Synthesis, molecular structures, fluxional properties and catalytic activity of a series of alkyne complexes of molybdenum(II) and tungsten(II) containing phosphite donor ligands
Baker, Paul K.; Drew, Michael G. B.; Evans, Deborah S.; Johans, Archie W.; Meehan, Margaret M.; Journal of the Chemical Society, Dalton Transactions  (1999) 2541–; doi:10.1039/a902224d

data_7027399
_publ_section_title
;
 Synthesis, molecular structures, fluxional properties and catalytic
 activity of a series of alkyne complexes of molybdenum(II) and
 tungsten(II) containing phosphite donor ligands
;
_journal_issue                   15
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2541
_journal_paper_doi               10.1039/a902224d
_journal_year                    1999
_chemical_formula_moiety         Mo(CO)(MeCCPh)I2(P(OPh)3)2
_chemical_formula_sum            'C46 H35 I2 Mo O7 P2'
_chemical_formula_weight         1111.42
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 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                 112.475(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.08(2)
_cell_length_b                   11.581(17)
_cell_length_c                   23.65(3)
_cell_measurement_reflns_used    all
_cell_measurement_temperature    293(2)
_cell_volume                     4576(10)
_computing_cell_refinement       XDS
_computing_data_collection       'XDS (Kabsch, 1991)'
_computing_data_reduction        XDS
_computing_molecular_graphics    PLATON(Spek,1994)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Marresearch Image Plate'
_diffrn_measurement_method
'95 frames at 2^o intervals, counting time 2 min.'
_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  0.0763
_diffrn_reflns_av_sigmaI/netI    0.1012
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            5649
_diffrn_reflns_theta_max         26.06
_diffrn_reflns_theta_min         2.14
_diffrn_standards_number         n/a
_exptl_absorpt_coefficient_mu    1.754
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.183
_exptl_absorpt_correction_type   'DIFABS(Stuart and Walker,1983)'
_exptl_crystal_density_diffrn    1.614
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2180
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.077
_refine_diff_density_min         -0.925
_refine_diff_density_rms         0.157
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(7)
_refine_ls_extinction_coef       0.0011(3)
_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_ref   0.949
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     446
_refine_ls_number_reflns         3702
_refine_ls_number_restraints     219
_refine_ls_restrained_S_all      0.930
_refine_ls_R_factor_all          0.1771
_refine_ls_R_factor_gt           0.0814
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1656P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2125
_refine_ls_wR_factor_ref         0.2693
_reflns_number_gt                1695
_reflns_number_total             3702
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            902224dsup1.cif
_cod_data_source_block           4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1656P)^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^)+(0.1656P)^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        4575(10)
_cod_original_sg_symbol_H-M      Cc
_cod_database_code               7027399