Water-reservoir properties dependent on packing modes of [Ni(ii)3L6] cages
Gwak, Geonwoo; An, Seonghyeon; Kim, Dongwon; Di Serio, Martino; Jung, Ok-Sang; New Journal of Chemistry 46 (2022) 23239–23244; doi:10.1039/D2NJ04751A

data_7062112
_publ_section_title
;
 Water-reservoir properties dependent on packing modes of [Ni(ii)3L6]
 cages
;
_journal_issue                   48
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              23239
_journal_page_last               23244
_journal_paper_doi               10.1039/D2NJ04751A
_journal_volume                  46
_journal_year                    2022
_chemical_formula_moiety         'C84 H90 F18 N12 Ni3 O6 Si6, 6Br, 34(H2O)'
_chemical_formula_sum            'C84 H170 Br6 F18 N12 Ni3 O40 Si6'
_chemical_formula_weight         3154.44
_space_group_crystal_system      tetragonal
_space_group_IT_number           114
_space_group_name_Hall           'P -4 2n'
_space_group_name_H-M_alt        'P -4 21 c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2019/2
_audit_update_record
;
2022-11-05 deposited with the CCDC.	2022-11-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   30.232(4)
_cell_length_b                   30.232(4)
_cell_length_c                   30.935(6)
_cell_measurement_reflns_used    344639
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      33.974
_cell_measurement_theta_min      0.435
_cell_volume                     28274(8)
_computing_cell_refinement       'HKL3000sm (Otwinowski & Minor, 1997)'
_computing_data_collection       'PAL BL2D-SMDC Program (Shin et. al, 2016)'
_computing_data_reduction        'HKL3000sm (Otwinowski & Minor, 1997)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick, 2013)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Rayonix MX225HS CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.760
_diffrn_reflns_av_R_equivalents  0.0964
_diffrn_reflns_av_unetI/netI     0.0578
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            177141
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        27.129
_diffrn_reflns_theta_max         28.000
_diffrn_reflns_theta_min         1.581
_diffrn_source                   'PLSII 2D bending magnet'
_exptl_absorpt_coefficient_mu    2.638
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.856
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'HKL3000sm Scalepack(Otwinowski et.al,2003)'
_exptl_crystal_colour            'pale green'
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_description       block
_exptl_crystal_F_000             12944
_exptl_crystal_size_max          0.090
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.780
_refine_diff_density_min         -0.623
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details
;
 Flack x determined using 5530 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.034(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.950
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1256
_refine_ls_number_reflns         27646
_refine_ls_number_restraints     1190
_refine_ls_restrained_S_all      0.953
_refine_ls_R_factor_all          0.1134
_refine_ls_R_factor_gt           0.0670
_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^)+(0.1335P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1819
_refine_ls_wR_factor_ref         0.2112
_reflns_Friedel_coverage         0.891
_reflns_Friedel_fraction_full    0.993
_reflns_Friedel_fraction_max     0.992
_reflns_number_gt                15665
_reflns_number_total             27646
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj04751a2.cif
_cod_data_source_block           NiBr2_L1
_cod_depositor_comments
'Adding full bibliography for 7062110--7062113.cif.'
_cod_original_cell_volume        28273(10)
_cod_database_code               7062112
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_min   0.797
_shelx_estimated_absorpt_t_max   0.879
_shelx_res_checksum              51170
_shelx_fab_checksum              37791