Organometallic Selenolates. 5.1 Synthesis and Complexing Properties of 2-Propene- and 2-Methyl-2-propeneselenolato Molybdenum and Tungsten Compounds. Crystal Structures of cp(CO)3WSeCH2C(CH3)CH2, [cp(CO)2MoSeCH2C(CH3)CH2]2, [cp(CO)3Mo(μ-SeCH2C(CH3)CH2)W(CO)5], [cp(CO)3Mo(μ-SeCH2C(CH3)CH2)Mo(CO)5], and [cp(CO)3Mo(μ-SeCH2CHCH2)Mo(CO)5]
Peter G. Jones; Jörg Laube; Carsten Thöne; Inorganic Chemistry 36 (1997) 2097–2102; doi:10.1021/ic961199c

data_4323420
_publ_contact_author
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        Carsten Th\"one
        Institut f\"ur Anorganische und Analytische Chemie
        Technische Universit\"at Braunschweig
        Postfach 3329
        38023 Braunschweig
        Germany
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_publ_contact_author_email       thoene@xray36.anchem.nat.tu-bs.de
_publ_contact_author_fax         '049 531 391-5387'
_publ_contact_author_phone       '049 531 391-7350'
_publ_section_title
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 Organometallic Selenolates. 5.1 Synthesis and Complexing Properties of
 2-Propene- and 2-Methyl-2-propeneselenolato Molybdenum and Tungsten
 Compounds. Crystal Structures of cp(CO)3WSeCH2C(CH3)CH2,
 [cp(CO)2MoSeCH2C(CH3)CH2]2, [cp(CO)3Mo(\m-SeCH2C(CH3)CH2)W(CO)5],
 [cp(CO)3Mo(\m-SeCH2C(CH3)CH2)Mo(CO)5], and
 [cp(CO)3Mo(\m-SeCH2CHCH2)Mo(CO)5]
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2097
_journal_page_last               2102
_journal_paper_doi               10.1021/ic961199c
_journal_volume                  36
_journal_year                    1997
_chemical_formula_sum            'C17 H12 Mo O8 Se W'
_chemical_formula_weight         703.02
_chemical_name_systematic
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 ?
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_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                 103.030(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.708(2)
_cell_length_b                   9.837(2)
_cell_length_c                   14.958(2)
_cell_measurement_reflns_used    54
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      4
_cell_volume                     2108.4(6)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens Xscans'
_computing_molecular_graphics    'Siemens XP'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       Omega-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  0.0198
_diffrn_reflns_av_sigmaI/netI    0.0301
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            8416
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.03
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 247
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    7.811
_exptl_absorpt_correction_T_max  0.831
_exptl_absorpt_correction_T_min  0.493
_exptl_absorpt_correction_type   Psi-scans
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.215
_exptl_crystal_description       prism
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.36
_refine_diff_density_max         0.872
_refine_diff_density_min         -0.955
_refine_diff_density_rms         0.106
_refine_ls_extinction_coef       0.00120(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   0.958
_refine_ls_goodness_of_fit_obs   1.006
_refine_ls_hydrogen_treatment    'rigid methyl, others riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         4832
_refine_ls_number_restraints     112
_refine_ls_restrained_S_all      0.947
_refine_ls_restrained_S_obs      0.993
_refine_ls_R_factor_all          0.0274
_refine_ls_R_factor_obs          0.0206
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0220P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0429
_refine_ls_wR_factor_obs         0.0416
_reflns_number_observed          4157
_reflns_number_total             4832
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic961199c_3.cif
_cod_data_source_block           zksed
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0220P)^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^)+(0.0220P)^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 
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_cod_database_code               4323420