Water vapour induced structural flexibility in a square lattice coordination network
Zaworotko, Michael; Koupepidou, Kyriaki; Bezrukov, Andrey A.; Castell, Dominic C.; Sensharma, Debobroto; Mukherjee, Soumya; Chemical Communications  (2023) –; doi:10.1039/D3CC04109C

data_7132278
_publ_section_title
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 Water vapour induced structural flexibility in a square lattice
 coordination network
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_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D3CC04109C
_journal_year                    2023
_chemical_formula_moiety
'C30 H23 N6 Ni O5, 2.5(C H4 O), 0.5(H2 O), 1.5[CH4O]'
_chemical_formula_sum            'C34.08 H37.75 N6 Ni O8.59'
_chemical_formula_weight         727.53
_chemical_name_common            sql-(1,3-bib)(ndc)-Ni-gamma
_space_group_crystal_system      orthorhombic
_space_group_IT_number           36
_space_group_name_Hall           'C 2c -2'
_space_group_name_H-M_alt        'C m c 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2023-10-08
_audit_creation_method
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Olex2 1.5-alpha
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
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_audit_update_record
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2023-10-08 deposited with the CCDC.	2023-10-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.0063(17)
_cell_length_b                   16.5739(13)
_cell_length_c                   18.9230(14)
_cell_measurement_reflns_used    9310
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      25.72
_cell_measurement_theta_min      2.68
_cell_volume                     6901.8(9)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'APEX3 (Bruker, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150.00
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.994
_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  0.0845
_diffrn_reflns_av_unetI/netI     0.0652
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            42736
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.102
_diffrn_reflns_theta_min         3.037
_exptl_absorpt_coefficient_mu    0.624
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.5667
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0813 before and 0.0709 after correction.
The Ratio of minimum to maximum transmission is 0.7604.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.400
_exptl_crystal_description       plate
_exptl_crystal_F_000             3047
_exptl_crystal_size_max          0.381
_exptl_crystal_size_mid          0.169
_exptl_crystal_size_min          0.094
_refine_diff_density_max         0.959
_refine_diff_density_min         -0.541
_refine_diff_density_rms         0.110
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.15(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     315
_refine_ls_number_reflns         6777
_refine_ls_number_restraints     304
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.1232
_refine_ls_R_factor_gt           0.0738
_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^)+(0.1123P)^2^+36.6550P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1842
_refine_ls_wR_factor_ref         0.2290
_reflns_Friedel_coverage         0.878
_reflns_Friedel_fraction_full    0.948
_reflns_Friedel_fraction_max     0.933
_reflns_number_gt                4464
_reflns_number_total             6777
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc04109c2.cif
_cod_data_source_block           sql-(13-bib)(ndc)-ni-gamma
_cod_database_code               7132278
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
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1. Twinned data refinement
 Scales: 0.85(5)
 0.15(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
3. Restrained distances
 C1C-O1C
 1.4 with sigma of 0.02
 O1-H1A = O1-H1B
 0.87 with sigma of 0.02
 O1A-H1AA
 0.87 with sigma of 0.02
 H1A-H1B
 1.38 with sigma of 0.04
 Ni1-H1A \\sim Ni1-H1B
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
Uanis(C17) = Uanis(N6) = Uanis(C15) = Uanis(N5) = Uanis(C16) = Uanis(C18) =
Uanis(C21) = Uanis(C20) = Uanis(C19)
Uanis(O1E) = Uanis(C1E)
Uanis(C6) = Uanis(O1D)
Uanis(C13) = Uanis(C14) = Uanis(C11) = Uanis(C12) = Uanis(N4) = Uanis(C8) =
Uanis(N3) = Uanis(C9) = Uanis(C10)
Uanis(C25) = Uanis(C24) = Uanis(C23) = Uanis(C32) = Uanis(C31) = Uanis(C30) =
Uanis(C29) = Uanis(C28) = Uanis(C27) = Uanis(C26)
Uanis(C1C) = Uanis(O1C)
Uanis(C1B) = Uanis(O1B)
Uanis(O1B) = Uanis(C1B)
5. Rigid body (RIGU) restrains
 C6, O1D
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1B, O1B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1C, O1C
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(O1E)=Sof(C1E)=Sof(H1EA)=Sof(H1EB)=Sof(H1EC)=FVAR(1)
 Sof(C1C)=Sof(H1CA)=Sof(H1CB)=Sof(H1CC)=FVAR(2)
 Fixed Sof: C1B(0.5) H1BA(0.5) H1BB(0.5) H1BC(0.5)
7.a Aromatic/amide H refined with riding coordinates:
 C32(H32), C28(H28), C1(H1), C19(H19), C2(H2), C5(H5), C10(H10), C31(H31),
 C8(H8), C3(H3), C21(H21), C7(H7), C13(H13), C9(H9), C27(H27), C15(H15),
 C25(H25), C17(H17), C26(H26), C16(H16), C14(H14), C12(H12), C20(H20), C34(H34)
7.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C1B(H1BA,H1BB,H1BC), C1C(H1CA,H1CB,H1CC), C1E(H1EA,H1EB,H1EC)
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_smtbx_masks_special_details
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A solvent mask was calculated and 224 electrons were 
found in a volume of 596\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
1.5[CH4O] per Asymmetric Unit 
which account for 216 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              19852
_shelx_hkl_checksum              95139
_shelx_fab_checksum              83729
_olex2_submission_special_instructions 'No special instructions were received'