Formation and Ligand-Based Reductivity of Bridged Bis-alkylidene Scandium(III) Complexes
Ma, Wangyang; yu, chao; Chi, Yue; Chen, Tianyang; Wang, Lianjun; Yin, Jianhao; Wei, Baosheng; Xu, Ling; Zhang, Wen-Xiong; Xi, Zhenfeng; Chem. Sci.  (2017) –; doi:10.1039/C7SC02018J

data_1546745
_publ_section_title
;
 Formation and Ligand-Based Reductivity of Bridged Bis-alkylidene
 Scandium(III) Complexes
;
_journal_name_full               'Chem. Sci.'
_journal_paper_doi               10.1039/C7SC02018J
_journal_year                    2017
_chemical_formula_moiety         'C38 H60 Cl2 Li O4 Sc Si2'
_chemical_formula_sum            'C38 H60 Cl2 Li O4 Sc Si2'
_chemical_formula_weight         759.84
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_block_doi                 10.5517/ccdc.csd.cc1mh90f
_audit_creation_date             2016-12-03
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-12-05 deposited with the CCDC.
2017-07-31 downloaded from the CCDC.
;
_cell_angle_alpha                89.102(12)
_cell_angle_beta                 69.720(16)
_cell_angle_gamma                89.532(10)
_cell_formula_units_Z            2
_cell_length_a                   12.5970(16)
_cell_length_b                   13.4393(15)
_cell_length_c                   15.161(3)
_cell_measurement_reflns_used    1784
_cell_measurement_temperature    180.01(10)
_cell_measurement_theta_max      23.4210
_cell_measurement_theta_min      3.0060
_cell_volume                     2407.3(7)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      180.01(10)
_diffrn_detector_area_resol_mean 10.3914
_diffrn_measured_fraction_theta_full 0.884
_diffrn_measured_fraction_theta_max 0.908
_diffrn_measurement_details
;
  1 omega  -63.00   30.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       10.7017  -57.0000  150.0000 93

  2 omega  -15.00   88.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       10.7017   77.0000  -90.0000 103

  3 omega  -78.00   18.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.7954  -57.0000    0.0000 96
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0219227000
_diffrn_orient_matrix_UB_12      0.0455003000
_diffrn_orient_matrix_UB_13      0.0093758000
_diffrn_orient_matrix_UB_21      0.0302873000
_diffrn_orient_matrix_UB_22      -0.0263917000
_diffrn_orient_matrix_UB_23      0.0246188000
_diffrn_orient_matrix_UB_31      0.0469628000
_diffrn_orient_matrix_UB_32      -0.0044224000
_diffrn_orient_matrix_UB_33      -0.0423448000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.2377
_diffrn_reflns_Laue_measured_fraction_full 0.884
_diffrn_reflns_Laue_measured_fraction_max 0.908
_diffrn_reflns_point_group_measured_fraction_full 0.884
_diffrn_reflns_point_group_measured_fraction_max 0.908
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.025
_diffrn_reflns_theta_min         3.013
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.344
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.01423
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.048
_exptl_crystal_F_000             812
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.470
_refine_diff_density_min         -0.291
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.852
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     439
_refine_ls_number_reflns         7687
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.852
_refine_ls_R_factor_all          0.1991
_refine_ls_R_factor_gt           0.0878
_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/[\s^2^(Fo^2^)+(0.0400P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1534
_refine_ls_wR_factor_ref         0.1937
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3006
_reflns_number_total             7687
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc02018j2.cif
_cod_data_source_block           exp_6852-sr
_cod_database_code               1546745
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         'Sc Si C H Cl Li'
_shelx_estimated_absorpt_t_max   0.966
_shelx_estimated_absorpt_t_min   0.950
_reflns_odcompleteness_completeness 99.67
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,
 H27B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B),
 C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B),
  C37(H37A,H37B), C38(H38A,H38B)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C12(H12), C13(H13), C14(H14),
 C15(H15), C16(H16)
2.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,
 H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C)
;
_olex2_submission_special_instructions 'No special instructions were received'