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_4076251
_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            'C50 H81 Mo2 N7 O9'
_chemical_formula_weight         1116.10
_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                   11.8918(8)
_cell_length_b                   17.5341(12)
_cell_length_c                   26.0493(16)
_cell_measurement_reflns_used    184
_cell_measurement_temperature    293(2)
_cell_volume                     5431.6(6)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens 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 0.947
_diffrn_measured_fraction_theta_max 0.947
_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  0.0658
_diffrn_reflns_av_sigmaI/netI    0.0753
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            34195
_diffrn_reflns_theta_full        28.33
_diffrn_reflns_theta_max         28.33
_diffrn_reflns_theta_min         1.95
_exptl_absorpt_coefficient_mu    0.520
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.365
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2344
_exptl_crystal_size_max          .35
_exptl_crystal_size_mid          .30
_exptl_crystal_size_min          .20
_refine_diff_density_max         2.193
_refine_diff_density_min         -0.474
_refine_diff_density_rms         0.130
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.08(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
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_refine_ls_matrix_type           full
_refine_ls_number_parameters     682
_refine_ls_number_reflns         12535
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0870
_refine_ls_R_factor_gt           0.0590
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0850P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1403
_refine_ls_wR_factor_ref         0.1541
_reflns_number_gt                8751
_reflns_number_total             12535
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om034260bsi20031024_025413.cif
_cod_data_source_block           kk07
_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_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_database_code               4076251