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_7132279
_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, 4(H2 O)'
_chemical_formula_sum            'C30 H26.76 N6 Ni O8.76'
_chemical_formula_weight         670.12
_chemical_name_common            sql-(1,3-bib)(ndc)-Ni-alpha_prime
_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             2023-10-06
_audit_creation_method
;
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                   21.9932(12)
_cell_length_b                   14.6091(8)
_cell_length_c                   19.5808(12)
_cell_measurement_reflns_used    9962
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      66.45
_cell_measurement_theta_min      3.63
_cell_volume                     6291.3(6)
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0823
_diffrn_reflns_av_unetI/netI     0.0550
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            32644
_diffrn_reflns_point_group_measured_fraction_full 0.892
_diffrn_reflns_point_group_measured_fraction_max 0.892
_diffrn_reflns_theta_full        66.664
_diffrn_reflns_theta_max         66.664
_diffrn_reflns_theta_min         3.632
_exptl_absorpt_coefficient_mu    1.421
_exptl_absorpt_correction_T_max  0.7503
_exptl_absorpt_correction_T_min  0.5282
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1676 before and 0.0978 after correction.
The Ratio of minimum to maximum transmission is 0.7040.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_description       plate
_exptl_crystal_F_000             2774
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.201
_exptl_crystal_size_min          0.094
_refine_diff_density_max         0.988
_refine_diff_density_min         -0.658
_refine_diff_density_rms         0.131
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.33(8)
_refine_ls_extinction_coef       0.0012(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     396
_refine_ls_number_reflns         5109
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0970
_refine_ls_R_factor_gt           0.0813
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1708P)^2^+7.5726P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2268
_refine_ls_wR_factor_ref         0.2440
_reflns_Friedel_coverage         0.741
_reflns_Friedel_fraction_full    0.786
_reflns_Friedel_fraction_max     0.786
_reflns_number_gt                4355
_reflns_number_total             5109
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc04109c2.cif
_cod_data_source_block           sql-(13-bib)(ndc)-ni-alpha_prime
_cod_database_code               7132279
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
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1. Twinned data refinement
 Scales: 0.67(8)
 0.33(8)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
3. Restrained distances
 O1C-H1C
 0.87 with sigma of 0.02
 O1-H1A = O1-H1B
 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
C2 \\sim C3 \\sim N1 \\sim C1 \\sim N2: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
Uanis(C16) = Uanis(N5) = Uanis(C15) = Uanis(N6) = Uanis(C17)
Uanis(N1) = Uanis(C1) = Uanis(N2) = Uanis(C2) = Uanis(C3) = Uanis(C4) =
Uanis(C5) = Uanis(C7) = Uanis(C6)
Uanis(C13) = Uanis(C14) = Uanis(C11) = Uanis(C12)
5. Rigid body (RIGU) restrains
 C3, N1, C1, N2, C2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(O1E)=Sof(H1E)=FVAR(1)
 Sof(O1G)=Sof(H1GA)=Sof(H1GB)=FVAR(2)
 Fixed Sof: O1B(0.5) O1C(0.5) H1C(0.5) O1D(0.5) O1H(0.25) O1F(0.25)
7.a Free rotating group:
 O1A(H1AA), O1E(H1E), O1G(H1GA,H1GB)
7.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C1(H1), C19(H19), C14(H14), C20(H20), C12(H12), C25(H25), C21(H21),
 C9(H9), C15(H15), C17(H17), C5(H5), C28(H28), C32(H32), C8(H8), C26(H26),
 C16(H16), C2(H2), C10(H10), C3(H3), C31(H31), C7(H7), C27(H27), C6(H6)
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_shelx_res_checksum              89845
_shelx_hkl_checksum              63395
_olex2_submission_special_instructions 'No special instructions were received'