Experimental and Theoretical Studies of Carbodiphosphorane-CX2 Adducts with Unusual Bonding Situations: Preparation, Crystal Structures, and Bonding Analyses of S2CC(PPh3)2, O2CC(PPh3)2, and [(CO)4MS2CC(PPh3)2] (M = Cr, Mo, W)
Wolfgang Petz; Christian Kutschera; Maya Heitbaum; Gernot Frenking; Ralf Tonner; Bernhard Neumüller; Inorganic Chemistry 44 (2005) 1263–1274; doi:10.1021/ic048397l

data_4308648
_publ_contact_author
;
        Gernot Frenking
        Fachbereich Chemie
        Universit\"at Marburg
        Hans-Meerwein-Strasse
        35032 Marburg
        Germany
;
_publ_contact_author_email       frenking@chemie.uni-marburg.de
_publ_contact_author_fax         'int. 6421-28-25566'
_publ_contact_author_phone       'int. 6421-28-25563'
_publ_section_title
;
Experimental and Theoretical Studies of Carbodiphosphorane-CX2 Adducts
with Unusual Bonding Situations: Preparation, Crystal Structures, and
Bonding Analyses of S2CC(PPh3)2, O2CC(PPh3)2, and [(CO)4MS2CC(PPh3)2] (M =
Cr, Mo, W)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1263
_journal_page_last               1274
_journal_paper_doi               10.1021/ic048397l
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         '[Cr(CO)~4~{S~2~CC(PPh~3~)~2~}]^.^2THF'
_chemical_formula_sum            'C50 H46 Cr O6 P2 S2'
_chemical_formula_weight         920.93
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.37(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.493(1)
_cell_length_b                   22.302(3)
_cell_length_c                   20.261(2)
_cell_measurement_reflns_used    4500
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      26.12
_cell_measurement_theta_min      1.83
_cell_volume                     4612.9(9)
_computing_cell_refinement       'IPDS I (Stoe)'
_computing_data_collection       'IPDS I (Stoe)'
_computing_data_reduction        'IPDS I (Stoe)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1996)'
_computing_publication_material
'SHELXL-97 (Sheldrick, 1997), PLATON-98 (Spek, 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.954
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_device_type  'IPDS I (Stoe)'
_diffrn_measurement_method       'IPDS I (Stoe)'
_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  0.3601
_diffrn_reflns_av_sigmaI/netI    0.3532
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            35628
_diffrn_reflns_theta_full        26.12
_diffrn_reflns_theta_max         26.12
_diffrn_reflns_theta_min         1.83
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.456
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.22
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.326
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'small plates'
_exptl_crystal_F_000             1920
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.811
_refine_diff_density_min         -0.641
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.779
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     408
_refine_ls_number_reflns         8758
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.779
_refine_ls_R_factor_all          0.2288
_refine_ls_R_factor_gt           0.0888
_refine_ls_shift/su_max          0.042
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0642P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1715
_refine_ls_wR_factor_ref         0.2165
_reflns_number_gt                2721
_reflns_number_total             8758
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic048397lsi20041124_051054_3.cif
_cod_data_source_block           pe52
_cod_depositor_comments
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The following automatic conversions were performed:
data name '_publ_contact_autor' replaced with '_publ_contact_author'
as specified in the replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 4998 2017-03-02 13:24:31Z antanas 
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_cod_database_code               4308648