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_4310717
_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 Cl3 Cs7 Mo4 N12 Na4 Se4'
_chemical_formula_weight         2140.52
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           160
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  'R 3 -2"'
_symmetry_space_group_name_H-M   'R 3 m :H'
_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                120.00
_cell_formula_units_Z            3
_cell_length_a                   11.5386(10)
_cell_length_b                   11.5386(10)
_cell_length_c                   28.264(3)
_cell_measurement_temperature    110(2)
_cell_volume                     3258.9(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_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  0.0912
_diffrn_reflns_av_sigmaI/netI    0.0809
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            7033
_diffrn_reflns_theta_full        28.34
_diffrn_reflns_theta_max         28.34
_diffrn_reflns_theta_min         2.16
_exptl_absorpt_coefficient_mu    10.510
_exptl_crystal_density_diffrn    3.272
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2820
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.620
_refine_diff_density_min         -2.583
_refine_diff_density_rms         0.285
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(3)
_refine_ls_extinction_coef       0.00006(2)
_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   1.139
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     99
_refine_ls_number_reflns         2011
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.139
_refine_ls_R_factor_all          0.0690
_refine_ls_R_factor_gt           0.0448
_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^)+(0.0376P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0962
_refine_ls_wR_factor_ref         0.1043
_reflns_number_gt                1550
_reflns_number_total             2011
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic035050usi20031203_012455_3.cif
_cod_data_source_block           Na4Cs7Mo4Se4(CN)12Cl3_(6)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Rhombohedral' changed to 'rhombohedral'
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        3258.8(6)
_cod_original_sg_symbol_H-M      'R 3 m'
_cod_database_code               4310717