Glass-phase coordination polymer displaying proton conductivity and guest-accessible porosity
Inukai, Munehiro; Nishiyama, Yusuke; Honjo, Kayako; Das, Chinmoy; Kitagawa, Susumu; Horike, Satoshi; Chemical Communications  (2019) –; doi:10.1039/C9CC02744K

data_7123723
_publ_section_title
;
 Glass-phase coordination polymer displaying proton conductivity and
 guest-accessible porosity
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC02744K
_journal_year                    2019
_chemical_formula_moiety
'H4 O12 P3 Zn2, 2(C7 H6 Cl N2), H2 O4 P, C H4 O'
_chemical_formula_sum            'C15 H22 Cl2 N4 O17 P4 Zn2'
_chemical_formula_weight         855.88
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_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
_audit_creation_date             2019-05-09
_audit_creation_method
;
Olex2 1.3-dev
(compiled 2019.03.18 svn.r3573 for OlexSys, GUI svn.r5585)
;
_audit_update_record
;
2019-06-10 deposited with the CCDC.    2019-06-24 downloaded from the CCDC.
;
_cell_angle_alpha                97.386(10)
_cell_angle_beta                 91.735(8)
_cell_angle_gamma                96.000(12)
_cell_formula_units_Z            2
_cell_length_a                   5.159(3)
_cell_length_b                   15.964(8)
_cell_length_c                   18.237(10)
_cell_measurement_reflns_used    3185
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      27.4816
_cell_measurement_theta_min      3.2003
_cell_volume                     1479.9(14)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      223.25
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0811
_diffrn_reflns_av_unetI/netI     0.1465
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            9800
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         1.825
_exptl_absorpt_coefficient_mu    2.099
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8179
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.921
_exptl_crystal_description       prism
_exptl_crystal_F_000             860
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.049
_refine_diff_density_min         -0.764
_refine_diff_density_rms         0.170
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     405
_refine_ls_number_reflns         5078
_refine_ls_number_restraints     151
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.1488
_refine_ls_R_factor_gt           0.0865
_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^)+(0.0536P)^2^+14.3541P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1671
_refine_ls_wR_factor_ref         0.2031
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2957
_reflns_number_total             5078
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc02744k2.cif
_cod_data_source_block           znpclbim
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_cell_volume        1479.8(13)
_cod_database_code               7123723
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.679
_shelx_estimated_absorpt_t_min   0.679
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 H11-O1S
 1 with sigma of 0.1
3. Rigid body (RIGU) restrains
 C4, N1, C1, C2, N2, C3, C7, C6, C5, Cl1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C8, N3, C9, N4, C10, C14, C11, C13, C12, Cl2
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4.a Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), N3(H3A), N4(H4), C1(H1A), C3(H3), C5(H5A), C6(H6A), C8(H8),
 C10(H10), C11(H11A), C13(H13)
4.b Idealised Me refined as rotating group:
 C1S(H1SA,H1SB,H1SC)
4.c Idealised tetrahedral OH refined as rotating group:
 O5(H5), O6(H6), O11(H11), O12(H12), O14(H14), O15(H15), O1S(H1S)
;
_smtbx_masks_void_probe_radius   0.9
_smtbx_masks_void_truncation_radius 1.0
_shelx_res_checksum              99753
_olex2_submission_special_instructions 'No special instructions were received'