Redox transmetallation approaches to the synthesis of extremely bulky amido-lanthanoid(ii) and -calcium(ii) complexes.
de Bruin-Dickason, Caspar N; Boutland, Aaron J.; Dange, Deepak; Deacon, Glen B.; Jones, Cameron; Dalton transactions (Cambridge, England : 2003) 47 (2018) 9512–9520; doi:10.1039/c8dt02138d

data_7046817
_publ_section_title
;
 Redox transmetallation approaches to the synthesis of extremely bulky
 amido-lanthanoid(ii) and -calcium(ii) complexes.
;
_journal_issue                   28
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9512
_journal_page_last               9520
_journal_paper_doi               10.1039/c8dt02138d
_journal_volume                  47
_journal_year                    2018
_chemical_formula_sum            'C76 H80 N2 Si2 Yb'
_chemical_formula_weight         1250.64
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2018-05-25 deposited with the CCDC.
2018-06-22 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 113.47(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.442(3)
_cell_length_b                   21.321(4)
_cell_length_c                   19.126(4)
_cell_measurement_reflns_used    13249
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.00
_cell_measurement_theta_min      1.39
_cell_volume                     6150(2)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'Blu-Ice (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics    X-Seed
_computing_publication_material  CifTAB
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_radiation_source         'Australian Synchrotron'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.71090
_diffrn_reflns_av_R_equivalents  0.1516
_diffrn_reflns_av_sigmaI/netI    0.0724
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            92209
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.39
_exptl_absorpt_coefficient_mu    1.605
_exptl_absorpt_correction_T_max  0.924
_exptl_absorpt_correction_T_min  0.866
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   XDS
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2592
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.712
_refine_diff_density_min         -1.879
_refine_diff_density_rms         0.121
_refine_ls_extinction_coef       0.00124(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     747
_refine_ls_number_reflns         13249
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.1068
_refine_ls_R_factor_gt           0.0645
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0501P)^2^+32.7475P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1375
_refine_ls_wR_factor_ref         0.1581
_reflns_number_gt                8913
_reflns_number_total             13249
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8dt02138d2.cif
_cod_data_source_block           compound8
_cod_depositor_comments
'Adding full bibliography for 7046810--7046818.cif.'
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7046817