Synthesis and characterisation of {Mo(η-L)(CO)3}+ (η-L = C5H5 or C5Me5) fragments ligated with [CB11H12]− and derivatives. Isolation and structural characterisation of an intermediate in a silver salt metathesis reaction
Patmore, Nathan J.; Mahon, Mary F.; Steed, Jonathan W.; Weller, Andrew S.; Journal of the Chemical Society, Dalton Transactions  (2001) 277–; doi:10.1039/b008222h

data_7010358
_publ_section_title
;
 Synthesis and characterisation of {Mo(\h-L)(CO)3}+
 (\h-L&#x2005;=&#x2005;C5H5 or C5Me5) fragments ligated with
 [CB11H12]&#x2212; and derivatives. Isolation and structural
 characterisation of an intermediate in a silver salt metathesis
 reaction
;
_journal_issue                   3
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              277
_journal_paper_doi               10.1039/b008222h
_journal_year                    2001
_chemical_formula_sum            'C9 H11 Ag B11 Br6 I Mo O3'
_chemical_formula_weight         1096.26
_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                90.871(5)
_cell_angle_beta                 96.678(4)
_cell_angle_gamma                90.355(5)
_cell_formula_units_Z            2
_cell_length_a                   7.7200(7)
_cell_length_b                   11.8360(8)
_cell_length_c                   14.7530(15)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      18
_cell_measurement_theta_min      12
_cell_volume                     1338.7(2)
_computing_molecular_graphics    'ORTEX (P.McArdle, 1995)'
_computing_publication_material  'SHELXL-97/2 (Sheldrick,1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      170(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  '4-circle diffractometer'
_diffrn_measurement_method       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0967
_diffrn_reflns_av_sigmaI/netI    0.1156
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            11052
_diffrn_reflns_theta_full        25.17
_diffrn_reflns_theta_max         25.17
_diffrn_reflns_theta_min         3.56
_exptl_absorpt_coefficient_mu    11.320
_exptl_absorpt_correction_T_max  1.012
_exptl_absorpt_correction_T_min  0.982
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    2.720
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.598
_refine_diff_density_min         -2.947
_refine_diff_density_rms         0.369
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     295
_refine_ls_number_reflns         4679
_refine_ls_number_restraints     115
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.1324
_refine_ls_R_factor_gt           0.0917
_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^)+(0.1718P)^2^+29.3778P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2541
_refine_ls_wR_factor_ref         0.2844
_reflns_number_gt                3236
_reflns_number_total             4679
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b008222h.txt
_cod_data_source_block           compound3
_cod_depositor_comments
;
The following automatic conversions were performed:
'_atom_site_symetry_multiplicity' tag replaced with
'_atom_site_symmetry_multiplicity'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 

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_sg_symbol_H-M      P-1
_cod_database_code               7010358