Insulator-to-Proton-Conductor Transition in a Dense Metal-Organic Framework.
Tominaka, Satoshi; Coudert, François-Xavier; Dao, Thang D.; Nagao, Tadaaki; Cheetham, Anthony K.; Journal of the American Chemical Society 137 (2015) 6428–6431; doi:10.1021/jacs.5b02777

data_4123616
_publ_section_title
;
 Insulator-to-Proton-Conductor Transition in a Dense Metal-Organic
 Framework.
;
_journal_issue                   20
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6428
_journal_page_last               6431
_journal_paper_doi               10.1021/jacs.5b02777
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety         'C8 Li2 O16 Zr, 2(C2 H8 N)'
_chemical_formula_sum            'C12 H16 Li2 N2 O16 Zr'
_chemical_formula_weight         549.37
_chemical_name_common            dma2[Li2Zr(ox)4]
_chemical_name_systematic        'Lithium Zirconium Oxalate Dimethylammonium'
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-01-20
_audit_creation_method
;
Olex2 1.2
(compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.834(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.0091(8)
_cell_length_b                   16.6385(9)
_cell_length_c                   15.3534(7)
_cell_measurement_reflns_used    7476
_cell_measurement_temperature    120.00(14)
_cell_measurement_theta_max      67.5110
_cell_measurement_theta_min      3.9130
_cell_volume                     4089.2(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      120.00(14)
_diffrn_detector_area_resol_mean 16.1183
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0079189000
_diffrn_orient_matrix_UB_12      -0.0306215000
_diffrn_orient_matrix_UB_13      0.0942376000
_diffrn_orient_matrix_UB_21      0.0950318000
_diffrn_orient_matrix_UB_22      -0.0145888000
_diffrn_orient_matrix_UB_23      0.0046349000
_diffrn_orient_matrix_UB_31      0.0131734000
_diffrn_orient_matrix_UB_32      0.0861290000
_diffrn_orient_matrix_UB_33      0.0341650000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0315
_diffrn_reflns_av_unetI/netI     0.0176
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            21297
_diffrn_reflns_theta_full        67.86
_diffrn_reflns_theta_max         67.86
_diffrn_reflns_theta_min         3.83
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.206
_exptl_absorpt_correction_T_max  0.798
_exptl_absorpt_correction_T_min  0.251
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.785
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2208
_exptl_crystal_size_max          0.6843
_exptl_crystal_size_mid          0.0519
_exptl_crystal_size_min          0.0467
_refine_diff_density_max         1.022
_refine_diff_density_min         -0.795
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     302
_refine_ls_number_reflns         3697
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0376
_refine_ls_R_factor_gt           0.0322
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0659P)^2^+1.6469P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0903
_refine_ls_wR_factor_ref         0.0969
_reflns_number_gt                3110
_reflns_number_total             3697
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja5b02777_si_002.cif
_cod_data_source_block           PhaseI_120K
_cod_depositor_comments
'Adding full bibliography for 4123615--4123618.cif.'
_cod_original_cell_volume        4089.2(3)
_cod_database_code               4123616
_chemical_oxdiff_formula         'Li2 Zr C12 O16 N2 H16'
_reflns_odcompleteness_completeness 98.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 N22(H22A,H22B), N1(H1D,H1E)
2.b Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C29(H29A,H29B,H29C), C1(H1A,H1B,H1C), C2(H2A,H2B,H2C)
;