Disordered sodium alkoxides from powder data: crystal structures of sodium ethoxide, propoxide, butoxide and pentoxide, and some of their solvates
Beske, Maurice; Cronje, Stephanie; Schmidt, Martin U.; Tapmeyer, Lukas; Acta Crystallographica Section B 77 (2021) –; doi:10.1107/S205252062001584X

data_2108750
_publ_section_title
;
 Disordered sodium alkoxides from powder data: crystal structures of
 sodium ethoxide, propoxide, butoxide and pentoxide, and some of their
 solvates
;
_journal_coeditor_code           NE5003SUP1
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S205252062001584X
_journal_volume                  77
_journal_year                    2021
_chemical_compound_source        synthesis
_chemical_formula_moiety         'C2 H5 O 1-, Na 1+, 2(C2 H6 O)'
_chemical_formula_sum            'C6 H17 Na O3'
_chemical_formula_weight         160.18
_chemical_name_common            'sodium ethanolate ethanol disolvate'
_chemical_name_systematic        'sodium ethoxide ethanol disolvate'
_chemical_properties_physical
'air-sensitive, moisture-sensitive, hygroscopic,Air-sensitive,Moisture-sensitive,Hygroscopic,Heat-sensitive'
_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_block_doi                 10.5517/ccdc.csd.cc237p13
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-07-29 deposited with the CCDC. 2020-04-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.08(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.622(6)
_cell_length_b                   5.1926(9)
_cell_length_c                   17.682(6)
_cell_measurement_reflns_used    1441
_cell_measurement_temperature    238(2)
_cell_measurement_theta_max      40.7214
_cell_measurement_theta_min      4.1353
_cell_volume                     1035.0(7)
_computing_cell_refinement       'Bruker APEX3 v2016.1-0'
_computing_data_collection       'Bruker APEX3 v2016.1-0'
_computing_data_reduction        'Bruker APEX3 v2016.1-0'
_computing_molecular_graphics    shelXle
_computing_publication_material  'shelXle, Mercury, ORTEPIII'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_pressure         101.3
_diffrn_ambient_temperature      238(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.735
_diffrn_measurement_device_type  'apex2 detector'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.3172
_diffrn_reflns_av_unetI/netI     0.1469
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.735
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5735
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.735
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         59.909
_diffrn_reflns_theta_min         4.136
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Incoatec microfocus tube'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.006
_exptl_absorpt_correction_T_max  0.7486
_exptl_absorpt_correction_T_min  0.2700
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.028
_exptl_crystal_density_method    'none applied'
_exptl_crystal_description       'fine needle'
_exptl_crystal_F_000             352
_exptl_crystal_recrystallization_method
'Crystallized from ethanolic solution of sodium ethoxide at room temperature'
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.160
_refine_diff_density_min         -0.203
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.980
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     94
_refine_ls_number_reflns         1124
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.980
_refine_ls_R_factor_all          0.1691
_refine_ls_R_factor_gt           0.0842
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1281P)^2^]  where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2178
_refine_ls_wR_factor_ref         0.2709
_reflns_Friedel_coverage         0.000
_reflns_number_gt                488
_reflns_number_total             1124
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ne5003sup1.cif
_cod_data_source_block           NaOEt2EtOH
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2108750
_publcif_datablock.id            {65c314dd-bb9c-486a-8bcd-3c65ed9bd08e}
_shelx_res_checksum              49098
_shelx_hkl_checksum              57399
_cod_database_fobs_code 2108750