Stepwise reduction of a phosphaalkyne PC bond to a phosphaalkene and a phosphine at the FeH(dppe)2 centre. Crystal and molecular structure of the η1-co-ordinated phosphaalkyne complex trans-[FeH(η1-PCBut)(dppe)2][BPh4]
Meidine, Mohamed F.; Amélia N. D. A.Lemos, Maria; Pombeiro, Armando J. L.; Nixon, John F.; Hitchcock, Peter B.; Journal of the Chemical Society, Dalton Transactions  (1998) 3319–; doi:10.1039/a804803g

data_7028134
_publ_section_title
;
 Stepwise reduction of a phosphaalkyne P&#xE007;C bond to a phosphaalkene
 and a phosphine at the FeH(dppe)2 centre. Crystal and molecular structure
 of the \h1-co-ordinated phosphaalkyne complex
 trans-[FeH(\h1-P&#xE007;CBut)(dppe)2][BPh4]
;
_journal_issue                   19
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3319
_journal_paper_doi               10.1039/a804803g
_journal_year                    1998
_chemical_formula_structural     '[(dppe)2FeH(PCtBu)][BPh4]'
_chemical_formula_sum            'C81 H78 B Fe P5'
_chemical_formula_weight         1272.94
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 98.86(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.186(3)
_cell_length_b                   17.812(4)
_cell_length_c                   34.237(9)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      10
_cell_measurement_theta_min      7
_cell_volume                     6740(3)
_computing_cell_refinement       'Enraf-Nonius CAD4'
_computing_data_collection       'Enraf-Nonius CAD4'
_computing_molecular_graphics    'CAMERON (Watkin and Pearce,1993)'
_computing_publication_material  SHELXL-93
_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'
_diffrn_measurement_method       \w--2\q
_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  0.0494
_diffrn_reflns_av_sigmaI/netI    0.0840
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            9876
_diffrn_reflns_theta_max         22.98
_diffrn_reflns_theta_min         2.04
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.387
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.254
_exptl_crystal_F_000             2680
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.445
_refine_diff_density_min         -0.304
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.026
_refine_ls_goodness_of_fit_obs   0.989
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     797
_refine_ls_number_reflns         9258
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.335
_refine_ls_restrained_S_obs      0.989
_refine_ls_R_factor_all          0.1015
_refine_ls_R_factor_obs          0.0534
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+15.2449P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1719
_refine_ls_wR_factor_obs         0.1022
_reflns_number_observed          6224
_reflns_number_total             9338
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            g804803sup1.cif
_cod_data_source_block           may1397
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+15.2449P] 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^)+(0.0000P)^2^+15.2449P] 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        6740.2(29)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7028134