Cyanide-Limited Complexation of Molybdenum(III): Synthesis of Octahedral [Mo(CN)6]3- and Cyano-Bridged [Mo2(CN)11]5-
Laurance G. Beauvais; Jeffrey R. Long; Journal of the American Chemical Society 124 (2002) 2110–2111; doi:10.1021/ja0175901

data_4114661
_publ_contact_author
;
        Jeffrey R. Long
        Department of Chemistry
        University of California, Berkeley
        United States of America
;
_publ_contact_author_email       jlong@cchem.berkeley.edu
_publ_contact_author_fax         '510 643-3832'
_publ_contact_author_phone       '510 642-0860'
_publ_section_title
;
 Cyanide-Limited Complexation of Molybdenum(III): Synthesis of Octahedral
 [Mo(CN)6]3- and Cyano-Bridged [Mo2(CN)11]5-
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2110
_journal_page_last               2111
_journal_paper_doi               10.1021/ja0175901
_journal_volume                  124
_journal_year                    2002
_chemical_compound_source        synthetic
_chemical_formula_structural     (Et4N)5[Mo2(CN)11]-2DMF-2MeOH
_chemical_formula_sum            'C59 H122 Mo2 N18 O4'
_chemical_formula_weight         1339.63
_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
_cell_angle_alpha                96.6270(10)
_cell_angle_beta                 107.7700(10)
_cell_angle_gamma                94.8600(10)
_cell_formula_units_Z            1
_cell_length_a                   10.6037(2)
_cell_length_b                   11.9623(3)
_cell_length_c                   15.23160(10)
_cell_measurement_temperature    293(2)
_cell_volume                     1812.82(6)
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction
;
  SAINT (Siemens, 1995), XPREP (Siemens, 1995)
;
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_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  0.0355
_diffrn_reflns_av_sigmaI/netI    0.0599
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8372
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         2.03
_exptl_absorpt_coefficient_mu    0.399
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, Acta Cryst. (1995) A51 33-38'
_exptl_crystal_colour            'olive green'
_exptl_crystal_density_diffrn    1.227
_exptl_crystal_description       plate
_exptl_crystal_F_000             718
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.392
_refine_diff_density_min         -1.146
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.034
_refine_ls_goodness_of_fit_obs   1.085
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         5071
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_restrained_S_obs      1.085
_refine_ls_R_factor_all          0.0768
_refine_ls_R_factor_obs          0.0604
_refine_ls_shift/esd_max         0.018
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1294P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1840
_refine_ls_wR_factor_obs         0.1642
_reflns_number_observed          4128
_reflns_number_total             5085
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja0175901_s2_1.cif
_cod_data_source_block           compound2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1294P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1294P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4114661