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_2243546
_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          '[Er4 (C12 H10 N)8 O2], 2C6 H6'
_chemical_formula_moiety         'C96 H80 Er4 N8 O2, 2(C6 H6)'
_chemical_formula_sum            'C108 H92 Er4 N8 O2'
_chemical_formula_weight         2202.93
_chemical_name_systematic
;Bis(\m-diphenylamido-\k^2^<i>N</i>:<i>N</i>)bis[\m-1\k<i>N</i>:2(\h^6^)-diphenylamido]tetrakis(diphenylamido-\k<i>N</i>)di-\m~3~-oxido-tetraerbium(III)
benzene disolvate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -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                61.3447(8)
_cell_angle_beta                 82.7796(10)
_cell_angle_gamma                83.0804(10)
_cell_formula_units_Z            1
_cell_length_a                   12.8857(8)
_cell_length_b                   13.6846(9)
_cell_length_c                   13.7411(9)
_cell_measurement_reflns_used    8814
_cell_measurement_temperature    88(2)
_cell_measurement_theta_max      29.08
_cell_measurement_theta_min      2.19
_cell_volume                     2104.4(2)
_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>SHELXS</i> (Sheldrick, 2008c)
;
_diffrn_ambient_temperature      88(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.899
_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  0.0519
_diffrn_reflns_av_unetI/netI     0.0463
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            51658
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.161
_diffrn_reflns_theta_min         1.597
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    4.007
_exptl_absorpt_correction_T_max  0.4318
_exptl_absorpt_correction_T_min  0.2539
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>TWINABS</i>; Sheldrick, 2012)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.738
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1084
_exptl_crystal_size_max          0.347
_exptl_crystal_size_mid          0.278
_exptl_crystal_size_min          0.106
_refine_diff_density_max         1.619
_refine_diff_density_min         -1.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.963
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     552
_refine_ls_number_reflns         10308
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.963
_refine_ls_R_factor_all          0.0317
_refine_ls_R_factor_gt           0.0273
_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^)+(0.0328P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0612
_refine_ls_wR_factor_ref         0.0624
_reflns_number_gt                9209
_reflns_number_total             10308
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            zl2782sup1.cif
_cod_data_source_block           3-Er
_cod_database_code               2243546
_cod_database_fobs_code          2243546
_shelx_estimated_absorpt_t_min   0.337
_shelx_estimated_absorpt_t_max   0.676
_shelx_hkl_checksum              93182
_shelx_res_checksum              6833