Reactions of a cyanosilane with an iron(II) centre. Synthesis and crystal structure of the isocyanotriphenylborate complex trans-[FeH(CNBPh3)(Ph2PCH2CH2PPh2)2] and anodic deprotonation of the hydrogen isocyanide (CNH) analogue
Almeida, Sílvia S. P. R.; da Silva, M. Fátima C. Guedes; Fraústoda Silva, João J. R.; Pombeiro, Armando J. L.; Journal of the Chemical Society, Dalton Transactions  (1999) 467–; doi:10.1039/a807707j

data_7027131
_publ_section_title
;
 Reactions of a cyanosilane with an iron(II) centre. Synthesis and crystal
 structure of the isocyanotriphenylborate complex
 trans-[FeH(CNBPh3)(Ph2PCH2CH2PPh2)2] and anodic deprotonation of the
 hydrogen isocyanide (CNH) analogue
;
_journal_issue                   3
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              467
_journal_paper_doi               10.1039/a807707j
_journal_year                    1999
_chemical_formula_sum            'C72 H69 B Fe N2 O2 P4'
_chemical_formula_weight         1184.97
_chemical_name_systematic
; 
 ? 
;
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                109.10(2)
_cell_angle_beta                 102.78(2)
_cell_angle_gamma                63.49(2)
_cell_formula_units_Z            2
_cell_length_a                   13.685(3)
_cell_length_b                   13.746(3)
_cell_length_c                   19.616(4)
_cell_measurement_temperature    293(2)
_cell_volume                     3107.9(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.636
_diffrn_measured_fraction_theta_max 0.636
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0216
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7012
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         2.08
_exptl_absorpt_coefficient_mu    0.392
_exptl_crystal_density_diffrn    1.266
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1227
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.480
_refine_diff_density_min         -0.319
_refine_diff_density_rms         0.053
_refine_ls_extinction_coef       0.0017(6)
_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   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1014
_refine_ls_number_reflns         7012
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_obs          0.0397
_refine_ls_shift/su_max          2.654
_refine_ls_shift/su_mean         0.070
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0853P)^2^+1.5296P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1111
_refine_ls_wR_factor_obs         0.1111
_reflns_number_gt                7012
_reflns_number_total             7012
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            807707jsup1.cif
_cod_data_source_block           pmb02
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0853P)^2^+1.5296P] 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^)+(0.0853P)^2^+1.5296P] 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        3107.9(12)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7027131