Geometrical isomerism in pentadecanuclear high-spin Ni9W6 clusters with symmetrical bidentate ligands detected
Nowicka, Beata; Stadnicka, Katarzyna; Nitek, Wojciech; Rams, Michał; Sieklucka, Barbara; CrystEngComm 14 (2012) 6559–; doi:10.1039/c2ce25537e

data_7208687
_publ_section_title
;
 Geometrical isomerism in pentadecanuclear high-spin Ni9W6 clusters with
 symmetrical bidentate ligands detected
;
_journal_issue                   20
_journal_name_full               CrystEngComm
_journal_page_first              6559
_journal_paper_doi               10.1039/c2ce25537e
_journal_volume                  14
_journal_year                    2012
_chemical_formula_sum            'C148 H89 N65 Ni9 O12 W6'
_chemical_formula_weight         4601.10
_chemical_name_common            (Ni(Ni(5,5'dmbpy)(H2O))8(W(CN)8)6)*8H2O
_chemical_name_systematic
;
{Ni[Ni(5,5'dmbpy)(H2O)]8[W(CN)8]6}*8H2O
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                89.305(5)
_cell_angle_beta                 90.024(5)
_cell_angle_gamma                73.132(5)
_cell_formula_units_Z            2
_cell_length_a                   19.899(5)
_cell_length_b                   20.113(5)
_cell_length_c                   31.475(5)
_cell_measurement_temperature    293(2)
_cell_volume                     12054(5)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL DENZO and Scalepack (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'Ortep3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR-92 (ALTOMARE et al., 1994)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       '\f and \o scans to fill Ewald sphere'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0520
_diffrn_reflns_av_sigmaI/netI    0.1322
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            79308
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         1.06
_exptl_absorpt_coefficient_mu    3.586
_exptl_absorpt_correction_T_max  0.8412
_exptl_absorpt_correction_T_min  0.6730
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(DENZO-SMN; Otwinowski & Minor, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.268
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             4448.0
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.384
_refine_diff_density_min         -0.906
_refine_diff_density_rms         0.188
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1100
_refine_ls_number_reflns         54307
_refine_ls_number_restraints     75
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.1964
_refine_ls_R_factor_gt           0.0955
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0900P)^2^+119.9078P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2047
_refine_ls_wR_factor_ref         0.2551
_reflns_number_gt                27806
_reflns_number_total             54307
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ce25537e.txt
_cod_data_source_block           3b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' 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      P-1
_cod_database_code               7208687