Reactivity of Hydrides FeH2(CO)2P2 (P = Phosphites) with Aryldiazonium Cations: Preparation, Characterization, X-ray Crystal Structure, and Electrochemical Studies of Mono- and Binuclear Aryldiazenido Complexes
Gabriele Albertin; Stefano Antoniutti; Alessia Bacchi; Davide Barbera; Emilio Bordignon; Giancarlo Pelizzi; Paolo Ugo; Inorganic Chemistry 37 (1998) 5602–5610; doi:10.1021/ic980430e

data_4323100
_publ_section_title
;
 Reactivity of Hydrides FeH2(CO)2P2 (P = Phosphites) with Aryldiazonium
 Cations: Preparation, Characterization, X-ray Crystal Structure, and
 Electrochemical Studies of Mono- and Binuclear Aryldiazenido Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5602
_journal_page_last               5610
_journal_paper_doi               10.1021/ic980430e
_journal_volume                  37
_journal_year                    1998
_chemical_formula_structural
;
{[Fe(CO)2{P(OEt)3}2(N=N-C7H6)]2}(BPh4)2
;
_chemical_formula_sum            'C90 H112 B2 Fe2 N4 O16 P4'
_chemical_formula_weight         1763.04
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     patt
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                99.560(10)
_cell_angle_beta                 102.800(10)
_cell_angle_gamma                65.300(10)
_cell_formula_units_Z            1
_cell_length_a                   15.008(4)
_cell_length_b                   17.094(5)
_cell_length_c                   10.553(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_volume                     2390.2(12)
_computing_molecular_graphics    'ZORTEP (Zsolnai, Pritzkow, 1994)'
_computing_publication_material
;
 PARST95 (Nardelli, 1995)
;
_computing_structure_refinement  'SHELXL-96 (Sheldrick, 1996)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens AED diffractometer'
_diffrn_measurement_method       '\q/2\q scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71068
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1321
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            11524
_diffrn_reflns_theta_max         28.03
_diffrn_reflns_theta_min         3.03
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 100
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    0.432
_exptl_crystal_density_diffrn    1.225
_exptl_crystal_F_000             930
_refine_diff_density_max         0.407
_refine_diff_density_min         -0.364
_refine_diff_density_rms         0.064
_refine_ls_extinction_coef       0.0017(16)
_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_all   0.875
_refine_ls_goodness_of_fit_obs   1.100
_refine_ls_matrix_type           full
_refine_ls_number_parameters     492
_refine_ls_number_reflns         11524
_refine_ls_number_restraints     234
_refine_ls_restrained_S_all      0.869
_refine_ls_restrained_S_obs      1.069
_refine_ls_R_factor_all          0.2474
_refine_ls_R_factor_obs          0.0717
_refine_ls_shift/esd_max         0.056
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1470P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3003
_refine_ls_wR_factor_obs         0.1893
_reflns_number_observed          3117
_reflns_number_total             11524
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic980430e.cif
_cod_data_source_block           compound_5b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1470P)^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^)+(0.1470P)^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_database_code               4323100