Synthesis and crystallographic characterization of diphenylamide rare-earth metal complexes <i>Ln</i>(NPh~2~)~3~(THF)~2~ and [(Ph~2~N)~2~<i>Ln</i>(μ-NPh~2~)]~2~
Palumbo, Chad T.; Kotyk, Christopher M.; Ziller, Joseph W.; Evans, William J.; Acta Crystallographica Section E 76 (2020) 1447–1453; doi:10.1107/S2056989020009998

data_2243542
_publ_section_title
;
 Synthesis and crystallographic characterization of diphenylamide
 rare-earth metal complexes <i>Ln</i>(NPh~2~)~3~(THF)~2~ and
 [(Ph~2~N)~2~<i>Ln</i>(\m-NPh~2~)]~2~
;
_journal_coeditor_code           ZL2782
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1447
_journal_page_last               1453
_journal_paper_doi               10.1107/S2056989020009998
_journal_volume                  76
_journal_year                    2020
_chemical_formula_iupac          '[Y (C12 H10 N)3 (C4 H8 O)2]'
_chemical_formula_moiety         'C44 H46 N3 O2 Y'
_chemical_formula_sum            'C44 H46 N3 O2 Y'
_chemical_formula_weight         737.75
_chemical_name_systematic
;
Tris(diphenylamido-\k<i>N</i>)bis(tetrahydrofuran-\k<i>O</i>)yttrium(III)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 107.2070(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.3539(9)
_cell_length_b                   12.5259(7)
_cell_length_c                   20.2511(12)
_cell_measurement_reflns_used    9981
_cell_measurement_temperature    143(2)
_cell_measurement_theta_max      28.19
_cell_measurement_theta_min      2.19
_cell_volume                     3720.4(4)
_computing_cell_refinement
;
SAINT (Bruker, 2009)
;
_computing_data_collection
;
APEX2 (Bruker, 2011)
;
_computing_data_reduction
;
SAINT (Bruker, 2009)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008d)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008d)
;
_computing_structure_refinement
;
<i>SHELXL2014/7</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXS2008/4</i> (Sheldrick, 2008c)
;
_diffrn_ambient_temperature      143(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.940
_diffrn_measurement_device_type  'Bruker SMART APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0254
_diffrn_reflns_av_unetI/netI     0.0221
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            42053
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.460
_diffrn_reflns_theta_min         1.388
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.608
_exptl_absorpt_correction_T_max  0.6828
_exptl_absorpt_correction_T_min  0.5366
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
(SADABS; Krause et al., 2015)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.317
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1544
_exptl_crystal_size_max          0.520
_exptl_crystal_size_mid          0.377
_exptl_crystal_size_min          0.373
_refine_diff_density_max         0.807
_refine_diff_density_min         -0.465
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         8829
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0313
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0440P)^2^+1.6736P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0771
_refine_ls_wR_factor_ref         0.0812
_reflns_number_gt                7562
_reflns_number_total             8829
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            zl2782sup1.cif
_cod_data_source_block           1-Y
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2243542
_cod_database_fobs_code          2243542
_shelx_estimated_absorpt_t_min   0.488
_shelx_estimated_absorpt_t_max   0.585
_shelx_hkl_checksum              84328
_shelx_res_checksum              50241