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_7217742
_publ_section_title
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 High Nuclearity Ni(II) Cages from Hydroxamate Ligands
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_journal_name_full               'RSC Advances'
_journal_paper_doi               10.1039/C4RA06064D
_journal_year                    2014
_chemical_formula_sum            'C61 H67 Cl2 N13 Ni5 O17'
_chemical_formula_weight         1618.71
_chemical_name_common            '[Ni5(L)4(py)5](ClO4)2.1H2O'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 93.552(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.6573(4)
_cell_length_b                   15.1811(4)
_cell_length_c                   29.7812(11)
_cell_measurement_reflns_used    9811
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      2.9030
_cell_volume                     6614.0(4)
_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 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_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  -77.00   54.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.2653    0.0000 -180.0000 131
  
  2 omega  -48.00   10.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.2653  -37.0000  -60.0000 58
  
  3 omega  -67.00  -41.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.2653  -37.0000   30.0000 26
  
  4 omega   30.00   87.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       22.7028 -137.0000    0.0000 57
  
  5 omega   30.00   88.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       22.7028 -137.0000 -179.0000 58
  
  6 omega   34.00   88.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       22.7028  179.0000  -60.0000 54
  
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0209052000
_diffrn_orient_matrix_UB_12      0.0111263000
_diffrn_orient_matrix_UB_21      0.0388913000
_diffrn_orient_matrix_UB_22      0.0158982000
_diffrn_orient_matrix_UB_23      0.0128757000
_diffrn_orient_matrix_UB_31      0.0200309000
_diffrn_orient_matrix_UB_32      -0.0424910000
_diffrn_orient_matrix_UB_33      -0.0004406000
_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  0.0785
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            52717
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         2.9030
_exptl_absorpt_coefficient_mu    1.558
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95873
_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    1.624
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Parallelepiped
_exptl_crystal_F_000             3328
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.374
_refine_diff_density_min         -0.770
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     886
_refine_ls_number_reflns         12096
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0854
_refine_ls_R_factor_gt           0.0482
_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^)+(0.0422P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0993
_refine_ls_wR_factor_ref         0.1139
_reflns_number_gt                8299
_reflns_number_total             12096
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ra06064d2.cif
_cod_data_source_block           cmd211e2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7217742