#------------------------------------------------------------------------------
#$Date: 2019-11-23 11:47:41 +0200 (Sat, 23 Nov 2019) $
#$Revision: 233156 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/85/4348599.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_4348599
loop_
_publ_author_name
'Chow, Chun Y.'
'Guillot, Régis'
'Rivière, Eric'
'Kampf, Jeff W.'
'Mallah, Talal'
'Pecoraro, Vincent L.'
_publ_section_title
;
 Synthesis and Magnetic Characterization of Fe(III)-Based 9-Metallacrown-3
 Complexes Which Exhibit Magnetorefrigerant Properties.
;
_journal_issue                   20
_journal_name_full               'Inorganic chemistry'
_journal_page_first              10238
_journal_page_last               10247
_journal_paper_doi               10.1021/acs.inorgchem.6b01404
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C45 H39 Fe4 N3 O18 + (solvent)'
_chemical_formula_sum            'C45 H39 Fe4 N3 O18'
_chemical_formula_weight         1133.19
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   18.44496(20)
_cell_length_b                   18.44496(20)
_cell_length_c                   31.7624(3)
_cell_measurement_reflns_used    26850
_cell_measurement_temperature    85(2)
_cell_measurement_theta_max      73.5230
_cell_measurement_theta_min      3.0690
_cell_volume                     9358.35(17)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r16 (Rigaku, 2014)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_diffrn_ambient_temperature      85(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku Saturn 944+ CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0762
_diffrn_reflns_av_unetI/netI     0.0216
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            82010
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.847
_diffrn_reflns_theta_min         3.097
_diffrn_source                   'micro-focus rotating anode'
_exptl_absorpt_coefficient_mu    7.826
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45926
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015) 
Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.206
_exptl_crystal_description       cube
_exptl_crystal_F_000             3468
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.512
_refine_diff_density_min         -0.508
_refine_diff_density_rms         0.078
_refine_ls_extinction_coef       0.000143(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     213
_refine_ls_number_reflns         4218
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0431
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0844P)²+9.8939P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1243
_refine_ls_wR_factor_ref         0.1274
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3943
_reflns_number_total             4218
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic6b01404_si_002.cif
_cod_data_source_block           1-OBz
_cod_original_cell_volume        9358.3(2)
_cod_database_code               4348599
_shelx_space_group_comment
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;
_shelx_estimated_absorpt_t_min   0.573
_shelx_estimated_absorpt_t_max   0.573
_shelxl_version_number           2014/6
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
N1 N 1.03644(11) 0.12225(11) 0.16827(6) 0.0330(4) Uani 1 1 d . . .
Fe1 Fe 1.0000 0.0000 0.10059(2) 0.02825(16) Uani 1 3 d S T P
Fe2 Fe 0.91102(2) 0.08597(2) 0.16242(2) 0.03131(14) Uani 1 1 d . U .
O1 O 0.86666(11) 0.00740(10) 0.21049(5) 0.0396(4) Uani 1 1 d . . .
O2 O 0.90296(9) -0.02121(9) 0.13810(5) 0.0315(3) Uani 1 1 d . . .
O3 O 0.93741(10) 0.17844(10) 0.19966(5) 0.0382(4) Uani 1 1 d . . .
O100 O 0.92969(11) 0.13974(11) 0.10616(5) 0.0412(4) Uani 1 1 d . . .
O101 O 0.97037(10) 0.07010(10) 0.06383(5) 0.0352(3) Uani 1 1 d . . .
C1 C 0.85859(14) -0.06520(14) 0.20449(7) 0.0348(5) Uani 1 1 d . . .
C2 C 1.04803(16) 0.17514(16) 0.23876(8) 0.0415(5) Uani 1 1 d . . .
C3 C 1.0912(2) 0.1921(3) 0.27695(10) 0.0653(9) Uani 1 1 d . . .
H3 H 1.1341 0.1784 0.2800 0.078 Uiso 1 1 calc R U .
C4 C 1.0730(3) 0.2280(3) 0.31009(11) 0.0871(13) Uani 1 1 d . . .
H4 H 1.1028 0.2387 0.3359 0.105 Uiso 1 1 calc R U .
C5 C 1.0105(3) 0.2486(3) 0.30546(10) 0.0764(11) Uani 1 1 d . . .
H5 H 0.9981 0.2744 0.3281 0.092 Uiso 1 1 calc R U .
C6 C 0.9669(2) 0.2321(2) 0.26879(9) 0.0556(7) Uani 1 1 d . . .
H6 H 0.9244 0.2467 0.2662 0.067 Uiso 1 1 calc R U .
C7 C 0.98311(16) 0.19414(15) 0.23479(7) 0.0400(5) Uani 1 1 d . . .
C100 C 0.94538(14) 0.12169(14) 0.07021(7) 0.0346(4) Uani 1 1 d . . .
C101 C 0.93224(15) 0.16297(15) 0.03310(7) 0.0378(5) Uani 1 1 d . . .
C102 C 0.9035(2) 0.21903(19) 0.03831(9) 0.0527(7) Uani 1 1 d . . .
H102 H 0.8951 0.2339 0.0658 0.063 Uiso 1 1 calc R U .
C103 C 0.8870(3) 0.2533(2) 0.00306(10) 0.0688(9) Uani 1 1 d . . .
H103 H 0.8669 0.2914 0.0065 0.083 Uiso 1 1 calc R U .
C104 C 0.8996(2) 0.2325(2) -0.03674(10) 0.0652(8) Uani 1 1 d . . .
H104 H 0.8881 0.2561 -0.0606 0.078 Uiso 1 1 calc R U .
C105 C 0.92905(19) 0.17716(19) -0.04220(8) 0.0510(6) Uani 1 1 d . . .
H105 H 0.9383 0.1634 -0.0697 0.061 Uiso 1 1 calc R U .
C106 C 0.94492(15) 0.14217(15) -0.00749(8) 0.0401(5) Uani 1 1 d . . .
H106 H 0.9645 0.1038 -0.0112 0.048 Uiso 1 1 calc R U .
O200 O 0.78809(10) 0.05579(11) 0.15135(6) 0.0455(4) Uani 1 1 d . U .
H200 H 0.7797 0.0958 0.1366 0.055 Uiso 1 1 calc R U .
C200 C 0.7163(2) -0.0183(3) 0.1637(2) 0.116(2) Uani 1 1 d . U .
H20A H 0.6663 -0.0168 0.1546 0.175 Uiso 1 1 calc R U .
H20B H 0.7167 -0.0663 0.1507 0.175 Uiso 1 1 calc R U .
H20C H 0.7158 -0.0236 0.1944 0.175 Uiso 1 1 calc R U .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 '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 N1 O2 111.84(17) 3_765 3_765
C1 N1 Fe2 123.28(15) 3_765 .
O2 N1 Fe2 120.50(12) 3_765 .
O101 Fe1 O101 89.65(7) . 2_645
O101 Fe1 O101 89.65(7) . 3_765
O101 Fe1 O101 89.65(7) 2_645 3_765
O101 Fe1 O2 93.62(6) . 3_765
O101 Fe1 O2 176.04(6) 2_645 3_765
O101 Fe1 O2 88.14(6) 3_765 3_765
O101 Fe1 O2 176.04(6) . 2_645
O101 Fe1 O2 88.14(6) 2_645 2_645
O101 Fe1 O2 93.62(6) 3_765 2_645
O2 Fe1 O2 88.71(6) 3_765 2_645
O101 Fe1 O2 88.14(6) . .
O101 Fe1 O2 93.62(6) 2_645 .
O101 Fe1 O2 176.04(6) 3_765 .
O2 Fe1 O2 88.71(6) 3_765 .
O2 Fe1 O2 88.71(6) 2_645 .
O3 Fe2 O1 90.20(7) . .
O3 Fe2 O100 101.89(7) . .
O1 Fe2 O100 164.54(7) . .
O3 Fe2 O2 161.02(7) . .
O1 Fe2 O2 77.36(6) . .
O100 Fe2 O2 93.05(6) . .
O3 Fe2 N1 84.94(7) . .
O1 Fe2 N1 98.83(7) . .
O100 Fe2 N1 91.87(7) . .
O2 Fe2 N1 82.91(6) . .
O3 Fe2 O200 95.74(7) . .
O1 Fe2 O200 86.45(7) . .
O100 Fe2 O200 82.83(8) . .
O2 Fe2 O200 97.71(7) . .
N1 Fe2 O200 174.68(8) . .
C1 O1 Fe2 116.02(14) . .
N1 O2 Fe1 116.70(11) 2_645 .
N1 O2 Fe2 112.99(11) 2_645 .
Fe1 O2 Fe2 113.85(7) . .
C7 O3 Fe2 123.75(14) . .
C100 O100 Fe2 133.36(15) . .
C100 O101 Fe1 135.23(15) . .
O1 C1 N1 121.6(2) . 2_645
O1 C1 C2 118.8(2) . 2_645
N1 C1 C2 119.6(2) 2_645 2_645
C3 C2 C7 118.7(2) . .
C3 C2 C1 117.1(2) . 3_765
C7 C2 C1 124.2(2) . 3_765
C4 C3 C2 121.7(3) . .
C4 C3 H3 119.1 . .
C2 C3 H3 119.1 . .
C3 C4 C5 119.1(3) . .
C3 C4 H4 120.4 . .
C5 C4 H4 120.4 . .
C6 C5 C4 120.5(3) . .
C6 C5 H5 119.8 . .
C4 C5 H5 119.8 . .
C5 C6 C7 121.5(3) . .
C5 C6 H6 119.2 . .
C7 C6 H6 119.2 . .
O3 C7 C6 118.8(2) . .
O3 C7 C2 122.7(2) . .
C6 C7 C2 118.4(2) . .
O100 C100 O101 124.1(2) . .
O100 C100 C101 117.7(2) . .
O101 C100 C101 118.2(2) . .
C102 C101 C106 119.6(2) . .
C102 C101 C100 120.5(2) . .
C106 C101 C100 119.9(2) . .
C101 C102 C103 119.6(3) . .
C101 C102 H102 120.2 . .
C103 C102 H102 120.2 . .
C104 C103 C102 120.5(3) . .
C104 C103 H103 119.8 . .
C102 C103 H103 119.8 . .
C103 C104 C105 120.3(3) . .
C103 C104 H104 119.9 . .
C105 C104 H104 119.9 . .
C106 C105 C104 119.8(3) . .
C106 C105 H105 120.1 . .
C104 C105 H105 120.1 . .
C105 C106 C101 120.3(2) . .
C105 C106 H106 119.8 . .
C101 C106 H106 119.8 . .
C200 O200 Fe2 125.9(2) . .
C200 O200 H200 117.1 . .
Fe2 O200 H200 117.1 . .
O200 C200 H20A 109.5 . .
O200 C200 H20B 109.5 . .
H20A C200 H20B 109.5 . .
O200 C200 H20C 109.5 . .
H20A C200 H20C 109.5 . .
H20B C200 H20C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
N1 C1 1.314(3) 3_765
N1 O2 1.414(2) 3_765
N1 Fe2 2.0703(18) .
Fe1 O101 2.0101(15) .
Fe1 O101 2.0102(15) 2_645
Fe1 O101 2.0102(15) 3_765
Fe1 O2 2.0189(15) 3_765
Fe1 O2 2.0189(15) 2_645
Fe1 O2 2.0190(15) .
Fe2 O3 1.9273(16) .
Fe2 O1 1.9786(17) .
Fe2 O100 1.9884(17) .
Fe2 O2 2.0574(15) .
Fe2 O200 2.0767(17) .
O1 C1 1.286(3) .
O2 N1 1.414(2) 2_645
O3 C7 1.340(3) .
O100 C100 1.263(3) .
O101 C100 1.264(3) .
C1 N1 1.314(3) 2_645
C1 C2 1.471(3) 2_645
C2 C3 1.398(4) .
C2 C7 1.411(3) .
C2 C1 1.472(3) 3_765
C3 C4 1.371(4) .
C3 H3 0.9500 .
C4 C5 1.391(5) .
C4 H4 0.9500 .
C5 C6 1.360(4) .
C5 H5 0.9500 .
C6 C7 1.399(3) .
C6 H6 0.9500 .
C100 C101 1.487(3) .
C101 C102 1.388(4) .
C101 C106 1.398(3) .
C102 C103 1.392(4) .
C102 H102 0.9500 .
C103 C104 1.374(5) .
C103 H103 0.9500 .
C104 C105 1.385(4) .
C104 H104 0.9500 .
C105 C106 1.381(3) .
C105 H105 0.9500 .
C106 H106 0.9500 .
O200 C200 1.402(4) .
O200 H200 0.9500 .
C200 H20A 0.9800 .
C200 H20B 0.9800 .
C200 H20C 0.9800 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O200 H200 O3 0.95 1.75 2.611(2) 148.4 13_655
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
Fe2 O1 C1 N1 -0.9(3) . 2_645
Fe2 O1 C1 C2 -179.18(17) . 2_645
C7 C2 C3 C4 -1.3(6) . .
C1 C2 C3 C4 176.3(4) 3_765 .
C2 C3 C4 C5 -0.4(7) . .
C3 C4 C5 C6 1.1(7) . .
C4 C5 C6 C7 0.1(6) . .
Fe2 O3 C7 C6 -149.3(2) . .
Fe2 O3 C7 C2 31.7(3) . .
C5 C6 C7 O3 179.1(3) . .
C5 C6 C7 C2 -1.8(5) . .
C3 C2 C7 O3 -178.6(3) . .
C1 C2 C7 O3 4.0(4) 3_765 .
C3 C2 C7 C6 2.4(4) . .
C1 C2 C7 C6 -175.0(3) 3_765 .
Fe2 O100 C100 O101 -15.7(3) . .
Fe2 O100 C100 C101 163.31(16) . .
Fe1 O101 C100 O100 -2.5(3) . .
Fe1 O101 C100 C101 178.48(15) . .
O100 C100 C101 C102 -0.2(3) . .
O101 C100 C101 C102 178.9(2) . .
O100 C100 C101 C106 -177.0(2) . .
O101 C100 C101 C106 2.1(3) . .
C106 C101 C102 C103 0.5(5) . .
C100 C101 C102 C103 -176.3(3) . .
C101 C102 C103 C104 -0.5(6) . .
C102 C103 C104 C105 -0.1(6) . .
C103 C104 C105 C106 0.7(6) . .
C104 C105 C106 C101 -0.7(4) . .
C102 C101 C106 C105 0.1(4) . .
C100 C101 C106 C105 176.9(2) . .
