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_4323422
_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
;
 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            'C16 H10 Mo2 O8 Se'
_chemical_formula_weight         601.08
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.638(4)
_cell_length_b                   9.707(2)
_cell_length_c                   11.169(3)
_cell_measurement_reflns_used    62
_cell_measurement_temperature    143(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      10
_cell_volume                     2020.7(8)
_computing_cell_refinement       'Stoe DIF4'
_computing_data_collection       'Stoe DIF4'
_computing_data_reduction        'Stoe REDU4'
_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      143(2)
_diffrn_measurement_device       'Stoe STADI4'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0331
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4654
_diffrn_reflns_theta_max         27.54
_diffrn_reflns_theta_min         3.03
_diffrn_standards_decay_%        2
_diffrn_standards_interval_count 247
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.080
_exptl_absorpt_correction_T_max  0.939
_exptl_absorpt_correction_T_min  0.604
_exptl_absorpt_correction_type   Psi-scans
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.976
_exptl_crystal_description       tablet
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.639
_refine_diff_density_min         -1.115
_refine_diff_density_rms         0.113
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.109(12)
_refine_ls_extinction_method     shelxl
_refine_ls_goodness_of_fit_all   1.078
_refine_ls_goodness_of_fit_obs   1.052
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         4652
_refine_ls_number_restraints     104
_refine_ls_restrained_S_all      1.067
_refine_ls_restrained_S_obs      1.040
_refine_ls_R_factor_all          0.0410
_refine_ls_R_factor_obs          0.0360
_refine_ls_shift/esd_max         0.004
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0454P)^2^+3.4828P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0915
_refine_ls_wR_factor_obs         0.0864
_reflns_number_observed          4374
_reflns_number_total             4652
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic961199c_5.cif
_cod_data_source_block           spee
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0454P)^2^+3.4828P] 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^)+(0.0454P)^2^+3.4828P] 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_original_cell_volume        2020.8(8)
_cod_database_code               4323422