#------------------------------------------------------------------------------
#$Date: 2016-03-22 21:07:06 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179012 $
#$URL: svn://www.crystallography.net/cod/cif/4/12/10/4121007.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_4121007
loop_
_publ_author_name
'Eugenio Coronado'
'Mónica Giménez-Marqués'
'Guillermo Mínguez Espallargas'
'Fernando Rey'
'Iñigo J. Vitórica-Yrezábal'
_publ_section_title
;
 Spin-Crossover Modification through Selective CO2 Sorption
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15986
_journal_page_last               15989
_journal_paper_doi               10.1021/ja407135k
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C30 H30 Cl2 Fe N24 O8'
_chemical_formula_weight         981.53
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           176
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_space_group_name_H-M   'P 63/m'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   10.5117(7)
_cell_length_b                   10.5117(7)
_cell_length_c                   23.576(2)
_cell_measurement_reflns_used    376
_cell_measurement_temperature    240(2)
_cell_measurement_theta_max      24.9905
_cell_measurement_theta_min      3.4179
_cell_volume                     2256.0(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      240(2)
_diffrn_detector_area_resol_mean 16.0267
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type
'SuperNova, Single source at offset), Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Mo) x-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1962
_diffrn_reflns_av_sigmaI/netI    0.1724
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            8181
_diffrn_reflns_theta_full        25.04
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         3.42
_exptl_absorpt_coefficient_mu    0.527
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64784
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.445
_exptl_crystal_description       block
_exptl_crystal_F_000             1004
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.840
_refine_diff_density_min         -0.679
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     97
_refine_ls_number_reflns         1377
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.2033
_refine_ls_R_factor_gt           0.0984
_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)+(0.1379P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2367
_refine_ls_wR_factor_ref         0.2975
_reflns_number_gt                632
_reflns_number_total             1377
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja407135k_si_002.cif
_cod_data_source_block           sx285bb
_cod_original_cell_volume        2256.1(3)
_cod_database_code               4121007
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -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_group
Fe1 Fe 1.0000 1.0000 0.5000 0.0281(8) Uani 1 6 d S .
O1 O 0.8020(10) 0.4505(9) 0.4954(3) 0.098(3) Uiso 1 1 d . .
Cl1 Cl 0.6667 0.3333 0.5075(5) 0.035(2) Uiso 0.64(2) 3 d SP 1
O2 O 0.6667 0.3333 0.5655(10) 0.106(10) Uiso 0.64(2) 3 d SP 1
Cl1' Cl 0.6667 0.3333 0.4871(11) 0.056(5) Uiso 0.36(2) 3 d SP 2
O2' O 0.6667 0.3333 0.4284(15) 0.079(14) Uiso 0.36(2) 3 d SP 2
N1 N 0.9551(7) 0.8137(7) 0.5525(2) 0.0370(17) Uani 1 1 d . .
C2 C 1.0339(9) 0.7515(9) 0.5620(3) 0.038(2) Uani 1 1 d . .
H2 H 1.1210 0.7738 0.5428 0.046 Uiso 1 1 calc R .
N3 N 0.9733(8) 0.6528(7) 0.6027(3) 0.0418(19) Uani 1 1 d . .
N4 N 0.8471(8) 0.6465(9) 0.6184(3) 0.062(2) Uani 1 1 d . .
N5 N 0.8391(8) 0.7484(9) 0.5887(3) 0.058(2) Uani 1 1 d . .
C6 C 1.0125(11) 0.5480(10) 0.6262(3) 0.055(3) Uani 1 1 d . .
H6A H 1.1095 0.5716 0.6120 0.082 Uiso 1 1 calc R .
H6B H 0.9413 0.4488 0.6132 0.082 Uiso 1 1 calc R .
C7 C 1.0152(9) 0.5501(9) 0.6909(3) 0.040(2) Uani 1 1 d . .
C8 C 1.1143(10) 0.6718(10) 0.7201(3) 0.062(3) Uani 1 1 d . .
H8 H 1.1828 0.7560 0.7002 0.075 Uiso 1 1 calc R .
C9 C 0.9163(10) 0.4277(9) 0.7208(3) 0.051(3) Uani 1 1 d . .
H9 H 0.8480 0.3431 0.7011 0.061 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'
O O 0.0106 0.0060 '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'
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
N1 Fe1 N1 180.000(1) 2_765 8_566
N1 Fe1 N1 90.4(2) 2_765 3_675
N1 Fe1 N1 89.6(2) 8_566 3_675
N1 Fe1 N1 90.4(2) 2_765 .
N1 Fe1 N1 89.6(2) 8_566 .
N1 Fe1 N1 90.4(2) 3_675 .
N1 Fe1 N1 89.6(2) 2_765 9_656
N1 Fe1 N1 90.4(2) 8_566 9_656
N1 Fe1 N1 180.0(2) 3_675 9_656
N1 Fe1 N1 89.6(2) . 9_656
N1 Fe1 N1 89.6(2) 2_765 7_776
N1 Fe1 N1 90.4(2) 8_566 7_776
N1 Fe1 N1 89.6(2) 3_675 7_776
N1 Fe1 N1 180.0(2) . 7_776
N1 Fe1 N1 90.4(2) 9_656 7_776
O1 Cl1 O1 115.8(4) 3_665 .
O1 Cl1 O1 115.8(4) 3_665 2_655
O1 Cl1 O1 115.8(4) . 2_655
O1 Cl1 O2 102.0(5) 3_665 .
O1 Cl1 O2 102.0(5) . .
O1 Cl1 O2 102.0(5) 2_655 .
O1 Cl1' O1 117.9(6) 3_665 .
O1 Cl1' O1 117.9(6) 3_665 2_655
O1 Cl1' O1 117.9(6) . 2_655
O1 Cl1' O2' 98.3(12) 3_665 .
O1 Cl1' O2' 98.3(12) . .
O1 Cl1' O2' 98.3(12) 2_655 .
C2 N1 N5 105.8(6) . .
C2 N1 Fe1 130.3(5) . .
N5 N1 Fe1 123.5(5) . .
N1 C2 N3 109.9(7) . .
N1 C2 H2 125.1 . .
N3 C2 H2 125.1 . .
C2 N3 N4 108.4(7) . .
C2 N3 C6 131.3(7) . .
N4 N3 C6 120.0(7) . .
N5 N4 N3 106.0(6) . .
N4 N5 N1 109.8(7) . .
N3 C6 C7 112.2(7) . .
N3 C6 H6A 109.2 . .
C7 C6 H6A 109.2 . .
N3 C6 H6B 109.2 . .
C7 C6 H6B 109.2 . .
H6A C6 H6B 107.9 . .
C8 C7 C9 118.9(7) . .
C8 C7 C6 121.2(8) . .
C9 C7 C6 119.9(8) . .
C7 C8 C8 120.3(5) . 10_557
C7 C8 H8 119.9 . .
C8 C8 H8 119.9 10_557 .
C7 C9 C9 120.8(5) . 10_557
C7 C9 H9 119.6 . .
C9 C9 H9 119.6 10_557 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 N1 2.160(6) 2_765
Fe1 N1 2.160(6) 8_566
Fe1 N1 2.160(6) 3_675
Fe1 N1 2.160(6) .
Fe1 N1 2.160(6) 9_656
Fe1 N1 2.160(6) 7_776
O1 Cl1' 1.352(10) .
O1 Cl1 1.367(9) .
Cl1 O1 1.367(9) 3_665
Cl1 O1 1.367(9) 2_655
Cl1 O2 1.37(2) .
Cl1' O1 1.352(10) 3_665
Cl1' O1 1.352(10) 2_655
Cl1' O2' 1.38(4) .
N1 C2 1.306(9) .
N1 N5 1.361(8) .
C2 N3 1.319(9) .
C2 H2 0.9400 .
N3 N4 1.346(9) .
N3 C6 1.466(10) .
N4 N5 1.316(10) .
C6 C7 1.525(11) .
C6 H6A 0.9800 .
C6 H6B 0.9800 .
C7 C8 1.364(11) .
C7 C9 1.377(11) .
C8 C8 1.412(16) 10_557
C8 H8 0.9400 .
C9 C9 1.378(14) 10_557
C9 H9 0.9400 .
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_4
Cl1' O1 Cl1 O1 70.2(8) . 3_665
Cl1' O1 Cl1 O1 -70.2(8) . 2_655
Cl1' O1 Cl1 O2 180.0 . .
Cl1 O1 Cl1' O1 -75.9(19) . 3_665
Cl1 O1 Cl1' O1 75.9(19) . 2_655
Cl1 O1 Cl1' O2' 180.000(1) . .
N1 Fe1 N1 C2 -63.3(8) 2_765 .
N1 Fe1 N1 C2 116.7(8) 8_566 .
N1 Fe1 N1 C2 -153.7(6) 3_675 .
N1 Fe1 N1 C2 26.3(6) 9_656 .
N1 Fe1 N1 N5 108.1(5) 2_765 .
N1 Fe1 N1 N5 -71.9(5) 8_566 .
N1 Fe1 N1 N5 17.6(6) 3_675 .
N1 Fe1 N1 N5 -162.4(6) 9_656 .
N5 N1 C2 N3 -0.7(8) . .
Fe1 N1 C2 N3 171.7(5) . .
N1 C2 N3 N4 2.7(9) . .
N1 C2 N3 C6 175.5(8) . .
C2 N3 N4 N5 -3.5(9) . .
C6 N3 N4 N5 -177.3(7) . .
N3 N4 N5 N1 3.1(10) . .
C2 N1 N5 N4 -1.5(9) . .
Fe1 N1 N5 N4 -174.6(5) . .
C2 N3 C6 C7 132.2(8) . .
N4 N3 C6 C7 -55.7(11) . .
N3 C6 C7 C8 -64.6(11) . .
N3 C6 C7 C9 115.3(9) . .
C9 C7 C8 C8 -0.3(10) . 10_557
C6 C7 C8 C8 179.6(5) . 10_557
C8 C7 C9 C9 0.3(10) . 10_557
C6 C7 C9 C9 -179.6(5) . 10_557
