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_1546744
_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         'C11 H22 Cl2 N O2 S2 Sc'
_chemical_formula_sum            'C11 H22 Cl2 N O2 S2 Sc'
_chemical_formula_weight         380.27
_chemical_name_systematic
;
 ?
;
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_block_doi                 10.5517/ccdc.csd.cc1mzndn
_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                90
_cell_angle_beta                 101.302(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.6252(3)
_cell_length_b                   17.9614(5)
_cell_length_c                   12.5733(4)
_cell_measurement_reflns_used    10274
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      30.2190
_cell_measurement_theta_min      3.4920
_cell_volume                     1688.64(10)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector_area_resol_mean 10.3914
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -15.00   86.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       13.6191   77.0000  -90.0000 101

  2 omega  -13.00   84.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       13.6191   42.0000 -176.0000 97

  3 omega  -60.00   42.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       13.6191  -57.0000  150.0000 102

  4 omega  -60.00   43.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       13.6191  -57.0000   30.0000 103

  5 omega  -13.00   89.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       13.6191   38.0000   90.0000 102

  6 omega    3.00   72.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       13.6191 -126.0000  -27.5811 69
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0430905000
_diffrn_orient_matrix_UB_12      -0.0061789000
_diffrn_orient_matrix_UB_13      -0.0545706000
_diffrn_orient_matrix_UB_21      0.0690355000
_diffrn_orient_matrix_UB_22      0.0198260000
_diffrn_orient_matrix_UB_23      -0.0181402000
_diffrn_orient_matrix_UB_31      0.0486616000
_diffrn_orient_matrix_UB_32      -0.0336189000
_diffrn_orient_matrix_UB_33      -0.0006843000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0422
_diffrn_reflns_av_unetI/netI     0.0242
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            21950
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.020
_diffrn_reflns_theta_min         2.806
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.996
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63646
_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_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_description       block
_exptl_crystal_F_000             792
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.314
_refine_diff_density_min         -0.295
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     174
_refine_ls_number_reflns         3333
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0333
_refine_ls_R_factor_gt           0.0250
_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^)+(0.0280P)^2^+0.8590P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0597
_refine_ls_wR_factor_ref         0.0649
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2846
_reflns_number_total             3333
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc02018j2.cif
_cod_data_source_block           exp_8027
_cod_original_cell_volume        1688.64(9)
_cod_database_code               1546744
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         'C1 H1 Si1 Sc1 N1 Cl1 S1 Li1'
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C8(H8A,H8B), C11(H11A,H11B), C7(H7A,H7B), C9(H9A,H9B), C6(H6A,
 H6B), C5(H5A,H5B), C10(H10A,H10B)
2.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C)
;
_olex2_submission_special_instructions 'No special instructions were received'