{Ni<sub>4</sub>} Cubanes from enantiomerically pure 2-(1-hydroxyethyl)pyridine ligands: supramolecular chirality.
Mayans, Julia; Athanasopoulou, Angeliki A.; Pham, Amy Trinh; Font-Bardia, Mercè; Mazarakioti, Eleni C.; Pilkington, Melanie; Stamatatos, Theocharis C.; Escuer, Albert; Dalton transactions (Cambridge, England : 2003) 48 (2019) 10427–10434; doi:10.1039/c9dt01026b

data_7701512
_publ_section_title
;
 {Ni<sub>4</sub>} Cubanes from enantiomerically pure
 2-(1-hydroxyethyl)pyridine ligands: supramolecular chirality.
;
_journal_issue                   28
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10427
_journal_page_last               10434
_journal_paper_doi               10.1039/c9dt01026b
_journal_volume                  48
_journal_year                    2019
_chemical_absolute_configuration rm
_chemical_formula_moiety         '2(C36 H44 N4 Ni4 O12), 13(H2 O)'
_chemical_formula_sum            'C72 H114 N8 Ni8 O37'
_chemical_formula_weight         2153.39
_space_group_crystal_system      orthorhombic
_space_group_IT_number           20
_space_group_name_Hall           'C 2c 2'
_space_group_name_H-M_alt        'C 2 2 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-02-12 deposited with the CCDC.	2019-05-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.8143(11)
_cell_length_b                   31.128(3)
_cell_length_c                   11.9196(10)
_cell_measurement_reflns_used    9888
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.67
_cell_measurement_theta_min      2.35
_cell_volume                     5125.6(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0940
_diffrn_reflns_av_unetI/netI     0.0580
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            28130
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        24.661
_diffrn_reflns_theta_max         24.661
_diffrn_reflns_theta_min         2.350
_diffrn_source                   microfocus
_exptl_absorpt_coefficient_mu    1.515
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.5448
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.395
_exptl_crystal_description       prism
_exptl_crystal_F_000             2244
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile/diethylether'
_exptl_crystal_size_max          0.289
_exptl_crystal_size_mid          0.125
_exptl_crystal_size_min          0.095
_refine_diff_density_max         1.292
_refine_diff_density_min         -0.506
_refine_diff_density_rms         0.099
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.04(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         4339
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0594
_refine_ls_R_factor_gt           0.0452
_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^)+(0.0649P)^2^+2.9525P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1093
_refine_ls_wR_factor_ref         0.1181
_reflns_Friedel_coverage         0.787
_reflns_Friedel_fraction_full    0.993
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                3649
_reflns_number_total             4339
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01026b2.cif
_cod_data_source_block           mo_i06sb178_0m_a_aa
_cod_database_code               7701512
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              577