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_1546746
_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         'C12 H18 Cl O2 Sc'
_chemical_formula_sum            'C12 H18 Cl O2 Sc'
_chemical_formula_weight         274.67
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yac'
_space_group_name_H-M_alt        'P 1 n 1'
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_space_group_name_H-M   'P 1 n 1'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/ccdc.csd.cc1np08m
_audit_creation_date             2017-03-10
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_audit_update_record
;
2017-03-22 deposited with the CCDC.
2017-07-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.433(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.0301(3)
_cell_length_b                   10.1171(5)
_cell_length_c                   9.2007(4)
_cell_measurement_reflns_used    8456
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      30.3630
_cell_measurement_theta_min      4.0280
_cell_volume                     641.41(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.7e (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.7e (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.7e (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -34.00  25.00   0.50    0.71    --    1.40 -38.00 -60.00  118
  2  \w      1.00  35.00   0.50    0.71    --    1.40 -82.00  30.00   68
  3  \w      3.00  35.00   0.50    0.71    --    1.40 -80.00 155.76   64
  4  \w    -33.00  -8.00   0.50    0.71    --    1.40 -80.00 155.76   50
  5  \w    -85.00  31.00   0.50    0.71    --    1.40 -24.00  25.20  232
  6  \w    -18.00  33.00   0.50    0.71    --    1.40 -77.00-180.00  102
  7  \w    -43.00  27.00   0.50    0.71    --    1.40 -57.00 -90.00  140
  8  \w    -87.00  25.00   0.50    0.71    --    1.40 -41.00-156.74  224
  9  \w    -87.00 -53.00   0.50    0.71    --    1.40 -38.00 -60.00   68
 10  \w    -88.00  31.00   0.50    0.71    --    1.40 -23.00 114.37  238
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Pro: Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0616897000
_diffrn_orient_matrix_UB_12      -0.0408376000
_diffrn_orient_matrix_UB_13      -0.0516225000
_diffrn_orient_matrix_UB_21      0.0539472000
_diffrn_orient_matrix_UB_22      -0.0563409000
_diffrn_orient_matrix_UB_23      0.0298298000
_diffrn_orient_matrix_UB_31      -0.0622701000
_diffrn_orient_matrix_UB_32      -0.0085889000
_diffrn_orient_matrix_UB_33      0.0512923000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0430
_diffrn_reflns_av_unetI/netI     0.0288
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            14657
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.017
_diffrn_reflns_theta_min         3.906
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.765
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88786
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.7e (Rigaku Oxford Diffraction, 2015)
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    1.422
_exptl_crystal_description       block
_exptl_crystal_F_000             288
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.718
_refine_diff_density_min         -0.614
_refine_diff_density_rms         0.086
_refine_ls_abs_structure_details
;
 Flack x determined using 1189 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.037(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     147
_refine_ls_number_reflns         2510
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0407
_refine_ls_R_factor_gt           0.0400
_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^)+(0.0655P)^2^+0.9477P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1167
_refine_ls_wR_factor_ref         0.1173
_reflns_Friedel_coverage         0.975
_reflns_Friedel_fraction_full    0.981
_reflns_Friedel_fraction_max     0.981
_reflns_number_gt                2462
_reflns_number_total             2510
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc02018j2.cif
_cod_data_source_block           7
_cod_database_code               1546746
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         'c H O Sc Si Li Cl'
_shelx_estimated_absorpt_t_max   0.914
_shelx_estimated_absorpt_t_min   0.894
_reflns_odcompleteness_completeness 99.61
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_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 Ternary CH refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8)
2.b Secondary CH2 refined with riding coordinates:
 C10(H10a,H10b), C11(H11a,H11b)
2.c Idealised Me refined as rotating group:
 C9(H9a,H9b,H9c), C12(H12a,H12b,H12c)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.311
_oxdiff_exptl_absorpt_empirical_full_min 0.719