Synthesis of homometallic divalent lanthanide organoimides from benzyl complexes.
Wolf, Benjamin M.; Stuhl, Christoph; Anwander, Reiner; Chemical communications (Cambridge, England) 54 (2018) 8826–8829; doi:10.1039/c8cc05234d

data_7121958
_publ_section_title
;
 Synthesis of homometallic divalent lanthanide organoimides from benzyl
 complexes.
;
_journal_issue                   64
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              8826
_journal_page_last               8829
_journal_paper_doi               10.1039/c8cc05234d
_journal_volume                  54
_journal_year                    2018
_chemical_formula_sum            'C72 H116 N4 O6 Yb4'
_chemical_formula_weight         1825.84
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yc'
_space_group_name_H-M_alt        'P 1 c 1'
_symmetry_space_group_name_Hall  'P -2yc'
_symmetry_space_group_name_H-M   'P 1 c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-06-28 deposited with the CCDC.
2018-07-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.614(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.2322(8)
_cell_length_b                   16.2283(10)
_cell_length_c                   17.9608(11)
_cell_measurement_reflns_used    9828
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      29.5479
_cell_measurement_theta_min      2.7005
_cell_volume                     3585.6(4)
_computing_cell_refinement       'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_data_collection       'Bruker Apex3'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'XT, VERSION 2014/5'
_diffrn_ambient_temperature      140(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Smart Apex III Duo'
_diffrn_measurement_method       omega/phi-scans
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0355
_diffrn_reflns_av_unetI/netI     0.0331
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            96339
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.578
_diffrn_reflns_theta_min         1.255
_diffrn_source                   Imus-tube
_exptl_absorpt_coefficient_mu    5.219
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.4649
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.691
_exptl_crystal_description       block
_exptl_crystal_F_000             1808
_exptl_crystal_size_max          0.466
_exptl_crystal_size_mid          0.458
_exptl_crystal_size_min          0.258
_refine_diff_density_max         1.396
_refine_diff_density_min         -0.993
_refine_diff_density_rms         0.099
_refine_ls_abs_structure_details
;
 Flack x determined using 9466 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.014(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     905
_refine_ls_number_reflns         20088
_refine_ls_number_restraints     418
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0246
_refine_ls_R_factor_gt           0.0237
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0351P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0573
_refine_ls_wR_factor_ref         0.0577
_reflns_Friedel_coverage         0.993
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                19608
_reflns_number_total             20088
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc05234d2.cif
_cod_data_source_block           2-Yb_mo_FK20_0m_a
_cod_depositor_comments
'Adding full bibliography for 7121956--7121961.cif.'
_cod_database_code               7121958
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.195
_shelx_estimated_absorpt_t_max   0.346
_shelx_res_checksum              50714