Unexpected Ni(ii) and Cu(ii) polynuclear assemblies—a balance between ligand and metal ion coordination preferences
Shuvaev, Kontantin V.; Tandon, Santokh S.; Dawe, Louise N.; Thompson, Laurence K.; Chemical Communications 46 (2010) 4755–4757; doi:10.1039/c0cc00150c

data_7111661
_publ_section_title
;
 Unexpected Ni(ii) and Cu(ii) polynuclear assemblies---a balance between
 ligand and metal ion coordination preferences
;
_journal_issue                   26
_journal_name_full               'Chemical Communications'
_journal_page_first              4755
_journal_page_last               4757
_journal_paper_doi               10.1039/c0cc00150c
_journal_volume                  46
_journal_year                    2010
_chemical_formula_moiety
'[3(C28 H18 O2 N12), Cu11, 2(OH)], 4(C2 H3 O2), 4(Cl O4), Na, (O H), 55 (H2 O)'
_chemical_formula_sum            'C92 H179 Cl4 Cu11 N36 Na O88'
_chemical_formula_weight         4061.42
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                67.954(10)
_cell_angle_beta                 78.882(12)
_cell_angle_gamma                86.105(14)
_cell_formula_units_Z            2
_cell_length_a                   18.024(7)
_cell_length_b                   20.901(6)
_cell_length_c                   24.333(7)
_cell_measurement_reflns_used    26278
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      29.7530
_cell_measurement_theta_min      1.7118
_cell_volume                     8337(5)
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_molecular_graphics    'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)'
_computing_publication_material  'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 14.63
_diffrn_measured_fraction_theta_full 0.948
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'graphite - Rigaku SHINE'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0642
_diffrn_reflns_av_sigmaI/netI    0.1011
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            58641
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_theta_min         2.54
_exptl_absorpt_coefficient_mu    1.548
_exptl_absorpt_correction_T_max  0.9635
_exptl_absorpt_correction_T_min  0.8206
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(T. Higashi, 2000)'
_exptl_crystal_colour            'Dark Brown'
_exptl_crystal_density_diffrn    1.618
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             4170
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_platon_squeeze_details
;
The Platon Squeeze procedure was applied to recover 853 electrons per
unit cell in one void (total volume 2835 ^A^3); that is 426.5 electrons
per formula unit. Disordered solvent lattice water molecules (approx. 42
molecules) were present,however, a good point atom model could not be
achieved. The application of Squeeze gave a good improvement in the data
statistics and allowed for a full anisotropic refinement of the structure.
PLATON Reference : Spek, A.L. (2003), J.Appl.Cryst. 36, 7-13
;
_refine_diff_density_max         2.046
_refine_diff_density_min         -1.492
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1712
_refine_ls_number_reflns         32789
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0901
_refine_ls_R_factor_gt           0.0735
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1286P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2073
_refine_ls_wR_factor_ref         0.2273
_reflns_number_gt                23554
_reflns_number_total             32789
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            C0CC00150Csup1.cif
_cod_data_source_block           5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Numerical' changed to
'numerical' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
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_cod_database_code               7111661