Formation of a Heterometallic AlIII/SmIIIComplex Involving a Novel [EtAl(2-py)2O]2–Ligand (2-py = 2-Pyridyl)
García-Rodríguez, Raúl; Simmonds, Hayley R.; Wright, Dominic S.; Organometallics 33 (2014) 7113–; doi:10.1021/om5009132

data_4084772
_publ_section_title
;
 Formation of a Heterometallic AlIII/SmIIIComplex Involving a Novel
 [EtAl(2-py)2O]2--Ligand (2-py = 2-Pyridyl)
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              7113
_journal_paper_doi               10.1021/om5009132
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C54 H52 Al4 N10 O2 Sm2,4(C4 H8 O)'
_chemical_formula_sum            'C70 H84 Al4 N10 O6 Sm2'
_chemical_formula_weight         1570.09
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                105.8620(10)
_cell_angle_beta                 94.2120(10)
_cell_angle_gamma                118.2890(10)
_cell_formula_units_Z            1
_cell_length_a                   12.73690(10)
_cell_length_b                   13.0219(2)
_cell_length_c                   13.3823(3)
_cell_measurement_reflns_used    15231
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      32.03
_cell_measurement_theta_min      1.00
_cell_volume                     1825.28(6)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius B.V. 1998)'
_computing_data_reduction
;
 HKL Denzo and Scalepack (Otwinowski & Minor 1997)
;
_computing_publication_material  'SHELXL-97 (Sheldrick 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick 1997)'
_computing_structure_solution    'SIR-92 (Altomare et al. 1994)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'Thin slice \w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0547
_diffrn_reflns_av_sigmaI/netI    0.0784
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            25758
_diffrn_reflns_theta_full        32.00
_diffrn_reflns_theta_max         32.00
_diffrn_reflns_theta_min         3.56
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.696
_exptl_absorpt_correction_T_max  0.970
_exptl_absorpt_correction_T_min  0.834
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.428
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             798
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.914
_refine_diff_density_min         -0.923
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     405
_refine_ls_number_reflns         12480
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0595
_refine_ls_R_factor_gt           0.0381
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0385P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0848
_refine_ls_wR_factor_ref         0.0915
_reflns_number_gt                9293
_reflns_number_total             12480
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5009132_si_002.cif
_cod_data_source_block           dw1072
_cod_depositor_comments
'Adding full bibliography for 4084770--4084773.cif.'
_cod_original_cell_volume        1825.28(5)
_cod_database_code               4084772