Synthesis and Characterization of Bi- and Trinuclear Molybdenum Carbonyl Compounds Obtained by Ligand Exchange Reactions of [Et4N]3[Mo3(CO)9(OMe)3]
Adrian, Rafael A.; Yaklin, Marsha M.; Klausmeyer, Kevin K.; Organometallics 23 (2004) 1352–; doi:10.1021/om034260b

data_4076250
_publ_section_title
;
 Synthesis and Characterization of Bi- and Trinuclear Molybdenum Carbonyl
 Compounds Obtained by Ligand Exchange Reactions of
 [Et4N]3[Mo3(CO)9(OMe)3]
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1352
_journal_paper_doi               10.1021/om034260b
_journal_volume                  23
_journal_year                    2004
_chemical_formula_sum            'C36 H69 Mo3 N3 O12'
_chemical_formula_weight         1023.76
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           138
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4ac 2ac'
_symmetry_space_group_name_H-M   'P 42/n c m :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                   11.7204(9)
_cell_length_b                   11.7204(9)
_cell_length_c                   31.957(4)
_cell_measurement_reflns_used    6960
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      26.48
_cell_measurement_theta_min      2.15
_cell_volume                     4389.9(7)
_computing_cell_refinement       'Bruker APEX 2'
_computing_data_collection       'Bruker APEX 2'
_computing_data_reduction        'Bruker SAINTPLUS'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0428
_diffrn_reflns_av_sigmaI/netI    0.0267
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            59326
_diffrn_reflns_theta_full        31.95
_diffrn_reflns_theta_max         31.95
_diffrn_reflns_theta_min         2.54
_exptl_absorpt_coefficient_mu    0.903
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.549
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2112
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.915
_refine_diff_density_min         -1.407
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         4036
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0944
_refine_ls_R_factor_gt           0.0622
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0288P)^2^+15.1509P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1258
_refine_ls_wR_factor_ref         0.1356
_reflns_number_gt                2674
_reflns_number_total             4036
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om034260bsi20031024_025413.cif
_cod_data_source_block           kk010
_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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        4389.9(8)
_cod_original_sg_symbol_H-M      P4(2)/ncm
_cod_database_code               4076250