#------------------------------------------------------------------------------
#$Date: 2016-03-24 02:09:31 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179559 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/28/4502842.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_4502842
loop_
_publ_author_name
'Ormond-Prout, Johnathan E.'
'Smart, Paul'
'Brammer, Lee'
_publ_section_title
;
 Cyanometallates as Halogen Bond Acceptors
;
_journal_issue                   1
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              205
_journal_paper_doi               10.1021/cg200942u
_journal_volume                  12
_journal_year                    2012
_chemical_formula_sum            'C24 H18 Fe I6 N9'
_chemical_formula_weight         1249.72
_chemical_name_systematic
; 
 ? 
;
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 113.893(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.8980(6)
_cell_length_b                   15.4085(5)
_cell_length_c                   12.4411(3)
_cell_measurement_reflns_used    4905
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.34
_cell_measurement_theta_min      2.24
_cell_volume                     3487.54(18)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and 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  0.0505
_diffrn_reflns_av_sigmaI/netI    0.0544
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16922
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    5.773
_exptl_absorpt_correction_T_max  0.5960
_exptl_absorpt_correction_T_min  0.2763
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.380
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2276
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.330
_refine_diff_density_min         -1.371
_refine_diff_density_rms         0.209
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.310
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     186
_refine_ls_number_reflns         4008
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.310
_refine_ls_R_factor_all          0.0708
_refine_ls_R_factor_gt           0.0412
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0415P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0920
_refine_ls_wR_factor_ref         0.1140
_reflns_number_gt                2812
_reflns_number_total             4008
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg200942u_si_002.cif
_cod_data_source_block           ilb1626_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4502842
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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
I31 I 0.09495(3) 0.39736(3) 1.01367(3) 0.02888(16) Uani 1 1 d .
I21 I -0.02537(3) 0.10110(3) 0.07556(4) 0.03478(17) Uani 1 1 d .
I22 I 0.14432(3) 0.21160(3) -0.20568(4) 0.03940(18) Uani 1 1 d .
Fe1 Fe 0.7500 0.2500 1.0000 0.0345(4) Uani 1 2 d S
C13 C 0.6654(4) 0.2077(5) 1.0464(5) 0.0283(17) Uani 1 1 d .
C12 C 0.6936(4) 0.2093(5) 0.8268(6) 0.0294(17) Uani 1 1 d .
C23 C 0.0745(4) 0.1143(4) 0.0586(6) 0.0296(18) Uani 1 1 d .
C22 C 0.1377(5) 0.0784(5) 0.1406(6) 0.0332(19) Uani 1 1 d .
H22 H 0.1367 0.0516 0.2088 0.040 Uiso 1 1 calc R
C25 C 0.1415(4) 0.1565(5) -0.0534(6) 0.0304(18) Uani 1 1 d .
C26 C 0.2037(4) 0.1192(5) 0.0294(6) 0.0326(19) Uani 1 1 d .
H26 H 0.2485 0.1204 0.0192 0.039 Uiso 1 1 calc R
C24 C 0.0762(4) 0.1556(5) -0.0404(6) 0.0311(18) Uani 1 1 d .
H24 H 0.0335 0.1823 -0.0969 0.037 Uiso 1 1 calc R
N21 N 0.2010(4) 0.0807(4) 0.1255(5) 0.0321(15) Uani 1 1 d .
C21 C 0.2683(4) 0.0377(5) 0.2122(6) 0.042(2) Uani 1 1 d .
H21A H 0.2746 -0.0189 0.1816 0.063 Uiso 1 1 calc R
H21B H 0.2633 0.0297 0.2867 0.063 Uiso 1 1 calc R
H21C H 0.3113 0.0741 0.2252 0.063 Uiso 1 1 calc R
C11 C 0.7956(4) 0.1282(5) 1.0450(5) 0.0288(17) Uani 1 1 d .
C33 C 0.0381(4) 0.4621(4) 0.8530(5) 0.0234(16) Uani 1 1 d .
C32 C 0.0366(4) 0.5506(4) 0.8508(5) 0.0254(16) Uani 1 1 d .
H32 H 0.0617 0.5825 0.9212 0.031 Uiso 1 1 calc R
C34 C 0.0000 0.4165(6) 0.7500 0.027(2) Uani 1 2 d S
H34 H 0.0000 0.3549 0.7500 0.033 Uiso 1 2 calc SR
N11 N 0.8212(4) 0.0604(4) 1.0754(5) 0.0358(16) Uani 1 1 d .
N13 N 0.6210(4) 0.1832(4) 1.0751(5) 0.0382(17) Uani 1 1 d .
N12 N 0.6651(4) 0.1865(4) 0.7312(5) 0.0441(18) Uani 1 1 d .
N31 N 0.0000 0.5924(5) 0.7500 0.0234(19) Uani 1 2 d S
C31 C 0.0000 0.6874(6) 0.7500 0.036(3) Uani 1 2 d S
H31A H 0.0336 0.7086 0.7161 0.054 Uiso 0.50 1 calc PR
H31B H 0.0162 0.7086 0.8309 0.054 Uiso 0.50 1 calc PR
H31C H -0.0498 0.7086 0.7030 0.054 Uiso 0.50 1 calc PR
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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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
C11 Fe1 C11 179.998(1) 7_657 .
C11 Fe1 C12 90.0(3) 7_657 7_657
C11 Fe1 C12 90.0(3) . 7_657
C11 Fe1 C12 90.0(3) 7_657 .
C11 Fe1 C12 90.0(3) . .
C12 Fe1 C12 180.000(1) 7_657 .
C11 Fe1 C13 87.5(3) 7_657 7_657
C11 Fe1 C13 92.5(3) . 7_657
C12 Fe1 C13 92.0(3) 7_657 7_657
C12 Fe1 C13 88.0(3) . 7_657
C11 Fe1 C13 92.5(3) 7_657 .
C11 Fe1 C13 87.5(3) . .
C12 Fe1 C13 88.0(3) 7_657 .
C12 Fe1 C13 92.0(3) . .
C13 Fe1 C13 179.999(1) 7_657 .
N13 C13 Fe1 177.6(7) . .
N12 C12 Fe1 177.4(7) . .
C22 C23 C24 119.7(7) . .
C22 C23 I21 120.4(5) . .
C24 C23 I21 119.8(6) . .
N21 C22 C23 120.8(6) . .
N21 C22 H22 119.6 . .
C23 C22 H22 119.6 . .
C24 C25 C26 121.0(7) . .
C24 C25 I22 118.9(5) . .
C26 C25 I22 120.1(6) . .
N21 C26 C25 119.9(7) . .
N21 C26 H26 120.0 . .
C25 C26 H26 120.0 . .
C25 C24 C23 118.1(7) . .
C25 C24 H24 120.9 . .
C23 C24 H24 120.9 . .
C22 N21 C26 120.5(7) . .
C22 N21 C21 120.2(6) . .
C26 N21 C21 119.2(7) . .
N21 C21 H21A 109.5 . .
N21 C21 H21B 109.5 . .
H21A C21 H21B 109.5 . .
N21 C21 H21C 109.5 . .
H21A C21 H21C 109.5 . .
H21B C21 H21C 109.5 . .
N11 C11 Fe1 176.8(6) . .
C32 C33 C34 119.3(6) . .
C32 C33 I31 119.4(4) . .
C34 C33 I31 121.3(5) . .
N31 C32 C33 120.0(6) . .
N31 C32 H32 120.0 . .
C33 C32 H32 120.0 . .
C33 C34 C33 119.1(9) . 2_556
C33 C34 H34 120.4 . .
C33 C34 H34 120.4 2_556 .
C32 N31 C32 122.2(8) 2_556 .
C32 N31 C31 118.9(4) 2_556 .
C32 N31 C31 118.9(4) . .
N31 C31 H31A 109.5 . .
N31 C31 H31B 109.5 . .
H31A C31 H31B 109.5 . .
N31 C31 H31C 109.5 . .
H31A C31 H31C 109.5 . .
H31B C31 H31C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
I31 C33 2.107(6) .
I21 C23 2.091(7) .
I22 C25 2.097(7) .
Fe1 C11 2.061(8) 7_657
Fe1 C11 2.061(8) .
Fe1 C12 2.083(7) 7_657
Fe1 C12 2.083(7) .
Fe1 C13 2.093(8) 7_657
Fe1 C13 2.093(8) .
C13 N13 1.141(9) .
C12 N12 1.146(8) .
C23 C22 1.375(10) .
C23 C24 1.399(9) .
C22 N21 1.349(9) .
C22 H22 0.9500 .
C25 C24 1.373(10) .
C25 C26 1.375(10) .
C26 N21 1.355(8) .
C26 H26 0.9500 .
C24 H24 0.9500 .
N21 C21 1.491(9) .
C21 H21A 0.9800 .
C21 H21B 0.9800 .
C21 H21C 0.9800 .
C11 N11 1.157(9) .
C33 C32 1.364(9) .
C33 C34 1.387(8) .
C32 N31 1.334(7) .
C32 H32 0.9500 .
C34 C33 1.387(8) 2_556
C34 H34 0.9500 .
N31 C32 1.334(7) 2_556
N31 C31 1.464(12) .
C31 H31A 0.9800 .
C31 H31B 0.9800 .
C31 H31C 0.9800 .
