Hexacyanoosmate(iii) chemistry: preparation and magnetic properties of a pentanuclear cluster and a Prussian blue analogue with Ni(ii).
Hilfiger, Matthew G; Shatruk, Michael; Prosvirin, Andrey; Dunbar, Kim R; Chemical communications (Cambridge, England)  (2008) 5752–5754; doi:10.1039/b813413h

data_7103543
_publ_section_title
;
 Hexacyanoosmate(iii) chemistry: preparation and magnetic properties of
 a pentanuclear cluster and a Prussian blue analogue with Ni(ii).
;
_journal_issue                   44
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              5752
_journal_page_last               5754
_journal_paper_doi               10.1039/b813413h
_journal_year                    2008
_chemical_formula_sum            'C94.4 H76.8 N23.2 Ni2.4 Os1.6'
_chemical_formula_weight         1981.41
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 98.152(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            5
_cell_length_a                   19.403(14)
_cell_length_b                   25.613(18)
_cell_length_c                   24.962(17)
_cell_measurement_reflns_used    595
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      24.15
_cell_measurement_theta_min      1.57
_cell_volume                     12280(15)
_computing_cell_refinement       'SMART V5.625 (Bruker, 2000)'
_computing_data_collection       'SMART V5.625 (Bruker, 2000)'
_computing_data_reduction        'SAINT V6.32 (Bruker, 2001)'
_computing_molecular_graphics    'X-Seed (Barbour, 2001)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'SMART APEX CCD area-detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1331
_diffrn_reflns_av_sigmaI/netI    0.1194
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            83299
_diffrn_reflns_theta_full        24.16
_diffrn_reflns_theta_max         24.16
_diffrn_reflns_theta_min         1.33
_exptl_absorpt_coefficient_mu    2.570
_exptl_absorpt_correction_T_max  0.8823
_exptl_absorpt_correction_T_min  0.4263
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2.03 (Bruker, 2003)'
_exptl_crystal_colour            Orange-brown
_exptl_crystal_density_diffrn    1.340
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needles
_exptl_crystal_F_000             4972
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.952
_refine_diff_density_min         -1.577
_refine_diff_density_rms         0.265
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.149
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1308
_refine_ls_number_reflns         19015
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.149
_refine_ls_R_factor_all          0.1679
_refine_ls_R_factor_gt           0.0892
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1075P)^2^+181.9481P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2310
_refine_ls_wR_factor_ref         0.2768
_reflns_number_gt                10721
_reflns_number_total             19015
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b813413h.txt
_cod_data_source_block           c:\users\matthew\niostbp\p21-c.cif
_cod_original_formula_sum        'C94.40 H76.80 N23.20 Ni2.40 Os1.60'
_cod_database_code               7103543