data_2002093
_journal_name_full 'Acta Crystallographica, Section C'
_journal_year 1993
_journal_volume C49
_journal_page_first 147
_journal_page_last 151
_publ_section_title
;
FeCl~3~ Behavior in Acetonitrile: Structures of
[FeCl~2~(CH~3~CN)~4~][FeCl~4~] and
[AlCl(CH~3~CN)~5~][FeCl~4~]~2~[CH~3~CN]
;
loop_
_publ_author_name
'Gao, Y.'
'Guery, J.'
'Jacoboni, C.'
_chemical_formula_moiety 'C10 H15 Al Cl N5 2+ , (Cl4 Fe 1-)2 C2 H3 N '
_chemical_formula_sum 'C12 H18 N6 Al Cl9 Fe2'
_chemical_formula_structural '[AlC1(CH3CN)5] [FeCl4]2 [CH3CN]'
_chemical_formula_weight 703.75
_symmetry_cell_setting orthorhombic
_symmetry_space_group_name_H-M 'P 21 21 21'
loop_
_symmetry_equiv_pos_as_xyz
+x,+y,+z
1/2-x,-y,1/2+z
-x,1/2+y,1/2-z
1/2+x,1/2-y,-z
_cell_length_a 10.1025(5)
_cell_length_b 14.5130(10)
_cell_length_c 21.032(2)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 3083.69
_cell_formula_units_Z 4
_cell_measurement_reflns_used 32
_cell_measurement_theta_min 15
_cell_measurement_theta_max 16
_cell_measurement_temperature 293
_exptl_crystal_description needle
_exptl_crystal_colour green
_exptl_crystal_size_max 0.38
_exptl_crystal_size_mid 0.27
_exptl_crystal_size_min 0.27
_exptl_crystal_density_diffrn 1.516
_exptl_crystal_F_000 1400
_exptl_absorpt_coefficient_mu 17.58
_exptl_absorpt_correction_type 'Gaussian (Shelx76)'
_exptl_absorpt_correction_T_min 0.4465
_exptl_absorpt_correction_T_max 0.5932
_diffrn_ambient_temperature 293
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_source 'Fine focus Siemens Mo X-ray tube'
_diffrn_radiation_monochromator 'graphite'
_diffrn_measurement_device 'STOE-Siemens AED2'
_diffrn_measurement_method \q/2\q
_diffrn_reflns_number 4057
_diffrn_reflns_av_R_equivalents 0.02
_diffrn_reflns_theta_min 2.5
_diffrn_reflns_theta_max 30
_diffrn_reflns_limit_h_min 0
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_k_min -4
_diffrn_reflns_limit_k_max 20
_diffrn_reflns_limit_l_min -17
_diffrn_reflns_limit_l_max 29
_diffrn_standards_number 3
_diffrn_standards_interval_time 60
_diffrn_standards_decay_% 8.6
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
5 -2 -6
5 2 6
0 7 -4
_reflns_number_total 3325
_reflns_number_observed 1674
_reflns_observed_criterion 'I>3.0\s(I)'
_refine_ls_structure_factor_coef F
_refine_ls_matrix_type full
_refine_ls_R_factor_obs 0.042
_refine_ls_wR_factor_obs 0.042
_refine_ls_goodness_of_fit_obs 2.21
_refine_ls_number_reflns 1674
_refine_ls_number_parameters 290
_refine_ls_number_restraints 0
_refine_ls_number_constraints 2
_refine_ls_hydrogen_treatment refall
_refine_ls_weighting_scheme unit
_refine_ls_shift/esd_max 0.014
_refine_diff_density_max 0.296
_refine_diff_density_min -0.432
_refine_ls_extinction_method 'no extinction correction'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Fe Fe3+ 0.301 0.845 International_Tables_Vol_IV_Table_2.2B
Al Al3+ 0.056 0.052 International_Tables_Vol_IV_Table_2.2B
Cl Cl1- 0.132 0.159 International_Tables_Vol_IV_Table_2.2B
C C 0.002 0.002 Acta_Cryst.,_A24_(1968)
H H 0.0 0.0 Acta_Cryst.,_A24_(1968)
N N 0.004 0.003 Acta_Cryst.,_A24_(1968)
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_calc_attached_atom
_atom_site_refinement_flags
_atom_site_disorder_group
_atom_site_type_symbol
Fe(1) 0.4921(2) 0.4293(2) 0.50260(10)
0.0670(10)
 Uani ? ? ? ? Fe
Fe(2) 0.4934(2) 0.4322(2) 0.84380(10)
0.0680(10)
 Uani ? ? ? ? Fe
Al 0.6252(3) 0.3778(2) 0.1640(2) 0.040(2) Uani ? ? ? ? Al
Cl(1) 0.4141(3) 0.3438(2) 0.1602(2) 0.059(2) Uani ? ? ? ? Cl
Cl(2) 0.5602(4) 0.5723(3) 0.5025(2) 0.081(2) Uani ? ? ? ? Cl
Cl(3) 0.5712(5) 0.3621(3) 0.5866(2) 0.105(3) Uani ? ? ? ? Cl
Cl(4) 0.5679(5) 0.3643(3) 0.4175(2) 0.101(3) Uani ? ? ? ? Cl
Cl(5) 0.2783(4) 0.4258(5) 0.5092(2) 0.109(4) Uani ? ? ? ? Cl
Cl(6) 0.5761(4) 0.5692(3) 0.8336(2) 0.085(2) Uani ? ? ? ? Cl
Cl(7) 0.5638(5) 0.3453(4) 0.7671(2) 0.129(4) Uani ? ? ? ? Cl
Cl(8) 0.5602(5) 0.3755(4) 0.9330(2) 0.117(4) Uani ? ? ? ? Cl
Cl(9) 0.2796(3) 0.4377(3) 0.8383(2) 0.077(3) Uani ? ? ? ? Cl
N(1) 0.8184(8) 0.4044(7) 0.1669(5) 0.047(6) Uani ? ? ? ? N
N(2) 0.6070(10)
  0.4676(7) 0.2342(4) 0.047(6) Uani ? ? ? ? N
N(3) 0.6670(10)
  0.2844(7) 0.2291(4) 0.047(6) Uani ? ? ? ? N
N(4) 0.6730(10)
  0.2914(7) 0.0947(4) 0.045(6) Uani ? ? ? ? N
N(5) 0.6120(10)
  0.4775(7) 0.1008(4) 0.043(6) Uani ? ? ? ? N
N(6) 0.4160(10)
  0.1804(8) 0.3214(6) 0.076(8) Uani ? ? ? ? N
C(1) 0.9280(10)
  0.4139(9) 0.1671(6) 0.055(8) Uani ? ? ? ? C
C(3) 0.6000(10)
  0.5188(9) 0.2744(5) 0.048(8) Uani ? ? ? ? C
C(5) 0.6990(10)
  0.2392(9) 0.2693(6) 0.049(9) Uani ? ? ? ? C
C(7) 0.7110(10)
  0.2485(9) 0.0519(5) 0.048(8) Uani ? ? ? ? C
C(9) 0.6020(10)
  0.5345(8) 0.0656(5) 0.047(7) Uani ? ? ? ? C
C(11) 0.3470(10)
   0.2394(9) 0.3241(7) 0.060(9) Uani ? ? ? ? C
C(2) 1.0740(10)
  0.4230(10)
   0.1695(8) 0.074(9) Uani ? ? ? ? C
C(4) 0.5910(10)
  0.5862(8) 0.3237(6) 0.061(8) Uani ? ? ? ? C
C(6) 0.740(2) 0.1830(10)
   0.3235(7) 0.080(10)
 Uani ? ? ? ? C
C(8) 0.7480(10)
  0.1970(10)
   0.0003(6) 0.070(10)
 Uani ? ? ? ? C
C(10) 0.588(2) 0.6110(10)
0.0201(6) 0.070(10)
  Uani ? ? ? ? C
C(12) 0.263(2) 0.3160(10)
0.3281(8) 0.080(10)
  Uani ? ? ? ? C
H(1) 1.1150(10)
  0.4560(10)
   0.1280(8) 0.090(10)
 Uiso ? ? G ? H
H(2) 1.1120(10)
  0.3540(10)
   0.1733(8) 0.090(10)
 Uiso ? ? G ? H
H(3) 1.1000(10)
  0.4620(10)
   0.2113(8) 0.090(10)
 Uiso ? ? G ? H
H(4) 0.6550(10)
  0.5542(8) 0.3580(6) 0.090(10)
  Uiso ? ? G ? H
H(5) 0.4990(10)
  0.6041(8) 0.3462(6) 0.090(10)
  Uiso ? ? G ? H
H(6) 0.6380(10)
  0.6477(8) 0.3055(6) 0.090(10)
  Uiso ? ? G ? H
H(7) 0.832(2) 0.1500(10)
   0.3100(7) 0.090(10)
 Uiso ? ? G ? H
H(8) 0.666(2) 0.1310(10)
   0.3329(7) 0.090(10)
 Uiso ? ? G ? H
H(9) 0.757(2) 0.2230(10)
   0.3658(7) 0.090(10)
 Uiso ? ? G ? H
H(10) 0.8410(10)
   0.2130(10)
-0.0222(6) 0.090(10)
   Uiso ? ? D ? H
H(11) 0.6690(10)
   0.2020(10)
-0.0345(6) 0.090(10)
   Uiso ? ? G ? H
H(12) 0.7510(10)
   0.1280(10)
0.0197(6) 0.090(10)
  Uiso ? ? G ? H
H(13) 0.575(2) 0.5800(10)
-0.0260(6) 0.090(10)
   Uiso ? ? G ? H
H(14) 0.661(2) 0.6650(10)
0.0168(6) 0.090(10)
  Uiso ? ? G ? H
H(15) 0.495(2) 0.6400(10)
0.0360(6) 0.090(10)
  Uiso ? ? G ? H
H(16) 0.170(2) 0.2960(10)
0.3498(8) 0.090(10)
  Uiso ? ? G ? H
H(17) 0.244(2) 0.3420(10)
0.2810(8) 0.090(10)
  Uiso ? ? G ? H
H(18) 0.309(2) 0.3680(10)
0.3566(8) 0.090(10)
  Uiso ? ? G ? H