P‒C and C‒C Coupling Processes in the Reactions of the Phosphinidene-Bridged Complex [Fe2(η5-C5H5)2(μ-PCy)(μ-CO)(CO)2] with Alkynes
Alvarez, M. Angeles; García, M. Esther; González, Rocío; Ruiz, Miguel A.; Organometallics 32 (2013) 4601–; doi:10.1021/om4005669

data_4081325
_publ_section_title
;
 P--C and C--C Coupling Processes in the Reactions of the
 Phosphinidene-Bridged Complex [Fe2(\h5-C5H5)2(\m-PCy)(\m-CO)(CO)2] with
 Alkynes
;
_journal_issue                   16
_journal_name_full               Organometallics
_journal_page_first              4601
_journal_paper_doi               10.1021/om4005669
_journal_volume                  32
_journal_year                    2013
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C27 H29 Fe2 O7 P, C H2 Cl2'
_chemical_formula_sum            'C28 H31 Cl2 Fe2 O7 P'
_chemical_formula_weight         693.10
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 94.136(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.5419(17)
_cell_length_b                   24.032(4)
_cell_length_c                   12.901(2)
_cell_measurement_reflns_used    1381
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      27.6345
_cell_measurement_theta_min      2.73
_cell_measurement_wavelength     0.71073
_cell_volume                     2950.6(9)
_computing_cell_refinement       'Brucker Smart'
_computing_data_collection       'Brucker Smart'
_computing_data_reduction        'Brucker Smart'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0(1)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Smart-CCD-1000 BRUKER'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0397
_diffrn_reflns_av_unetI/netI     0.0338
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            27868
_diffrn_reflns_theta_full        26.73
_diffrn_reflns_theta_max         26.73
_diffrn_reflns_theta_min         1.69
_exptl_absorpt_coefficient_mu    1.263
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.797440
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'BRUKER Sadabs'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.56
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.151
_refine_diff_density_min         -1.753
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     368
_refine_ls_number_reflns         6247
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.13
_refine_ls_R_factor_all          0.0706
_refine_ls_R_factor_gt           0.0584
_refine_ls_shift/su_max          0.01
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1008P)^2^+7.2939P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1669
_refine_ls_wR_factor_ref         0.1761
_reflns_number_gt                5083
_reflns_number_total             6247
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om4005669_si_002.cif
_cod_data_source_block           compoundcis6
_cod_depositor_comments
;
The following automatic conversions were performed:
'_diffrn_radiation_monochromador' tag replaced with
'_diffrn_radiation_monochromator'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 
;
_cod_original_cell_volume        2950.7(9)
_cod_database_code               4081325