Isomerism and Ligand Rearrangement within thecyclo-P2S3Middle Deck in Dimolybdenum Triple-Decker Complexes
Gröger, Christian; Kubicki, Marek M.; Meier, Walter; Pronold, Michael; Wachter, Joachim; Zabel, Manfred; Organometallics 28 (2009) 5633–; doi:10.1021/om900600t

data_4070074
_publ_section_title
;
 Isomerism and Ligand Rearrangement within thecyclo-P2S3Middle Deck in
 Dimolybdenum Triple-Decker Complexes
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              5633
_journal_paper_doi               10.1021/om900600t
_journal_volume                  28
_journal_year                    2009
_chemical_compound_source        'see text'
_chemical_formula_moiety         'C25 H30 Mo2 O5 P2 S3 W, 0.5(C7 H8)'
_chemical_formula_sum            'C28.5 H34 Mo2 O5 P2 S3 W'
_chemical_formula_weight         990.42
_chemical_name_systematic        ?
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 103.909(12)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.7163(16)
_cell_length_b                   22.2865(17)
_cell_length_c                   21.587(2)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    123
_cell_measurement_theta_max      25.92
_cell_measurement_theta_min      2.12
_cell_volume                     6872.4(12)
_computing_cell_refinement       'STOE (1998)'
_computing_data_collection       'STOE (1998)'
_computing_data_reduction        'STOE (1998)'
_computing_molecular_graphics    'PLATON (Spek, 1990)'
_computing_publication_material  'PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-97 (Altomare, 1993)'
_diffrn_ambient_temperature      123(1)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'STOE-IPDS diffractometer'
_diffrn_measurement_method       rotation
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0376
_diffrn_reflns_av_sigmaI/netI    0.0228
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            94924
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        25.92
_diffrn_reflns_theta_max         25.92
_diffrn_reflns_theta_min         2.32
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.368
_exptl_absorpt_correction_T_max  0.5707
_exptl_absorpt_correction_T_min  0.4842
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
'analytical from crystal shape (X-SHAPE, X-RED. STOE, 1996)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.914
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3847
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.14
_refine_diff_density_max         2.340
_refine_diff_density_min         -0.906
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     807
_refine_ls_number_reflns         13298
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0401
_refine_ls_R_factor_gt           0.0322
_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^)+(0.0558P)^2^]         where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0791
_refine_ls_wR_factor_ref         0.0814
_reflns_number_gt                11176
_reflns_number_total             13298
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om900600t_si_001.cif
_cod_data_source_block           f084
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

2026-02-13
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C57 H68 Mo4 O10 P4 S6 W2'
_cod_original_formula_weight         1980.85
_cod_original_formula_moiety         '2(C25 H30 Mo2 O5 P2 S3 W), C7 H8'
_cod_original_formula_units_Z            4
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4070074