#------------------------------------------------------------------------------
#$Date: 2019-11-08 01:15:30 +0200 (Fri, 08 Nov 2019) $
#$Revision: 224453 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/87/7048738.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_7048738
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                 102.899(6)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   15.3530(17)
_cell_length_b                   11.0280(10)
_cell_length_c                   20.812(3)
_cell_measurement_reflns_used    4663
_cell_measurement_temperature    93
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      3.00
_cell_volume                     3434.8(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      93
_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  0.0472
_diffrn_reflns_av_unetI/netI     0.0456
_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       -26
_diffrn_reflns_number            13470
_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         3.001
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.283
_exptl_absorpt_correction_T_max  0.774
_exptl_absorpt_correction_T_min  0.671
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.864
_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         0.40
_refine_diff_density_min         -0.37
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.944
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     243
_refine_ls_number_reflns         3927
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0595
_refine_ls_R_factor_gt           0.0452
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.0439P)²+13.4451P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0959
_refine_ls_wR_factor_ref         0.1047
_reflns_number_gt                3269
_reflns_number_total             3927
_reflns_threshold_expression     F²>2.0σ(F²)
_cod_data_source_file            c8dt05104f2.cif
_cod_data_source_block           cubis_93K
_cod_depositor_comments
'Adding full bibliography for 7048738--7048744.cif.'
_cod_database_code               7048738
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 0.01906(13) Uani 1 2 d S
Cl1 Cl 0.12879(5) 0.20040(7) 0.22693(4) 0.02585(18) Uani 1 1 d .
Cl2 Cl -0.02861(5) -0.07138(7) 0.38950(4) 0.02757(18) Uani 1 1 d .
Cl3 Cl 0.0000 -0.54426(10) 0.2500 0.0490(4) Uani 1 2 d S
Cl4 Cl 0.18145(5) -0.12741(7) 0.28137(4) 0.0332(2) Uani 1 1 d .
F1 F 0.48023(14) 0.0920(2) 0.39776(11) 0.0434(5) Uani 1 1 d .
F2 F 0.45918(19) -0.0914(2) 0.42311(14) 0.0633(8) Uani 1 1 d .
F3 F 0.36323(15) -0.0002(2) 0.34643(11) 0.0542(7) Uani 1 1 d .
F4 F 0.15915(15) -0.13850(18) 0.54025(11) 0.0447(5) Uani 1 1 d .
F5 F 0.24146(16) -0.07684(19) 0.63188(10) 0.0431(5) Uani 1 1 d .
F6 F 0.29262(15) -0.20843(18) 0.57279(11) 0.0435(5) Uani 1 1 d .
O1 O 0.35286(16) 0.17064(19) 0.45382(11) 0.0313(5) Uani 1 1 d .
O2 O 0.24356(15) 0.09751(18) 0.54643(10) 0.0242(5) Uani 1 1 d .
N1 N 0.15448(18) 0.1842(2) 0.41864(12) 0.0251(6) Uani 1 1 d .
C1 C 0.0000 -0.0004(3) 0.2500 0.0170(8) Uani 1 2 d S
C2 C 0.1607(2) 0.2149(3) 0.35761(15) 0.0232(6) Uani 1 1 d .
H2 H 0.2014 0.2769 0.3520 0.028 Uiso 1 1 calc R
C3 C 0.1097(2) 0.1590(2) 0.30258(14) 0.0202(6) Uani 1 1 d .
C4 C 0.04986(19) 0.0646(2) 0.30755(14) 0.0179(6) Uani 1 1 d .
C5 C 0.04444(19) 0.0367(2) 0.37257(15) 0.0196(6) Uani 1 1 d .
C6 C 0.0958(2) 0.0979(3) 0.42592(15) 0.0230(6) Uani 1 1 d .
H6 H 0.0893 0.0781 0.4690 0.028 Uiso 1 1 calc R
C7 C 0.0000 -0.3875(4) 0.2500 0.0303(10) Uani 1 2 d S
C8 C 0.0801(2) -0.3265(3) 0.26521(15) 0.0283(7) Uani 1 1 d .
H8 H 0.1349 -0.3697 0.2751 0.034 Uiso 1 1 calc R
C9 C 0.0794(2) -0.2009(3) 0.26586(15) 0.0216(6) Uani 1 1 d .
C10 C 0.0000 -0.1341(3) 0.2500 0.0180(8) Uani 1 2 d S
C11 C 0.4181(2) 0.0139(3) 0.40559(17) 0.0350(8) Uani 1 1 d .
C12 C 0.3642(2) 0.0596(3) 0.45448(15) 0.0263(7) Uani 1 1 d .
C13 C 0.3309(2) -0.0298(3) 0.49176(15) 0.0280(7) Uani 1 1 d .
H13 H 0.3473 -0.1121 0.4876 0.034 Uiso 1 1 calc R
C14 C 0.2757(2) -0.0026(3) 0.53371(14) 0.0245(6) Uani 1 1 d .
C15 C 0.2430(2) -0.1080(3) 0.57014(17) 0.0328(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
Cu Cu 0.3201 1.2651
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
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)
;
O O 0.0106 0.0060
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 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)
;
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)
;
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 180.00(10) . 7_556
O2 Cu1 N1 90.12(9) . 7_556
O2 Cu1 N1 89.88(9) 7_556 7_556
O2 Cu1 N1 89.88(9) . .
O2 Cu1 N1 90.12(9) 7_556 .
N1 Cu1 N1 180.0 7_556 .
O2 Cu1 O1 90.33(9) . 7_556
O2 Cu1 O1 89.67(9) 7_556 7_556
N1 Cu1 O1 87.18(9) 7_556 7_556
N1 Cu1 O1 92.82(9) . 7_556
O2 Cu1 O1 89.67(9) . .
O2 Cu1 O1 90.33(9) 7_556 .
N1 Cu1 O1 92.82(9) 7_556 .
N1 Cu1 O1 87.18(9) . .
O1 Cu1 O1 180.00(9) 7_556 .
C12 O1 Cu1 120.1(2) . .
C14 O2 Cu1 125.8(2) . .
C2 N1 C6 118.6(3) . .
C2 N1 Cu1 119.4(2) . .
C6 N1 Cu1 121.2(2) . .
C4 C1 C4 121.1(3) . 2
C4 C1 C10 119.47(17) . .
C4 C1 C10 119.47(17) 2 .
N1 C2 C3 121.8(3) . .
N1 C2 H2 119.1 . .
C3 C2 H2 119.1 . .
C2 C3 C4 121.9(3) . .
C2 C3 Cl1 117.3(2) . .
C4 C3 Cl1 120.6(2) . .
C3 C4 C5 114.3(3) . .
C3 C4 C1 122.4(2) . .
C5 C4 C1 123.3(2) . .
C6 C5 C4 121.2(3) . .
C6 C5 Cl2 116.9(2) . .
C4 C5 Cl2 121.8(2) . .
N1 C6 C5 122.1(3) . .
N1 C6 H6 118.9 . .
C5 C6 H6 118.9 . .
C8 C7 C8 121.4(4) . 2
C8 C7 Cl3 119.3(2) . .
C8 C7 Cl3 119.3(2) 2 .
C7 C8 C9 118.9(3) . .
C7 C8 H8 120.5 . .
C9 C8 H8 120.5 . .
C8 C9 C10 122.1(3) . .
C8 C9 Cl4 117.6(2) . .
C10 C9 Cl4 120.1(2) . .
C9 C10 C9 116.4(4) 2 .
C9 C10 C1 121.79(18) 2 .
C9 C10 C1 121.79(18) . .
F1 C11 F2 106.9(3) . .
F1 C11 F3 106.6(3) . .
F2 C11 F3 108.2(3) . .
F1 C11 C12 112.3(3) . .
F2 C11 C12 113.4(3) . .
F3 C11 C12 109.1(3) . .
O1 C12 C13 128.8(3) . .
O1 C12 C11 114.4(3) . .
C13 C12 C11 116.7(3) . .
C14 C13 C12 122.8(3) . .
C14 C13 H13 118.6 . .
C12 C13 H13 118.6 . .
O2 C14 C13 130.4(3) . .
O2 C14 C15 112.0(3) . .
C13 C14 C15 117.6(3) . .
F5 C15 F6 107.8(3) . .
F5 C15 F4 106.8(3) . .
F6 C15 F4 106.9(3) . .
F5 C15 C14 111.0(3) . .
F6 C15 C14 113.7(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 1.953(2) .
Cu1 O2 1.953(2) 7_556
Cu1 N1 2.106(3) 7_556
Cu1 N1 2.106(3) .
Cu1 O1 2.205(2) 7_556
Cu1 O1 2.205(2) .
Cl1 C3 1.726(3) .
Cl2 C5 1.726(3) .
Cl3 C7 1.729(4) .
Cl4 C9 1.729(3) .
F1 C11 1.322(4) .
F2 C11 1.333(4) .
F3 C11 1.337(4) .
F4 C15 1.342(4) .
F5 C15 1.335(4) .
F6 C15 1.338(4) .
O1 C12 1.237(4) .
O2 C14 1.261(4) .
N1 C2 1.339(4) .
N1 C6 1.342(4) .
C1 C4 1.458(3) .
C1 C4 1.458(3) 2
C1 C10 1.474(5) .
C2 C3 1.380(4) .
C2 H2 0.9500 .
C3 C4 1.407(4) .
C4 C5 1.408(4) .
C5 C6 1.385(4) .
C6 H6 0.9500 .
C7 C8 1.375(4) .
C7 C8 1.375(4) 2
C8 C9 1.384(4) .
C8 H8 0.9500 .
C9 C10 1.400(3) .
C10 C9 1.400(3) 2
C11 C12 1.532(5) .
C12 C13 1.419(4) .
C13 C14 1.379(5) .
C13 H13 0.9500 .
C14 C15 1.532(4) .
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 15.8(2) . .
O2 Cu1 O1 C12 -164.2(2) 7_556 .
N1 Cu1 O1 C12 105.9(2) 7_556 .
N1 Cu1 O1 C12 -74.1(2) . .
O1 Cu1 O1 C12 -98(55) 7_556 .
O2 Cu1 O2 C14 75(100) 7_556 .
N1 Cu1 O2 C14 -106.8(2) 7_556 .
N1 Cu1 O2 C14 73.2(2) . .
O1 Cu1 O2 C14 166.0(2) 7_556 .
O1 Cu1 O2 C14 -14.0(2) . .
O2 Cu1 N1 C2 -144.7(2) . .
O2 Cu1 N1 C2 35.3(2) 7_556 .
N1 Cu1 N1 C2 -10(100) 7_556 .
O1 Cu1 N1 C2 125.0(2) 7_556 .
O1 Cu1 N1 C2 -55.0(2) . .
O2 Cu1 N1 C6 25.1(2) . .
O2 Cu1 N1 C6 -154.9(2) 7_556 .
N1 Cu1 N1 C6 160(100) 7_556 .
O1 Cu1 N1 C6 -65.3(2) 7_556 .
O1 Cu1 N1 C6 114.7(2) . .
C6 N1 C2 C3 -1.1(5) . .
Cu1 N1 C2 C3 169.0(2) . .
N1 C2 C3 C4 -1.6(5) . .
N1 C2 C3 Cl1 -176.2(2) . .
C2 C3 C4 C5 2.5(4) . .
Cl1 C3 C4 C5 176.9(2) . .
C2 C3 C4 C1 -175.9(3) . .
Cl1 C3 C4 C1 -1.5(4) . .
C4 C1 C4 C3 -49.6(2) 2 .
C10 C1 C4 C3 130.4(2) . .
C4 C1 C4 C5 132.2(3) 2 .
C10 C1 C4 C5 -47.8(3) . .
C3 C4 C5 C6 -0.9(4) . .
C1 C4 C5 C6 177.4(3) . .
C3 C4 C5 Cl2 177.0(2) . .
C1 C4 C5 Cl2 -4.7(4) . .
C2 N1 C6 C5 2.6(5) . .
Cu1 N1 C6 C5 -167.2(2) . .
C4 C5 C6 N1 -1.6(5) . .
Cl2 C5 C6 N1 -179.6(2) . .
C8 C7 C8 C9 0.8(2) 2 .
Cl3 C7 C8 C9 -179.2(2) . .
C7 C8 C9 C10 -1.5(4) . .
C7 C8 C9 Cl4 -177.00(19) . .
C8 C9 C10 C9 0.8(2) . 2
Cl4 C9 C10 C9 176.1(3) . 2
C8 C9 C10 C1 -179.2(2) . .
Cl4 C9 C10 C1 -3.9(3) . .
C4 C1 C10 C9 128.79(19) . 2
C4 C1 C10 C9 -51.21(19) 2 2
C4 C1 C10 C9 -51.21(19) . .
C4 C1 C10 C9 128.79(19) 2 .
Cu1 O1 C12 C13 -12.6(4) . .
Cu1 O1 C12 C11 164.1(2) . .
F1 C11 C12 O1 33.9(4) . .
F2 C11 C12 O1 155.2(3) . .
F3 C11 C12 O1 -84.1(4) . .
F1 C11 C12 C13 -148.9(3) . .
F2 C11 C12 C13 -27.6(4) . .
F3 C11 C12 C13 93.1(4) . .
O1 C12 C13 C14 1.9(5) . .
C11 C12 C13 C14 -174.8(3) . .
Cu1 O2 C14 C13 8.8(5) . .
Cu1 O2 C14 C15 -168.7(2) . .
C12 C13 C14 O2 1.6(5) . .
C12 C13 C14 C15 178.9(3) . .
O2 C14 C15 F5 -41.0(4) . .
C13 C14 C15 F5 141.2(3) . .
O2 C14 C15 F6 -162.8(3) . .
C13 C14 C15 F6 19.4(4) . .
O2 C14 C15 F4 77.2(3) . .
C13 C14 C15 F4 -100.6(3) . .
