Molecular ferroelectric pyridin-2-ylmethanaminium perchlorate with phase transition induced by disorder of perchlorate
Gan, Xuecheng; Tang, Zheng; Zhang, Wenjun; Xu, Cong; Sun, Xiaofan; Gao, Zhangran; Wu, Yizhang; Cai, Hong-Ling; Wu, X. S.; RSC Advances 9 (2019) 5470–; doi:10.1039/C8RA10031D

data_7232357
_publ_section_title
;
 Molecular ferroelectric pyridin-2-ylmethanaminium perchlorate with phase
 transition induced by disorder of perchlorate
;
_journal_issue                   10
_journal_name_full               'RSC Advances'
_journal_page_first              5470
_journal_paper_doi               10.1039/C8RA10031D
_journal_volume                  9
_journal_year                    2019
_chemical_formula_moiety         '2(Cl O4), C6 H10 N2'
_chemical_formula_sum            'C6 H10 Cl2 N2 O8'
_chemical_formula_weight         309.06
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-09-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-10-12 deposited with the CCDC.
2019-01-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.470(9)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.868(7)
_cell_length_b                   15.208(9)
_cell_length_c                   13.240(8)
_cell_measurement_temperature    293(2)
_cell_volume                     2387(2)
_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_temperature      293.15
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0401
_diffrn_reflns_av_unetI/netI     0.0542
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            17113
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.393
_diffrn_reflns_theta_min         1.718
_exptl_absorpt_coefficient_mu    0.580
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.720
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1264
_refine_diff_density_max         0.735
_refine_diff_density_min         -0.490
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     392
_refine_ls_number_reflns         5393
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.129
_refine_ls_R_factor_all          0.0902
_refine_ls_R_factor_gt           0.0631
_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^)+(0.1000P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1731
_refine_ls_wR_factor_ref         0.2007
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3894
_reflns_number_total             5393
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ra10031d2.cif
_cod_data_source_block           1
_cod_database_code               7232357
_shelxl_version_number           2013-2
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H,H) groups
2. Restrained distances
 Cl4-O0AA \\sim Cl4-O0AB
 with sigma of 0.02
 Cl4-O4 \\sim Cl4-O4A
 with sigma of 0.02
 Cl4-O2AA \\sim Cl4-O2AB
 with sigma of 0.02
 Cl3-O3 \\sim Cl3-O3A
 with sigma of 0.02
 Cl3-O5 \\sim Cl3-O5A
 with sigma of 0.02
 Cl3-O6 \\sim Cl3-O6A
 with sigma of 0.02
 Cl3-O1AA \\sim Cl3-O1AB
 with sigma of 0.02
3. Others
 Sof(O4A)=Sof(O0AB)=Sof(O2AB)=1-FVAR(1)
 Sof(O0AA)=Sof(O4)=Sof(O2AA)=FVAR(1)
 Sof(O1AB)=Sof(O3A)=Sof(O6A)=Sof(O5A)=1-FVAR(2)
 Sof(O3)=Sof(O5)=Sof(O6)=Sof(O1AA)=FVAR(2)
4.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C6(H6A,H6B)
4.b Aromatic/amide H refined with riding coordinates:
 N4(H4), N9(H9), C14(H14), C16(H16), C17(H17), C19(H19), C20(H20), C23(H23),
 C24(H24), C26(H26)
4.c Idealised Me refined as rotating group:
 N3(H3A,H3B,H3C), N5(H5A,H5B,H5C)
;
_shelx_res_checksum              97002
_olex2_submission_special_instructions 'No special instructions were received'