#------------------------------------------------------------------------------
#$Date: 2019-11-08 01:15:30 +0200 (Fri, 08 Nov 2019) $
#$Revision: 224453 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/87/7048740.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_7048740
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                 102.584(6)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   15.3404(18)
_cell_length_b                   11.0521(10)
_cell_length_c                   20.930(3)
_cell_measurement_reflns_used    4544
_cell_measurement_temperature    130
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      3.00
_cell_volume                     3463.3(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      130
_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  0.0448
_diffrn_reflns_av_unetI/netI     0.0444
_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            13575
_diffrn_reflns_point_group_measured_fraction_full 0.000
_diffrn_reflns_point_group_measured_fraction_max 0.000
_diffrn_reflns_theta_full        27.490
_diffrn_reflns_theta_max         27.490
_diffrn_reflns_theta_min         3.003
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.273
_exptl_absorpt_correction_T_max  0.963
_exptl_absorpt_correction_T_min  0.835
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.849
_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   0.965
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     243
_refine_ls_number_reflns         3956
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0647
_refine_ls_R_factor_gt           0.0473
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.0512P)²+9.3724P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1029
_refine_ls_wR_factor_ref         0.1129
_reflns_number_gt                3190
_reflns_number_total             3956
_reflns_threshold_expression     F²>2.0σ(F²)
_cod_data_source_file            c8dt05104f2.cif
_cod_data_source_block           cubis_130K
_cod_depositor_comments
'Adding full bibliography for 7048738--7048744.cif.'
_cod_database_code               7048740
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 0.02424(14) Uani 1 2 d S
Cl1 Cl 0.87125(6) 0.20069(7) 0.77255(4) 0.0349(2) Uani 1 1 d .
Cl2 Cl 1.02936(6) -0.07231(8) 0.61151(4) 0.0371(2) Uani 1 1 d .
Cl3 Cl 1.0000 -0.54269(11) 0.7500 0.0650(5) Uani 1 2 d S
Cl4 Cl 1.18122(5) -0.12713(8) 0.78203(5) 0.0443(2) Uani 1 1 d .
F1 F 0.52099(16) 0.0946(2) 0.60073(12) 0.0586(6) Uani 1 1 d .
F2 F 0.5430(2) -0.0881(2) 0.57776(16) 0.0850(10) Uani 1 1 d .
F3 F 0.63748(18) 0.0052(3) 0.65297(11) 0.0730(8) Uani 1 1 d .
F4 F 0.84086(17) -0.1378(2) 0.45847(13) 0.0595(7) Uani 1 1 d .
F5 F 0.75849(18) -0.0754(2) 0.36831(11) 0.0578(6) Uani 1 1 d .
F6 F 0.70738(18) -0.2065(2) 0.42721(12) 0.0579(7) Uani 1 1 d .
O1 O 0.65108(18) 0.1715(2) 0.54614(11) 0.0410(6) Uani 1 1 d .
O2 O 0.75814(16) 0.09791(19) 0.45393(10) 0.0314(5) Uani 1 1 d .
N1 N 0.8486(2) 0.1851(2) 0.58213(13) 0.0348(7) Uani 1 1 d .
C1 C 1.0000 -0.0001(4) 0.7500 0.0235(8) Uani 1 2 d S
C2 C 0.8418(2) 0.2156(3) 0.64294(16) 0.0339(8) Uani 1 1 d .
H2 H 0.8014 0.2779 0.6485 0.041 Uiso 1 1 calc R
C3 C 0.8917(2) 0.1592(3) 0.69751(15) 0.0272(7) Uani 1 1 d .
C4 C 0.9508(2) 0.0648(2) 0.69273(15) 0.0235(6) Uani 1 1 d .
C5 C 0.9567(2) 0.0363(3) 0.62828(16) 0.0280(7) Uani 1 1 d .
C6 C 0.9062(2) 0.0981(3) 0.57545(17) 0.0321(7) Uani 1 1 d .
H6 H 0.9129 0.0777 0.5327 0.039 Uiso 1 1 calc R
C7 C 1.0000 -0.3858(4) 0.7500 0.0392(12) Uani 1 2 d S
C8 C 1.0800(3) -0.3254(3) 0.76553(16) 0.0370(8) Uani 1 1 d .
H8 H 1.1348 -0.3686 0.7759 0.044 Uiso 1 1 calc R
C9 C 1.0791(2) -0.2003(3) 0.76578(15) 0.0275(6) Uani 1 1 d .
C10 C 1.0000 -0.1328(4) 0.7500 0.0247(9) Uani 1 2 d S
C11 C 0.5835(3) 0.0168(4) 0.5941(2) 0.0490(10) Uani 1 1 d .
C12 C 0.6380(2) 0.0606(3) 0.54546(16) 0.0352(8) Uani 1 1 d .
C13 C 0.6708(2) -0.0283(3) 0.50816(16) 0.0361(8) Uani 1 1 d .
H13 H 0.6542 -0.1102 0.5123 0.043 Uiso 1 1 calc R
C14 C 0.7256(2) -0.0017(3) 0.46622(15) 0.0314(7) Uani 1 1 d .
C15 C 0.7580(3) -0.1075(3) 0.42979(19) 0.0437(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 180.00(11) . 7_656
O2 Cu1 O1 89.89(9) . 7_656
O2 Cu1 O1 90.11(9) 7_656 7_656
O2 Cu1 O1 90.11(9) . .
O2 Cu1 O1 89.89(9) 7_656 .
O1 Cu1 O1 180.00(9) 7_656 .
O2 Cu1 N1 90.12(9) . 7_656
O2 Cu1 N1 89.88(9) 7_656 7_656
O1 Cu1 N1 87.07(10) 7_656 7_656
O1 Cu1 N1 92.93(10) . 7_656
O2 Cu1 N1 89.88(9) . .
O2 Cu1 N1 90.12(9) 7_656 .
O1 Cu1 N1 92.93(10) 7_656 .
O1 Cu1 N1 87.07(10) . .
N1 Cu1 N1 180.00(11) 7_656 .
C12 O1 Cu1 121.4(2) . .
C14 O2 Cu1 125.5(2) . .
C6 N1 C2 118.1(3) . .
C6 N1 Cu1 121.6(2) . .
C2 N1 Cu1 119.1(2) . .
C4 C1 C4 121.1(4) . 2_756
C4 C1 C10 119.45(18) . .
C4 C1 C10 119.45(18) 2_756 .
N1 C2 C3 121.8(3) . .
N1 C2 H2 119.1 . .
C3 C2 H2 119.1 . .
C2 C3 C4 122.0(3) . .
C2 C3 Cl1 117.0(2) . .
C4 C3 Cl1 120.7(2) . .
C3 C4 C5 114.4(3) . .
C3 C4 C1 122.3(3) . .
C5 C4 C1 123.3(3) . .
C6 C5 C4 121.0(3) . .
C6 C5 Cl2 117.0(2) . .
C4 C5 Cl2 122.0(2) . .
N1 C6 C5 122.7(3) . .
N1 C6 H6 118.7 . .
C5 C6 H6 118.7 . .
C8 C7 C8 121.8(4) . 2_756
C8 C7 Cl3 119.1(2) . .
C8 C7 Cl3 119.1(2) 2_756 .
C7 C8 C9 118.6(3) . .
C7 C8 H8 120.7 . .
C9 C8 H8 120.7 . .
C8 C9 C10 122.7(3) . .
C8 C9 Cl4 117.3(3) . .
C10 C9 Cl4 119.9(2) . .
C9 C10 C9 115.7(4) 2_756 .
C9 C10 C1 122.14(19) 2_756 .
C9 C10 C1 122.14(19) . .
F1 C11 F2 106.6(4) . .
F1 C11 F3 106.5(3) . .
F2 C11 F3 108.4(4) . .
F1 C11 C12 112.3(3) . .
F2 C11 C12 113.5(3) . .
F3 C11 C12 109.1(3) . .
O1 C12 C13 128.0(3) . .
O1 C12 C11 114.6(3) . .
C13 C12 C11 117.4(3) . .
C14 C13 C12 123.1(3) . .
C14 C13 H13 118.5 . .
C12 C13 H13 118.5 . .
O2 C14 C13 130.1(3) . .
O2 C14 C15 112.3(3) . .
C13 C14 C15 117.6(3) . .
F4 C15 F6 107.6(3) . .
F4 C15 F5 107.3(3) . .
F6 C15 F5 107.7(3) . .
F4 C15 C14 110.5(3) . .
F6 C15 C14 113.3(3) . .
F5 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 1.955(2) .
Cu1 O2 1.955(2) 7_656
Cu1 O1 2.151(3) 7_656
Cu1 O1 2.151(3) .
Cu1 N1 2.151(3) 7_656
Cu1 N1 2.151(3) .
Cl1 C3 1.729(3) .
Cl2 C5 1.726(3) .
Cl3 C7 1.734(4) .
Cl4 C9 1.730(3) .
F1 C11 1.318(4) .
F2 C11 1.325(5) .
F3 C11 1.333(5) .
F4 C15 1.325(5) .
F5 C15 1.336(4) .
F6 C15 1.336(4) .
O1 C12 1.241(4) .
O2 C14 1.258(4) .
N1 C6 1.334(4) .
N1 C2 1.343(4) .
C1 C4 1.458(4) .
C1 C4 1.458(4) 2_756
C1 C10 1.467(5) .
C2 C3 1.378(4) .
C2 H2 0.9500 .
C3 C4 1.400(4) .
C4 C5 1.407(4) .
C5 C6 1.384(5) .
C6 H6 0.9500 .
C7 C8 1.372(4) .
C7 C8 1.372(4) 2_756
C8 C9 1.383(4) .
C8 H8 0.9500 .
C9 C10 1.400(4) .
C10 C9 1.400(4) 2_756
C11 C12 1.529(5) .
C12 C13 1.414(5) .
C13 C14 1.373(5) .
C13 H13 0.9500 .
C14 C15 1.537(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 14.1(3) . .
O2 Cu1 O1 C12 -165.9(3) 7_656 .
O1 Cu1 O1 C12 -144(100) 7_656 .
N1 Cu1 O1 C12 104.2(3) 7_656 .
N1 Cu1 O1 C12 -75.8(3) . .
O2 Cu1 O2 C14 64(100) 7_656 .
O1 Cu1 O2 C14 167.8(3) 7_656 .
O1 Cu1 O2 C14 -12.2(3) . .
N1 Cu1 O2 C14 -105.1(3) 7_656 .
N1 Cu1 O2 C14 74.9(3) . .
O2 Cu1 N1 C6 22.8(3) . .
O2 Cu1 N1 C6 -157.2(3) 7_656 .
O1 Cu1 N1 C6 -67.1(3) 7_656 .
O1 Cu1 N1 C6 112.9(3) . .
N1 Cu1 N1 C6 176(100) 7_656 .
O2 Cu1 N1 C2 -144.5(3) . .
O2 Cu1 N1 C2 35.5(3) 7_656 .
O1 Cu1 N1 C2 125.6(3) 7_656 .
O1 Cu1 N1 C2 -54.4(3) . .
N1 Cu1 N1 C2 8(100) 7_656 .
C6 N1 C2 C3 -0.5(5) . .
Cu1 N1 C2 C3 167.3(3) . .
N1 C2 C3 C4 -1.6(5) . .
N1 C2 C3 Cl1 -176.1(3) . .
C2 C3 C4 C5 2.1(4) . .
Cl1 C3 C4 C5 176.3(2) . .
C2 C3 C4 C1 -176.3(3) . .
Cl1 C3 C4 C1 -2.1(4) . .
C4 C1 C4 C3 -49.1(2) 2_756 .
C10 C1 C4 C3 130.9(2) . .
C4 C1 C4 C5 132.6(3) 2_756 .
C10 C1 C4 C5 -47.4(3) . .
C3 C4 C5 C6 -0.7(4) . .
C1 C4 C5 C6 177.8(3) . .
C3 C4 C5 Cl2 177.0(2) . .
C1 C4 C5 Cl2 -4.6(4) . .
C2 N1 C6 C5 2.0(5) . .
Cu1 N1 C6 C5 -165.5(2) . .
C4 C5 C6 N1 -1.4(5) . .
Cl2 C5 C6 N1 -179.1(3) . .
C8 C7 C8 C9 0.4(2) 2_756 .
Cl3 C7 C8 C9 -179.6(2) . .
C7 C8 C9 C10 -0.9(4) . .
C7 C8 C9 Cl4 -177.2(2) . .
C8 C9 C10 C9 0.4(2) . 2_756
Cl4 C9 C10 C9 176.7(3) . 2_756
C8 C9 C10 C1 -179.6(2) . .
Cl4 C9 C10 C1 -3.3(3) . .
C4 C1 C10 C9 -51.37(19) . 2_756
C4 C1 C10 C9 128.63(19) 2_756 2_756
C4 C1 C10 C9 128.63(19) . .
C4 C1 C10 C9 -51.37(19) 2_756 .
Cu1 O1 C12 C13 -11.1(5) . .
Cu1 O1 C12 C11 165.4(2) . .
F1 C11 C12 O1 35.8(5) . .
F2 C11 C12 O1 156.8(3) . .
F3 C11 C12 O1 -82.1(4) . .
F1 C11 C12 C13 -147.4(3) . .
F2 C11 C12 C13 -26.3(5) . .
F3 C11 C12 C13 94.8(4) . .
O1 C12 C13 C14 1.0(6) . .
C11 C12 C13 C14 -175.4(3) . .
Cu1 O2 C14 C13 7.1(5) . .
Cu1 O2 C14 C15 -169.7(2) . .
C12 C13 C14 O2 2.1(6) . .
C12 C13 C14 C15 178.7(3) . .
O2 C14 C15 F4 76.5(4) . .
C13 C14 C15 F4 -100.8(4) . .
O2 C14 C15 F6 -162.7(3) . .
C13 C14 C15 F6 20.1(5) . .
O2 C14 C15 F5 -41.9(4) . .
C13 C14 C15 F5 140.8(3) . .
