Atomic layer deposition of sodium and potassium oxides: evaluation of precursors and deposition of thin films.
Ostreng, E.; Sønsteby, H H; Oien, S.; Nilsen, O.; Fjellvåg, H; Dalton transactions (Cambridge, England : 2003) 43 (2014) 16666–16672; doi:10.1039/c4dt01930j

data_7032635
_publ_section_title
;
 Atomic layer deposition of sodium and potassium oxides: evaluation of
 precursors and deposition of thin films.
;
_journal_issue                   44
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16666
_journal_page_last               16672
_journal_paper_doi               10.1039/c4dt01930j
_journal_volume                  43
_journal_year                    2014
_chemical_compound_source        'Commercially obtained'
_chemical_formula_moiety         'C24 H54 Na6 O6'
_chemical_formula_sum            'C24 H54 Na6 O6'
_chemical_formula_weight         576.61
_chemical_name_common            'Sodium tert-butoxide'
_chemical_name_systematic        'Sodium tert-butoxide'
_chemical_properties_physical
'Air-sensitive, Moisture-sensitive, Hygroscopic, Oxygen-sensitive'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-08-25
_audit_creation_method
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_audit_update_record
;
2014-08-25 

;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            20
_cell_length_a                   18.1583(16)
_cell_length_b                   19.2347(17)
_cell_length_c                   51.548(4)
_cell_measurement_reflns_used    8880
_cell_measurement_temperature    100
_cell_measurement_theta_max      20.84
_cell_measurement_theta_min      2.241
_cell_volume                     18004(3)
_computing_cell_refinement       'APEX2 v2013.6--2 (Bruker AXS)'
_computing_data_collection       'APEX2 v2013.6--2 (Bruker AXS)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Diamond v3.2i (Brandenburg, 2012)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.01
_diffrn_detector                 'Bruker PHOTON100 area detector'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.585
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type
'Bruker D8 Venture fixed-chi goniometer and Photon100 CMOS detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0691
_diffrn_reflns_av_unetI/netI     0.0464
_diffrn_reflns_Laue_measured_fraction_full 0.585
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            90802
_diffrn_reflns_point_group_measured_fraction_full 0.577
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         20.816
_diffrn_reflns_theta_min         2.208
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.133
_exptl_absorpt_correction_T_max  0.7446
_exptl_absorpt_correction_T_min  0.6311
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1571 before and 0.0589 after correction.
The Ratio of minimum to maximum transmission is 0.8476.
The \l/2 correction factor is 0.0000.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.064
_exptl_crystal_description       prism
_exptl_crystal_F_000             6240
_exptl_crystal_recrystallization_method Sublimation
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.25
_exptl_transmission_factor_max   1.0000
_exptl_transmission_factor_min   0.8467
_refine_diff_density_max         0.494
_refine_diff_density_min         -0.250
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details
;
 Flack x determined using 5453 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.57(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1711
_refine_ls_number_reflns         18808
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0846
_refine_ls_R_factor_gt           0.0580
_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^)+(0.0586P)^2^+26.9926P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1414
_refine_ls_wR_factor_ref         0.1565
_reflns_Friedel_coverage         0.831
_reflns_Friedel_fraction_full    0.568
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                14462
_reflns_number_total             18808
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt01930j2.cif
_cod_data_source_block           eo-big-p212121_a(2)
_cod_depositor_comments          'Adding full bibliography for 7032635.cif.'
_cod_database_code               7032635
_shelxl_version_number           2014-3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C162) \\sim Ueq, Uanis(C461) \\sim Ueq, Uanis(C312) \\sim Ueq: with sigma
of 0.02 and sigma for terminal atoms of 0.002
Uanis(C463) \\sim Ueq, Uanis(C151) \\sim Ueq, Uanis(C152) \\sim Ueq: with sigma
of 0.05 and sigma for terminal atoms of 0.1
3.a Idealised Me refined as rotating group:
 C111(H11A,H11B,H11C), C112(H11D,H11E,H11F), C113(H11G,H11H,H11I), C121(H12A,
 H12B,H12C), C122(H12D,H12E,H12F), C123(H12G,H12H,H12I), C131(H13A,H13B,H13C),
 C132(H13D,H13E,H13F), C133(H13G,H13H,H13I), C141(H14A,H14B,H14C), C142(H14D,
 H14E,H14F), C143(H14G,H14H,H14I), C151(H15A,H15B,H15C), C152(H15D,H15E,H15F),
 C153(H15G,H15H,H15I), C161(H16A,H16B,H16C), C162(H16D,H16E,H16F), C163(H16G,
 H16H,H16I), C211(H21A,H21B,H21C), C212(H21D,H21E,H21F), C213(H21G,H21H,H21I),
 C221(H22A,H22B,H22C), C222(H22D,H22E,H22F), C223(H22G,H22H,H22I), C231(H23A,
 H23B,H23C), C232(H23D,H23E,H23F), C233(H23G,H23H,H23I), C241(H24A,H24B,H24C),
 C242(H24D,H24E,H24F), C243(H24G,H24H,H24I), C251(H25A,H25B,H25C), C252(H25D,
 H25E,H25F), C253(H25G,H25H,H25I), C261(H26A,H26B,H26C), C262(H26D,H26E,H26F),
 C263(H26G,H26H,H26I), C311(H31A,H31B,H31C), C312(H31D,H31E,H31F), C313(H31G,
 H31H,H31I), C321(H32A,H32B,H32C), C322(H32D,H32E,H32F), C323(H32G,H32H,H32I),
 C331(H33A,H33B,H33C), C332(H33D,H33E,H33F), C333(H33G,H33H,H33I), C341(H34A,
 H34B,H34C), C342(H34D,H34E,H34F), C343(H34G,H34H,H34I), C351(H35A,H35B,H35C),
 C352(H35D,H35E,H35F), C353(H35G,H35H,H35I), C361(H36A,H36B,H36C), C362(H36D,
 H36E,H36F), C363(H36G,H36H,H36I), C411(H41A,H41B,H41C), C412(H41D,H41E,H41F),
 C413(H41G,H41H,H41I), C421(H42A,H42B,H42C), C422(H42D,H42E,H42F), C423(H42G,
 H42H,H42I), C431(H43A,H43B,H43C), C432(H43D,H43E,H43F), C433(H43G,H43H,H43I),
 C441(H44A,H44B,H44C), C442(H44D,H44E,H44F), C443(H44G,H44H,H44I), C451(H45A,
 H45B,H45C), C452(H45D,H45E,H45F), C453(H45G,H45H,H45I), C461(H46A,H46B,H46C),
 C462(H46D,H46E,H46F), C463(H46G,H46H,H46I), C511(H51A,H51B,H51C), C512(H51D,
 H51E,H51F), C513(H51G,H51H,H51I), C521(H52A,H52B,H52C), C522(H52D,H52E,H52F),
 C523(H52G,H52H,H52I), C531(H53A,H53B,H53C), C532(H53D,H53E,H53F), C533(H53G,
 H53H,H53I), C541(H54A,H54B,H54C), C542(H54D,H54E,H54F), C543(H54G,H54H,H54I),
 C551(H55A,H55B,H55C), C552(H55D,H55E,H55F), C553(H55G,H55H,H55I), C561(H56A,
 H56B,H56C), C562(H56D,H56E,H56F), C563(H56G,H56H,H56I)
;
_olex2_submission_special_instructions 'No special instructions were received'