#------------------------------------------------------------------------------
#$Date: 2016-03-26 16:01:19 +0100 (Sat 26 de Mar de 2016) $
#$Revision: 180368 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/37/7203784.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7203784
loop_
_publ_author_name
'Zordan, Fiorenzo'
'Purver, Stephen L.'
'Adams, Harry'
'Brammer, Lee'
_publ_section_title
;
 Halometallate and halide ions: nucleophiles in competition for
 hydrogen bond and halogen bond formation in halopyridinium salts of
 mixed halide--halometallate anions
;
_journal_issue                   57
_journal_name_full               CrystEngComm
_journal_page_first              350
_journal_paper_doi               10.1039/b503858h
_journal_volume                  7
_journal_year                    2005
_chemical_formula_moiety         '3(c5 h5 br n), 2(cl4 Fe), Cl'
_chemical_formula_sum            'C15 H15 Br3 Cl9 Fe2 N3'
_chemical_formula_weight         907.78
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.716(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.583(11)
_cell_length_b                   13.960(10)
_cell_length_c                   14.695(11)
_cell_measurement_reflns_used    3908
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.29
_cell_measurement_theta_min      3.134
_cell_volume                     2990(4)
_computing_cell_refinement       'Bruker Smart'
_computing_data_collection       'Bruker Smart'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.952
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_device_type  'Bruker Smart 1000 CCD'
_diffrn_measurement_method       ω-scans
_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  0.1409
_diffrn_reflns_av_sigmaI/netI    0.1412
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18984
_diffrn_reflns_theta_full        28.64
_diffrn_reflns_theta_max         28.64
_diffrn_reflns_theta_min         1.94
_exptl_absorpt_coefficient_mu    5.795
_exptl_absorpt_correction_T_max  0.2585
_exptl_absorpt_correction_T_min  0.1757
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.016
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1744
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.32
_refine_diff_density_max         1.817
_refine_diff_density_min         -1.678
_refine_diff_density_rms         0.193
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.909
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         7323
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.909
_refine_ls_R_factor_all          0.1413
_refine_ls_R_factor_gt           0.0712
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1001P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1691
_refine_ls_wR_factor_ref         0.2075
_reflns_number_gt                3550
_reflns_number_total             7323
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b503858h.txt
_cod_data_source_block           ilb18m
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7203784
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.82125(8) 0.28154(9) 0.67461(8) 0.0376(3) Uani 1 1 d . . .
Fe2 Fe 0.88270(8) 0.21401(9) 0.17264(8) 0.0356(3) Uani 1 1 d . . .
Cl1 Cl 0.77666(18) 0.2132(2) 0.79908(16) 0.0646(8) Uani 1 1 d . . .
Cl2 Cl 0.78292(16) 0.18656(18) 0.56182(14) 0.0529(6) Uani 1 1 d . . .
Cl3 Cl 0.76226(15) 0.42479(18) 0.65700(17) 0.0535(6) Uani 1 1 d . . .
Cl4 Cl 0.96995(14) 0.29815(18) 0.67773(16) 0.0529(6) Uani 1 1 d . . .
Cl5 Cl 0.82825(15) 0.13075(18) 0.28423(15) 0.0494(6) Uani 1 1 d . . .
Cl6 Cl 0.84656(16) 0.14638(18) 0.04220(15) 0.0494(6) Uani 1 1 d . . .
Cl7 Cl 0.82134(15) 0.35657(17) 0.17348(15) 0.0473(6) Uani 1 1 d . . .
Cl8 Cl 1.03106(14) 0.23146(17) 0.18987(15) 0.0470(6) Uani 1 1 d . . .
Cl9 Cl 0.38192(13) 0.57331(16) 0.04083(13) 0.0402(5) Uani 1 1 d . . .
N31 N 0.1797(5) 0.5361(5) 0.0918(4) 0.0406(17) Uani 1 1 d . . .
H31 H 0.2383 0.5226 0.0862 0.049 Uiso 1 1 calc R . .
C32 C 0.1274(6) 0.4741(6) 0.1366(6) 0.040(2) Uani 1 1 d . . .
H32 H 0.1530 0.4171 0.1619 0.048 Uiso 1 1 calc R . .
C33 C 0.0378(5) 0.4943(6) 0.1449(5) 0.0385(19) Uani 1 1 d . . .
H33 H -0.0007 0.4509 0.1758 0.046 Uiso 1 1 calc R . .
C34 C 0.0019(5) 0.5768(6) 0.1093(5) 0.0326(18) Uani 1 1 d . . .
Br34 Br -0.12177(6) 0.60697(7) 0.12263(6) 0.0480(3) Uani 1 1 d . . .
C35 C 0.0568(6) 0.6397(7) 0.0633(6) 0.047(2) Uani 1 1 d . . .
H35 H 0.0327 0.6972 0.0378 0.056 Uiso 1 1 calc R . .
C36 C 0.1479(6) 0.6160(7) 0.0558(5) 0.042(2) Uani 1 1 d . . .
H36 H 0.1878 0.6575 0.0244 0.050 Uiso 1 1 calc R . .
N11 N 0.4466(5) 0.7806(6) 0.0740(4) 0.0426(18) Uani 1 1 d . . .
H11 H 0.4065 0.7341 0.0653 0.051 Uiso 1 1 calc R . .
C12 C 0.4170(6) 0.8684(7) 0.0923(6) 0.050(2) Uani 1 1 d . . .
H12 H 0.3530 0.8802 0.0957 0.060 Uiso 1 1 calc R . .
C13 C 0.4778(6) 0.9417(8) 0.1061(6) 0.050(2) Uani 1 1 d . . .
H13 H 0.4571 1.0048 0.1184 0.059 Uiso 1 1 calc R . .
C14 C 0.5698(5) 0.9216(6) 0.1018(5) 0.0354(18) Uani 1 1 d . . .
Br14 Br 0.65704(6) 1.01802(8) 0.11914(7) 0.0538(3) Uani 1 1 d . . .
C15 C 0.5989(6) 0.8320(7) 0.0814(6) 0.048(2) Uani 1 1 d . . .
H15 H 0.6624 0.8185 0.0760 0.058 Uiso 1 1 calc R . .
C16 C 0.5344(7) 0.7619(7) 0.0687(6) 0.049(2) Uani 1 1 d . . .
H16 H 0.5536 0.6984 0.0558 0.058 Uiso 1 1 calc R . .
N21 N 0.5015(5) 0.4611(5) 0.1840(4) 0.0438(18) Uani 1 1 d . . .
H21 H 0.4816 0.4784 0.1293 0.053 Uiso 1 1 calc R . .
C22 C 0.5807(6) 0.4150(7) 0.1923(6) 0.048(2) Uani 1 1 d . . .
H22 H 0.6161 0.4025 0.1404 0.057 Uiso 1 1 calc R . .
C23 C 0.6110(6) 0.3857(6) 0.2771(6) 0.044(2) Uani 1 1 d . . .
H23 H 0.6661 0.3499 0.2842 0.053 Uiso 1 1 calc R . .
C24 C 0.5612(5) 0.4083(6) 0.3511(5) 0.0319(18) Uani 1 1 d . . .
Br24 Br 0.60462(7) 0.37148(7) 0.46750(6) 0.0488(3) Uani 1 1 d . . .
C26 C 0.4504(7) 0.4823(7) 0.2556(6) 0.050(2) Uani 1 1 d . . .
H26 H 0.3939 0.5153 0.2468 0.060 Uiso 1 1 calc R . .
C25 C 0.4795(6) 0.4565(6) 0.3408(5) 0.040(2) Uani 1 1 d . . .
H25 H 0.4441 0.4714 0.3921 0.049 Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl1 Fe1 Cl4 110.52(10) . . ?
Cl1 Fe1 Cl2 107.18(12) . . ?
Cl4 Fe1 Cl2 108.22(11) . . ?
Cl1 Fe1 Cl3 111.90(12) . . ?
Cl4 Fe1 Cl3 107.00(11) . . ?
Cl2 Fe1 Cl3 111.99(11) . . ?
Cl5 Fe2 Cl7 108.87(11) . . ?
Cl5 Fe2 Cl8 110.74(10) . . ?
Cl7 Fe2 Cl8 107.61(11) . . ?
Cl5 Fe2 Cl6 110.22(11) . . ?
Cl7 Fe2 Cl6 108.10(10) . . ?
Cl8 Fe2 Cl6 111.20(10) . . ?
C36 N31 C32 123.1(8) . . ?
N31 C32 C33 118.6(8) . . ?
C32 C33 C34 120.3(8) . . ?
C33 C34 C35 120.3(7) . . ?
C33 C34 Br34 120.7(6) . . ?
C35 C34 Br34 119.0(6) . . ?
C36 C35 C34 117.6(8) . . ?
N31 C36 C35 120.1(9) . . ?
C16 N11 C12 121.3(8) . . ?
N11 C12 C13 120.5(9) . . ?
C12 C13 C14 118.1(9) . . ?
C15 C14 C13 120.7(8) . . ?
C15 C14 Br14 118.6(6) . . ?
C13 C14 Br14 120.6(7) . . ?
C14 C15 C16 118.1(9) . . ?
N11 C16 C15 121.2(9) . . ?
C22 N21 C26 122.6(7) . . ?
N21 C22 C23 119.0(8) . . ?
C24 C23 C22 119.4(8) . . ?
C23 C24 C25 120.5(7) . . ?
C23 C24 Br24 119.3(6) . . ?
C25 C24 Br24 120.2(6) . . ?
N21 C26 C25 119.9(9) . . ?
C26 C25 C24 118.6(8) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 Cl1 2.180(3) . ?
Fe1 Cl4 2.180(3) . ?
Fe1 Cl2 2.182(3) . ?
Fe1 Cl3 2.189(3) . ?
Fe2 Cl5 2.179(3) . ?
Fe2 Cl7 2.182(3) . ?
Fe2 Cl8 2.184(3) . ?
Fe2 Cl6 2.187(3) . ?
N31 C36 1.314(11) . ?
N31 C32 1.340(11) . ?
C32 C33 1.346(11) . ?
C33 C34 1.363(12) . ?
C34 C35 1.379(12) . ?
C34 Br34 1.868(8) . ?
C35 C36 1.376(12) . ?
N11 C16 1.311(11) . ?
N11 C12 1.330(12) . ?
C12 C13 1.366(13) . ?
C13 C14 1.374(12) . ?
C14 C15 1.357(12) . ?
C14 Br14 1.864(8) . ?
C15 C16 1.367(12) . ?
N21 C22 1.325(11) . ?
N21 C26 1.341(11) . ?
C22 C23 1.372(11) . ?
C23 C24 1.363(11) . ?
C24 C25 1.372(11) . ?
C24 Br24 1.878(7) . ?
C26 C25 1.359(11) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C36 N31 C32 C33 0.3(12) . . . . ?
N31 C32 C33 C34 -0.8(12) . . . . ?
C32 C33 C34 C35 0.9(12) . . . . ?
C32 C33 C34 Br34 -178.6(6) . . . . ?
C33 C34 C35 C36 -0.4(13) . . . . ?
Br34 C34 C35 C36 179.1(6) . . . . ?
C32 N31 C36 C35 0.2(12) . . . . ?
C34 C35 C36 N31 -0.1(13) . . . . ?
C16 N11 C12 C13 -0.1(13) . . . . ?
N11 C12 C13 C14 -0.9(13) . . . . ?
C12 C13 C14 C15 2.1(12) . . . . ?
C12 C13 C14 Br14 179.6(6) . . . . ?
C13 C14 C15 C16 -2.5(13) . . . . ?
Br14 C14 C15 C16 -180.0(6) . . . . ?
C12 N11 C16 C15 -0.3(13) . . . . ?
C14 C15 C16 N11 1.5(13) . . . . ?
C26 N21 C22 C23 1.6(13) . . . . ?
N21 C22 C23 C24 -3.0(13) . . . . ?
C22 C23 C24 C25 2.7(13) . . . . ?
C22 C23 C24 Br24 -178.1(7) . . . . ?
C22 N21 C26 C25 0.1(14) . . . . ?
N21 C26 C25 C24 -0.4(14) . . . . ?
C23 C24 C25 C26 -1.1(13) . . . . ?
Br24 C24 C25 C26 179.7(7) . . . . ?
