C11 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C11 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C10 C18 H18A 109.5 . . ?
C10 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C10 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C13 C19 H19A 109.5 . . ?
C13 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C13 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C1 Sc1 C2 93.86(9) . 3 ?
C1 Sc1 C2 93.15(9) . . ?
C2 Sc1 C2 97.17(15) 3 . ?
C1 Sc1 C13 98.54(12) . . ?
C2 Sc1 C13 138.00(10) 3 . ?
C2 Sc1 C13 121.82(10) . . ?
C1 Sc1 C14 109.74(11) . . ?
C2 Sc1 C14 104.74(10) 3 . ?
C2 Sc1 C14 146.73(10) . . ?
C13 Sc1 C14 33.44(10) . . ?
C1 Sc1 C10 119.18(10) . . ?
C2 Sc1 C10 144.90(10) 3 . ?
C2 Sc1 C10 92.78(10) . . ?
C13 Sc1 C10 33.33(9) . . ?
C14 Sc1 C10 55.27(9) . . ?
C1 Sc1 C12 142.27(11) . . ?
C2 Sc1 C12 91.91(10) 3 . ?
C2 Sc1 C12 123.04(10) . . ?
C13 Sc1 C12 55.25(9) . . ?
C14 Sc1 C12 33.28(9) . . ?
C10 Sc1 C12 55.06(9) . . ?
C1 Sc1 C11 151.86(11) . . ?
C2 Sc1 C11 112.40(10) 3 . ?
C2 Sc1 C11 93.40(10) . . ?
C13 Sc1 C11 55.23(9) . . ?
C14 Sc1 C11 55.26(9) . . ?
C10 Sc1 C11 33.13(9) . . ?
C12 Sc1 C11 33.24(9) . . ?
C1 Sc1 Sc1 43.66(7) . 3 ?
C2 Sc1 Sc1 50.25(7) 3 3 ?
C2 Sc1 Sc1 95.80(7) . 3 ?
C13 Sc1 Sc1 130.23(6) . 3 ?
C14 Sc1 Sc1 117.45(7) . 3 ?
C10 Sc1 Sc1 161.12(6) . 3 ?
C12 Sc1 Sc1 130.46(7) . 3 ?
C11 Sc1 Sc1 161.27(7) . 3 ?
C1 Sc1 Sc1 43.65(7) . 2 ?
C2 Sc1 Sc1 96.33(7) 3 2 ?
C2 Sc1 Sc1 49.54(7) . 2 ?
C13 Sc1 Sc1 120.01(7) . 2 ?
C14 Sc1 Sc1 147.73(7) . 2 ?
C10 Sc1 Sc1 115.38(7) . 2 ?
C12 Sc1 Sc1 169.54(7) . 2 ?
C11 Sc1 Sc1 136.47(7) . 2 ?
Sc1 Sc1 Sc1 60.0 3 2 ?
C1 Sc1 H2C 114.0(12) . . ?
C2 Sc1 H2C 89.0(10) 3 . ?
C2 Sc1 H2C 21.9(11) . . ?
C13 Sc1 H2C 121.1(10) . . ?
C14 Sc1 H2C 133.0(11) . . ?
C10 Sc1 H2C 87.9(10) . . ?
C12 Sc1 H2C 103.3(11) . . ?
C11 Sc1 H2C 77.8(11) . . ?
Sc1 Sc1 H2C 106.0(11) 3 . ?
Sc1 Sc1 H2C 70.5(12) 2 . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 Sc1 2.130(2) 2 ?
C1 Sc1 2.130(2) 3 ?
C1 Sc1 2.130(2) . ?
C1 H1 0.97(7) . ?
C2 Sc1 2.379(3) 2 ?
C2 Sc1 2.404(3) . ?
C2 H2A 0.93(4) . ?
C2 H2B 0.95(5) . ?
C2 H2C 0.91(5) . ?
C10 C11 1.413(4) . ?
C10 C13 1.416(4) . ?
C10 C18 1.510(4) . ?
C10 Sc1 2.472(3) . ?
C11 C12 1.420(4) . ?
C11 C17 1.508(4) . ?
C11 Sc1 2.483(3) . ?
C12 C14 1.418(4) . ?
C12 C16 1.508(4) . ?
C12 Sc1 2.481(3) . ?
C13 C14 1.419(4) . ?
C13 C19 1.509(4) . ?
C13 Sc1 2.464(3) . ?
C14 C15 1.507(4) . ?
C14 Sc1 2.470(3) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
Sc1 Sc1 3.0819(8) 3 ?
Sc1 Sc1 3.0820(8) 2 ?
Sc1 H2C 2.38(4) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C13 C10 C11 C12 0.1(3) . . . . ?
C18 C10 C11 C12 -177.4(2) . . . . ?
Sc1 C10 C11 C12 65.56(18) . . . . ?
C13 C10 C11 C17 177.4(3) . . . . ?
C18 C10 C11 C17 -0.2(4) . . . . ?
Sc1 C10 C11 C17 -117.2(3) . . . . ?
C13 C10 C11 Sc1 -65.42(18) . . . . ?
C18 C10 C11 Sc1 117.1(3) . . . . ?
C10 C11 C12 C14 -0.1(3) . . . . ?
C17 C11 C12 C14 -177.3(3) . . . . ?
Sc1 C11 C12 C14 65.23(18) . . . . ?
C10 C11 C12 C16 175.6(2) . . . . ?
C17 C11 C12 C16 -1.6(4) . . . . ?
Sc1 C11 C12 C16 -119.0(3) . . . . ?
C10 C11 C12 Sc1 -65.37(18) . . . . ?
C17 C11 C12 Sc1 117.4(3) . . . . ?
C11 C10 C13 C14 -0.1(3) . . . . ?
C18 C10 C13 C14 177.4(3) . . . . ?
Sc1 C10 C13 C14 -66.05(18) . . . . ?
C11 C10 C13 C19 -178.4(3) . . . . ?
C18 C10 C13 C19 -0.9(4) . . . . ?
Sc1 C10 C13 C19 115.7(3) . . . . ?
C11 C10 C13 Sc1 65.95(18) . . . . ?
C18 C10 C13 Sc1 -116.6(3) . . . . ?
C11 C12 C14 C13 0.1(3) . . . . ?
C16 C12 C14 C13 -175.6(3) . . . . ?
Sc1 C12 C14 C13 65.64(18) . . . . ?
C11 C12 C14 C15 176.5(3) . . . . ?
C16 C12 C14 C15 0.9(4) . . . . ?
Sc1 C12 C14 C15 -117.9(3) . . . . ?
C11 C12 C14 Sc1 -65.57(18) . . . . ?
C16 C12 C14 Sc1 118.8(3) . . . . ?
C10 C13 C14 C12 0.0(3) . . . . ?
C19 C13 C14 C12 178.3(3) . . . . ?
Sc1 C13 C14 C12 -66.12(18) . . . . ?
C10 C13 C14 C15 -176.4(3) . . . . ?
C19 C13 C14 C15 1.8(4) . . . . ?
Sc1 C13 C14 C15 117.4(3) . . . . ?
C10 C13 C14 Sc1 66.14(18) . . . . ?
C19 C13 C14 Sc1 -115.6(3) . . . . ?
