Syntheses, properties and Mössbauer studies of mono- and di-nitrile phosphine complexes of iron(II). Crystal structures of trans-[Fe(NCR)2(Et2PCH2CH2PEt2)2][BF4]2 (R = Me or CH2C6H4OMe-4) †
Martins, Luísa M. D. R. S.; Duarte, M. Teresa; Galvão, Adelino M.; Resende, Catarina; Pombeiro, Armando J. L.; Henderson, Richard A.; Evans, David J.; Journal of the Chemical Society, Dalton Transactions  (1998) 3311–; doi:10.1039/a804193h

data_7028144
_publ_section_title
;
 Syntheses, properties and M\"ossbauer studies of mono- and di-nitrile
 phosphine complexes of iron(II). Crystal structures of
 trans-[Fe(NCR)2(Et2PCH2CH2PEt2)2][BF4]2 (R&#x2005;=&#x2005;Me or
 CH2C6H4OMe-4)&#x200A;&#x2020;
;
_journal_issue                   19
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3311
_journal_paper_doi               10.1039/a804193h
_journal_year                    1998
_chemical_formula_sum            'C24 H54 B2 F8 Fe N2 P4'
_chemical_formula_weight         724.04
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 93.414(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.265(4)
_cell_length_b                   14.8580(5)
_cell_length_c                   13.528(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      13
_cell_measurement_theta_min      8
_cell_volume                     3464.1(15)
_computing_cell_refinement       'CAD-4 software (Enraf Nonius, 1989)'
_computing_data_collection       'CAD-4 software (Enraf Nonius, 1989)'
_computing_data_reduction        'process-MolEN, (Fair, 1990)'
_computing_molecular_graphics    'ORTEP (Johnson, 1976)'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'CAD4-Enraf Nonius'
_diffrn_measurement_method       '\w-2\q scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0443
_diffrn_reflns_av_sigmaI/netI    0.0226
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            5175
_diffrn_reflns_theta_max         29.99
_diffrn_reflns_theta_min         1.81
_diffrn_standards_decay_%        0.027
_diffrn_standards_interval_count 100
_diffrn_standards_interval_time  3600
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.682
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.961
_exptl_absorpt_correction_type   'empirical via \y-scan North et al. (1968)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.388
_exptl_crystal_density_meas      ?
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.840
_refine_diff_density_min         -0.688
_refine_diff_density_rms         0.085
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.047
_refine_ls_goodness_of_fit_obs   1.085
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     185
_refine_ls_number_reflns         4505
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.109
_refine_ls_restrained_S_obs      1.085
_refine_ls_R_factor_all          0.0868
_refine_ls_R_factor_obs          0.0602
_refine_ls_shift/esd_max         -0.065
_refine_ls_shift/esd_mean        0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0905P)^2^+6.4112P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1934
_refine_ls_wR_factor_obs         0.1595
_reflns_number_observed          3593
_reflns_number_total             5024
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            h804193sup1.cif
_cod_data_source_block           reniob
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0905P)^2^+6.4112P] 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^)+(0.0905P)^2^+6.4112P] 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        3464.0(15)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7028144