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_7217744
_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            'C74 H116 Cl2 N20 Ni9 O52'
_chemical_formula_weight         2716.96
_chemical_name_common            '[Ni9]-(ClO4)2'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_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                 90.320(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.0036(7)
_cell_length_b                   25.0628(9)
_cell_length_c                   21.2234(5)
_cell_measurement_reflns_used    5730
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      3.1630
_cell_volume                     10640.1(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_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(2)
_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   -1.00   96.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       25.9059   77.0000  150.0000 97
  
  2 omega   -7.00   56.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       25.9059  -99.0000  -90.0000 63
  
  3 omega  -25.00   68.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       25.9059  -99.0000   30.0000 93
  
  4 omega   -2.00   77.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       25.9059   19.0000  120.0000 79
  
  5 omega   59.00   91.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       25.9059   57.0000  -60.0000 32
  
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0246176000
_diffrn_orient_matrix_UB_12      0.0203886000
_diffrn_orient_matrix_UB_21      0.0145709000
_diffrn_orient_matrix_UB_22      0.0119285000
_diffrn_orient_matrix_UB_23      0.0270784000
_diffrn_orient_matrix_UB_31      0.0209616000
_diffrn_orient_matrix_UB_32      0.0156109000
_diffrn_orient_matrix_UB_33      -0.0195342000
_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  0.0946
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            40644
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         3.16
_exptl_absorpt_coefficient_mu    1.708
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95840
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.656
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Parallelepiped
_exptl_crystal_F_000             5400
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.129
_refine_diff_density_min         -1.189
_refine_diff_density_rms         0.138
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.026(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1236
_refine_ls_number_reflns         16130
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0989
_refine_ls_R_factor_gt           0.0693
_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^)+(0.0930P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1594
_refine_ls_wR_factor_ref         0.1769
_reflns_number_gt                12123
_reflns_number_total             16130
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ra06064d2.cif
_cod_data_source_block           cmd263e5
_cod_original_sg_symbol_H-M      Cc
_cod_database_code               7217744