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_7062113
_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         'C102 H144  N12 Ni3 O6 Si6, 6Br, 38(H2O)'
_chemical_formula_sum            'C102 H220 Br6 N12 Ni3 O44 Si6'
_chemical_formula_weight         3143.02
_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                   31.291(4)
_cell_length_b                   31.291(4)
_cell_length_c                   31.796(6)
_cell_measurement_reflns_used    457515
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      33.858
_cell_measurement_theta_min      0.447
_cell_volume                     31132(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
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick, 2013)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Rayonix MX225HS CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.780
_diffrn_reflns_av_R_equivalents  0.0960
_diffrn_reflns_av_unetI/netI     0.0473
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_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            201340
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        27.905
_diffrn_reflns_theta_max         28.000
_diffrn_reflns_theta_min         1.406
_diffrn_source                   'PLSII 2D bending magnet'
_exptl_absorpt_coefficient_mu    2.542
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.878
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'HKL3000sm Scalepack(Otwinowski et.al,2003)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.341
_exptl_crystal_description       block
_exptl_crystal_F_000             13168
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.711
_refine_diff_density_min         -0.354
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details
;
 Flack x determined using 6886 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.035(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1254
_refine_ls_number_reflns         28460
_refine_ls_number_restraints     1972
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.0879
_refine_ls_R_factor_gt           0.0584
_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^)+(0.1144P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1672
_refine_ls_wR_factor_ref         0.1861
_reflns_Friedel_coverage         0.888
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                18768
_reflns_number_total             28460
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj04751a2.cif
_cod_data_source_block           NiBr2_L2
_cod_depositor_comments
'Adding full bibliography for 7062110--7062113.cif.'
_cod_original_cell_volume        31132(11)
_cod_database_code               7062113
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_min   0.430
_shelx_estimated_absorpt_t_max   0.630
_shelx_res_checksum              2168
_shelx_fab_checksum              98848