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_7111662
_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
'C144 H112 N80 Ni16 O34, 16 (N O3), 32 (H2 O)'
_chemical_formula_sum            'C144 H176 N96 Ni16 O96'
_chemical_formula_weight         5726.76
_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                111.723(6)
_cell_angle_beta                 94.468(6)
_cell_angle_gamma                97.249(7)
_cell_formula_units_Z            2
_cell_length_a                   19.483(6)
_cell_length_b                   24.701(8)
_cell_length_c                   26.510(9)
_cell_measurement_reflns_used    38098
_cell_measurement_temperature    128(2)
_cell_measurement_theta_max      31.2311
_cell_measurement_theta_min      2.3127
_cell_volume                     11649(7)
_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    'SHELXL-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      128(2)
_diffrn_detector_area_resol_mean 14.63
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.957
_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  0.0662
_diffrn_reflns_av_sigmaI/netI    0.0759
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            90389
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.50
_exptl_absorpt_coefficient_mu    1.372
_exptl_absorpt_correction_T_max  0.8466
_exptl_absorpt_correction_T_min  0.7486
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(T. Higashi, 2000)'
_exptl_crystal_colour            'Dark Red'
_exptl_crystal_density_diffrn    1.632
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             5856
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.19
_platon_squeeze_details
;
The Platon Squeeze procedure was applied to recover 1191 electrons per
unit cell in one void (total volume 4084 ^A^3); that is 595.5 electrons
per formula unit. Due to poor diffraction, and many, many peaks
associated with disordered lattice solvent and anions, charge could not
be conclusively balanced based on this X-ray analysis. The model formula
corresponds to (L-2H)8(Ni(II))16(H2O)15(NO3)3) Therefore, for charge
balance, an additional 13 nitrate anions per formula unit are required.
This would account for 416 electrons. The additional electron density
is attributed to partial occupancy, disordered, lattice solvent molecules;
that is, approximately 17 water molecules per formula unit, accounting
for another 170 electrons. The application of Squeeze gave a significant
improvement in the data statistics, however, this report is only intended
to support to the gross connectivity in the core of the structure. Further
conclusions based on the X-ray analysis would constitute over-interpretation
of a weak data set.
PLATON Reference : Spek, A.L. (2003), J.Appl.Cryst. 36, 7-13.
;
_refine_diff_density_max         2.999
_refine_diff_density_min         -0.756
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2585
_refine_ls_number_reflns         39271
_refine_ls_number_restraints     742
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.1609
_refine_ls_R_factor_gt           0.1299
_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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3304
_refine_ls_wR_factor_ref         0.3785
_reflns_number_gt                20567
_reflns_number_total             39271
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            C0CC00150Csup1.cif
_cod_data_source_block           6
_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_original_cell_volume        11649(6)
_cod_database_code               7111662