#------------------------------------------------------------------------------
#$Date: 2019-11-08 01:15:30 +0200 (Fri, 08 Nov 2019) $
#$Revision: 224453 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/87/7048744.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_7048744
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                 102.657(6)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   15.3379(18)
_cell_length_b                   11.0460(10)
_cell_length_c                   20.900(3)
_cell_measurement_reflns_used    4546
_cell_measurement_temperature    120
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      3.00
_cell_volume                     3454.9(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      120
_diffrn_detector_area_resol_mean 7.111
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0462
_diffrn_reflns_av_unetI/netI     0.0454
_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       23
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            13574
_diffrn_reflns_point_group_measured_fraction_full 0.000
_diffrn_reflns_point_group_measured_fraction_max 0.000
_diffrn_reflns_theta_full        27.480
_diffrn_reflns_theta_max         27.480
_diffrn_reflns_theta_min         3.231
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.276
_exptl_absorpt_correction_T_max  0.962
_exptl_absorpt_correction_T_min  0.840
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.853
_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         0.36
_refine_diff_density_min         -0.36
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.949
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     243
_refine_ls_number_reflns         3949
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0633
_refine_ls_R_factor_gt           0.0459
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.0520P)²+9.8753P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1016
_refine_ls_wR_factor_ref         0.1123
_reflns_number_gt                3177
_reflns_number_total             3949
_reflns_threshold_expression     F²>2.0σ(F²)
_cod_data_source_file            c8dt05104f2.cif
_cod_data_source_block           cubis_120K
_cod_depositor_comments
'Adding full bibliography for 7048738--7048744.cif.'
_cod_database_code               7048744
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 0.2500 0.2500 0.5000 0.02296(14) Uani 1 2 d S
Cl1 Cl 0.37128(6) 0.20066(7) 0.77267(4) 0.0332(2) Uani 1 1 d .
Cl2 Cl 0.52919(6) -0.07216(7) 0.61125(4) 0.0348(2) Uani 1 1 d .
Cl3 Cl 0.5000 -0.54310(11) 0.7500 0.0603(5) Uani 1 2 d S
Cl4 Cl 0.68116(5) -0.12732(8) 0.78192(5) 0.0416(2) Uani 1 1 d .
F1 F 0.02059(16) 0.0944(2) 0.60108(11) 0.0548(6) Uani 1 1 d .
F2 F 0.0425(2) -0.0888(2) 0.57756(16) 0.0805(9) Uani 1 1 d .
F3 F 0.13735(17) 0.0041(3) 0.65312(11) 0.0676(8) Uani 1 1 d .
F4 F 0.34099(16) -0.1382(2) 0.45869(12) 0.0562(6) Uani 1 1 d .
F5 F 0.25846(17) -0.0762(2) 0.36848(11) 0.0534(6) Uani 1 1 d .
F6 F 0.20754(17) -0.20697(19) 0.42737(11) 0.0545(6) Uani 1 1 d .
O1 O 0.15004(18) 0.1712(2) 0.54614(11) 0.0394(6) Uani 1 1 d .
O2 O 0.25787(15) 0.09783(18) 0.45389(10) 0.0290(5) Uani 1 1 d .
N1 N 0.3477(2) 0.1848(2) 0.58199(13) 0.0332(6) Uani 1 1 d .
C1 C 0.5000 -0.0008(4) 0.7500 0.0229(8) Uani 1 2 d S
C2 C 0.3413(2) 0.2159(3) 0.64274(16) 0.0312(7) Uani 1 1 d .
H2 H 0.3016 0.2790 0.6483 0.037 Uiso 1 1 calc R
C3 C 0.3910(2) 0.1587(3) 0.69740(15) 0.0256(6) Uani 1 1 d .
C4 C 0.45067(19) 0.0648(2) 0.69264(15) 0.0228(6) Uani 1 1 d .
C5 C 0.4563(2) 0.0364(3) 0.62795(16) 0.0265(6) Uani 1 1 d .
C6 C 0.4056(2) 0.0979(3) 0.57495(16) 0.0304(7) Uani 1 1 d .
H6 H 0.4121 0.0777 0.5321 0.036 Uiso 1 1 calc R
C7 C 0.5000 -0.3861(4) 0.7500 0.0372(12) Uani 1 2 d S
C8 C 0.5803(2) -0.3260(3) 0.76527(16) 0.0343(8) Uani 1 1 d .
H8 H 0.6351 -0.3695 0.7752 0.041 Uiso 1 1 calc R
C9 C 0.5795(2) -0.2003(3) 0.76588(15) 0.0271(7) Uani 1 1 d .
C10 C 0.5000 -0.1330(4) 0.7500 0.0237(9) Uani 1 2 d S
C11 C 0.0832(3) 0.0164(3) 0.59421(19) 0.0435(9) Uani 1 1 d .
C12 C 0.1373(2) 0.0606(3) 0.54535(16) 0.0332(7) Uani 1 1 d .
C13 C 0.1701(2) -0.0282(3) 0.50829(16) 0.0340(7) Uani 1 1 d .
H13 H 0.1531 -0.1101 0.5124 0.041 Uiso 1 1 calc R
C14 C 0.2256(2) -0.0024(3) 0.46632(15) 0.0293(7) Uani 1 1 d .
C15 C 0.2574(3) -0.1073(3) 0.42975(17) 0.0394(8) 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)
;
O O 0.0106 0.0060
;
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)
;
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 180.0 . 7_556
O2 Cu1 N1 90.16(9) . 7_556
O2 Cu1 N1 89.84(9) 7_556 7_556
O2 Cu1 N1 89.84(9) . .
O2 Cu1 N1 90.16(9) 7_556 .
N1 Cu1 N1 180.00(11) 7_556 .
O2 Cu1 O1 90.01(9) . .
O2 Cu1 O1 89.99(9) 7_556 .
N1 Cu1 O1 92.97(10) 7_556 .
N1 Cu1 O1 87.03(10) . .
O2 Cu1 O1 89.99(9) . 7_556
O2 Cu1 O1 90.01(9) 7_556 7_556
N1 Cu1 O1 87.03(10) 7_556 7_556
N1 Cu1 O1 92.97(10) . 7_556
O1 Cu1 O1 180.0 . 7_556
C12 O1 Cu1 121.1(2) . .
C14 O2 Cu1 125.7(2) . .
C6 N1 C2 118.5(3) . .
C6 N1 Cu1 121.3(2) . .
C2 N1 Cu1 119.3(2) . .
C10 C1 C4 119.71(17) . .
C10 C1 C4 119.71(17) . 2_656
C4 C1 C4 120.6(3) . 2_656
N1 C2 C3 121.7(3) . .
N1 C2 H2 119.2 . .
C3 C2 H2 119.2 . .
C2 C3 C4 122.1(3) . .
C2 C3 Cl1 117.1(2) . .
C4 C3 Cl1 120.7(2) . .
C3 C4 C5 114.3(3) . .
C3 C4 C1 122.5(3) . .
C5 C4 C1 123.2(2) . .
C6 C5 C4 121.1(3) . .
C6 C5 Cl2 117.0(2) . .
C4 C5 Cl2 121.8(2) . .
N1 C6 C5 122.3(3) . .
N1 C6 H6 118.8 . .
C5 C6 H6 118.8 . .
C8 C7 C8 122.3(4) 2_656 .
C8 C7 Cl3 118.9(2) 2_656 .
C8 C7 Cl3 118.9(2) . .
C7 C8 C9 118.4(3) . .
C7 C8 H8 120.8 . .
C9 C8 H8 120.8 . .
C8 C9 C10 122.4(3) . .
C8 C9 Cl4 117.4(2) . .
C10 C9 Cl4 120.1(2) . .
C9 C10 C9 116.1(4) 2_656 .
C9 C10 C1 121.93(19) 2_656 .
C9 C10 C1 121.93(19) . .
F1 C11 F3 106.7(3) . .
F1 C11 F2 106.7(3) . .
F3 C11 F2 108.3(3) . .
F1 C11 C12 112.2(3) . .
F3 C11 C12 109.3(3) . .
F2 C11 C12 113.4(3) . .
O1 C12 C13 128.4(3) . .
O1 C12 C11 114.4(3) . .
C13 C12 C11 117.1(3) . .
C14 C13 C12 123.3(3) . .
C14 C13 H13 118.3 . .
C12 C13 H13 118.3 . .
O2 C14 C13 129.5(3) . .
O2 C14 C15 112.3(3) . .
C13 C14 C15 118.1(3) . .
F5 C15 F6 107.8(3) . .
F5 C15 F4 106.8(3) . .
F6 C15 F4 106.9(3) . .
F5 C15 C14 111.1(3) . .
F6 C15 C14 113.7(3) . .
F4 C15 C14 110.4(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O2 1.954(2) .
Cu1 O2 1.954(2) 7_556
Cu1 N1 2.139(3) 7_556
Cu1 N1 2.139(3) .
Cu1 O1 2.165(3) .
Cu1 O1 2.165(3) 7_556
Cl1 C3 1.729(3) .
Cl2 C5 1.726(3) .
Cl3 C7 1.734(4) .
Cl4 C9 1.721(3) .
F1 C11 1.322(4) .
F2 C11 1.329(5) .
F3 C11 1.332(4) .
F4 C15 1.337(4) .
F5 C15 1.329(4) .
F6 C15 1.335(4) .
O1 C12 1.237(4) .
O2 C14 1.263(4) .
N1 C6 1.336(4) .
N1 C2 1.340(4) .
C1 C10 1.460(5) .
C1 C4 1.462(4) .
C1 C4 1.462(4) 2_656
C2 C3 1.380(4) .
C2 H2 0.9500 .
C3 C4 1.401(4) .
C4 C5 1.409(4) .
C5 C6 1.385(4) .
C6 H6 0.9500 .
C7 C8 1.373(4) 2_656
C7 C8 1.373(4) .
C8 C9 1.389(4) .
C8 H8 0.9500 .
C9 C10 1.404(4) .
C10 C9 1.404(4) 2_656
C11 C12 1.530(5) .
C12 C13 1.409(5) .
C13 C14 1.379(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 14.4(2) . .
O2 Cu1 O1 C12 -165.6(2) 7_556 .
N1 Cu1 O1 C12 104.5(3) 7_556 .
N1 Cu1 O1 C12 -75.5(3) . .
O1 Cu1 O1 C12 -131(100) 7_556 .
O2 Cu1 O2 C14 153(53) 7_556 .
N1 Cu1 O2 C14 -105.8(2) 7_556 .
N1 Cu1 O2 C14 74.2(2) . .
O1 Cu1 O2 C14 -12.8(2) . .
O1 Cu1 O2 C14 167.2(2) 7_556 .
O2 Cu1 N1 C6 23.4(3) . .
O2 Cu1 N1 C6 -156.6(3) 7_556 .
N1 Cu1 N1 C6 -111(14) 7_556 .
O1 Cu1 N1 C6 113.4(3) . .
O1 Cu1 N1 C6 -66.6(3) 7_556 .
O2 Cu1 N1 C2 -145.0(3) . .
O2 Cu1 N1 C2 35.0(3) 7_556 .
N1 Cu1 N1 C2 81(14) 7_556 .
O1 Cu1 N1 C2 -55.0(2) . .
O1 Cu1 N1 C2 125.0(2) 7_556 .
C6 N1 C2 C3 -1.6(5) . .
Cu1 N1 C2 C3 167.1(2) . .
N1 C2 C3 C4 -0.2(5) . .
N1 C2 C3 Cl1 -175.9(3) . .
C2 C3 C4 C5 1.2(4) . .
Cl1 C3 C4 C5 176.7(2) . .
C2 C3 C4 C1 -176.6(3) . .
Cl1 C3 C4 C1 -1.0(4) . .
C10 C1 C4 C3 130.4(2) . .
C4 C1 C4 C3 -49.6(2) 2_656 .
C10 C1 C4 C5 -47.2(3) . .
C4 C1 C4 C5 132.8(3) 2_656 .
C3 C4 C5 C6 -0.4(4) . .
C1 C4 C5 C6 177.4(3) . .
C3 C4 C5 Cl2 177.2(2) . .
C1 C4 C5 Cl2 -5.0(4) . .
C2 N1 C6 C5 2.5(5) . .
Cu1 N1 C6 C5 -166.0(2) . .
C4 C5 C6 N1 -1.5(5) . .
Cl2 C5 C6 N1 -179.2(3) . .
C8 C7 C8 C9 0.7(2) 2_656 .
Cl3 C7 C8 C9 -179.3(2) . .
C7 C8 C9 C10 -1.5(4) . .
C7 C8 C9 Cl4 -177.4(2) . .
C8 C9 C10 C9 0.8(2) . 2_656
Cl4 C9 C10 C9 176.6(3) . 2_656
C8 C9 C10 C1 -179.2(2) . .
Cl4 C9 C10 C1 -3.4(3) . .
C4 C1 C10 C9 -51.34(19) . 2_656
C4 C1 C10 C9 128.66(19) 2_656 2_656
C4 C1 C10 C9 128.66(19) . .
C4 C1 C10 C9 -51.34(19) 2_656 .
Cu1 O1 C12 C13 -11.3(5) . .
Cu1 O1 C12 C11 164.9(2) . .
F1 C11 C12 O1 35.6(5) . .
F3 C11 C12 O1 -82.5(4) . .
F2 C11 C12 O1 156.6(3) . .
F1 C11 C12 C13 -147.7(3) . .
F3 C11 C12 C13 94.2(4) . .
F2 C11 C12 C13 -26.7(5) . .
O1 C12 C13 C14 1.4(6) . .
C11 C12 C13 C14 -174.8(3) . .
Cu1 O2 C14 C13 8.0(5) . .
Cu1 O2 C14 C15 -169.8(2) . .
C12 C13 C14 O2 1.5(6) . .
C12 C13 C14 C15 179.2(3) . .
O2 C14 C15 F5 -41.2(4) . .
C13 C14 C15 F5 140.7(3) . .
O2 C14 C15 F6 -163.0(3) . .
C13 C14 C15 F6 18.9(5) . .
O2 C14 C15 F4 77.0(4) . .
C13 C14 C15 F4 -101.1(4) . .
