Synthesis and crystal structures of tetrameric [2-(4,4-dimethyl-2-oxazolin-2-yl)anilido]sodium and tris[2-(4,4-dimethyl-2-oxazolin-2-yl)anilido]ytterbium(III)
Gajecki, Leah; Twamley, Brendan; Berg, David J.; Acta Crystallographica Section E 76 (2020) 703–709; doi:10.1107/S2056989020005034

data_2243363
_publ_section_title
;
 Synthesis and crystal structures of tetrameric
 [2-(4,4-dimethyl-2-oxazolin-2-yl)anilido]sodium and
 tris[2-(4,4-dimethyl-2-oxazolin-2-yl)anilido]ytterbium(III)
;
_journal_coeditor_code           ZL2777
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              703
_journal_page_last               709
_journal_paper_doi               10.1107/S2056989020005034
_journal_volume                  76
_journal_year                    2020
_chemical_formula_iupac          '[Yb (C11 H13 N2 O)3]'
_chemical_formula_moiety         'C33 H39 N6 O3 Yb'
_chemical_formula_sum            'C33 H39 N6 O3 Yb'
_chemical_formula_weight         740.74
_chemical_name_systematic
;
Tris[2-(4,4-dimethyl-2-oxazolin-2-yl)anilinido]ytterbium(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   mixed
_atom_sites_solution_primary     heavy
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 94.7220(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.9428(5)
_cell_length_b                   9.8253(5)
_cell_length_c                   28.6089(14)
_cell_measurement_reflns_used    7270
_cell_measurement_temperature    86(2)
_cell_measurement_theta_max      24.56
_cell_measurement_theta_min      2.19
_cell_volume                     3065.5(3)
_computing_cell_refinement
;
SAINT (Bruker, 2003)
;
_computing_data_collection
;
SMART (Bruker, 2003)
;
_computing_data_reduction
;
SAINT (Bruker, 2003)
;
_computing_molecular_graphics
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
SHELXL (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS (Sheldrick, 2008)
;
_diffrn_ambient_temperature      86(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'SMART APEX CCD area detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0593
_diffrn_reflns_av_unetI/netI     0.0440
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            39651
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.553
_diffrn_reflns_theta_min         1.944
_diffrn_source                   'sealed X-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.095
_exptl_absorpt_correction_T_max  0.2617
_exptl_absorpt_correction_T_min  0.2185
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2016)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.605
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1492
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.831
_refine_diff_density_min         -1.192
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     394
_refine_ls_number_reflns         7061
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0320
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0248P)^2^+4.5847P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0687
_refine_ls_wR_factor_ref         0.0730
_reflns_number_gt                5882
_reflns_number_total             7061
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            zl2777sup1.cif
_cod_data_source_block           YbH-L133
_cod_database_code               2243363
_shelx_estimated_absorpt_t_min   0.549
_shelx_estimated_absorpt_t_max   0.861
_shelx_hkl_checksum              60844
_shelx_res_checksum              4209
_cod_database_fobs_code 2243363