#------------------------------------------------------------------------------
#$Date: 2019-11-08 01:15:30 +0200 (Fri, 08 Nov 2019) $
#$Revision: 224453 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/87/7048743.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_7048743
loop_
_publ_author_name
'Kimura, Shun'
'Uchida, Hikaru'
'Kusamoto, Tetsuro'
'Nishihara, Hiroshi'
_publ_section_title
;
 One-dimensional magnetic chain composed of CuII and
 polychlorinated dipyridylphenylmethyl radical: temperature-dependent
 Jahn-Teller distortion correlated to π-conjugation and magnetic
 properties.
;
_journal_issue                   21
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7090
_journal_page_last               7093
_journal_paper_doi               10.1039/c8dt05104f
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C27 H8 Cl7 Cu F12 N2 O4'
_chemical_formula_sum            'C27 H8 Cl7 Cu F12 N2 O4'
_chemical_formula_weight         964.07
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_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_update_record
;
2019-01-14 deposited with the CCDC.
2019-01-21 downloaded from the CCDC.
;
_cell_angle_alpha                90.0000
_cell_angle_beta                 102.478(7)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   15.3428(18)
_cell_length_b                   11.0604(10)
_cell_length_c                   20.949(3)
_cell_measurement_reflns_used    4457
_cell_measurement_temperature    140
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      3.00
_cell_volume                     3471.0(7)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r3'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r3 (Rigaku, 2009)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r3'
_computing_molecular_graphics    'CrystalStructure 4.3'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2018)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla, et al., 2005)'
_diffrn_ambient_temperature      140
_diffrn_detector_area_resol_mean 7.111
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       ω
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0450
_diffrn_reflns_av_unetI/netI     0.0447
_diffrn_reflns_Laue_measured_fraction_full 0.000
_diffrn_reflns_Laue_measured_fraction_max 0.000
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            13594
_diffrn_reflns_point_group_measured_fraction_full 0.000
_diffrn_reflns_point_group_measured_fraction_max 0.000
_diffrn_reflns_theta_full        27.460
_diffrn_reflns_theta_max         27.460
_diffrn_reflns_theta_min         3.004
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.270
_exptl_absorpt_correction_T_max  0.963
_exptl_absorpt_correction_T_min  0.827
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.845
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chip
_exptl_crystal_F_000             1888.00
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.38
_refine_diff_density_min         -0.43
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.966
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     243
_refine_ls_number_reflns         3948
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0666
_refine_ls_R_factor_gt           0.0487
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.0488P)²+10.1367P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1042
_refine_ls_wR_factor_ref         0.1138
_reflns_number_gt                3172
_reflns_number_total             3948
_reflns_threshold_expression     F²>2.0σ(F²)
_cod_data_source_file            c8dt05104f2.cif
_cod_data_source_block           cubis_140K
_cod_depositor_comments
'Adding full bibliography for 7048738--7048744.cif.'
_cod_database_code               7048743
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
Cu1 Cu 0.7500 0.2500 0.5000 0.02584(15) Uani 1 2 d S
Cl1 Cl 0.62874(6) 0.20088(8) 0.22760(4) 0.0371(2) Uani 1 1 d .
Cl2 Cl 0.47054(6) -0.07238(8) 0.38829(4) 0.0396(2) Uani 1 1 d .
Cl3 Cl 0.5000 -0.54211(11) 0.2500 0.0691(5) Uani 1 2 d S
Cl4 Cl 0.68118(6) -0.12708(8) 0.28207(5) 0.0471(3) Uani 1 1 d .
F1 F 0.97850(17) 0.0952(2) 0.39951(13) 0.0636(7) Uani 1 1 d .
F2 F 0.9566(2) -0.0874(3) 0.42214(17) 0.0930(11) Uani 1 1 d .
F3 F 0.86229(19) 0.0067(3) 0.34709(12) 0.0796(9) Uani 1 1 d .
F4 F 0.65890(18) -0.1380(2) 0.54163(13) 0.0647(7) Uani 1 1 d .
F5 F 0.74146(19) -0.0754(2) 0.63162(11) 0.0622(7) Uani 1 1 d .
F6 F 0.79231(19) -0.2061(2) 0.57272(12) 0.0618(7) Uani 1 1 d .
O1 O 0.84850(19) 0.1718(2) 0.45394(12) 0.0438(6) Uani 1 1 d .
O2 O 0.74146(16) 0.09767(19) 0.54605(10) 0.0325(5) Uani 1 1 d .
N1 N 0.6516(2) 0.1851(2) 0.41757(14) 0.0369(7) Uani 1 1 d .
C1 C 0.5000 -0.0002(4) 0.2500 0.0238(9) Uani 1 2 d S
C2 C 0.6578(3) 0.2156(3) 0.35718(17) 0.0354(8) Uani 1 1 d .
H2 H 0.6976 0.2786 0.3517 0.043 Uiso 1 1 calc R
C3 C 0.6087(2) 0.1591(3) 0.30236(16) 0.0285(7) Uani 1 1 d .
C4 C 0.5492(2) 0.0649(3) 0.30736(15) 0.0256(6) Uani 1 1 d .
C5 C 0.5429(2) 0.0367(3) 0.37174(16) 0.0287(7) Uani 1 1 d .
C6 C 0.5932(2) 0.0980(3) 0.42431(17) 0.0340(7) Uani 1 1 d .
H6 H 0.5864 0.0778 0.4670 0.041 Uiso 1 1 calc R
C7 C 0.5000 -0.3850(4) 0.2500 0.0409(13) Uani 1 2 d S
C8 C 0.5802(3) -0.3251(3) 0.26552(17) 0.0383(8) Uani 1 1 d .
H8 H 0.6349 -0.3684 0.2758 0.046 Uiso 1 1 calc R
C9 C 0.5791(2) -0.2002(3) 0.26573(16) 0.0305(7) Uani 1 1 d .
C10 C 0.5000 -0.1326(4) 0.2500 0.0258(9) Uani 1 2 d S
C11 C 0.9155(3) 0.0176(4) 0.4060(2) 0.0503(10) Uani 1 1 d .
C12 C 0.8615(3) 0.0611(3) 0.45483(17) 0.0375(8) Uani 1 1 d .
C13 C 0.8290(3) -0.0276(3) 0.49168(17) 0.0397(8) Uani 1 1 d .
H13 H 0.8462 -0.1093 0.4875 0.048 Uiso 1 1 calc R
C14 C 0.7737(2) -0.0022(3) 0.53352(15) 0.0324(7) Uani 1 1 d .
C15 C 0.7420(3) -0.1068(3) 0.57026(19) 0.0457(9) Uani 1 1 d .
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 for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
Cl Cl 0.1484 0.1585
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Cu Cu 0.3201 1.2651
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
F F 0.0171 0.0103
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
N N 0.0061 0.0033
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
O O 0.0106 0.0060
;
International Tables for Crystallography
(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
O2 Cu1 O2 180.000(1) 7_656 .
O2 Cu1 O1 89.81(9) 7_656 .
O2 Cu1 O1 90.19(9) . .
O2 Cu1 O1 90.19(9) 7_656 7_656
O2 Cu1 O1 89.81(9) . 7_656
O1 Cu1 O1 180.000(1) . 7_656
O2 Cu1 N1 90.11(10) 7_656 .
O2 Cu1 N1 89.89(10) . .
O1 Cu1 N1 86.85(10) . .
O1 Cu1 N1 93.15(11) 7_656 .
O2 Cu1 N1 89.89(10) 7_656 7_656
O2 Cu1 N1 90.11(10) . 7_656
O1 Cu1 N1 93.15(11) . 7_656
O1 Cu1 N1 86.85(10) 7_656 7_656
N1 Cu1 N1 180.000(1) . 7_656
C12 O1 Cu1 121.2(2) . .
C14 O2 Cu1 125.4(2) . .
C2 N1 C6 117.9(3) . .
C2 N1 Cu1 119.6(2) . .
C6 N1 Cu1 121.5(2) . .
C4 C1 C4 121.0(4) 2_655 .
C4 C1 C10 119.50(18) 2_655 .
C4 C1 C10 119.50(18) . .
N1 C2 C3 122.5(3) . .
N1 C2 H2 118.8 . .
C3 C2 H2 118.8 . .
C2 C3 C4 121.4(3) . .
C2 C3 Cl1 117.6(2) . .
C4 C3 Cl1 120.9(2) . .
C3 C4 C5 114.6(3) . .
C3 C4 C1 122.2(3) . .
C5 C4 C1 123.2(3) . .
C6 C5 C4 120.9(3) . .
C6 C5 Cl2 117.2(2) . .
C4 C5 Cl2 121.9(2) . .
N1 C6 C5 122.7(3) . .
N1 C6 H6 118.7 . .
C5 C6 H6 118.7 . .
C8 C7 C8 122.3(4) . 2_655
C8 C7 Cl3 118.9(2) . .
C8 C7 Cl3 118.9(2) 2_655 .
C7 C8 C9 118.2(3) . .
C7 C8 H8 120.9 . .
C9 C8 H8 120.9 . .
C8 C9 C10 122.9(3) . .
C8 C9 Cl4 117.2(3) . .
C10 C9 Cl4 119.8(2) . .
C9 C10 C9 115.6(4) 2_655 .
C9 C10 C1 122.2(2) 2_655 .
C9 C10 C1 122.2(2) . .
F1 C11 F2 106.1(4) . .
F1 C11 F3 106.2(3) . .
F2 C11 F3 108.6(4) . .
F1 C11 C12 112.3(3) . .
F2 C11 C12 113.7(3) . .
F3 C11 C12 109.7(4) . .
O1 C12 C13 128.6(4) . .
O1 C12 C11 114.2(3) . .
C13 C12 C11 117.1(3) . .
C14 C13 C12 123.3(3) . .
C14 C13 H13 118.4 . .
C12 C13 H13 118.4 . .
O2 C14 C13 129.5(3) . .
O2 C14 C15 112.2(3) . .
C13 C14 C15 118.3(3) . .
F5 C15 F6 107.5(3) . .
F5 C15 F4 107.2(3) . .
F6 C15 F4 107.1(3) . .
F5 C15 C14 111.0(3) . .
F6 C15 C14 113.5(3) . .
F4 C15 C14 110.3(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O2 1.960(2) 7_656
Cu1 O2 1.960(2) .
Cu1 O1 2.143(3) .
Cu1 O1 2.143(3) 7_656
Cu1 N1 2.157(3) .
Cu1 N1 2.157(3) 7_656
Cl1 C3 1.723(3) .
Cl2 C5 1.724(3) .
Cl3 C7 1.738(5) .
Cl4 C9 1.730(3) .
F1 C11 1.321(5) .
F2 C11 1.329(5) .
F3 C11 1.331(5) .
F4 C15 1.332(5) .
F5 C15 1.333(4) .
F6 C15 1.337(4) .
O1 C12 1.240(4) .
O2 C14 1.261(4) .
N1 C2 1.333(4) .
N1 C6 1.343(4) .
C1 C4 1.463(4) 2_655
C1 C4 1.463(4) .
C1 C10 1.465(6) .
C2 C3 1.379(5) .
C2 H2 0.9500 .
C3 C4 1.404(4) .
C4 C5 1.408(4) .
C5 C6 1.379(5) .
C6 H6 0.9500 .
C7 C8 1.373(4) .
C7 C8 1.373(4) 2_655
C8 C9 1.381(4) .
C8 H8 0.9500 .
C9 C10 1.403(4) .
C10 C9 1.403(4) 2_655
C11 C12 1.527(5) .
C12 C13 1.405(5) .
C13 C14 1.375(5) .
C13 H13 0.9500 .
C14 C15 1.526(5) .
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
O2 Cu1 O1 C12 -166.2(3) 7_656 .
O2 Cu1 O1 C12 13.8(3) . .
O1 Cu1 O1 C12 85(100) 7_656 .
N1 Cu1 O1 C12 -76.0(3) . .
N1 Cu1 O1 C12 104.0(3) 7_656 .
O2 Cu1 O2 C14 -134(100) 7_656 .
O1 Cu1 O2 C14 -12.5(3) . .
O1 Cu1 O2 C14 167.5(3) 7_656 .
N1 Cu1 O2 C14 74.4(3) . .
N1 Cu1 O2 C14 -105.6(3) 7_656 .
O2 Cu1 N1 C2 35.0(3) 7_656 .
O2 Cu1 N1 C2 -145.0(3) . .
O1 Cu1 N1 C2 -54.8(3) . .
O1 Cu1 N1 C2 125.2(3) 7_656 .
N1 Cu1 N1 C2 176(100) 7_656 .
O2 Cu1 N1 C6 -156.9(3) 7_656 .
O2 Cu1 N1 C6 23.1(3) . .
O1 Cu1 N1 C6 113.3(3) . .
O1 Cu1 N1 C6 -66.7(3) 7_656 .
N1 Cu1 N1 C6 -16(100) 7_656 .
C6 N1 C2 C3 -1.7(5) . .
Cu1 N1 C2 C3 166.8(3) . .
N1 C2 C3 C4 -0.4(5) . .
N1 C2 C3 Cl1 -175.8(3) . .
C2 C3 C4 C5 1.6(5) . .
Cl1 C3 C4 C5 176.9(2) . .
C2 C3 C4 C1 -176.7(3) . .
Cl1 C3 C4 C1 -1.4(4) . .
C4 C1 C4 C3 -49.4(2) 2_655 .
C10 C1 C4 C3 130.6(2) . .
C4 C1 C4 C5 132.5(3) 2_655 .
C10 C1 C4 C5 -47.5(3) . .
C3 C4 C5 C6 -0.8(4) . .
C1 C4 C5 C6 177.5(3) . .
C3 C4 C5 Cl2 177.6(2) . .
C1 C4 C5 Cl2 -4.1(4) . .
C2 N1 C6 C5 2.6(5) . .
Cu1 N1 C6 C5 -165.8(3) . .
C4 C5 C6 N1 -1.3(5) . .
Cl2 C5 C6 N1 -179.8(3) . .
C8 C7 C8 C9 0.4(2) 2_655 .
Cl3 C7 C8 C9 -179.6(2) . .
C7 C8 C9 C10 -0.9(5) . .
C7 C8 C9 Cl4 -177.3(2) . .
C8 C9 C10 C9 0.4(2) . 2_655
Cl4 C9 C10 C9 176.8(3) . 2_655
C8 C9 C10 C1 -179.6(2) . .
Cl4 C9 C10 C1 -3.2(3) . .
C4 C1 C10 C9 -51.4(2) 2_655 2_655
C4 C1 C10 C9 128.6(2) . 2_655
C4 C1 C10 C9 128.6(2) 2_655 .
C4 C1 C10 C9 -51.4(2) . .
Cu1 O1 C12 C13 -10.9(5) . .
Cu1 O1 C12 C11 165.2(2) . .
F1 C11 C12 O1 36.3(5) . .
F2 C11 C12 O1 156.8(4) . .
F3 C11 C12 O1 -81.5(4) . .
F1 C11 C12 C13 -147.1(4) . .
F2 C11 C12 C13 -26.7(5) . .
F3 C11 C12 C13 95.1(4) . .
O1 C12 C13 C14 1.3(6) . .
C11 C12 C13 C14 -174.7(3) . .
Cu1 O2 C14 C13 7.9(5) . .
Cu1 O2 C14 C15 -170.3(2) . .
C12 C13 C14 O2 1.2(6) . .
C12 C13 C14 C15 179.3(3) . .
O2 C14 C15 F5 -41.4(4) . .
C13 C14 C15 F5 140.2(3) . .
O2 C14 C15 F6 -162.6(3) . .
C13 C14 C15 F6 19.0(5) . .
O2 C14 C15 F4 77.3(4) . .
C13 C14 C15 F4 -101.1(4) . .
