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_7132276
_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, 0.5(C4 H9 N O), 2.5(H2 O)'
_chemical_formula_sum            'C32 H30.83 N6.5 Ni O7.96'
_chemical_formula_weight         692.43
_chemical_name_common            sql-(1,3-bib)(ndc)-Ni-alpha
_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             2023-10-05
_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                   21.9995(8)
_cell_length_b                   14.6850(5)
_cell_length_c                   19.4382(6)
_cell_measurement_reflns_used    9920
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      28.26
_cell_measurement_theta_min      2.97
_cell_volume                     6279.8(4)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0416
_diffrn_reflns_av_unetI/netI     0.0203
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            83467
_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         26.372
_diffrn_reflns_theta_min         2.797
_exptl_absorpt_coefficient_mu    0.681
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6897
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0669 before and 0.0611 after correction.
The Ratio of minimum to maximum transmission is 0.9249.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.465
_exptl_crystal_description       plate
_exptl_crystal_F_000             2880
_exptl_crystal_size_max          0.597
_exptl_crystal_size_mid          0.513
_exptl_crystal_size_min          0.118
_refine_diff_density_max         0.672
_refine_diff_density_min         -0.571
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.140(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     476
_refine_ls_number_reflns         6602
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0377
_refine_ls_R_factor_gt           0.0331
_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^)+(0.0469P)^2^+8.5016P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0843
_refine_ls_wR_factor_ref         0.0877
_reflns_Friedel_coverage         0.939
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                6140
_reflns_number_total             6602
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc04109c2.cif
_cod_data_source_block           sql-(13-bib)(ndc)-ni-alpha
_cod_original_formula_sum        'C32 H30.83 N6.50 Ni O7.96'
_cod_database_code               7132276
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.924
_shelx_estimated_absorpt_t_min   0.687
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.860(16)
 0.140(16)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All H(H) groups, All C(H,H,H) groups, All O(H,H) groups
3. Restrained distances
 O1D-H1DA = O1D-H1DB
 0.87 with sigma of 0.02
 O1E-H1EA = O1E-H1EB
 0.87 with sigma of 0.02
 H1DA-H1DB
 1.38 with sigma of 0.04
 H1EA-H1EB
 1.38 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
Uanis(C1A) = Uanis(C2A) = Uanis(N1A) = Uanis(C4A) = Uanis(O1A)
5. Others
 Sof(O1D)=Sof(H1DA)=Sof(H1DB)=Sof(H1C)=FVAR(1)
 Sof(O1E)=Sof(H1EA)=Sof(H1EB)=FVAR(2)
 Fixed Sof: H3AA(0.5) H3AB(0.5) H3AC(0.5) C2A(0.5) H2AA(0.5) H2AB(0.5)
 H2AC(0.5) C4A(0.5) O1A(0.5) C1A(0.5) H1AA(0.5) H1AB(0.5) H1AC(0.5)
6.a Rotating group:
 O1(H1A,H1B)
6.b Aromatic/amide H refined with riding coordinates:
 C20(H20), C32(H32), C21(H21), C7(H7), C15(H15), C25(H25), C9(H9), C3(H3),
 C31(H31), C13(H13), C28(H28), C8(H8), C26(H26), C5(H5), C14(H14), C19(H19),
 C2(H2), C27(H27), C12(H12), C10(H10), C6(H6), C17(H17), C16(H16), C1(H1)
6.c Idealised Me refined as rotating group:
 C3A(H3AA,H3AB,H3AC), C2A(H2AA,H2AB,H2AC), C1A(H1AA,H1AB,H1AC)
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_shelx_res_checksum              3264
_shelx_hkl_checksum              58614
_olex2_submission_special_instructions 'No special instructions were received'