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_7217741
_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_formula_sum            'C42 H64 Cl2 N8 Ni5 O22'
_chemical_formula_weight         1397.46
_chemical_name_common            Ni5-MeOH
_chemical_name_systematic        'Ni5(1)-MeOH '
_chemical_properties_physical    Hygroscopic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                70.12(3)
_cell_angle_beta                 63.48(3)
_cell_angle_gamma                64.17(3)
_cell_formula_units_Z            1
_cell_length_a                   11.191(2)
_cell_length_b                   12.389(3)
_cell_length_c                   12.401(3)
_cell_measurement_reflns_used    7266
_cell_measurement_temperature    150.1(2)
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      3.2841
_cell_volume                     1361.9(7)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug  2 2010,13:00:58)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug  2 2010,13:00:58)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug  2 2010,13:00:58)
;
_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      150.1(1)
_diffrn_detector_area_resol_mean 16.1048
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -64.00   14.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.4216  -77.0000  -60.0000 78
  
  2 omega  -67.00    1.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.4216  -37.0000  -60.0000 68
  
  3 omega  -47.00  -18.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       22.7028  -77.0000  -30.0000 29
  
  4 omega   -3.00   87.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       22.7028   77.0000 -150.0000 90
  
  5 omega  -45.00   51.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       22.7028  -77.0000   90.0000 96
  
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0195679000
_diffrn_orient_matrix_UB_12      -0.0524981000
_diffrn_orient_matrix_UB_21      -0.0659540000
_diffrn_orient_matrix_UB_22      0.0301805000
_diffrn_orient_matrix_UB_23      -0.0101055000
_diffrn_orient_matrix_UB_31      0.0329522000
_diffrn_orient_matrix_UB_32      -0.0236038000
_diffrn_orient_matrix_UB_33      -0.0545760000
_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  0.0169
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10303
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         3.29
_exptl_absorpt_coefficient_mu    1.880
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85835
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug  2 2010,13:00:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.704
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Parallelepiped
_exptl_crystal_F_000             722
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.447
_refine_diff_density_min         -0.989
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     366
_refine_ls_number_reflns         4974
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0349
_refine_ls_R_factor_gt           0.0308
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+3.1746P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0736
_refine_ls_wR_factor_ref         0.0758
_reflns_number_gt                4541
_reflns_number_total             4974
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ra06064d2.cif
_cod_data_source_block           cmd207e4
_cod_original_cell_volume        1362.0(5)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7217741