Synthesis and Characterization of Paramagnetic Lanthanide Benzyl Complexes
Huang, Wenliang; Upton, Brianna M.; Khan, Saeed I.; Diaconescu, Paula L.; Organometallics 32 (2013) 1379–; doi:10.1021/om3010433

data_4080284
_publ_section_title
;
 Synthesis and Characterization of Paramagnetic Lanthanide Benzyl
 Complexes
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1379
_journal_paper_doi               10.1021/om3010433
_journal_volume                  32
_journal_year                    2013
_chemical_formula_sum            'C33 H53 Fe Gd N2 O Si2'
_chemical_formula_weight         763.05
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.555(3)
_cell_length_b                   17.625(6)
_cell_length_c                   20.422(6)
_cell_measurement_temperature    100(2)
_cell_volume                     3439.2(19)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.959
_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  0.0690
_diffrn_reflns_av_sigmaI/netI    0.0731
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            31004
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         30.64
_diffrn_reflns_theta_min         3.72
_exptl_absorpt_coefficient_mu    2.430
_exptl_absorpt_correction_T_max  0.7272
_exptl_absorpt_correction_T_min  0.4586
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs (Bruker)'
_exptl_crystal_density_diffrn    1.474
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1564
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_refine_diff_density_max         2.199
_refine_diff_density_min         -1.695
_refine_diff_density_rms         0.191
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.251(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     362
_refine_ls_number_reflns         9737
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0481
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+19.2498P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1110
_refine_ls_wR_factor_ref         0.1133
_reflns_number_gt                8599
_reflns_number_total             9737
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om3010433_si_003.cif
_cod_data_source_block           (NNfc)GdBn(THF)
_cod_original_sg_symbol_H-M      Pca21
_cod_database_code               4080284