Missing link in the ligand-field photolysis of [Mo(CN)8]4-: synthesis, X-ray crystal structure, and physicochemical properties of [Mo(CN)6]2-.
Szklarzewicz, Janusz; Matoga, Dariusz; Niezgoda, Agnieszka; Yoshioka, Daisuke; Mikuriya, Masahiro; Inorganic chemistry 46 (2007) 9531–9533; doi:10.1021/ic701395r

data_4339653
_publ_section_title
;
 Missing link in the ligand-field photolysis of [Mo(CN)8]4-: synthesis,
 X-ray crystal structure, and physicochemical properties of [Mo(CN)6]2-.
;
_journal_issue                   23
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9531
_journal_page_last               9533
_journal_paper_doi               10.1021/ic701395r
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C14 H26 Mo N8 O'
_chemical_formula_weight         418.37
_chemical_name_systematic
; 
 (Me4N)2(Mo(CN)6).H2O 
;
_space_group_IT_number           225
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  '-F 4 2 3'
_symmetry_space_group_name_H-M   'F m -3 m'
_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                   12.5900(13)
_cell_length_b                   12.5900(13)
_cell_length_c                   12.5900(13)
_cell_measurement_temperature    293
_cell_volume                     1995.6(4)
_computing_cell_refinement       'BRUKER SMART'
_computing_data_collection       'BRUKER SMART'
_computing_data_reduction        'BRUKER SAINT'
_computing_molecular_graphics    'BRUKER SHELXL'
_computing_publication_material  'BRUKER SHELXL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'psi and omega 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  0.0268
_diffrn_reflns_av_sigmaI/netI    0.0074
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            3099
_diffrn_reflns_theta_full        28.35
_diffrn_reflns_theta_max         28.35
_diffrn_reflns_theta_min         2.80
_exptl_absorpt_coefficient_mu    0.675
_exptl_absorpt_correction_T_max  0.9056
_exptl_absorpt_correction_T_min  0.8769
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.669
_refine_diff_density_min         -0.415
_refine_diff_density_rms         0.063
_refine_ls_extinction_coef       0.0017(12)
_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   1.202
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     17
_refine_ls_number_reflns         165
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.202
_refine_ls_R_factor_all          0.0712
_refine_ls_R_factor_gt           0.0670
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0692P)^2^+9.8430P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1666
_refine_ls_wR_factor_ref         0.1729
_reflns_number_gt                157
_reflns_number_total             165
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic701395r-file001.cif
_cod_data_source_block           mocn6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Cubic' changed to 'cubic' 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      Fm-3m
_cod_database_code               4339653