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_4123618
_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_absolute_configuration ad
_chemical_formula_moiety         '0.5(C16 H2 Li4 O33 Zr2), 2(C2 H8 N)'
_chemical_formula_sum            'C12 H17 Li2 N2 O16.5 Zr'
_chemical_formula_weight         558.38
_chemical_name_systematic        'Lithium zirconium oxalate dimethylammonium'
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-02-08
_audit_creation_method
;
Olex2 1.2
(compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736)
;
_cell_angle_alpha                78.177(3)
_cell_angle_beta                 89.232(3)
_cell_angle_gamma                69.334(3)
_cell_formula_units_Z            2
_cell_length_a                   8.4752(3)
_cell_length_b                   8.4797(3)
_cell_length_c                   16.1725(5)
_cell_measurement_reflns_used    7735
_cell_measurement_temperature    120.05(10)
_cell_measurement_theta_max      67.7610
_cell_measurement_theta_min      2.7870
_cell_volume                     1062.21(7)
_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      120.05(10)
_diffrn_detector_area_resol_mean 16.1183
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0036516000
_diffrn_orient_matrix_UB_12      0.1163649000
_diffrn_orient_matrix_UB_13      -0.0872141000
_diffrn_orient_matrix_UB_21      -0.1837865000
_diffrn_orient_matrix_UB_22      0.0171376000
_diffrn_orient_matrix_UB_23      -0.0186708000
_diffrn_orient_matrix_UB_31      -0.0640993000
_diffrn_orient_matrix_UB_32      0.1602387000
_diffrn_orient_matrix_UB_33      0.0394491000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_av_unetI/netI     0.0485
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14809
_diffrn_reflns_theta_full        67.66
_diffrn_reflns_theta_max         67.66
_diffrn_reflns_theta_min         2.80
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.039
_exptl_absorpt_correction_T_max  0.793
_exptl_absorpt_correction_T_min  0.491
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.746
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             562
_exptl_crystal_size_max          0.1921
_exptl_crystal_size_mid          0.0687
_exptl_crystal_size_min          0.0558
_refine_diff_density_max         1.728
_refine_diff_density_min         -0.547
_refine_diff_density_rms         0.114
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.35(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     613
_refine_ls_number_reflns         6913
_refine_ls_number_restraints     399
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0532
_refine_ls_R_factor_gt           0.0459
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1038P)^2^+1.7169P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1350
_refine_ls_wR_factor_ref         0.1517
_reflns_number_gt                6204
_reflns_number_total             6913
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja5b02777_si_004.cif
_cod_data_source_block           PhaseII_120K
_cod_depositor_comments
'Adding full bibliography for 4123615--4123618.cif.'
_cod_original_cell_volume        1062.20(6)
_cod_original_formula_sum        'C12 H17 Li2 N2 O16.50 Zr'
_cod_database_code               4123618
_chemical_oxdiff_formula         'Zr Li2 N2 C12 O16.5 H17'
_reflns_odcompleteness_completeness 97.71
_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, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C46) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C54) \\sim Ueq, Uanis(C49)
\\sim Ueq, Uanis(C50) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C44) \\sim Ueq,
Uanis(C34) \\sim Ueq, Uanis(C62) \\sim Ueq, Uanis(C61) \\sim Ueq, Uanis(C57)
\\sim Ueq, Uanis(C58) \\sim Ueq, Uanis(C55) \\sim Ueq, Uanis(C56) \\sim Ueq,
Uanis(C60) \\sim Ueq, Uanis(C59) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(O5) \\sim Ueq, Uanis(O14) \\sim Ueq, Uanis(O20) \\sim Ueq, Uanis(O21)
\\sim Ueq, Uanis(O72) \\sim Ueq, Uanis(O35) \\sim Ueq, Uanis(O28) \\sim Ueq,
Uanis(O8) \\sim Ueq, Uanis(O11) \\sim Ueq, Uanis(O25) \\sim Ueq, Uanis(O26)
\\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(O24) \\sim Ueq, Uanis(O15) \\sim Ueq,
Uanis(O1) \\sim Ueq, Uanis(O9) \\sim Ueq, Uanis(O73) \\sim Ueq, Uanis(O74)
\\sim Ueq, Uanis(O75) \\sim Ueq, Uanis(O76) \\sim Ueq, Uanis(O77) \\sim Ueq,
Uanis(O79) \\sim Ueq, Uanis(O80) \\sim Ueq, Uanis(O78) \\sim Ueq, Uanis(O7)
\\sim Ueq, Uanis(O17) \\sim Ueq, Uanis(O23) \\sim Ueq, Uanis(O3) \\sim Ueq,
Uanis(O12) \\sim Ueq, Uanis(O10) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(O16)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O6) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(Li9) \\sim Ueq, Uanis(Li7) \\sim Ueq, Uanis(Li10) \\sim Ueq, Uanis(Li1)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(N10) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(N9) \\sim
Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C8) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C2) \\sim
Ueq, Uanis(C14) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C13) \\sim Ueq,
Uanis(C10) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O14) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
3.a Rotating group:
 O6(H6A,H6B)
3.b Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), N2(H2D,H2E), N10(H10D,H10E), N9(H9D,H9E)
3.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C7(H7A,H7B,H7C), C4(H4A,H4B,H4C), C14(H14A,H14B,H14C),
 C10(H10A,H10B,H10C), C13(H13A,H13B,H13C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C)
;