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_1543108
_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_absolute_configuration unk
_chemical_formula_moiety         'C3 H3 O6 Zn, H4.5 N1.5 O0.5'
_chemical_formula_sum            'C3 H7.5 N1.5 O6.5 Zn'
_chemical_formula_weight         233.97
_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             2016-03-17
_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                   8.61779(12)
_cell_length_b                   7.73073(10)
_cell_length_c                   11.50052(16)
_cell_measurement_reflns_used    5878
_cell_measurement_temperature    119.8(6)
_cell_measurement_theta_max      45.2920
_cell_measurement_theta_min      3.5350
_cell_volume                     766.185(18)
_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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      119.8(6)
_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 0.996
_diffrn_measurement_details
;
  1 omega  -67.00   54.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.1328   77.0000  -90.0000 121

  2 omega  -67.00   54.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.1328   77.0000 -120.0000 121

  3 omega  -67.00   54.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.1328   77.0000  150.0000 121

  4 omega   23.00  144.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       63.7857   77.0000 -120.0000 121

  5 omega   23.00  144.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       63.7857   77.0000  -90.0000 121

  6 omega   23.00  144.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       63.7857   77.0000 -180.0000 121

  7 omega -106.00   16.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.7232   77.0000  150.0000 122

  8 omega   -9.00   96.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       25.1953   57.0000   60.0000 105

  9 omega  -25.00   28.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       25.1953   96.0000  177.0000 53
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0702531000
_diffrn_orient_matrix_UB_12      -0.0461682000
_diffrn_orient_matrix_UB_13      -0.0083533000
_diffrn_orient_matrix_UB_21      0.0425640000
_diffrn_orient_matrix_UB_22      0.0724268000
_diffrn_orient_matrix_UB_23      0.0204164000
_diffrn_orient_matrix_UB_31      -0.0049723000
_diffrn_orient_matrix_UB_32      -0.0324042000
_diffrn_orient_matrix_UB_33      0.0575723000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_av_unetI/netI     0.0319
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            18244
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         45.478
_diffrn_reflns_theta_min         1.771
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.205
_exptl_absorpt_correction_T_max  0.532
_exptl_absorpt_correction_T_min  0.443
_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_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.028
_exptl_crystal_description       block
_exptl_crystal_F_000             472
_exptl_crystal_size_max          0.2905
_exptl_crystal_size_mid          0.2851
_exptl_crystal_size_min          0.231
_refine_diff_density_max         0.603
_refine_diff_density_min         -0.687
_refine_diff_density_rms         0.093
_refine_ls_abs_structure_details
;
 Flack x determined using 1845 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.005(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     141
_refine_ls_number_reflns         5999
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0393
_refine_ls_R_factor_gt           0.0264
_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^)+(0.0232P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0537
_refine_ls_wR_factor_ref         0.0581
_reflns_Friedel_coverage         0.937
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                4821
_reflns_number_total             5999
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6sc01247g2.cif
_cod_data_source_block           Zn-hox-48_120K
_cod_depositor_comments
'Adding full bibliography for 1543107--1543108.cif.'
_cod_original_cell_volume        766.186(18)
_cod_original_formula_sum        'C3 H7.50 N1.50 O6.50 Zn'
_cod_database_code               1543108
_chemical_oxdiff_formula         'Zn1 O6.5 N1.5 H7 C3'
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.58144 0.41856
2. Fixed Uiso
 At 1.5 times of:
  All N(H,H) groups, All N(H,H,H) groups, All O(H) groups
3. Restrained distances
 N2-H2A
 0.87 with sigma of 0.02
 N2-H2B
 0.87 with sigma of 0.02
 N1-H1A = N1-H1B = N1-H1C
 0.87 with sigma of 0.001
 O7-H7
 0.82 with sigma of 0.02
 N1-H2B = N1-H1A
 1.95 with sigma of 0.04
4. Others
 Sof(N2)=Sof(H2A)=Sof(H2B)=1-FVAR(1)
 Sof(O7)=Sof(H7)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_original_sample_id solidsolution_NH3NH2ZnHCOO3
_olex2_submission_special_instructions 'No special instructions were received'