{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_7701514
_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 syn
_chemical_formula_moiety         'C48 H68 N4 Ni4 O12'
_chemical_formula_sum            'C48 H68 N4 Ni4 O12'
_chemical_formula_weight         1127.90
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2019-02-12 deposited with the CCDC.	2019-05-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.276(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.548(3)
_cell_length_b                   20.583(6)
_cell_length_c                   12.063(3)
_cell_measurement_reflns_used    9735
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      2.71
_cell_volume                     2840.1(13)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.997
_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  0.0399
_diffrn_reflns_av_unetI/netI     0.0347
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            20232
_diffrn_reflns_point_group_measured_fraction_full 0.861
_diffrn_reflns_point_group_measured_fraction_max 0.884
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.206
_exptl_absorpt_coefficient_mu    1.362
_exptl_absorpt_correction_T_max  0.930
_exptl_absorpt_correction_T_min  0.770
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.319
_exptl_crystal_description       plate
_exptl_crystal_F_000             1184
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.642
_refine_diff_density_min         -0.610
_refine_diff_density_rms         0.085
_refine_ls_abs_structure_details
;
 Flack x determined using 1737 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.123(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     256
_refine_ls_number_reflns         4437
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0532
_refine_ls_R_factor_gt           0.0495
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0342P)^2^+14.0735P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1148
_refine_ls_wR_factor_ref         0.1183
_reflns_Friedel_coverage         0.720
_reflns_Friedel_fraction_full    0.744
_reflns_Friedel_fraction_max     0.764
_reflns_number_gt                4202
_reflns_number_total             4437
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01026b2.cif
_cod_data_source_block           api266c_0m_a_sq
_cod_original_sg_symbol_H-M      'C 2'
_cod_database_code               7701514
_shelxl_version_number           2014-3
_shelx_res_checksum              35561
_shelx_fab_checksum              62634