Tuneable mechanical and dynamical properties in the ferroelectric perovskite solid solution [NH3NH2]1−x[NH3OH]xZn(HCOO)3
Kieslich, Gregor; Kumagai, Shohei; Forse, Alexander C.; Sun, Shijing; Henke, Sebastian; Yamashita, Masahiro; Grey, Clare P.; Cheetham, Anthony K.; Chem. Sci. 7 (2016) 5108–; doi:10.1039/C6SC01247G

data_1543107
_publ_section_title
;
 Tuneable mechanical and dynamical properties in the ferroelectric
 perovskite solid solution [NH3NH2]1&#x2212;x[NH3OH]xZn(HCOO)3
;
_journal_issue                   8
_journal_name_full               'Chem. Sci.'
_journal_page_first              5108
_journal_paper_doi               10.1039/C6SC01247G
_journal_volume                  7
_journal_year                    2016
_chemical_formula_moiety         'C3 H3 O6 Zn, H5 N2'
_chemical_formula_sum            'C3 H8 N2 O6 Zn'
_chemical_formula_weight         233.48
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-02-25
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-03-18 deposited with the CCDC.
2016-04-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.6706(2)
_cell_length_b                   7.72008(19)
_cell_length_c                   11.4872(3)
_cell_measurement_reflns_used    6673
_cell_measurement_temperature    123(3)
_cell_measurement_theta_max      45.1660
_cell_measurement_theta_min      1.7810
_cell_volume                     768.93(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
;
_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_environment      N~2~
_diffrn_ambient_temperature      123(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1183
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega -117.00  -35.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.0078 -178.0000   60.0000 82

  2 omega -106.00   58.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.0078   19.0000  -30.0000 164

  3 omega  100.00  147.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       63.7857  111.0000 -180.0000 47

  4 omega  100.00  147.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       63.7857  111.0000   90.0000 47

  5 omega  100.00  147.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       63.7857  111.0000   60.0000 47

  6 omega -147.00  -79.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.7232 -111.0000  -30.0000 68

  7 omega -139.00  -30.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.7232  -61.0000   60.0000 109

  8 omega  -48.00   17.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.7232   30.0000 -120.0000 65

  9 omega -132.00  -32.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.7232  178.0000  -90.0000 100

 10 omega  -33.00   14.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0703  111.0000   79.0000 47

 11 omega -101.00    9.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.0078  -55.0000 -141.0000 110

 12 omega -142.00  -78.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.7232  -45.0000  120.0000 64
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0183510000
_diffrn_orient_matrix_UB_12      -0.0473518000
_diffrn_orient_matrix_UB_13      -0.0510209000
_diffrn_orient_matrix_UB_21      0.0512818000
_diffrn_orient_matrix_UB_22      0.0527624000
_diffrn_orient_matrix_UB_23      -0.0326168000
_diffrn_orient_matrix_UB_31      0.0610478000
_diffrn_orient_matrix_UB_32      -0.0584626000
_diffrn_orient_matrix_UB_33      0.0119922000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0283
_diffrn_reflns_av_unetI/netI     0.0290
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            17865
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         45.249
_diffrn_reflns_theta_min         1.773
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.191
_exptl_absorpt_correction_T_max  0.950
_exptl_absorpt_correction_T_min  0.912
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
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)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    2.017
_exptl_crystal_description       block
_exptl_crystal_F_000             472
_exptl_crystal_size_max          0.5448
_exptl_crystal_size_mid          0.4692
_exptl_crystal_size_min          0.2716
_refine_diff_density_max         0.750
_refine_diff_density_min         -0.802
_refine_diff_density_rms         0.086
_refine_ls_abs_structure_details
;
 Flack x determined using 2043 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.005(6)
_refine_ls_extinction_coef       0.0463(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     118
_refine_ls_number_reflns         5935
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0299
_refine_ls_R_factor_gt           0.0233
_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^)+(0.0214P)^2^+0.0654P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0512
_refine_ls_wR_factor_ref         0.0541
_reflns_Friedel_coverage         0.937
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                5169
_reflns_number_total             5935
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6sc01247g2.cif
_cod_data_source_block           Zn-hox-0_120K
_cod_depositor_comments
'Adding full bibliography for 1543107--1543108.cif.'
_cod_database_code               1543107
_chemical_oxdiff_formula         'Zn1 O6 C3 N2 H8'
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.541(10) 0.459(10)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups, All N(H,H,H) groups
3. Restrained distances
 N2-H2B
 1.01 with sigma of 0.02
 H2B-H2A
 1.49 with sigma of 0.04
 N1-H2B = N1-H2A
 1.97 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
Uiso(H2B) = Uiso(H2A) = Uiso(H1C)
5.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C3(H3), C4(H4)
5.b Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_shelx_res_checksum              34487
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'