Synthesis of novel chiral heterometallic terpene oximates: unusual generation of an aluminium enolate by a cooperative effect.
Fernández-Millán, María; Temprado, Manuel; Cano, Jesús; Cuenca, Tomás; Mosquera, Marta E. G.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 10514–10518; doi:10.1039/c6dt02116f

data_7039549
_publ_section_title
;
 Synthesis of novel chiral heterometallic terpene oximates: unusual
 generation of an aluminium enolate by a cooperative effect.
;
_journal_issue                   26
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10514
_journal_page_last               10518
_journal_paper_doi               10.1039/c6dt02116f
_journal_volume                  45
_journal_year                    2016
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C52 H77 Al2 K2 N4 O2.C6 D6'
_chemical_formula_sum            'C58 H77 Al2 D6 K2 N4 O2'
_chemical_formula_weight         1006.48
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-03-22 deposited with the CCDC.
2016-06-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   32.214(11)
_cell_length_b                   11.964(8)
_cell_length_c                   15.575(14)
_cell_measurement_reflns_used    22
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      16.076
_cell_measurement_theta_min      2.986
_cell_volume                     6003(7)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      200
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1692
_diffrn_reflns_av_unetI/netI     0.1432
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            92427
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        19.997
_diffrn_reflns_theta_max         19.997
_diffrn_reflns_theta_min         3.049
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.228
_exptl_absorpt_correction_T_max  1.093
_exptl_absorpt_correction_T_min  0.942
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.114
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2156
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.15
_platon_squeeze_details
;
 A molecule of deuterated benzene crystallized with every molecule of this 
 compound but presented severe disorder and it was not possible to get a 
 chemical sensible model for it, so Squeeze procedure was used to remove 
 their contribution to the structure factors.
;
_refine_diff_density_max         0.323
_refine_diff_density_min         -0.281
_refine_diff_density_rms         0.065
_refine_ls_abs_structure_details
;
 Flack x determined using 872 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.02(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     549
_refine_ls_number_reflns         5580
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.1572
_refine_ls_R_factor_gt           0.0998
_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^)+(0.1452P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2245
_refine_ls_wR_factor_ref         0.2563
_reflns_Friedel_coverage         0.767
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                3230
_reflns_number_total             5580
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02116f2.cif
_cod_data_source_block           1R4S_1a
_cod_depositor_comments
'Adding full bibliography for 7039548--7039551.cif.'
_cod_database_code               7039549
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              74648