Synthesis and Structural Characterization of Bi- and Trimetallic Octacyanometalate(IV) Complexes: [Δ,Λ-MII(en)3][cis-MII(en)2(OH2)][MIV(CN)8]·2H2O and [cis-MII(en)2(OH2)]2[(μ-NC)2MIV(CN)6]·4H2O (MII= Mn, Co, Ni; MIV= Mo, W)
Withers, Jeffrey R.; Ruschmann, Chad; Bojang, Pasano; Parkin, Sean; Holmes, Stephen M.; Inorganic Chemistry 44 (2005) 352–358; doi:10.1021/ic048936m

data_4308406
_publ_section_title
;
 Synthesis and Structural Characterization of Bi- and Trimetallic
 Octacyanometalate(IV) Complexes:
 [\D,\L-MII(en)3][cis-MII(en)2(OH2)][MIV(CN)8]&#x00B7;2H2O and
 [cis-MII(en)2(OH2)]2[(\m-NC)2MIV(CN)6]&#x00B7;4H2O
 (MII= Mn, Co, Ni; MIV= Mo, W)
;
_journal_coden_ASTM              INOCAJ
_journal_issue                   2
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              352
_journal_page_last               358
_journal_paper_doi               10.1021/ic048936m
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C8 H22 Co N8 O3 W0.5'
_chemical_formula_weight         429.19
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_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                 108.783(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.1162(3)
_cell_length_b                   11.0546(2)
_cell_length_c                   17.6671(3)
_cell_measurement_reflns_used    3792
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.00
_cell_volume                     3164.82(15)
_computing_cell_refinement       'SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'XP in Siemens SHELXTL (Sheldrick, 1994)'
_computing_publication_material
;
SHELX97-2 (Sheldrick, 1997) and local procedures
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90.0(2)
_diffrn_detector_area_resol_mean 18
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Nonius KappaCCD diffractometer'
_diffrn_measurement_method       '\w scans at fixed \c = 55\%'
_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  0.0234
_diffrn_reflns_av_sigmaI/netI    0.0343
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            7003
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.23
_diffrn_standards_decay_%        <1
_exptl_absorpt_coefficient_mu    4.719
_exptl_absorpt_correction_T_max  0.6497
_exptl_absorpt_correction_T_min  0.6013
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Scalepack (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.802
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'block (cut)'
_exptl_crystal_F_000             1712
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.944
_refine_diff_density_min         -1.346
_refine_diff_density_rms         0.100
_refine_ls_extinction_coef       0.00023(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         3636
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0236
_refine_ls_R_factor_gt           0.0200
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0172P)^2^+1.5027P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0423
_refine_ls_wR_factor_ref         0.0430
_reflns_number_gt                3363
_reflns_number_total             3636
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic048936msi20041109_053940_2.cif
_cod_data_source_block           k02273
_cod_depositor_comments
;
The following automatic conversions were performed:
_cell_measurement_temperature value '90.02)' changed to '90(2)'-
fixed precision.
Automatic conversion script
Id: cif_fix_values 1382 2010-08-28 14:56:29Z saulius 
;
_cod_original_cell_volume        3164.82(10)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C8 H22 Co N8 O3 W0.50'
_cod_database_code               4308406