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_4310718
_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            'C12 Mo4 N12 Na8 Se4'
_chemical_formula_weight         1195.76
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           141
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4bd 2'
_symmetry_space_group_name_H-M   'I 41/a m d :2'
_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                   15.362(2)
_cell_length_b                   15.362(2)
_cell_length_c                   11.055(2)
_cell_measurement_temperature    110(2)
_cell_volume                     2608.9(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0583
_diffrn_reflns_av_sigmaI/netI    0.0279
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            14021
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         2.65
_exptl_absorpt_coefficient_mu    7.626
_exptl_absorpt_correction_T_max  0.4002
_exptl_absorpt_correction_T_min  0.2256
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    3.044
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2192
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.978
_refine_diff_density_min         -0.923
_refine_diff_density_rms         0.435
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.295
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     54
_refine_ls_number_reflns         876
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.295
_refine_ls_R_factor_all          0.0651
_refine_ls_R_factor_gt           0.0462
_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^)+(0.0629P)^2^+13.7767P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1013
_refine_ls_wR_factor_ref         0.1190
_reflns_number_gt                711
_reflns_number_total             876
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic035050usi20031203_012455_4.cif
_cod_data_source_block           Na8Mo4Se4(CN)12_(7)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
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        2609.0(7)
_cod_original_sg_symbol_H-M      'I 41/a m d'
_cod_database_code               4310718