Cyanide-Melt Synthesis of Reduced Molybdenum Selenide Clusters
Carmela Magliocchi; Xiaobing Xie; Timothy Hughbanks; Inorganic Chemistry 43 (2004) 1902–1911; doi:10.1021/ic035050u

data_4310715
_publ_section_title
;
 Cyanide-Melt Synthesis of Reduced Molybdenum Selenide Clusters
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1902
_journal_page_last               1911
_journal_paper_doi               10.1021/ic035050u
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C6 Mo6 N6 Na8 O20 Se8'
_chemical_formula_weight         1867.36
_chemical_name_systematic
; 
 ? 
;
_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                105.587(3)
_cell_angle_beta                 111.282(2)
_cell_angle_gamma                104.176(2)
_cell_formula_units_Z            1
_cell_length_a                   10.5887(14)
_cell_length_b                   10.7696(14)
_cell_length_c                   11.6714(15)
_cell_measurement_temperature    110(2)
_cell_volume                     1104.2(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.916
_diffrn_measured_fraction_theta_max 0.916
_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  0.0484
_diffrn_reflns_av_sigmaI/netI    0.0727
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            7133
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         2.04
_exptl_absorpt_coefficient_mu    8.390
_exptl_absorpt_correction_T_max  0.8501
_exptl_absorpt_correction_T_min  0.2847
_exptl_crystal_density_diffrn    2.808
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             850
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.297
_refine_diff_density_min         -1.868
_refine_diff_density_rms         0.278
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.921
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         5046
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.921
_refine_ls_R_factor_all          0.0696
_refine_ls_R_factor_gt           0.0436
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0524P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1006
_refine_ls_wR_factor_ref         0.1083
_reflns_number_gt                3394
_reflns_number_total             5046
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic035050usi20031203_012455_1.cif
_cod_data_source_block           Na8Mo6Se8(CN)6_20H2O_(4)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        1104.2(2)
_cod_database_code               4310715