#------------------------------------------------------------------------------
#$Date: 2016-03-23 20:35:46 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179414 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/11/4331190.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_4331190
loop_
_publ_author_name
'Eugenio Coronado'
'Mónica Giménez-Marqués'
'Carlos J. Gómez-García'
'Guillermo Mínguez Espallargas'
_publ_section_title
;
 Dynamic Magnetic Materials Based on the Cationic Coordination Polymer
 [Cu(btix)2]n2n+ [btix = 1,4-Bis(triazol-1-ylmethyl)benzene]: Tuning the
 Structural and Magnetic Properties through Anion Exchange
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12938
_journal_page_last               12947
_journal_paper_doi               10.1021/ic302066e
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C24 H24 B2 Cu F8 N12'
_chemical_formula_weight         717.71
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_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_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 123.97(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.820(9)
_cell_length_b                   9.5063(15)
_cell_length_c                   15.544(6)
_cell_measurement_reflns_used    428
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      24.9915
_cell_measurement_theta_min      2.3759
_cell_volume                     2919(3)
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_collection       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1448
_diffrn_reflns_av_sigmaI/netI    0.2228
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            6214
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.38
_exptl_absorpt_coefficient_mu    0.840
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83163
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.633
_exptl_crystal_description       block
_exptl_crystal_F_000             1452
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.591
_refine_diff_density_min         -0.503
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.973
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     212
_refine_ls_number_reflns         2576
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.973
_refine_ls_R_factor_all          0.1946
_refine_ls_R_factor_gt           0.0763
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0246P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1130
_refine_ls_wR_factor_ref         0.1510
_reflns_number_gt                1179
_reflns_number_total             2576
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302066e_si_001.cif
_cod_data_source_block           1
_cod_database_code               4331190
#BEGIN Tags that were not found in dictionaries:
_cell_oxdiff_measurement_reflns_used 428
#END Tags that were not found in dictionaries
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.7500 1.2500 0.5000 0.0254(4) Uani 1 2 d S . .
N1 N 0.5950(3) 1.2205(5) 0.1896(4) 0.0209(15) Uani 1 1 d . . .
N2 N 0.5565(3) 1.2363(6) 0.2283(4) 0.0295(16) Uani 1 1 d . . .
C3 C 0.6025(4) 1.2358(7) 0.3292(5) 0.0257(19) Uani 1 1 d . . .
H3 H 0.5911 1.2448 0.3785 0.031 Uiso 1 1 calc R . .
N4 N 0.6672(3) 1.2214(5) 0.3572(4) 0.0227(16) Uani 1 1 d . . .
C5 C 0.6601(4) 1.2122(6) 0.2663(5) 0.0229(19) Uani 1 1 d . . .
H5 H 0.6963 1.2014 0.2575 0.027 Uiso 1 1 calc R . .
C6 C 0.5637(4) 1.2277(7) 0.0783(5) 0.027(2) Uani 1 1 d . . .
H6A H 0.5291 1.1528 0.0433 0.041 Uiso 1 1 calc R . .
H6B H 0.5984 1.2124 0.0630 0.041 Uiso 1 1 calc R . .
C11 C 0.5311(4) 1.3686(7) 0.0377(5) 0.0220(19) Uani 1 1 d . . .
C12 C 0.5670(4) 1.4919(8) 0.0813(5) 0.031(2) Uani 1 1 d . . .
H12 H 0.6132 1.4876 0.1376 0.037 Uiso 1 1 calc R . .
C13 C 0.5362(4) 1.6216(7) 0.0434(6) 0.028(2) Uani 1 1 d . . .
H13 H 0.5617 1.7052 0.0737 0.034 Uiso 1 1 calc R . .
N21 N 0.8221(3) 0.8429(6) 0.5613(5) 0.0250(16) Uani 1 1 d . . .
N22 N 0.8190(3) 0.8590(6) 0.4730(4) 0.0267(17) Uani 1 1 d . . .
C23 C 0.7940(4) 0.9856(7) 0.4430(5) 0.030(2) Uani 1 1 d . . .
H23 H 0.7855 1.0267 0.3810 0.037 Uiso 1 1 calc R . .
N24 N 0.7814(3) 1.0524(6) 0.5056(4) 0.0210(15) Uani 1 1 d . . .
C25 C 0.7996(4) 0.9581(7) 0.5802(6) 0.0236(19) Uani 1 1 d . . .
H25 H 0.7968 0.9716 0.6382 0.028 Uiso 1 1 calc R . .
C26 C 0.8532(4) 0.7211(7) 0.6269(6) 0.034(2) Uani 1 1 d . A .
H26A H 0.8376 0.6355 0.5831 0.051 Uiso 1 1 calc R . .
H26B H 0.8382 0.7140 0.6746 0.051 Uiso 1 1 calc R . .
C31 C 0.9295(4) 0.7261(7) 0.6899(6) 0.030(2) Uani 1 1 d . . .
B1 B 0.8159(5) 1.3742(9) 0.3519(7) 0.027(2) Uani 1 1 d . . .
F1 F 0.8178(3) 1.3310(5) 0.4380(4) 0.0532(15) Uani 1 1 d . . .
F2 F 0.8052(2) 1.2523(5) 0.2941(3) 0.0533(14) Uani 1 1 d . . .
F3 F 0.8753(3) 1.4311(4) 0.3771(4) 0.0629(17) Uani 1 1 d . . .
F4 F 0.7626(2) 1.4652(4) 0.2941(3) 0.0466(14) Uani 1 1 d . . .
C32A C 0.9664(9) 0.6173(14) 0.6770(11) 0.028(4) Uiso 0.50 1 d P A -1
H32A H 0.9430 0.5436 0.6284 0.033 Uiso 0.50 1 calc PR A -1
C33A C 0.9642(10) 0.8361(19) 0.7414(15) 0.034(5) Uiso 0.50 1 d P A -1
H33A H 0.9401 0.9178 0.7383 0.041 Uiso 0.50 1 calc PR A -1
C32B C 1.0366(9) 0.6217(16) 0.7366(13) 0.036(4) Uiso 0.50 1 d P . -1
H32B H 1.0615 0.5529 0.7268 0.043 Uiso 0.50 1 calc PR . -1
C33B C 1.0353(11) 0.8417(19) 0.8018(14) 0.035(5) Uiso 0.50 1 d P . -1
H33B H 1.0581 0.9262 0.8362 0.042 Uiso 0.50 1 calc PR . -1
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 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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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
N4 Cu1 N4 180.000(1) 7_676 .
N4 Cu1 N24 91.9(2) 7_676 7_676
N4 Cu1 N24 88.1(2) . 7_676
N4 Cu1 N24 88.1(2) 7_676 .
N4 Cu1 N24 91.9(2) . .
N24 Cu1 N24 180.000(2) 7_676 .
C5 N1 N2 110.3(6) . .
C5 N1 C6 129.6(7) . .
N2 N1 C6 119.8(6) . .
C3 N2 N1 102.1(6) . .
N2 C3 N4 115.0(7) . .
N2 C3 H3 122.5 . .
N4 C3 H3 122.5 . .
C5 N4 C3 102.7(6) . .
C5 N4 Cu1 130.5(5) . .
C3 N4 Cu1 125.6(5) . .
N4 C5 N1 109.9(7) . .
N4 C5 H5 125.0 . .
N1 C5 H5 125.0 . .
N1 C6 C11 110.1(5) . .
N1 C6 H6A 109.6 . .
C11 C6 H6A 109.6 . .
N1 C6 H6B 109.6 . .
C11 C6 H6B 109.6 . .
H6A C6 H6B 108.1 . .
C13 C11 C12 118.3(7) 5_685 .
C13 C11 C6 120.5(6) 5_685 .
C12 C11 C6 121.2(7) . .
C11 C12 C13 120.6(7) . .
C11 C12 H12 119.7 . .
C13 C12 H12 119.7 . .
C11 C13 C12 121.1(7) 5_685 .
C11 C13 H13 119.5 5_685 .
C12 C13 H13 119.5 . .
C25 N21 N22 109.6(6) . .
C25 N21 C26 128.2(7) . .
N22 N21 C26 121.9(7) . .
C23 N22 N21 103.0(6) . .
N22 C23 N24 115.0(6) . .
N22 C23 H23 122.5 . .
N24 C23 H23 122.5 . .
C23 N24 C25 102.7(6) . .
C23 N24 Cu1 130.3(5) . .
C25 N24 Cu1 126.9(5) . .
N21 C25 N24 109.8(6) . .
N21 C25 H25 125.1 . .
N24 C25 H25 125.1 . .
N21 C26 C31 112.9(6) . .
N21 C26 H26A 109.0 . .
C31 C26 H26A 109.0 . .
N21 C26 H26B 109.0 . .
C31 C26 H26B 109.0 . .
H26A C26 H26B 107.8 . .
C33A C31 C33B 29.8(9) . 2_756
C33A C31 C32B 101.1(12) . 2_756
C33B C31 C32B 117.6(13) 2_756 2_756
C33A C31 C32A 115.9(13) . .
C33B C31 C32A 101.7(12) 2_756 .
C32B C31 C32A 58.7(8) 2_756 .
C33A C31 C26 123.2(11) . .
C33B C31 C26 123.3(10) 2_756 .
C32B C31 C26 116.7(9) 2_756 .
C32A C31 C26 119.6(9) . .
F3 B1 F4 111.8(7) . .
F3 B1 F1 112.2(8) . .
F4 B1 F1 109.9(8) . .
F3 B1 F2 107.6(7) . .
F4 B1 F2 109.3(7) . .
F1 B1 F2 105.8(6) . .
C32B C32A C31 119.1(13) . .
C32B C32A H32A 120.4 . .
C31 C32A H32A 120.4 . .
C31 C33A C33B 123.9(19) . .
C31 C33A H33A 118.1 . .
C33B C33A H33A 118.1 . .
C31 C32B C32A 120.2(15) 2_756 .
C31 C32B H32B 119.9 2_756 .
C32A C32B H32B 119.9 . .
C31 C33B C33A 119.2(18) 2_756 .
C31 C33B H33B 120.4 2_756 .
C33A C33B H33B 120.4 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N4 2.000(6) 7_676
Cu1 N4 2.000(6) .
Cu1 N24 2.006(5) 7_676
Cu1 N24 2.006(5) .
N1 C5 1.329(8) .
N1 N2 1.357(8) .
N1 C6 1.453(8) .
N2 C3 1.319(8) .
C3 N4 1.354(9) .
C3 H3 0.9500 .
N4 C5 1.329(8) .
C5 H5 0.9500 .
C6 C11 1.499(9) .
C6 H6A 0.9900 .
C6 H6B 0.9900 .
C11 C13 1.381(10) 5_685
C11 C12 1.385(9) .
C12 C13 1.387(9) .
C12 H12 0.9500 .
C13 C11 1.381(10) 5_685
C13 H13 0.9500 .
N21 C25 1.323(8) .
N21 N22 1.340(8) .
N21 C26 1.445(8) .
N22 C23 1.307(8) .
C23 N24 1.329(8) .
C23 H23 0.9500 .
N24 C25 1.332(8) .
C25 H25 0.9500 .
C26 C31 1.508(10) .
C26 H26A 0.9900 .
C26 H26B 0.9900 .
C31 C33A 1.295(19) .
C31 C33B 1.34(2) 2_756
C31 C32B 1.382(16) 2_756
C31 C32A 1.443(17) .
B1 F3 1.353(10) .
B1 F4 1.375(10) .
B1 F1 1.376(10) .
B1 F2 1.401(10) .
C32A C32B 1.39(2) .
C32A H32A 0.9500 .
C33A C33B 1.405(17) .
C33A H33A 0.9500 .
C32B C31 1.382(16) 2_756
C32B H32B 0.9500 .
C33B C31 1.344(19) 2_756
C33B H33B 0.9500 .
