Humidity-sensitive irreversible phase transformation of open-framework zinc phosphate and its water-assisted high proton conduction properties.
Yu, Jing-Wei; Yu, Hai-Jiao; Ren, Qiu; Zhang, Jin; Zou, Yang; Luo, Hong-Bin; Wang, Lifeng; Ren, Xiao-Ming; Dalton transactions (Cambridge, England : 2003) 50 (2021) 8070–8075; doi:10.1039/d1dt00296a

data_7707395
_publ_section_title
;
 Humidity-sensitive irreversible phase transformation of open-framework
 zinc phosphate and its water-assisted high proton conduction properties.
;
_journal_issue                   23
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8070
_journal_page_last               8075
_journal_paper_doi               10.1039/d1dt00296a
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'H6 O16 P4 Zn2, 2(C4 H12 N)'
_chemical_formula_sum            'C8 H30 N2 O16 P4 Zn2'
_chemical_formula_weight         664.96
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yc'
_space_group_name_H-M_alt        'P 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc26ry0y
_audit_creation_date             2019-10-25
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-12-07 deposited with the CCDC.	2021-05-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.872(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.4561(8)
_cell_length_b                   13.7954(14)
_cell_length_c                   10.1880(11)
_cell_measurement_reflns_used    9856
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      27.42
_cell_measurement_theta_min      2.49
_cell_volume                     1188.3(2)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0411
_diffrn_reflns_av_unetI/netI     0.0518
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            10899
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.478
_diffrn_reflns_theta_min         1.476
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.361
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4516
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1448 before and 0.0765 after correction.
The Ratio of minimum to maximum transmission is 0.6057.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.858
_exptl_crystal_description       block
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.038
_refine_diff_density_min         -0.593
_refine_diff_density_rms         0.140
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.86(2)
_refine_ls_extinction_coef       0.040(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     305
_refine_ls_number_reflns         4215
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0468
_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^)+(0.0545P)^2^+5.3826P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1199
_refine_ls_wR_factor_ref         0.1206
_reflns_Friedel_coverage         0.994
_reflns_Friedel_fraction_full    0.991
_reflns_Friedel_fraction_max     0.990
_reflns_number_gt                4097
_reflns_number_total             4215
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00296a2.cif
_cod_data_source_block           mono
_cod_depositor_comments
'Adding full bibliography for 7707395--7707396.cif.'
_cod_database_code               7707395
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.834
_shelx_estimated_absorpt_t_min   0.650
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.14(2)
 0.86(2)
2. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
3.a Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,
 H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C)
3.b Idealised tetrahedral OH refined as rotating group:
 O2(H2), O4(H4), O7(H7), O11(H11), O14(H14), O16(H16)
;
_shelx_res_checksum              72430
_olex2_submission_special_instructions 'No special instructions were received'