Synthesis and structural diversity of trivalent rare-earth metal diisopropylamide complexes.
Spallek, Tatiana; Heß, Oliver; Meermann-Zimmermann, Melanie; Meermann, Christian; Klimpel, Michael G.; Estler, Frank; Schneider, David; Scherer, Wolfgang; Tafipolsky, Maxim; Törnroos, Karl W; Maichle-Mössmer, Cäcilia; Sirsch, Peter; Anwander, Reiner; Dalton transactions (Cambridge, England : 2003) 45 (2016) 13750–13765; doi:10.1039/c6dt01568a

data_7039868
_publ_section_title
;
 Synthesis and structural diversity of trivalent rare-earth metal
 diisopropylamide complexes.
;
_journal_issue                   35
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13750
_journal_page_last               13765
_journal_paper_doi               10.1039/c6dt01568a
_journal_volume                  45
_journal_year                    2016
_chemical_formula_sum            'C32 H72 Cl2 Lu2 N4 O2'
_chemical_formula_weight         965.77
_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   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-05-25 deposited with the CCDC.
2016-05-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.5440(10)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   13.5111(3)
_cell_length_b                   28.9345(6)
_cell_length_c                   32.5140(7)
_cell_measurement_reflns_used    9708
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      60.93
_cell_measurement_theta_min      4.53
_cell_volume                     12496.3(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Smart Apex II Duo'
_diffrn_measurement_method       omega/phi-scans
_diffrn_radiation_monochromator  multilayer
_diffrn_radiation_source         'Imus-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0422
_diffrn_reflns_av_unetI/netI     0.0323
_diffrn_reflns_Laue_measured_fraction_full 0.999
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_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            530264
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.666
_diffrn_reflns_theta_min         1.274
_exptl_absorpt_coefficient_mu    4.870
_exptl_absorpt_correction_T_max  0.9600
_exptl_absorpt_correction_T_min  0.9480
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.540
_exptl_crystal_description       block
_exptl_crystal_F_000             5808
_exptl_crystal_size_max          0.255
_exptl_crystal_size_mid          0.221
_exptl_crystal_size_min          0.195
_refine_diff_density_max         4.296
_refine_diff_density_min         -2.158
_refine_diff_density_rms         0.163
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.495(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2443
_refine_ls_number_reflns         72956
_refine_ls_number_restraints     3806
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0385
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0181P)^2^+53.4579P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0749
_refine_ls_wR_factor_ref         0.0777
_reflns_Friedel_coverage         0.999
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.978
_reflns_number_gt                64801
_reflns_number_total             72956
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt01568a2.cif
_cod_data_source_block           5d_(ohlu1a07)
_cod_depositor_comments
'Adding full bibliography for 7039866--7039885.cif.'
_cod_database_code               7039868
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.370
_shelx_estimated_absorpt_t_max   0.450
_shelx_res_checksum              1033