Reactions of alkynes with molybdenum and tungsten bis(alkyne) complexes [M(SR)(CF3CCCF3)2(η5-C5H5)] (M = Mo, R = C6F5; M = W, R = C6H4Me-4): crystal and molecular structure of [Mo{η4-C(CF3)C(CF3)C(CO2Me)C(CO2Me)(SC6F5)}(CF3CCCF3)(η5-C5H5)] †
Agh-Atabay, Naz M.; Davidson, Jack L.; Dullweber, Uta; Douglas, Graeme; Muir, Kenneth W.; Journal of the Chemical Society, Dalton Transactions  (1999) 3883–; doi:10.1039/a905297f

data_7027663
_publ_section_title
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 Reactions of alkynes with molybdenum and tungsten bis(alkyne) complexes
 [M(SR)(CF3C&#xE007;CCF3)2(\h5-C5H5)] (M&#x2005;=&#x2005;Mo,
 R&#x2005;=&#x2005;C6F5; M&#x2005;=&#x2005;W, R&#x2005;=&#x2005;C6H4Me-4):
 crystal and molecular structure of
 [Mo{\h4-C(CF3)&#xE006;C(CF3)C(CO2Me)C(CO2Me)(SC6F5)}(CF3C&#xE007;CCF3)(\h5-C5H5)]&#x200A;&#x2020;
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_journal_issue                   21
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3883
_journal_paper_doi               10.1039/a905297f
_journal_year                    1999
_chemical_formula_moiety         'C25 H11 F17 Mo O4 S'
_chemical_formula_sum            'C25 H11 F17 Mo O4 S'
_chemical_formula_weight         826.34
_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                 103.8900(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.8780(10)
_cell_length_b                   15.3020(15)
_cell_length_c                   17.119(2)
_cell_measurement_reflns_used    22
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14.0
_cell_measurement_theta_min      11.0
_cell_volume                     2766.2(5)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf-Nonius CAD4 diffractometer'
_diffrn_measurement_method       '\w/2\q 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  0.032
_diffrn_reflns_av_sigmaI/netI    0.0722
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            11329
_diffrn_reflns_theta_max         27.0
_diffrn_reflns_theta_min         2.02
_diffrn_standards_decay_%        25.0
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.699
_exptl_absorpt_correction_T_max  0.9559
_exptl_absorpt_correction_T_min  0.7039
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.984
_exptl_crystal_description       plate
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.40
_refine_diff_density_min         -0.53
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.987
_refine_ls_goodness_of_fit_obs   1.138
_refine_ls_matrix_type           full
_refine_ls_number_parameters     435
_refine_ls_number_reflns         6012
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.987
_refine_ls_restrained_S_obs      1.138
_refine_ls_R_factor_all          0.0920
_refine_ls_R_factor_obs          0.0367
_refine_ls_shift/esd_max         0.033
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0515P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0975
_refine_ls_wR_factor_obs         0.0850
_reflns_number_observed          3609
_reflns_number_total             6012
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            905297fsup1.cif
_cod_data_source_block           n002
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0515P)^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^)+(0.0515P)^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_sg_symbol_H-M      'P 2(1)/n'
_cod_database_code               7027663