Deprotonation, insertion and isomerisation in the post-functionalisation of tris-pyridyl aluminates.
Plajer, Alex J.; Kopf, Sara; Colebatch, Annie L.; Bond, Andrew D.; Wright, Dominic S.; García-Rodríguez, Raúl; Dalton transactions (Cambridge, England : 2003) 48 (2019) 5692–5697; doi:10.1039/c9dt00869a

data_7049507
_publ_section_title
;
 Deprotonation, insertion and isomerisation in the post-functionalisation
 of tris-pyridyl aluminates.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5692
_journal_page_last               5697
_journal_paper_doi               10.1039/c9dt00869a
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C54 H58 Li2 N6 O2 Al2, 4(C7 H8)'
_chemical_formula_sum            'C82 H90 Al2 Li2 N6 O2'
_chemical_formula_weight         1259.43
_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
_audit_creation_method           SHELXL-2018/1
_audit_update_record
;
2019-02-15 deposited with the CCDC.    2019-03-26 downloaded from the CCDC.
;
_cell_angle_alpha                72.5308(19)
_cell_angle_beta                 75.6187(18)
_cell_angle_gamma                68.8699(16)
_cell_formula_units_Z            1
_cell_length_a                   10.7764(4)
_cell_length_b                   11.6195(4)
_cell_length_c                   15.5555(6)
_cell_measurement_reflns_used    9812
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      66.82
_cell_measurement_theta_min      3.02
_cell_volume                     1711.41(11)
_computing_cell_refinement       'SAINT (Bruker, 2016)'
_computing_data_collection       'APEX3 (Bruker, 2016)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
_computing_publication_material  SHELXL
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker D8-QUEST PHOTON-100'
_diffrn_measurement_method       '\w and \f-scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0585
_diffrn_reflns_av_unetI/netI     0.0380
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            34421
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        66.993
_diffrn_reflns_theta_max         66.993
_diffrn_reflns_theta_min         3.016
_diffrn_source                   'Incoatec I\mS Cu microsource'
_exptl_absorpt_coefficient_mu    0.790
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.5477
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.222
_exptl_crystal_description       lath
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.080
_platon_squeeze_details
;
The data prior to SQUEEZE indicate two toluene sites per asymmetric unit
(= four per unit cell). These occupy layers in the ab planes and there must
be alternative orientations for these layers relative to the layers of
complexes. The diffraction pattern shows clear streaking along c* indicative
of layer stacking disorder. It also shows possible modulation peaks in the 
hk planes, but interpretation of these was not attempted. This could be an 
interesting system for further study, but we were interested solely in the
chemical interpretation (which is clear).
;
_refine_diff_density_max         0.380
_refine_diff_density_min         -0.251
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     302
_refine_ls_number_reflns         5992
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0667
_refine_ls_R_factor_gt           0.0563
_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^)+(0.0687P)^2^+1.3001P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1466
_refine_ls_wR_factor_ref         0.1550
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4995
_reflns_number_total             5992
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00869a2.cif
_cod_data_source_block           DW_B2_0295_sq
_cod_depositor_comments
'Adding full bibliography for 7049506--7049509.cif.'
_cod_database_code               7049507
_cambridge_user_name             'Alex Plajer'
_cambridge_user_crsid            ajp233
_cambridge_supervisor_name       'Dominic Wright'
_cambridge_supervisor_crsid      dsw1000
_cambridge_crystallographer_name 'Andrew Bond'
_cambridge_crystallographer_crsid adb29
_cambridge_sample_id             AP-4
_cambridge_data_id               DW_B2_0295
_shelx_estimated_absorpt_t_min   0.827
_shelx_estimated_absorpt_t_max   0.939
_shelx_res_checksum              91659
_shelx_hkl_checksum              84245
_shelx_fab_checksum              38051
_platon_squeeze_void_probe_radius 1.20