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#$Date: 2016-03-22 12:55:48 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178967 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/96/4119607.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_4119607
loop_
_publ_author_name
'Yi-Tong Wang'
'Shu-Tao Li'
'Shu-Qi Wu'
'Ai-Li Cui'
'De-Zhong Shen'
'Hui-Zhong Kou'
_publ_contact_author_address
;
Department of Chemistry
Tsinghua University
Beijing 100084
People's Republic of China
;
_publ_contact_author_email       kouhz@mail.tsinghua.edu.cn
_publ_contact_author_name        'Dr. Hui-Zhong Kou'
_publ_contact_author_phone       86-10-62771748
_publ_section_title
;
 Spin Transitions in Fe(II) Metallogrids Modulated by Substituents,
 Counteranions, and Solvents
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5942
_journal_page_last               5945
_journal_paper_doi               10.1021/ja312622c
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C64 H58 B4 Br8 F16 Fe4 N32 O7'
_chemical_formula_weight         2597.34
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           59
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ab 2a'
_symmetry_space_group_name_H-M   'P m m n :2'
_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                90.00
_cell_formula_units_Z            2
_cell_length_a                   21.262(4)
_cell_length_b                   25.265(5)
_cell_length_c                   8.0593(16)
_cell_measurement_reflns_used    16067
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      31.4713
_cell_measurement_theta_min      2.4184
_cell_volume                     4329.3(15)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  Saturn724+
_diffrn_measurement_method       dtprofit.ref
_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  0.0543
_diffrn_reflns_av_sigmaI/netI    0.0335
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            56006
_diffrn_reflns_theta_full        31.47
_diffrn_reflns_theta_max         31.47
_diffrn_reflns_theta_min         3.00
_exptl_absorpt_coefficient_mu    4.453
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7168
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.992
_exptl_crystal_description       stick
_exptl_crystal_F_000             2520
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.707
_refine_diff_density_min         -1.953
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     347
_refine_ls_number_reflns         7479
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0804
_refine_ls_R_factor_gt           0.0729
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0709P)²+18.7870P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1709
_refine_ls_wR_factor_ref         0.1757
_reflns_number_gt                6847
_reflns_number_total             7479
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja312622c_si_002_3.cif
_cod_data_source_block           2
_cod_original_cell_volume        4329.5(15)
_cod_original_sg_symbol_H-M      'P m m n'
_cod_database_code               4119607
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-x, y+1/2, -z'
'x+1/2, -y, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'x, -y-1/2, z'
'-x-1/2, y, z'
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
Fe1 Fe 0.60751(3) 0.62994(2) -0.31228(6) 0.01780(12) Uani 1 1 d .
Br1 Br 0.56006(3) 0.537194(18) -0.64163(6) 0.03565(14) Uani 1 1 d .
Br2 Br 0.49515(2) 0.57932(3) -0.00230(7) 0.04975(19) Uani 1 1 d .
B1 B 0.7500 0.4754(6) 0.305(2) 0.074(4) Uani 1 2 d S
B2 B 0.5514(7) 0.2500 -0.0645(17) 0.065(3) Uani 1 2 d S
F1 F 0.7500 0.4361(4) 0.4085(11) 0.109(3) Uani 1 2 d S
F2 F 0.7500 0.5162(5) 0.437(3) 0.221(9) Uani 1 2 d S
F3 F 0.6958(3) 0.4815(4) 0.2304(8) 0.141(3) Uani 1 1 d .
F4 F 0.5763(8) 0.2909(9) -0.149(2) 0.142(8) Uani 0.50 1 d P
F5 F 0.560(3) 0.2500 0.087(3) 0.19(2) Uani 0.50 2 d SP
F6 F 0.4922(8) 0.2500 -0.142(2) 0.094(5) Uani 0.50 2 d SP
F7 F 0.5236(11) 0.2500 0.085(4) 0.129(11) Uani 0.50 2 d SP
F8 F 0.6133(12) 0.2500 0.004(4) 0.141(11) Uani 0.50 2 d SP
F9 F 0.5320(19) 0.2975(7) -0.098(3) 0.28(2) Uani 0.50 1 d P
C1 C 0.5998(2) 0.51373(17) -0.4452(5) 0.0259(8) Uani 1 1 d .
C2 C 0.6118(2) 0.45963(18) -0.4341(6) 0.0324(9) Uani 1 1 d .
H2A H 0.6015 0.4371 -0.5212 0.039 Uiso 1 1 calc R
C3 C 0.6392(2) 0.44006(18) -0.2924(6) 0.0338(10) Uani 1 1 d .
H3A H 0.6479 0.4041 -0.2823 0.041 Uiso 1 1 calc R
C4 C 0.6536(2) 0.47498(18) -0.1638(6) 0.0290(8) Uani 1 1 d .
H4A H 0.6722 0.4627 -0.0667 0.035 Uiso 1 1 calc R
C5 C 0.63963(19) 0.52862(16) -0.1834(5) 0.0232(7) Uani 1 1 d .
C6 C 0.65071(19) 0.56686(16) -0.0530(5) 0.0232(7) Uani 1 1 d .
H6A H 0.6679 0.5581 0.0495 0.028 Uiso 1 1 calc R
C7 C 0.63109(19) 0.70294(16) -0.0564(4) 0.0207(7) Uani 1 1 d .
C8 C 0.6399(3) 0.7500 0.0287(7) 0.0247(11) Uani 1 2 d S
H8A H 0.6514 0.7500 0.1401 0.030 Uiso 1 2 calc SR
C9 C 0.6057(2) 0.7500 -0.2933(6) 0.0172(9) Uani 1 2 d S
H9A H 0.5940 0.7500 -0.4045 0.021 Uiso 1 2 calc SR
C10 C 0.4687(2) 0.62049(18) -0.1845(5) 0.0271(8) Uani 1 1 d .
C11 C 0.4052(2) 0.6334(2) -0.1910(6) 0.0327(9) Uani 1 1 d .
H11A H 0.3781 0.6235 -0.1060 0.039 Uiso 1 1 calc R
C12 C 0.3832(2) 0.6613(2) -0.3263(6) 0.0330(9) Uani 1 1 d .
H12A H 0.3413 0.6716 -0.3315 0.040 Uiso 1 1 calc R
C13 C 0.4244(2) 0.67373(17) -0.4551(6) 0.0268(8) Uani 1 1 d .
H13A H 0.4104 0.6914 -0.5493 0.032 Uiso 1 1 calc R
C14 C 0.48713(19) 0.65882(15) -0.4383(5) 0.0226(7) Uani 1 1 d .
C15 C 0.53282(19) 0.66837(15) -0.5686(5) 0.0229(7) Uani 1 1 d .
H15A H 0.5226 0.6837 -0.6700 0.027 Uiso 1 1 calc R
C16 C 0.69436(19) 0.64970(15) -0.5683(4) 0.0202(7) Uani 1 1 d .
C17 C 0.7500 0.6562(2) -0.6541(7) 0.0243(11) Uani 1 2 d S
H17A H 0.7500 0.6646 -0.7664 0.029 Uiso 1 2 calc SR
C18 C 0.7500 0.6292(2) -0.3303(6) 0.0187(9) Uani 1 2 d S
H18A H 0.7500 0.6197 -0.2187 0.022 Uiso 1 2 calc SR
N1 N 0.61281(16) 0.54925(13) -0.3267(4) 0.0212(6) Uani 1 1 d .
N2 N 0.63427(16) 0.61451(13) -0.0930(4) 0.0206(6) Uani 1 1 d .
N3 N 0.64150(18) 0.65563(13) 0.0156(4) 0.0236(7) Uani 1 1 d .
H3B H 0.6516 0.6517 0.1182 0.028 Uiso 1 1 calc R
N4 N 0.61324(15) 0.70280(13) -0.2214(4) 0.0188(6) Uani 1 1 d .
N5 N 0.51100(16) 0.63348(13) -0.3000(4) 0.0215(6) Uani 1 1 d .
N6 N 0.58917(16) 0.65341(13) -0.5300(4) 0.0203(6) Uani 1 1 d .
N7 N 0.63785(16) 0.65927(14) -0.6397(4) 0.0223(6) Uani 1 1 d .
N8 N 0.69414(15) 0.63531(12) -0.4025(4) 0.0179(6) Uani 1 1 d .
O1W O 0.7500 0.3429(3) -0.4096(10) 0.079(2) Uani 1 2 d S
O2W O 0.7500 0.2500 0.4143(15) 0.076(3) Uani 1 4 d S
O3W O 0.7213(10) 0.2500 0.080(2) 0.100(7) Uani 0.50 2 d SP
O4W O 0.7500 0.3436(14) -0.066(3) 0.45(3) Uani 1 2 d S
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'
B B 0.0013 0.0007 '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'
F F 0.0171 0.0103 '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
N6 Fe1 N2 171.80(15) . .
N6 Fe1 N8 80.24(14) . .
N2 Fe1 N8 94.40(14) . .
N6 Fe1 N4 93.67(14) . .
N2 Fe1 N4 80.13(14) . .
N8 Fe1 N4 90.84(13) . .
N6 Fe1 N1 105.73(14) . .
N2 Fe1 N1 80.29(14) . .
N8 Fe1 N1 89.78(13) . .
N4 Fe1 N1 160.40(13) . .
N6 Fe1 N5 79.93(14) . .
N2 Fe1 N5 105.28(14) . .
N8 Fe1 N5 160.17(13) . .
N4 Fe1 N5 90.19(14) . .
N1 Fe1 N5 95.80(14) . .
F1 B1 F3 112.7(7) . 8_755
F1 B1 F3 112.7(7) . .
F3 B1 F3 123.2(12) 8_755 .
F1 B1 F2 94.3(14) . .
F3 B1 F2 104.3(11) 8_755 .
F3 B1 F2 104.3(10) . .
F5 B2 F9 104.6(14) . .
F5 B2 F9 104.6(14) . 7_565
F9 B2 F9 135(3) . 7_565
F5 B2 F7 35(3) . .
F9 B2 F7 92.6(18) . .
F9 B2 F7 92.6(18) 7_565 .
F5 B2 F4 116.2(19) . 7_565
F9 B2 F4 137(2) . 7_565
F9 B2 F4 46.4(19) 7_565 7_565
F7 B2 F4 128.9(11) . 7_565
F5 B2 F4 116.2(19) . .
F9 B2 F4 46.4(19) . .
F9 B2 F4 137(2) 7_565 .
F7 B2 F4 128.9(11) . .
F4 B2 F4 100(2) 7_565 .
F5 B2 F6 125(3) . .
F9 B2 F6 67.9(15) . .
F9 B2 F6 67.9(15) 7_565 .
F7 B2 F6 90.3(17) . .
F4 B2 F6 97.3(12) 7_565 .
F4 B2 F6 97.3(12) . .
F5 B2 F8 58(2) . .
F9 B2 F8 111.9(16) . .
F9 B2 F8 111.9(16) 7_565 .
F7 B2 F8 93.3(18) . .
F4 B2 F8 80.4(14) 7_565 .
F4 B2 F8 80.4(14) . .
F6 B2 F8 176(2) . .
F9 F4 B2 64.1(15) . .
F7 F5 B2 80(3) . .
F7 F5 F8 149(3) . .
B2 F5 F8 68(2) . .
B2 F6 F9 52.7(10) . .
B2 F6 F9 52.7(10) . 7_565
F9 F6 F9 105(2) . 7_565
F5 F7 B2 65(3) . .
F5 F8 B2 53.3(13) . .
F4 F9 B2 69.4(19) . .
F4 F9 F6 107(2) . .
B2 F9 F6 59.4(12) . .
N1 C1 C2 125.0(4) . .
N1 C1 Br1 118.6(3) . .
C2 C1 Br1 116.3(3) . .
C3 C2 C1 119.0(4) . .
C3 C2 H2A 120.5 . .
C1 C2 H2A 120.5 . .
C2 C3 C4 118.9(4) . .
C2 C3 H3A 120.6 . .
C4 C3 H3A 120.6 . .
C3 C4 C5 118.9(4) . .
C3 C4 H4A 120.6 . .
C5 C4 H4A 120.6 . .
N1 C5 C4 123.1(4) . .
N1 C5 C6 114.8(3) . .
C4 C5 C6 122.1(4) . .
N2 C6 C5 113.3(3) . .
N2 C6 H6A 123.3 . .
C5 C6 H6A 123.3 . .
N3 C7 N4 117.2(3) . .
N3 C7 C8 121.7(3) . .
N4 C7 C8 121.0(4) . .
C7 C8 C7 118.2(5) . 7_575
C7 C8 H8A 120.9 . .
C7 C8 H8A 120.9 7_575 .
N4 C9 N4 126.5(5) . 7_575
N4 C9 H9A 116.7 . .
N4 C9 H9A 116.7 7_575 .
N5 C10 C11 124.7(4) . .
N5 C10 Br2 118.6(3) . .
C11 C10 Br2 116.6(3) . .
C12 C11 C10 118.6(4) . .
C12 C11 H11A 120.7 . .
C10 C11 H11A 120.7 . .
C11 C12 C13 119.4(4) . .
C11 C12 H12A 120.3 . .
C13 C12 H12A 120.3 . .
C14 C13 C12 117.9(4) . .
C14 C13 H13A 121.0 . .
C12 C13 H13A 121.0 . .
N5 C14 C13 123.7(4) . .
N5 C14 C15 114.5(3) . .
C13 C14 C15 121.7(4) . .
N6 C15 C14 113.4(3) . .
N6 C15 H15A 123.3 . .
C14 C15 H15A 123.3 . .
N7 C16 C17 121.8(3) . .
N7 C16 N8 117.0(3) . .
C17 C16 N8 121.2(4) . .
C16 C17 C16 118.0(5) 8_755 .
C16 C17 H17A 121.0 8_755 .
C16 C17 H17A 121.0 . .
N8 C18 N8 126.2(5) 8_755 .
N8 C18 H18A 116.9 8_755 .
N8 C18 H18A 116.9 . .
C1 N1 C5 115.2(3) . .
C1 N1 Fe1 134.2(3) . .
C5 N1 Fe1 110.5(3) . .
C6 N2 N3 121.1(3) . .
C6 N2 Fe1 120.3(3) . .
N3 N2 Fe1 118.3(2) . .
C7 N3 N2 112.3(3) . .
C7 N3 H3B 123.8 . .
N2 N3 H3B 123.8 . .
C9 N4 C7 116.6(3) . .
C9 N4 Fe1 131.4(3) . .
C7 N4 Fe1 112.0(3) . .
C10 N5 C14 115.4(3) . .
C10 N5 Fe1 134.0(3) . .
C14 N5 Fe1 110.4(3) . .
C15 N6 N7 120.8(3) . .
C15 N6 Fe1 120.4(3) . .
N7 N6 Fe1 118.5(3) . .
C16 N7 N6 112.1(3) . .
C18 N8 C16 116.7(3) . .
C18 N8 Fe1 131.3(3) . .
C16 N8 Fe1 112.0(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 N6 1.892(3) .
Fe1 N2 1.897(3) .
Fe1 N8 1.985(3) .
Fe1 N4 1.985(3) .
Fe1 N1 2.045(3) .
Fe1 N5 2.056(3) .
Br1 C1 1.890(4) .
Br2 C10 1.885(4) .
B1 F1 1.294(13) .
B1 F3 1.311(9) 8_755
B1 F3 1.311(9) .
B1 F2 1.48(2) .
B2 F5 1.23(2) .
B2 F9 1.296(16) .
B2 F9 1.296(17) 7_565
B2 F7 1.34(3) .
B2 F4 1.348(19) 7_565
B2 F4 1.348(19) .
B2 F6 1.40(2) .
B2 F8 1.43(3) .
F4 F9 1.04(4) .
F5 F7 0.78(6) .
F5 F8 1.31(5) .
F6 F9 1.51(3) .
F6 F9 1.51(3) 7_565
C1 N1 1.339(5) .
C1 C2 1.393(6) .
C2 C3 1.374(7) .
C2 H2A 0.9300 .
C3 C4 1.395(7) .
C3 H3A 0.9300 .
C4 C5 1.396(6) .
C4 H4A 0.9300 .
C5 N1 1.389(5) .
C5 C6 1.447(6) .
C6 N2 1.294(5) .
C6 H6A 0.9300 .
C7 N3 1.347(5) .
C7 N4 1.383(5) .
C7 C8 1.385(5) .
C8 C7 1.385(5) 7_575
C8 H8A 0.9300 .
C9 N4 1.335(4) .
C9 N4 1.335(4) 7_575
C9 H9A 0.9300 .
C10 N5 1.335(5) .
C10 C11 1.392(6) .
C11 C12 1.378(7) .
C11 H11A 0.9300 .
C12 C13 1.394(7) .
C12 H12A 0.9300 .
C13 C14 1.393(6) .
C13 H13A 0.9300 .
C14 N5 1.382(5) .
C14 C15 1.451(6) .
C15 N6 1.294(5) .
C15 H15A 0.9300 .
C16 N7 1.354(5) .
C16 C17 1.380(5) .
C16 N8 1.385(5) .
C17 C16 1.380(5) 8_755
C17 H17A 0.9300 .
C18 N8 1.332(4) 8_755
C18 N8 1.332(4) .
C18 H18A 0.9300 .
N2 N3 1.367(5) .
N3 H3B 0.8600 .
N6 N7 1.369(5) .
O3W O3W 1.22(4) 2_655
