Synthesis and Structures of New Mixed-Metal Lanthanide/Magnesium Allyl Complexes
Sánchez-Barba, Luis F.; Hughes, David L.; Humphrey, Simon M.; Bochmann, Manfred; Organometallics 24 (2005) 5329–; doi:10.1021/om0505155

data_4076066
_publ_section_title
;
 Synthesis and Structures of New Mixed-Metal Lanthanide/Magnesium Allyl
 Complexes
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              5329
_journal_paper_doi               10.1021/om0505155
_journal_volume                  24
_journal_year                    2005
_chemical_formula_moiety         '2(C12 H20 Sm), C24 H48 Mg O6, 2(C4 H8 O)'
_chemical_formula_sum            'C56 H104 Mg O8 Sm2'
_chemical_formula_weight         1230.40
_chemical_name_common            'Compound 5'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.2519(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.3797(4)
_cell_length_b                   21.6107(4)
_cell_length_c                   12.3467(3)
_cell_measurement_reflns_used    10496
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.02
_cell_volume                     6072.1(2)
_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 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'Thin slice \w and \f scans'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0533
_diffrn_reflns_av_sigmaI/netI    0.0608
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            18960
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.52
_exptl_absorpt_coefficient_mu    1.972
_exptl_absorpt_correction_T_max  0.953
_exptl_absorpt_correction_T_min  0.861
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.346
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       shard
_exptl_crystal_F_000             2560
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.920
_refine_diff_density_min         -0.619
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         6915
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0658
_refine_ls_R_factor_gt           0.0391
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0212P)^2^+20.7124P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0747
_refine_ls_wR_factor_ref         0.0838
_reflns_number_gt                5125
_reflns_number_total             6915
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            om0505155si20050622_103451.cif
_cod_data_source_block           ua0441
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4076066