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_2243543
_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          '[Er (C12 H10 N)3 (C4 H8 O)2]'
_chemical_formula_sum            'C44 H46 Er N3 O2'
_chemical_formula_weight         816.10
_chemical_name_systematic
;
Tris(diphenylamido-\k<i>N</i>)bis(tetrahydrofuran-\k<i>O</i>)erbium(III)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                 91.3697(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.0946(5)
_cell_length_b                   19.1086(8)
_cell_length_c                   16.3609(7)
_cell_measurement_reflns_used    9998
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.04
_cell_measurement_theta_min      2.47
_cell_volume                     3780.1(3)
_computing_cell_refinement
;
SAINT (Bruker, 2009)
;
_computing_data_collection
;
APEX2 (Bruker, 2014)
;
_computing_data_reduction
;
SAINT (Bruker, 2013)
;
_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>SHELXT</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.943
_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  0.0178
_diffrn_reflns_av_unetI/netI     0.0138
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            46529
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.225
_diffrn_reflns_theta_min         1.639
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.260
_exptl_absorpt_correction_T_max  0.6946
_exptl_absorpt_correction_T_min  0.5570
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause et al., 2015)
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1660
_exptl_crystal_size_max          0.482
_exptl_crystal_size_mid          0.389
_exptl_crystal_size_min          0.332
_refine_diff_density_max         0.700
_refine_diff_density_min         -0.417
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     462
_refine_ls_number_reflns         9687
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0225
_refine_ls_R_factor_gt           0.0194
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0257P)^2^+1.7012P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0488
_refine_ls_wR_factor_ref         0.0504
_reflns_number_gt                8834
_reflns_number_total             9687
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            zl2782sup1.cif
_cod_data_source_block           1-Er
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2243543
_cod_database_fobs_code          2243543
_shelx_estimated_absorpt_t_min   0.409
_shelx_estimated_absorpt_t_max   0.521
_shelx_hkl_checksum              29946
_shelx_res_checksum              2665