Dimetallagermanes of molybdenum and tungsten: synthesis, structure and reactions
Filippou, Alexander C.; Winter, Johannes G.; Kociok-Köhn, Gabriele; Hinz, Isolde; Journal of the Chemical Society, Dalton Transactions  (1998) 2029–; doi:10.1039/a801380b

data_7027908
_publ_contact_author
;
    Alexander C. Filippou
    Institut f\"ur Anorganische und Allgemeine Chemie der
    Humboldt Universit\"at zu Berlin
    Hessische Strasse 1-2
    10115 Berlin
    Bundesrepublik Deutschland
;
_publ_section_title
;
 Dimetallagermanes of molybdenum and tungsten: synthesis, structure and
 reactions&#x200A;
;
_journal_issue                   12
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2029
_journal_paper_doi               10.1039/a801380b
_journal_year                    1998
_chemical_formula_moiety         'C18 H19 Cl2 Ge Mo2 O5 P'
_chemical_formula_structural
;
 ((C5 H5) Mo (C O)3)) Ge Cl2 ((C5 H5) Mo (C O)2 (P(C H3)3)'
;
_chemical_formula_sum            'C18 H19 Cl2 Ge Mo2 O5 P'
_chemical_formula_weight         681.69
_chemical_name_systematic
; 
 ? 
;
_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
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 116.203(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.876(3)
_cell_length_b                   15.859(3)
_cell_length_c                   18.691(3)
_cell_measurement_reflns_used    2000
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      26
_cell_measurement_theta_min      2.1
_cell_volume                     4754.3(15)
_computing_cell_refinement       'IPDS (STOE, 1996)'
_computing_data_collection       'IPDS (STOE, 1996)'
_computing_data_reduction        'IPDS (Software 2.65, 1996)'
_computing_molecular_graphics
;
 L.Zsolnai,H.Pritzkow,ZORTEP,ORTEP program for PC,Universit\"at 
Heidelberg 1994
;
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measurement_device       STOE-IPDS
_diffrn_measurement_method       \f-rotation
_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  0.0669
_diffrn_reflns_av_sigmaI/netI    0.0611
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            33291
_diffrn_reflns_theta_max         26.08
_diffrn_reflns_theta_min         2.11
_diffrn_standards_number         200
_exptl_absorpt_coefficient_mu    2.482
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.905
_exptl_crystal_description       'irregular shape'
_exptl_crystal_F_000             2656
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.19
_refine_diff_density_max         1.717
_refine_diff_density_min         -1.639
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.917
_refine_ls_goodness_of_fit_obs   1.033
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     542
_refine_ls_number_reflns         9200
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_restrained_S_obs      1.033
_refine_ls_R_factor_all          0.0520
_refine_ls_R_factor_obs          0.0328
_refine_ls_shift/esd_max         -0.022
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0339P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0822
_refine_ls_wR_factor_obs         0.0707
_reflns_number_observed          6708
_reflns_number_total             9213
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            B801380sup1.cif
_cod_data_source_block           hansi18
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0339P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0339P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        4754.4(14)
_cod_database_code               7027908