Particle size dependence of proton conduction in a cationic lanthanum phosphonate MOF.
Levenson, Daniel A.; Zhang, Jinfeng; Gelfand, Benjamin S.; Kammampata, Sanoop P.; Thangadurai, Venkataraman; Shimizu, George K. H.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 4022–4029; doi:10.1039/c9dt04229f

data_7703835
_publ_section_title
;
 Particle size dependence of proton conduction in a cationic lanthanum
 phosphonate MOF.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4022
_journal_page_last               4029
_journal_paper_doi               10.1039/c9dt04229f
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C22 H46 La2 N3 O15 P3'
_chemical_formula_sum            'C22 H46 La2 N3 O15 P3'
_chemical_formula_weight         963.35
_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
_audit_creation_date             2018-02-15
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2019-10-31 deposited with the CCDC.	2020-03-12 downloaded from the CCDC.
;
_cell_angle_alpha                95.434(7)
_cell_angle_beta                 106.266(7)
_cell_angle_gamma                91.765(9)
_cell_formula_units_Z            2
_cell_length_a                   9.6056(16)
_cell_length_b                   15.424(3)
_cell_length_c                   16.780(3)
_cell_measurement_reflns_used    9780
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.37
_cell_measurement_theta_min      2.99
_cell_volume                     2371.6(7)
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.982
_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  0.0872
_diffrn_reflns_av_unetI/netI     0.1072
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            32249
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.443
_diffrn_reflns_theta_min         2.587
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.928
_exptl_absorpt_correction_T_max  0.9311
_exptl_absorpt_correction_T_min  0.6412
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0901 before and 0.0665 after correction.
The Ratio of minimum to maximum transmission is 0.6886.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.349
_exptl_crystal_description       rod
_exptl_crystal_F_000             956
_exptl_crystal_size_max          0.308
_exptl_crystal_size_mid          0.157
_exptl_crystal_size_min          0.084
_refine_diff_density_max         2.867
_refine_diff_density_min         -1.330
_refine_diff_density_rms         0.186
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.968
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     410
_refine_ls_number_reflns         11739
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.968
_refine_ls_R_factor_all          0.0768
_refine_ls_R_factor_gt           0.0494
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0573P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1156
_refine_ls_wR_factor_ref         0.1272
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8076
_reflns_number_total             11739
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04229f2.cif
_cod_data_source_block           1_sq
_cod_depositor_comments          'Adding full bibliography for 7703835.cif.'
_cod_original_cell_volume        2371.5(7)
_cod_database_code               7703835
_shelx_shelxl_version_number     2017/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2.a Rotating group:
 O15(H15A,H15B), O14(H14A,H14B)
2.b Ternary CH refined with riding coordinates:
 N3(H3), C16(H16), N2(H2), N1(H1), C7(H7), C4(H4)
2.c Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C12(H12A,H12B), C15(H15C,H15D), C18(H18A,H18B), C9(H9A,H9B),
 C13(H13A,H13B), C10(H10A,H10B), C11(H11A,H11B), C8(H8A,H8B), C14(H14C,H14D),
 C1(H1A,H1B), C6(H6A,H6B), C2(H2A,H2B), C5(H5A,H5B), C3(H3A,H3B)
2.d Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C22(H22A,H22B,H22C)
;
_shelx_res_checksum              9441
_shelx_fab_checksum              16065
_olex2_submission_special_instructions 'No special instructions were received'