Solvate sponge crystals of (DMF)3NaClO4: reversible pressure/temperature controlled juicing in a melt/press-castable sodium-ion conductor
Prakash, Prabhat; Ardhra, Shylendran; Fall, Birane; Zdilla, Michael J.; Wunder, Stephanie L.; Venkatnathan, Arun; Chemical Science 12 (2021) 5574–5581; doi:10.1039/D0SC06455F

data_1560726
_publ_section_title
;
 Solvate sponge crystals of (DMF)3NaClO4: reversible pressure/temperature
 controlled juicing in a melt/press-castable sodium-ion conductor
;
_journal_issue                   15
_journal_name_full               'Chemical Science'
_journal_page_first              5574
_journal_page_last               5581
_journal_paper_doi               10.1039/D0SC06455F
_journal_volume                  12
_journal_year                    2021
_chemical_formula_moiety         'C6 H14 Cl N2 Na O6'
_chemical_formula_sum            'C6 H14 Cl N2 Na O6'
_chemical_formula_weight         268.63
_chemical_name_systematic
'bis(N,N-dimetylformamide)-perchlorato sodium'
_chemical_properties_physical    Moisture-sensitive,Hygroscopic
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-06-20
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-07-24 deposited with the CCDC.	2021-03-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.244(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.1493(14)
_cell_length_b                   10.1833(15)
_cell_length_c                   13.220(2)
_cell_measurement_reflns_used    2807
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.72
_cell_measurement_theta_min      2.58
_cell_volume                     1169.8(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'COSMO (BrukerAXS)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      99.98
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.844
_diffrn_measured_fraction_theta_max 0.843
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0157
_diffrn_reflns_av_unetI/netI     0.0210
_diffrn_reflns_Laue_measured_fraction_full 0.844
_diffrn_reflns_Laue_measured_fraction_max 0.843
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            5501
_diffrn_reflns_point_group_measured_fraction_full 0.844
_diffrn_reflns_point_group_measured_fraction_max 0.843
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.810
_diffrn_reflns_theta_min         2.000
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.378
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6381
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0329 before and 0.0249 after correction. The Ratio of minimum to maximum transmission is 0.8558. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'clear white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_description       block
_exptl_crystal_F_000             560
_exptl_crystal_recrystallization_method 'From the Melt'
_exptl_crystal_size_max          0.152
_exptl_crystal_size_mid          0.121
_exptl_crystal_size_min          0.076
_refine_diff_density_max         0.502
_refine_diff_density_min         -0.305
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     159
_refine_ls_number_reflns         2335
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0414
_refine_ls_R_factor_gt           0.0320
_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^)+(0.0413P)^2^+0.6704P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0816
_refine_ls_wR_factor_ref         0.0869
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1954
_reflns_number_total             2335
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc06455f5.cif
_cod_data_source_block           mo_3183_0m
_cod_depositor_comments          'Adding full bibliography for 1560726.cif.'
_cod_database_code               1560726
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.972
_shelx_estimated_absorpt_t_min   0.945
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C1T(H1TA,H1TB,H1TC), C2T(H2TA,H2TB,H2TC), C3T(H3TA,H3TB,H3TC), C4T(H4TA,H4TB,
 H4TC)
;
_shelx_res_checksum              55075
_shelx_hkl_checksum              19706
_olex2_submission_special_instructions 'No special instructions were received'