<i>In Situ</i> Aliovalent Nickle Substitution and Acidic Modification of Nanowalls Promoted Proton Conductivity in InOF with 1D Helical Channel.
Gao, Hui; He, Yan-Bin; Hou, Juan-Juan; Zhang, Xian-Ming; ACS applied materials & interfaces 13 (2021) 38289–38295; doi:10.1021/acsami.1c09001

data_4518950
_publ_section_title
;
 <i>In Situ</i> Aliovalent Nickle Substitution and Acidic Modification of
 Nanowalls Promoted Proton Conductivity in InOF with 1D Helical Channel.
;
_journal_issue                   32
_journal_name_full               'ACS applied materials &amp; interfaces'
_journal_page_first              38289
_journal_page_last               38295
_journal_paper_doi               10.1021/acsami.1c09001
_journal_volume                  13
_journal_year                    2021
_chemical_formula_moiety         'C18 H10 Ni2 O12, 3(O)'
_chemical_formula_sum            'C18 H10 Ni2 O15'
_chemical_formula_weight         583.68
_space_group_crystal_system      tetragonal
_space_group_IT_number           98
_space_group_name_Hall           'I 4bw 2bw'
_space_group_name_H-M_alt        'I 41 2 2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-11-04
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.1751(3)
_cell_length_b                   15.1751(3)
_cell_length_c                   12.0768(4)
_cell_measurement_reflns_used    9904
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      3.37
_cell_volume                     2781.09(12)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-III CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0602
_diffrn_reflns_av_unetI/netI     0.0252
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            15576
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.677
_diffrn_reflns_theta_min         2.684
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.415
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6685
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0809 before and 0.0738 after correction.
The Ratio of minimum to maximum transmission is 0.8970.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_description       rod
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.234
_refine_diff_density_min         -0.764
_refine_diff_density_rms         0.172
_refine_ls_abs_structure_details
;
 Flack x determined using 501 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.023(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.195
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     106
_refine_ls_number_reflns         1326
_refine_ls_number_restraints     56
_refine_ls_restrained_S_all      1.234
_refine_ls_R_factor_all          0.0619
_refine_ls_R_factor_gt           0.0575
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1043P)^2^+17.4977P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1656
_refine_ls_wR_factor_ref         0.1711
_reflns_Friedel_coverage         0.691
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                1255
_reflns_number_total             1326
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            am1c09001_si_004.cif
_cod_data_source_block           201020a_a_pl
_cod_original_cell_volume        2781.09(14)
_cod_database_code               4518950
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.946
_shelx_estimated_absorpt_t_min   0.849
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All O(H) groups
2. Restrained distances
 O3-O4
 2.25 with sigma of 0.01
 C6-O3 \\sim C6-O4
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
O3 \\sim O4 \\sim C6: within 2A with sigma of 0.01 and sigma for terminal atoms
of 0.02 within 2A
Uanis(O5) \\sim Ueq, Uanis(O5A) \\sim Ueq, Uanis(O7) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(O3) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(C6) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(O4) \\sim Ueq: with sigma of 0.003 and sigma for terminal atoms of 0.006
Uanis(O7A) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(O5A) \\sim Ueq: with sigma of
0.006 and sigma for terminal atoms of 0.012
Uanis(O5) \\sim Ueq: with sigma of 0.003 and sigma for terminal atoms of 0.006
Uanis(O5A) = Uanis(O5)
Uanis(O7) = Uanis(O7A)
4. Others
 Fixed Sof: O4(0.5) H4(0.5) C6(0.5) H6(0.5) O5(0.32) O5A(0.16) O7(0.16)
 O7A(0.11)
5.a Riding coordinates:
 O4(H4)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C6(H6)
;
_shelx_res_checksum              68428
_shelx_hkl_checksum              75072
_olex2_submission_special_instructions 'No special instructions were received'