High Nuclearity Ni(II) Cages from Hydroxamate Ligands
jones, leigh Fon; McDonald, Cecelia; Brechin, Euan Kenneth; Sanz, Sergio; Rajaraman, Gopalan; Singh, Mukesh Kumar; Gaynor, Declan; RSC Advances  (2014) –; doi:10.1039/C4RA06064D

data_7217743
_publ_section_title
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 High Nuclearity Ni(II) Cages from Hydroxamate Ligands
;
_journal_name_full               'RSC Advances'
_journal_paper_doi               10.1039/C4RA06064D
_journal_year                    2014
_chemical_absolute_configuration ad
_chemical_formula_sum            'C70 H130 N20 Ni9 O57 S'
_chemical_formula_weight         2724.18
_chemical_name_common            Ni9-SO4.29H2O
_chemical_name_systematic        'Ni9-SO4 '
_chemical_properties_physical    Hygroscopic
_space_group_IT_number           46
_space_group_name_Hall           'I 2 -2a'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'I 2 -2a'
_symmetry_space_group_name_H-M   'I m a 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            4
_cell_length_a                   29.1847(11)
_cell_length_b                   21.2385(7)
_cell_length_c                   19.7536(6)
_cell_measurement_reflns_used    6970
_cell_measurement_temperature    214.0(9)
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      3.3570
_cell_volume                     12244.1(7)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_molecular_graphics    'ORTEX (P.McArdle, 1995)'
_computing_publication_material  'SHELXL-97/2 (Sheldrick,1997)'
_computing_structure_refinement  'SHELXL-97/2 (Sheldrick,1997)'
_computing_structure_solution    SHELXS97
_diffrn_ambient_temperature      214.0(9)
_diffrn_detector_area_resol_mean 16.1048
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega  -61.00  -35.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.1403 -178.0000  -60.0000 26
  
  2 omega   -1.00   25.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.1403  -99.0000 -180.0000 26
  
  3 omega   -6.00   91.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5934   77.0000 -150.0000 97
  
  4 omega    2.00   36.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5934   57.0000  -30.0000 34
  
  5 omega  -46.00   36.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5934  -57.0000  -30.0000 82
  
  6 omega  -47.00   37.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5934  -57.0000   90.0000 84
  
  7 omega  -44.00  -18.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5934  -37.0000 -120.0000 26
  
  8 omega   -9.00   36.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5934   77.0000   90.0000 45
  
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0201068000
_diffrn_orient_matrix_UB_12      0.0092332000
_diffrn_orient_matrix_UB_21      -0.0061592000
_diffrn_orient_matrix_UB_22      0.0198188000
_diffrn_orient_matrix_UB_23      0.0274329000
_diffrn_orient_matrix_UB_31      0.0121789000
_diffrn_orient_matrix_UB_32      0.0252566000
_diffrn_orient_matrix_UB_33      -0.0150987000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.1403
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            52181
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    1.431
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61718
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.192
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Parallelepiped
_exptl_crystal_F_000             4480
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
Electron density representing the equivalent of 29 water molecules 
per cage were removed during the SQUEEZE process 
;
_refine_diff_density_max         0.994
_refine_diff_density_min         -0.621
_refine_diff_density_rms         0.106
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.009(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.964
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     568
_refine_ls_number_reflns         11376
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.964
_refine_ls_R_factor_all          0.0844
_refine_ls_R_factor_gt           0.0598
_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^)+(0.0774P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1455
_refine_ls_wR_factor_ref         0.1531
_reflns_number_gt                7684
_reflns_number_total             11376
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ra06064d2.cif
_cod_data_source_block           ni9(4)sq
_cod_original_sg_symbol_H-M      Ima2
_cod_database_code               7217743