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_7111660
_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         '(C18 H14 O2 N10)3 Ni4 (Cl O4)2 (H2 O)7.5'
_chemical_formula_sum            'C54 H57 Cl2 N30 Ni4 O21.5'
_chemical_formula_weight         1776.04
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 115.296(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   41.051(9)
_cell_length_b                   9.569(2)
_cell_length_c                   19.109(4)
_cell_measurement_reflns_used    12074
_cell_measurement_temperature    138(2)
_cell_measurement_theta_max      30.8212
_cell_measurement_theta_min      2.3808
_cell_volume                     6787(3)
_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    'Patterson search(DIRDIF,Beurskens,1992)'
_diffrn_ambient_temperature      138(2)
_diffrn_detector_area_resol_mean 14.63
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0504
_diffrn_reflns_av_sigmaI/netI    0.0722
_diffrn_reflns_limit_h_max       51
_diffrn_reflns_limit_h_min       -50
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14603
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_theta_min         2.60
_exptl_absorpt_coefficient_mu    1.272
_exptl_absorpt_correction_T_max  0.9660
_exptl_absorpt_correction_T_min  0.9042
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.738
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             3636
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.948
_refine_diff_density_min         -0.629
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.144
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     524
_refine_ls_number_reflns         6979
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.144
_refine_ls_R_factor_all          0.1149
_refine_ls_R_factor_gt           0.0907
_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^)+(0.0924P)^2^+33.0701P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2153
_refine_ls_wR_factor_ref         0.2352
_reflns_number_gt                5288
_reflns_number_total             6979
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            C0CC00150Csup1.cif
_cod_data_source_block           2
_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 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C54 H57 Cl2 N30 Ni4 O21.50'
_cod_database_code               7111660