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_4076252
_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            'C53 H75 Mo2 N7 O9'
_chemical_formula_weight         1146.08
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                   15.089(3)
_cell_length_b                   19.2429(15)
_cell_length_c                   19.329(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      16
_cell_measurement_theta_min      8
_cell_volume                     5612.3(15)
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_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      293(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Enraf Nonius CAD4'
_diffrn_measurement_method       '\w 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  0.0120
_diffrn_reflns_av_sigmaI/netI    0.0759
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -2
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            5903
_diffrn_reflns_theta_full        25.08
_diffrn_reflns_theta_max         25.08
_diffrn_reflns_theta_min         1.71
_diffrn_standards_decay_%        .95
_diffrn_standards_interval_count 7200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.505
_exptl_absorpt_correction_T_max  0.9142
_exptl_absorpt_correction_T_min  0.8833
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.356
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             2392
_exptl_crystal_size_max          .52
_exptl_crystal_size_mid          .25
_exptl_crystal_size_min          .19
_refine_diff_density_max         0.549
_refine_diff_density_min         -0.380
_refine_diff_density_rms         0.093
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.09(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     642
_refine_ls_number_reflns         5761
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0659
_refine_ls_R_factor_gt           0.0494
_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^)+(0.0472P)^2^+1.6758P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1031
_refine_ls_wR_factor_ref         0.1088
_reflns_number_gt                4790
_reflns_number_total             5761
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om034260bsi20031024_025413.cif
_cod_data_source_block           kk12
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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        5612.1(13)
_cod_original_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_database_code               4076252