Exploring Reversible Thermochromic Behavior in a Rare Ni(II)-MOF System.
Zhang, Shihui; Zhang, Shuyu; Yin, Nan; Huang, Zhenqi; Xu, Wenhua; Yue, Kefen; Li, Xiuyuan; Li, Dongsheng; ACS applied materials & interfaces 13 (2021) 6430–6441; doi:10.1021/acsami.0c21116

data_4518517
_publ_section_title
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 Exploring Reversible Thermochromic Behavior in a Rare Ni(II)-MOF System.
;
_journal_issue                   5
_journal_name_full               'ACS applied materials &amp; interfaces'
_journal_page_first              6430
_journal_page_last               6441
_journal_paper_doi               10.1021/acsami.0c21116
_journal_volume                  13
_journal_year                    2021
_chemical_formula_moiety         'C31 H30 N12 Ni2 O10 S2, C H4 O, H2 O'
_chemical_formula_sum            'C32 H36 N12 Ni2 O12 S2'
_chemical_formula_weight         962.27
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-05-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.18 svn.r3508 for OlexSys, GUI svn.r5497)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   21.5743(8)
_cell_length_b                   21.5743(8)
_cell_length_c                   34.449(2)
_cell_measurement_reflns_used    6298
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      23.37
_cell_measurement_theta_min      2.72
_cell_volume                     16034.3(13)
_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      296.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0629
_diffrn_reflns_av_unetI/netI     0.0471
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            44264
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.336
_diffrn_reflns_theta_min         1.888
_exptl_absorpt_coefficient_mu    1.120
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.594
_exptl_crystal_description       block
_exptl_crystal_F_000             7936
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.589
_refine_diff_density_min         -0.499
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     575
_refine_ls_number_reflns         8135
_refine_ls_number_restraints     848
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0605
_refine_ls_R_factor_gt           0.0394
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0510P)^2^+18.9800P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0957
_refine_ls_wR_factor_ref         0.1063
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6145
_reflns_number_total             8135
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            am0c21116_si_005.cif
_cod_data_source_block           xb1397_0m
_cod_original_cell_volume        16034.1(16)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               4518517
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.887
_shelx_estimated_absorpt_t_min   0.868
_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 C(H,H,H,H,H,H) groups, All O(H) groups, All O(H,H)
  groups
2. Restrained distances
 O9A-H9AA
 0.85 with sigma of 0.01
 O9-H9B
 0.85 with sigma of 0.01
 H0AB-H0AA
 1.42 with sigma of 0.005
 H1AA-H1AB
 1.42 with sigma of 0.005
 O1AA-H1AA = O1AA-H1AB = O0AA-H0AB = O0AA-H0AA
 0.85 with sigma of 0.005
 C31-H9AA
 1.911993 with sigma of 0.02
 Ni2-H9AA
 2.776755 with sigma of 0.02
 C31-H9B
 1.91144 with sigma of 0.02
 Ni2-H9B
 2.771364 with sigma of 0.02
 O9A-C31 \\sim O9-C31
 with sigma of 0.02
 Ni2-O9A \\sim Ni2-O9
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17
\\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25
\\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim O1
\\sim O2 \\sim O3 \\sim O4 \\sim O5 \\sim O6 \\sim O7 \\sim O8 \\sim O9 \\sim
O10 \\sim O11 \\sim O9A \\sim O0AA \\sim O1AA: within 3.8A with sigma of 0.01
and sigma for terminal atoms of 0.02
Uanis(O11) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(H31D)=Sof(H31E)=Sof(H31F)=Sof(O9A)=Sof(H9AA)=1-FVAR(1)
 Sof(H31A)=Sof(H31B)=Sof(H31C)=Sof(O9)=Sof(H9B)=FVAR(1)
 Sof(O1AA)=Sof(H1AA)=Sof(H1AB)=1-FVAR(2)
 Sof(O0AA)=Sof(H0AA)=Sof(H0AB)=FVAR(2)
5.a Riding coordinates:
 O0AA(H0AA,H0AB), O1AA(H1AA,H1AB)
5.b Rotating group:
 O10(H10A,H10B)
5.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C5(H5), C7(H7), C9(H9), C11(H11), C12(H12), C14(H14),
 C15(H15), C16(H16), C17(H17), C20(H20), C22(H22), C24(H24), C26(H26), C27(H27),
  C29(H29), C30(H30), N2(H2A), N3(H3), N8(H8), N9(H9A), N11(H11A)
5.d Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C31(H31D,H31E,H31F), C32(H32A,H32B,H32C)
5.e Idealised tetrahedral OH refined as rotating group:
 O11(H11B)
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_shelx_res_checksum              46640
_shelx_hkl_checksum              18113
_olex2_submission_special_instructions 'No special instructions were received'