Synthesis, crystal structure, and magnetic properties of hexanuclear [{MnL2}4{Nb(CN)8}2] and Nonanuclear [{MnL2}6{Nb(CN)8}3] heterometallic clusters (L=bpy, phen).
Venkatakrishnan, Thengarai S.; Rajamani, Raghunathan; Ramasesha, S.; Sutter, Jean-Pascal; Inorganic chemistry 46 (2007) 9569–9574; doi:10.1021/ic062383t

data_4339666
_publ_section_title
;
 Synthesis, crystal structure, and magnetic properties of hexanuclear
 [{MnL2}4{Nb(CN)8}2] and Nonanuclear [{MnL2}6{Nb(CN)8}3] heterometallic
 clusters (L=bpy, phen).
;
_journal_issue                   23
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9569
_journal_page_last               9574
_journal_paper_doi               10.1021/ic062383t
_journal_volume                  46
_journal_year                    2007
_chemical_compound_source        synthesis
_chemical_formula_moiety         'C96 H64 Mn4 N32 Nb2, (H2 O)11.62 '
_chemical_formula_sum            'C96 H87.25 Mn4 N32 Nb2 O11.62'
_chemical_formula_weight         2280.73
_chemical_name_systematic
;
tetra(bis(2,2'-bipyridyl)Manganese(II))di(octacyano Niobium(IV)) cluster
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           CRYSTALS_ver_12.51
_cell_angle_alpha                90
_cell_angle_beta                 97.776(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.923(5)
_cell_length_b                   19.690(5)
_cell_length_c                   47.387(5)
_cell_measurement_reflns_used    9479
_cell_measurement_temperature    180
_cell_measurement_theta_max      29
_cell_measurement_theta_min      3
_cell_volume                     22116(8)
_computing_cell_refinement       'CrysAlis RED, (Oxford Diffraction, 2002)'
_computing_data_collection       'Xcalibur, (Oxford Diffraction, 2002)'
_computing_data_reduction        'CrysAlis RED, (Oxford Diffraction, 2002)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      180
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Oxford Diffraction XCALIBUR'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.149
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       64
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            201758
_diffrn_reflns_theta_full        29.078
_diffrn_reflns_theta_max         29.078
_diffrn_reflns_theta_min         2.603
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.713
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.90
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.37
_exptl_crystal_description       planar
_exptl_crystal_F_000             9112
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.48
_refine_diff_density_min         -1.11
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1138
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1097
_refine_ls_number_reflns         11242
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.2909
_refine_ls_R_factor_gt           0.0944
_refine_ls_shift/su_max          0.002030
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 7.19 4.79 6.23 1.77 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1324
_refine_ls_wR_factor_gt          0.0946
_refine_ls_wR_factor_ref         0.0946
_reflns_limit_h_max              32
_reflns_limit_h_min              -32
_reflns_limit_k_max              26
_reflns_limit_k_min              0
_reflns_limit_l_max              64
_reflns_limit_l_min              0
_reflns_number_gt                11242
_reflns_number_total             59125
_reflns_threshold_expression     >1.9\s(I)
_cod_data_source_file            ic062383t-file003.cif
_cod_data_source_block           cluster_1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from
2011-04-26.

'_refine_ls_hydrogen_treatment' value 'refu' changed to
'refU' according to
/usr/data/users/saulius/automatic-downloads/retrospective/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      'P 1 2/c 1 '
_cod_database_code               4339666