Selective Mono- and Dimetallation of a Group 3 Sandwich Complex
Martinez-Martinez, Antonio J.; Kennedy, Alan; Paprocki, Valerie; Fantuzzi, Felipe; Dewhurst, Rian David; O'Hara, Charles T.; Braunschweig, Holger; Mulvey, Robert E.; Chemical Communications  (2019) –; doi:10.1039/C9CC03825F

data_7123893
_publ_section_title
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 Selective Mono- and Dimetallation of a Group 3 Sandwich Complex
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_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC03825F
_journal_year                    2019
_chemical_formula_moiety         'C34 H56 Al Li N O Sc'
_chemical_formula_sum            'C34 H56 Al Li N O Sc'
_chemical_formula_weight         573.67
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_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
_audit_creation_method           SHELXL-2014/7
_audit_update_record
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2019-06-12 deposited with the CCDC.    2019-07-19 downloaded from the CCDC.
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_cell_angle_alpha                90.0
_cell_angle_beta                 97.9689(14)
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   11.11866(14)
_cell_length_b                   15.1374(2)
_cell_length_c                   19.5596(3)
_cell_measurement_reflns_used    8973
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      73.1030
_cell_measurement_theta_min      3.7000
_cell_volume                     3260.24(8)
_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
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_av_unetI/netI     0.0481
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            22387
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        70.000
_diffrn_reflns_theta_max         73.428
_diffrn_reflns_theta_min         3.706
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    2.367
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65221
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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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            'pale yellow'
_exptl_crystal_density_diffrn    1.169
_exptl_crystal_description       block
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.347
_refine_diff_density_min         -0.294
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         22387
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0565
_refine_ls_R_factor_gt           0.0463
_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^)+(0.0596P)^2^+1.6419P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1175
_refine_ls_wR_factor_ref         0.1266
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19031
_reflns_number_total             22387
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc03825f2.cif
_cod_data_source_block           ame73smarthklf5
_cod_original_cell_volume        3260.26(8)
_cod_database_code               7123893
_shelx_shelxl_version_number     2014/7
_exptl_absorpt_special_details
;

Once refined ROTEX suggested that the data was twinned by a 
180 degree rotation about 1 0 0. 
Applying the matrix 1 0 0 0 -1 0 -0.487 0 -1 gave an hklf 5 
formatted reflection file and refinement against this 
modified data improved R (-2%) and residual Q peaks (-40%). 
BASF refined to 0.0908(9).

The HKLF 5 card forces MERG 0, i.e. neither a number of unique reflections
nor an internal R value can be determined. The figures given here are taken
from an HKLF 4 file
 in the integration which led to this file the twinning
was ignored. Hence these figures are approximations.

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_shelx_res_checksum              63156