Alkali metal-templated assembly of the tetrahedral cyanometallate cages [M⊂Mo4(μ-CN)6(CO)12]5− (M = Li, Na)
Contakes, Stephen M.; Rauchfuss, Thomas B.; Chemical Communications  (2001) 553–; doi:10.1039/b010192n

data_7114909
_publ_section_title
;
 Alkali metal-templated assembly of the tetrahedral cyanometallate cages
 [M&#x2282;Mo4(\m-CN)6(CO)12]5&#x2212; (M = Li, Na)
;
_journal_issue                   6
_journal_name_full               'Chemical Communications'
_journal_page_first              553
_journal_paper_doi               10.1039/b010192n
_journal_year                    2001
_chemical_formula_sum            'C66 H112 Mo4 N15 Na O12'
_chemical_formula_weight         1714.30
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 96.764(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.1292(16)
_cell_length_b                   19.3643(16)
_cell_length_c                   24.966(2)
_cell_measurement_temperature    193(2)
_cell_volume                     9183.6(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0652
_diffrn_reflns_av_sigmaI/netI    0.0619
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            28888
_diffrn_reflns_theta_full        20.00
_diffrn_reflns_theta_max         20.00
_diffrn_reflns_theta_min         1.07
_exptl_absorpt_coefficient_mu    0.599
_exptl_crystal_density_diffrn    1.240
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3852
_refine_diff_density_max         0.701
_refine_diff_density_min         -0.741
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1455
_refine_ls_number_reflns         8574
_refine_ls_number_restraints     596
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.1052
_refine_ls_R_factor_gt           0.0735
_refine_ls_shift/su_max          0.425
_refine_ls_shift/su_mean         0.061
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1256P)^2^+30.6583P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1894
_refine_ls_wR_factor_ref         0.2107
_reflns_number_gt                6135
_reflns_number_total             8574
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b010192n.txt
_cod_data_source_block           p21cas
_cod_original_cell_volume        9183.7(13)
_cod_database_code               7114909