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_7132280
_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, (H2 O)'
_chemical_formula_sum            'C30 H25.5 N6 Ni O6'
_chemical_formula_weight         624.77
_chemical_name_common            sql-(1,3-bib)(ndc)-Ni-beta_vacuum
_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             2023-09-30
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_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                   21.925(4)
_cell_length_b                   13.614(3)
_cell_length_c                   19.848(3)
_cell_measurement_reflns_used    9798
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      24.60
_cell_measurement_theta_min      2.70
_cell_volume                     5924.4(19)
_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  0.0951
_diffrn_reflns_av_unetI/netI     0.0393
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            91643
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.099
_diffrn_reflns_theta_max         25.099
_diffrn_reflns_theta_min         2.704
_exptl_absorpt_coefficient_mu    0.708
_exptl_absorpt_correction_T_max  0.960
_exptl_absorpt_correction_T_min  0.668
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1134 before and 0.0912 after correction.
The Ratio of minimum to maximum transmission is 0.6954.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.401
_exptl_crystal_description       plate
_exptl_crystal_F_000             2588
_exptl_crystal_size_max          0.576
_exptl_crystal_size_mid          0.202
_exptl_crystal_size_min          0.058
_refine_diff_density_max         1.285
_refine_diff_density_min         -0.632
_refine_diff_density_rms         0.117
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.10(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         5408
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.1042
_refine_ls_R_factor_gt           0.0796
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1256P)^2^+42.3540P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2076
_refine_ls_wR_factor_ref         0.2344
_reflns_Friedel_coverage         0.934
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                4214
_reflns_number_total             5408
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc04109c2.cif
_cod_data_source_block           sql-(13-bib)(ndc)-ni-beta_vacuum
_cod_original_cell_volume        5924.5(18)
_cod_original_formula_sum        'C30 H25.50 N6 Ni O6'
_cod_database_code               7132280
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.960
_shelx_estimated_absorpt_t_min   0.686
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.90(5)
 0.10(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
3. Restrained distances
 C2-C6A
 1.4 with sigma of 0.02
 C7B-C6B
 1.4 with sigma of 0.02
 C4A-C5
 1.4 with sigma of 0.02
 C4B-C5
 1.4 with sigma of 0.02
 O1A-H1AA
 0.87 with sigma of 0.02
 O1B-H1BA = O1B-H1BB
 0.87 with sigma of 0.02
 H1BA-H1BB
 1.38 with sigma of 0.04
 N2-C4A \\sim N2-C4B
 with sigma of 0.02
 C5-C4A \\sim C5-C4B
 with sigma of 0.02
 C4A-C2 \\sim C4B-C7B
 with sigma of 0.02
 C2-C6A \\sim C7B-C6B
 with sigma of 0.02
 N2-C2 \\sim N2-C7B
 with sigma of 0.04
 C5-C2 \\sim C5-C7B
 with sigma of 0.04
 C4A-C6A \\sim C4B-C6B
 with sigma of 0.04
 N1-C3A \\sim N1-C3B
 with sigma of 0.02
 N2-C2A \\sim N2-C2B
 with sigma of 0.02
 C3A-C2A \\sim C3B-C2B
 with sigma of 0.02
 N1-C2A \\sim N1-C2B
 with sigma of 0.04
 N2-C3A \\sim N2-C3B
 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
Uanis(C5) = Uanis(C4A) = Uanis(C2) = Uanis(C6A)
Uanis(N2) = Uanis(C1) = Uanis(N1) = Uanis(C3A) = Uanis(C2A)
Uanis(C28) = Uanis(C27) = Uanis(C26) = Uanis(C25) = Uanis(C24) = Uanis(C23) =
Uanis(C32) = Uanis(C31) = Uanis(C30) = Uanis(C29)
Uanis(C2B) = Uanis(C3B) = Uanis(N1) = Uanis(C1) = Uanis(N2)
Uanis(C4A) = Uanis(C5) = Uanis(C2) = Uanis(C6A)
Uanis(C3A) = Uanis(N1) = Uanis(C1) = Uanis(N2) = Uanis(C2A)
Uanis(C6B) = Uanis(C7B) = Uanis(C4B) = Uanis(C5) = Uanis(C2B) = Uanis(N2) =
Uanis(C1) = Uanis(N1) = Uanis(C3B)
Uanis(C12) = Uanis(C13) = Uanis(N3) = Uanis(C9) = Uanis(C10)
Uanis(C14) = Uanis(C11) = Uanis(N4) = Uanis(C8) = Uanis(N3) = Uanis(C9) =
Uanis(C10) = Uanis(C13) = Uanis(C12)
Uanis(C13) = Uanis(C12)
Uanis(C21) = Uanis(C18) = Uanis(C19) = Uanis(C20)
Uanis(C17B) = Uanis(C16B) = Uanis(N6) = Uanis(C15B) = Uanis(N5B)
5. Others
 Sof(C4B)=Sof(C7B)=Sof(H7B)=1-FVAR(1)
 Sof(C4A)=Sof(C2)=Sof(H2)=FVAR(1)
 Sof(C3B)=Sof(H3B)=Sof(C2B)=Sof(H2B)=1-FVAR(2)
 Sof(C3A)=Sof(H3A)=Sof(C2A)=Sof(H2A)=FVAR(2)
 Fixed Sof: H1AA(0.5) H5A(0.25) H5B(0.25) C6A(0.25) H6A(0.25) C6B(0.25)
 H6B(0.25)
6.a Rotating group:
 O1(H1A,H1B)
6.b Aromatic/amide H refined with riding coordinates:
 C31(H31), C32(H32), C1(H1), C9(H9), C10(H10), C14(H14), C26(H26), C17B(H17B),
 C25(H25), C27(H27), C16B(H16B), C28(H28), C21(H21), C5(H5A), C5(H5B),
 C15B(H15B), C3A(H3A), C12(H12), C13(H13), C20(H20), C2A(H2A), C2(H2), C19(H19),
  C6A(H6A), C7B(H7B), C6B(H6B), C3B(H3B), C2B(H2B), C8(H8)
;
_shelx_res_checksum              41119
_shelx_hkl_checksum              40395
_olex2_submission_special_instructions 'No special instructions were received'