Molecular and supramolecular Ni(II) wheels from α-benzoin oxime
Karotsis, Georgios; Stoumpos, Constantinos; Collins, Anna; White, Fraser; Parsons, Simon; Slawin, Alexandra M. Z.; Papaefstathiou, Giannis S.; Brechin, Euan K.; Dalton Transactions  (2009) 3388–3390; doi:10.1039/b902002k

data_7001201
_publ_section_title
;
 Molecular and supramolecular Ni(II) wheels from \a-benzoin oxime
;
_journal_issue                   18
_journal_name_full               'Dalton Transactions'
_journal_page_first              3388
_journal_page_last               3390
_journal_paper_doi               10.1039/b902002k
_journal_year                    2009
_chemical_compound_source        'Giorgos Karotsis'
_chemical_formula_moiety
'[Ni8 (C14H11NO2)8 (Et2O)2 (MeOH)2 (H2O)], 2(Et2O)'
_chemical_formula_sum            'C130 H158 N8 Ni8 O23'
_chemical_formula_weight         2670.32
_chemical_name_systematic
;
?
;
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   22.4470(6)
_cell_length_b                   55.1580(13)
_cell_length_c                   21.2010(5)
_cell_measurement_reflns_used    9428
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.3105
_cell_measurement_theta_min      2.2705
_cell_volume                     26249.6(11)
_computing_cell_refinement       Saint
_computing_data_reduction        Saint
_computing_molecular_graphics    Shelxp
_computing_publication_material  'Platon, encifer'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'Shelxs Sheldrick'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker Smart Apex CCD'
_diffrn_measurement_method       'Omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0565
_diffrn_reflns_av_sigmaI/netI    0.0485
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       68
_diffrn_reflns_limit_k_min       -68
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            67387
_diffrn_reflns_theta_full        26.41
_diffrn_reflns_theta_max         26.41
_diffrn_reflns_theta_min         1.37
_exptl_absorpt_coefficient_mu    1.190
_exptl_absorpt_correction_T_max  0.7699
_exptl_absorpt_correction_T_min  0.6658
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2007/2'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             11216
_exptl_crystal_recrystallization_method 'Diffusion of ET2O into MeOH solution'
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.574
_refine_diff_density_min         -0.405
_refine_diff_density_rms         0.074
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.000(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     714
_refine_ls_number_reflns         13364
_refine_ls_number_restraints     176
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.0623
_refine_ls_R_factor_gt           0.0551
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0426P)^2^+111.8372P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1190
_refine_ls_wR_factor_ref         0.1219
_reflns_number_gt                12122
_reflns_number_total             13364
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b902002k.txt
_cod_data_source_block           eb8055
_cod_database_code               7001201