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#$Date: 2017-10-28 05:33:50 +0300 (Sat, 28 Oct 2017) $
#$Revision: 202391 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/45/7044571.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_7044571
loop_
_publ_author_name
'Zhang, Yanpeng'
'Mei, Tao'
'Yang, Dawei'
'Zhang, Yixin'
'Wang, Baomin'
'Qu, Jingping'
_publ_section_title
;
 Synthesis and reactivity of thiolate-bridged multi-iron complexes
 supported by cyclic (alkyl)(amino)carbene
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT03353B
_journal_year                    2017
_chemical_formula_sum            'C44 H72 Br2 Cl4 Fe2 N2 S2'
_chemical_formula_weight         1106.48
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           Orthorhombic'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2017-08-22 deposited with the CCDC.
2017-10-17 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.487(4)
_cell_length_b                   18.279(6)
_cell_length_c                   28.035(10)
_cell_measurement_reflns_used    9911
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      21.3851
_cell_measurement_theta_min      2.3439
_cell_volume                     5374(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      300(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_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  0.1075
_diffrn_reflns_av_sigmaI/netI    0.0429
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            73129
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.34
_exptl_absorpt_coefficient_mu    2.333
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             2288
_refine_diff_density_max         1.259
_refine_diff_density_min         -0.861
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         4726
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.1171
_refine_ls_R_factor_gt           0.0704
_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)+(0.1112P)²+15.0861P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1950
_refine_ls_wR_factor_ref         0.2143
_reflns_number_gt                3058
_reflns_number_total             4726
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7dt03353b2.cif
_cod_data_source_block           1_CCDC1
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               7044571
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, 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 0.07978(9) 0.01148(5) 0.54735(3) 0.0407(3) Uani 1 1 d .
Br1 Br 0.07319(9) -0.09616(4) 0.59630(3) 0.0657(3) Uani 1 1 d .
S1 S -0.14468(17) 0.02324(9) 0.53109(6) 0.0442(4) Uani 1 1 d .
N1 N 0.2205(5) 0.1182(3) 0.61306(18) 0.0395(12) Uani 1 1 d .
C1 C 0.1713(6) 0.1047(3) 0.5712(2) 0.0392(15) Uani 1 1 d .
C6 C 0.2803(8) 0.1939(4) 0.6206(3) 0.056(2) Uani 1 1 d .
C9 C 0.2255(7) 0.0623(3) 0.6501(2) 0.0423(16) Uani 1 1 d .
C2 C 0.1956(8) 0.1726(4) 0.5400(2) 0.0545(19) Uani 1 1 d .
C11 C 0.0057(8) 0.1046(4) 0.6813(3) 0.059(2) Uani 1 1 d .
H11A H 0.0174 0.1426 0.6571 0.071 Uiso 1 1 calc R
C10 C 0.1251(8) 0.0571(4) 0.6824(2) 0.0510(18) Uani 1 1 d .
C18 C 0.4336(7) 0.0120(5) 0.6132(3) 0.065(2) Uani 1 1 d .
H18A H 0.4242 0.0559 0.5934 0.078 Uiso 1 1 calc R
C17 C 0.3263(7) 0.0129(4) 0.6498(3) 0.0544(19) Uani 1 1 d .
C5 C 0.2417(10) 0.2301(4) 0.5743(3) 0.083(3) Uani 1 1 d .
H5A H 0.1745 0.2654 0.5801 0.100 Uiso 1 1 calc R
H5B H 0.3141 0.2558 0.5607 0.100 Uiso 1 1 calc R
C16 C 0.3293(10) -0.0398(4) 0.6857(3) 0.073(3) Uani 1 1 d .
H16A H 0.3981 -0.0718 0.6872 0.088 Uiso 1 1 calc R
C8 C 0.2270(12) 0.2311(5) 0.6639(4) 0.104(4) Uani 1 1 d .
H8A H 0.2548 0.2057 0.6920 0.156 Uiso 1 1 calc R
H8B H 0.1356 0.2306 0.6625 0.156 Uiso 1 1 calc R
H8C H 0.2566 0.2808 0.6650 0.156 Uiso 1 1 calc R
C19 C 0.5676(8) 0.0148(6) 0.6360(4) 0.099(3) Uani 1 1 d .
H19A H 0.5736 0.0568 0.6565 0.148 Uiso 1 1 calc R
H19B H 0.6309 0.0182 0.6114 0.148 Uiso 1 1 calc R
H19C H 0.5815 -0.0288 0.6544 0.148 Uiso 1 1 calc R
C14 C 0.1339(10) 0.0029(5) 0.7177(3) 0.073(2) Uani 1 1 d .
H14A H 0.0708 -0.0003 0.7409 0.087 Uiso 1 1 calc R
C4 C 0.0781(10) 0.1973(5) 0.5140(4) 0.098(4) Uani 1 1 d .
H4A H 0.0507 0.1596 0.4926 0.147 Uiso 1 1 calc R
H4B H 0.0968 0.2409 0.4963 0.147 Uiso 1 1 calc R
H4C H 0.0116 0.2073 0.5367 0.147 Uiso 1 1 calc R
C15 C 0.2351(11) -0.0458(5) 0.7184(3) 0.084(3) Uani 1 1 d .
H15A H 0.2383 -0.0825 0.7414 0.100 Uiso 1 1 calc R
C20 C 0.4229(10) -0.0538(6) 0.5805(4) 0.096(3) Uani 1 1 d .
H20A H 0.4913 -0.0529 0.5577 0.144 Uiso 1 1 calc R
H20B H 0.3428 -0.0522 0.5639 0.144 Uiso 1 1 calc R
H20C H 0.4278 -0.0978 0.5990 0.144 Uiso 1 1 calc R
C7 C 0.4210(10) 0.1903(5) 0.6272(5) 0.108(4) Uani 1 1 d .
H7A H 0.4590 0.1668 0.6000 0.162 Uiso 1 1 calc R
H7B H 0.4401 0.1628 0.6554 0.162 Uiso 1 1 calc R
H7C H 0.4545 0.2389 0.6303 0.162 Uiso 1 1 calc R
C12 C -0.1106(8) 0.0599(6) 0.6682(3) 0.082(3) Uani 1 1 d .
H12A H -0.1844 0.0910 0.6677 0.123 Uiso 1 1 calc R
H12B H -0.1226 0.0218 0.6913 0.123 Uiso 1 1 calc R
H12C H -0.0987 0.0387 0.6372 0.123 Uiso 1 1 calc R
C13 C -0.0185(11) 0.1421(6) 0.7297(3) 0.097(3) Uani 1 1 d .
H13A H 0.0549 0.1705 0.7384 0.145 Uiso 1 1 calc R
H13B H -0.0338 0.1056 0.7536 0.145 Uiso 1 1 calc R
H13C H -0.0915 0.1735 0.7272 0.145 Uiso 1 1 calc R
C3 C 0.3019(12) 0.1514(6) 0.5037(4) 0.109(4) Uani 1 1 d .
H3A H 0.3766 0.1359 0.5207 0.163 Uiso 1 1 calc R
H3B H 0.3223 0.1930 0.4842 0.163 Uiso 1 1 calc R
H3C H 0.2721 0.1122 0.4837 0.163 Uiso 1 1 calc R
Cl2 Cl 0.1400(7) 0.1953(4) 0.2975(2) 0.239(3) Uani 1 1 d .
Cl1 Cl 0.3312(10) 0.2195(5) 0.3705(3) 0.340(6) Uani 1 1 d .
C21 C -0.2184(10) 0.1113(5) 0.5299(3) 0.088(3) Uani 1 1 d .
H21A H -0.2440 0.1247 0.5616 0.132 Uiso 1 1 calc R
H21B H -0.2919 0.1099 0.5095 0.132 Uiso 1 1 calc R
H21C H -0.1589 0.1468 0.5179 0.132 Uiso 1 1 calc R
C22 C 0.2166(19) 0.1688(9) 0.3474(8) 0.197(9) Uani 1 1 d .
H22B H 0.2525 0.1209 0.3412 0.237 Uiso 1 1 calc R
H22A H 0.1524 0.1625 0.3720 0.237 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'
S S 0.1246 0.1234 '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
C1 Fe1 S1 112.63(19) . 5_556
C1 Fe1 Br1 120.26(18) . .
S1 Fe1 Br1 108.48(6) 5_556 .
C1 Fe1 S1 116.24(19) . .
S1 Fe1 S1 97.36(7) 5_556 .
Br1 Fe1 S1 98.82(6) . .
C21 S1 Fe1 110.2(3) . 5_556
C21 S1 Fe1 120.5(4) . .
Fe1 S1 Fe1 82.64(7) 5_556 .
C1 N1 C9 121.4(5) . .
C1 N1 C6 117.1(5) . .
C9 N1 C6 121.3(5) . .
N1 C1 C2 107.0(5) . .
N1 C1 Fe1 129.1(4) . .
C2 C1 Fe1 123.8(4) . .
C7 C6 C8 106.8(8) . .
C7 C6 C5 113.0(8) . .
C8 C6 C5 113.4(8) . .
C7 C6 N1 112.4(7) . .
C8 C6 N1 111.6(6) . .
C5 C6 N1 99.7(5) . .
C10 C9 C17 122.4(6) . .
C10 C9 N1 119.0(6) . .
C17 C9 N1 118.5(6) . .
C4 C2 C5 111.3(7) . .
C4 C2 C1 112.5(6) . .
C5 C2 C1 104.7(5) . .
C4 C2 C3 110.2(8) . .
C5 C2 C3 111.2(8) . .
C1 C2 C3 106.8(6) . .
C12 C11 C10 111.1(7) . .
C12 C11 C13 108.8(7) . .
C10 C11 C13 111.8(7) . .
C9 C10 C14 117.2(7) . .
C9 C10 C11 124.7(6) . .
C14 C10 C11 118.1(7) . .
C20 C18 C17 111.2(7) . .
C20 C18 C19 110.1(8) . .
C17 C18 C19 113.1(8) . .
C16 C17 C9 117.4(8) . .
C16 C17 C18 117.6(8) . .
C9 C17 C18 125.0(7) . .
C2 C5 C6 109.2(6) . .
C15 C16 C17 122.0(9) . .
C10 C14 C15 121.0(8) . .
C16 C15 C14 119.8(8) . .
Cl2 C22 Cl1 120.8(10) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 C1 2.067(6) .
Fe1 S1 2.388(2) 5_556
Fe1 Br1 2.4000(13) .
Fe1 S1 2.407(2) .
S1 C21 1.787(9) .
S1 Fe1 2.388(2) 5_556
N1 C1 1.305(8) .
N1 C9 1.459(8) .
N1 C6 1.534(8) .
C1 C2 1.541(9) .
C6 C7 1.488(12) .
C6 C8 1.500(12) .
C6 C5 1.512(11) .
C9 C10 1.392(10) .
C9 C17 1.390(10) .
C2 C4 1.501(11) .
C2 C5 1.505(10) .
C2 C3 1.558(13) .
C11 C12 1.514(12) .
C11 C10 1.524(11) .
C11 C13 1.540(11) .
C10 C14 1.402(10) .
C18 C20 1.517(12) .
C18 C17 1.522(11) .
C18 C19 1.545(12) .
C17 C16 1.394(11) .
C16 C15 1.353(13) .
C14 C15 1.387(13) .
Cl2 C22 1.685(19) .
Cl1 C22 1.65(2) .
