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_2243362
_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          '[Na4 (C11 H13 N2 O)4]'
_chemical_formula_moiety         'C44 H52 N8 Na4 O4'
_chemical_formula_sum            'C44 H52 N8 Na4 O4'
_chemical_formula_weight         848.89
_chemical_name_systematic
Poly[bis[\m~3~-2-(4,4-dimethyl-2-oxazolin-2-yl)anilinido][\m~2~-2-(4,4-dimethyl-2-oxazolin-2-yl)aniline]tetrasodium(I)]
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                105.2660(10)
_cell_angle_beta                 97.4460(10)
_cell_angle_gamma                106.1200(10)
_cell_formula_units_Z            2
_cell_length_a                   10.9545(5)
_cell_length_b                   11.8785(5)
_cell_length_c                   18.8415(8)
_cell_measurement_reflns_used    9632
_cell_measurement_temperature    87(2)
_cell_measurement_theta_max      29.90
_cell_measurement_theta_min      2.24
_cell_volume                     2217.20(17)
_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      87(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.960
_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_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0536
_diffrn_reflns_av_unetI/netI     0.0773
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            33551
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.047
_diffrn_reflns_theta_min         1.870
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.116
_exptl_absorpt_correction_T_max  0.9828
_exptl_absorpt_correction_T_min  0.776082
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2016)
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.272
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.490
_refine_diff_density_min         -0.311
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     565
_refine_ls_number_reflns         12487
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0970
_refine_ls_R_factor_gt           0.0659
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0734P)^2^+0.1127P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1443
_refine_ls_wR_factor_ref         0.1577
_reflns_number_gt                8858
_reflns_number_total             12487
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            zl2777sup1.cif
_cod_data_source_block           Na4H-L142
_cod_database_code               2243362
_shelx_estimated_absorpt_t_min   0.970
_shelx_estimated_absorpt_t_max   0.983
_shelx_hkl_checksum              63210
_shelx_res_checksum              43046
_cod_database_fobs_code 2243362