The Nature of Secondary Interactions at Electrophilic Metal Sites of Molecular and Silica-Supported Organolutetium Complexes from Solid-State NMR Spectroscopy.
Conley, Matthew P.; Lapadula, Giuseppe; Sanders, Kevin; Gajan, David; Lesage, Anne; Del Rosal, Iker; Maron, Laurent; Lukens, Wayne W.; Copéret, Christophe; Andersen, Richard A.; Journal of the American Chemical Society 138 (2016) 3831–3843; doi:10.1021/jacs.6b00071

data_4124938
_publ_section_title
;
 The Nature of Secondary Interactions at Electrophilic Metal Sites of
 Molecular and Silica-Supported Organolutetium Complexes from Solid-State
 NMR Spectroscopy.
;
_journal_issue                   11
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3831
_journal_page_last               3843
_journal_paper_doi               10.1021/jacs.6b00071
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         'C21 H57 Lu1 Si6, C3 Si0.74'
_chemical_formula_sum            'C24 H57 Lu Si6.73'
_chemical_formula_weight         709.85
_space_group_crystal_system      trigonal
_space_group_IT_number           159
_space_group_name_Hall           'P 3 -2c'
_space_group_name_H-M_alt        'P 3 1 c'
_symmetry_space_group_name_Hall  'P 3 -2c'
_symmetry_space_group_name_H-M   'P 3 1 c'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     heavy
_audit_creation_date             2015-03-25
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Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
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_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   16.1659(3)
_cell_length_b                   16.1659(3)
_cell_length_c                   8.57041(16)
_cell_measurement_reflns_used    14565
_cell_measurement_temperature    100
_cell_measurement_theta_max      37.5079
_cell_measurement_theta_min      2.9041
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_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
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_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
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_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 16.0839
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_details
;
  1 omega -107.00  -20.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.9735  -57.0000  -60.0000 87

  2 omega   22.00  115.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       38.5985 -164.0000  -32.0000 93

  3 omega  -16.00   -5.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       38.5985  -99.0000   60.0000 11

  4 omega   54.00  107.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       38.5985   57.0000   90.0000 53

  5 omega   13.00  108.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       38.5985   38.0000 -150.0000 95

  6 omega -108.00   -8.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.9735  -77.0000   30.0000 100

  7 omega   46.00   98.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       38.5985  165.0000 -147.0000 52
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0468104000
_diffrn_orient_matrix_UB_12      -0.0366477000
_diffrn_orient_matrix_UB_13      -0.0194736000
_diffrn_orient_matrix_UB_21      -0.0177813000
_diffrn_orient_matrix_UB_22      0.0099123000
_diffrn_orient_matrix_UB_23      0.0689558000
_diffrn_orient_matrix_UB_31      -0.0076016000
_diffrn_orient_matrix_UB_32      0.0335666000
_diffrn_orient_matrix_UB_33      -0.0414665000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0304
_diffrn_reflns_av_unetI/netI     0.0245
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            31730
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         37.597
_diffrn_reflns_theta_min         2.910
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.763
_exptl_absorpt_correction_T_max  0.841
_exptl_absorpt_correction_T_min  0.257
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
Analytical numeric absorption correction using a multifaceted crystal
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(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.215
_exptl_crystal_description       plate
_exptl_crystal_F_000             733
_exptl_crystal_size_max          1.7202
_exptl_crystal_size_mid          0.7231
_exptl_crystal_size_min          0.1314
_refine_diff_density_max         1.360
_refine_diff_density_min         -1.897
_refine_diff_density_rms         0.083
_refine_ls_abs_structure_details
;
 Flack x determined using 2880 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.130(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     174
_refine_ls_number_reflns         6518
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0277
_refine_ls_R_factor_gt           0.0252
_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^)+(0.0273P)^2^+0.5594P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0550
_refine_ls_wR_factor_ref         0.0558
_reflns_Friedel_coverage         0.940
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.922
_reflns_number_gt                6242
_reflns_number_total             6518
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b00071_si_001.cif
_cod_data_source_block           mpclu
_cod_depositor_comments
'Adding full bibliography for 4124937--4124939.cif.'
_cod_original_cell_volume        1939.69(8)
_cod_database_code               4124938
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         'Lu C10 N10 H30 Si3'
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     36.23
_olex2_refinement_description
;
;
_olex2_submission_special_instructions 'No special instructions were received'