A one-pot synthesis of a paramagnetic high-nuclearity nickel(II) cluster: an octadecanuclear Ni(II)16Na(I)2 metal aggregate.
Biswas, Biplab; Khanra, Sumit; Weyhermüller, Thomas; Chaudhuri, Phalguni; Chemical communications (Cambridge, England)  (2007) 1059–1061; doi:10.1039/b613782b

data_7101757
_publ_section_title
;
 A one-pot synthesis of a paramagnetic high-nuclearity nickel(II)
 cluster: an octadecanuclear Ni(II)16Na(I)2 metal aggregate.
;
_journal_issue                   10
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1059
_journal_page_last               1061
_journal_paper_doi               10.1039/b613782b
_journal_year                    2007
_chemical_formula_moiety
'[C102 H206 N12 Na2 Ni16 O68], 3 MeCN, 21 H2O'
_chemical_formula_sum            'C108 H257 N15 Na2 Ni16 O89'
_chemical_formula_weight         4175.63
_chemical_name_systematic
;
?
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.3308(6)
_cell_length_b                   26.0589(8)
_cell_length_c                   36.1281(12)
_cell_measurement_temperature    100(2)
_cell_volume                     18199.1(10)
_computing_cell_refinement       'Bruker AXS Collect Software'
_computing_data_collection       'Bruker AXS Collect Software'
_computing_data_reduction        'Bruker AXS Collect Software'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Nonius Kappa-CCD'
_diffrn_measurement_method
'1868 images at 0.3 deg. stepwise rotation in omega and phi, 90 sec./frame'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode, 50 kV, 80 mA'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1330
_diffrn_reflns_av_sigmaI/netI    0.0942
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            136036
_diffrn_reflns_theta_full        23.50
_diffrn_reflns_theta_max         23.50
_diffrn_reflns_theta_min         2.93
_exptl_absorpt_coefficient_mu    1.713
_exptl_absorpt_correction_T_max  0.9342
_exptl_absorpt_correction_T_min  0.7509
_exptl_absorpt_correction_type   gaussian
_exptl_crystal_colour            'light greenish blue'
_exptl_crystal_density_diffrn    1.524
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'transparent block'
_exptl_crystal_F_000             8768
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.956
_refine_diff_density_min         -0.678
_refine_diff_density_rms         0.110
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.028(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2093
_refine_ls_number_reflns         26843
_refine_ls_number_restraints     114
_refine_ls_restrained_S_all      1.137
_refine_ls_R_factor_all          0.1061
_refine_ls_R_factor_gt           0.0794
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0399P)^2^+104.0830P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1480
_refine_ls_wR_factor_ref         0.1592
_reflns_number_gt                21354
_reflns_number_total             26843
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b613782b.txt
_cod_data_source_block           5580
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'Gaussian' changed to 'gaussian'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0399P)^2^+104.0830P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0399P)^2^+104.0830P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_database_code               7101757