Tetracarbonyltungsten(0)-bis(μ-dimethylphosphido)-bis[dicyclopentadienylhydridomolybdenum(IV)]
Kubicki, Marek M.; Barré, Christophe; Moïse, Claude; Acta Crystallographica Section E 58 (2002) m152–m153; doi:10.1107/S1600536802004865

data_2201108
_publ_section_title
Tetracarbonyltungsten(0)-bis(\m-dimethylphosphido)-bis[dicyclopentadienylhydridomolybdenum(IV)]
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m152
_journal_page_last               m153
_journal_paper_doi               10.1107/S1600536802004865
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          '[Mo2 W1 H2 (C5 H5)4 (C2 H6 P1)2 (C1 O1)4]'
_chemical_formula_moiety         'C28 H34 Mo2 O4 P2 W'
_chemical_formula_sum            'C28 H34 Mo2 O4 P2 W'
_chemical_formula_weight         872.21
_chemical_name_systematic
;
tetracarbonyltungsten(0)-bis(\m-dimethylphosphido-dicyclopentadienyl
hydridomolybdenum(IV))
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 100.40(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.342(5)
_cell_length_b                   17.087(2)
_cell_length_c                   11.274(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14.2
_cell_measurement_theta_min      7.8
_cell_volume                     2906.9(11)
_computing_cell_refinement       'CAD-4 EXPRESS'
_computing_data_collection       'CAD-4 EXPRESS (Enraf-Nonius, 1992)'
_computing_data_reduction        'PROCESS in MolEN (Fair, 1990)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.00
_diffrn_measured_fraction_theta_max 1.00
_diffrn_measurement_device       'Enraf-Nonius CAD-4'
_diffrn_measurement_method       \w
_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  0.0486
_diffrn_reflns_av_sigmaI/netI    0.1446
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5899
_diffrn_reflns_theta_full        25.97
_diffrn_reflns_theta_max         25.97
_diffrn_reflns_theta_min         1.80
_diffrn_standards_decay_%        -4.1
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.939
_exptl_absorpt_correction_T_max  0.674
_exptl_absorpt_correction_T_min  0.595
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(DIFABS; Walker & Stuart, 1983)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.993
_exptl_crystal_density_meas      ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1688
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.434
_refine_diff_density_min         -1.457
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.995
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     342
_refine_ls_number_reflns         5683
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.1518
_refine_ls_R_factor_gt           0.0421
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0466P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1115
_refine_ls_wR_factor_ref         0.0840
_reflns_number_gt                2986
_reflns_number_total             5683
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            cv6099.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        2907.0(11)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2201108
_cod_database_fobs_code          2201108