#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/01/93/2019394.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_2019394
loop_
_publ_author_name
'Degtyarenko, Anna S.'
'Domasevitch, Konstantin V.'
_publ_section_title
;
Anion···\p interactions in copper(I) chloride and
bromide coordination polymers bearing 1,4-bis(pyridazin-4-yl)benzene
ligands
;
_journal_coeditor_code SF3217
_journal_issue 2
_journal_name_full 'Acta Crystallographica Section C'
_journal_page_first 173
_journal_page_last 177
_journal_paper_doi 10.1107/S2053229613034840
_journal_volume 70
_journal_year 2014
_chemical_formula_iupac '[Cu2 Cl2 (C14 H10 N4)]'
_chemical_formula_moiety 'C14 H10 Cl2 Cu2 N4'
_chemical_formula_sum 'C14 H10 Cl2 Cu2 N4'
_chemical_formula_weight 432.24
_chemical_name_systematic
;
poly[di-\m-chlorido-\m~4~-[1,4-bis(pyridazin-4-yl)benzene-
-1:2:3:4\k^4^N^1^:N^2^:N^1'^:N^2'^]dicopper(I)]
;
_space_group_IT_number 14
_space_group_name_Hall '-P 2ybc'
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2ybc'
_symmetry_space_group_name_H-M 'P 1 21/c 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL97
_cell_angle_alpha 90.00
_cell_angle_beta 115.198(10)
_cell_angle_gamma 90.00
_cell_formula_units_Z 2
_cell_length_a 7.0696(8)
_cell_length_b 17.2872(16)
_cell_length_c 6.6046(7)
_cell_measurement_reflns_used 8000
_cell_measurement_temperature 213(2)
_cell_measurement_theta_max 27.93
_cell_measurement_theta_min 2.36
_cell_volume 730.36(14)
_computing_cell_refinement 'IPDS Software (Stoe & Cie, 2000)'
_computing_data_collection 'IPDS Software (Stoe & Cie, 2000)'
_computing_data_reduction 'IPDS Software (Stoe & Cie, 2000)'
_computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)'
_computing_publication_material 'WinGX (Farrugia, 1999)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature 213(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type 'Stoe IPDS'
_diffrn_measurement_method '\f oscillation 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 0.0263
_diffrn_reflns_av_sigmaI/netI 0.0237
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_k_max 22
_diffrn_reflns_limit_k_min -20
_diffrn_reflns_limit_l_max 8
_diffrn_reflns_limit_l_min -8
_diffrn_reflns_number 6296
_diffrn_reflns_theta_full 27.93
_diffrn_reflns_theta_max 27.93
_diffrn_reflns_theta_min 2.36
_diffrn_standards_decay_% 0
_exptl_absorpt_coefficient_mu 3.276
_exptl_absorpt_correction_T_max 0.6059
_exptl_absorpt_correction_T_min 0.5070
_exptl_absorpt_correction_type numerical
_exptl_absorpt_process_details
'[X-RED (Stoe & Cie, 2001) and X-SHAPE (Stoe & Cie, 1999)]'
_exptl_crystal_colour red
_exptl_crystal_density_diffrn 1.965
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prism
_exptl_crystal_F_000 428
_exptl_crystal_size_max 0.24
_exptl_crystal_size_mid 0.20
_exptl_crystal_size_min 0.17
_refine_diff_density_max 0.385
_refine_diff_density_min -0.384
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.916
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 100
_refine_ls_number_reflns 1753
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 0.916
_refine_ls_R_factor_all 0.0282
_refine_ls_R_factor_gt 0.0225
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0362P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0519
_refine_ls_wR_factor_ref 0.0528
_reflns_number_gt 1440
_reflns_number_total 1753
_reflns_threshold_expression I>2\s(I)
_iucr_refine_instructions_details
;
TITL (I) in P2(1)/c
CELL 0.71073 7.0696 17.2872 6.6046 90.000 115.198 90.000
ZERR 2.00 0.0008 0.0016 0.0007 0.000 0.010 0.000
LATT 1
SYMM - X, 1/2 + Y, 1/2 - Z
SFAC C H N CL CU
UNIT 28 20 8 4 4
MERG 2
FMAP 2
OMIT 0
PLAN 20
SIZE 0.17 0.20 0.24
ACTA
BOND
BOND $H
CONF
L.S. 6
TEMP -60.00
WGHT 0.036200
FVAR 1.00371
CU1 5 0.168520 0.271681 0.067281 11.00000 0.03694 0.02870 =
0.02224 0.00161 0.00990 -0.00349
CL1 4 0.365450 0.309074 0.425399 11.00000 0.04610 0.04504 =
0.02616 -0.01082 0.01644 -0.02125
N1 3 -0.030100 0.187542 0.099147 11.00000 0.03077 0.02631 =
0.02104 0.00047 0.00775 -0.00398
N2 3 0.001254 0.160087 0.303306 11.00000 0.02603 0.02334 =
0.02050 -0.00085 0.00773 -0.00008
C1 1 -0.150460 0.148595 -0.083329 11.00000 0.03350 0.02883 =
0.02114 -0.00012 0.00928 -0.00734
AFIX 43
H1 2 -0.174029 0.170432 -0.222399 11.00000 -1.20000
AFIX 0
C2 1 -0.245891 0.076785 -0.084454 11.00000 0.02191 0.02373 =
0.02356 -0.00153 0.00831 -0.00002
C3 1 -0.204884 0.047792 0.126333 11.00000 0.02979 0.02322 =
0.02747 0.00062 0.01105 -0.00360
AFIX 43
H3 2 -0.257594 -0.000582 0.142547 11.00000 -1.20000
AFIX 0
C4 1 -0.084080 0.091965 0.312798 11.00000 0.03281 0.02735 =
0.02378 0.00262 0.01238 -0.00092
AFIX 43
H4 2 -0.060952 0.072698 0.454530 11.00000 -1.20000
AFIX 0
C5 1 -0.488180 0.080519 -0.492938 11.00000 0.02787 0.02045 =
0.02907 -0.00103 0.00857 -0.00129
AFIX 43
H5 2 -0.481001 0.134828 -0.488594 11.00000 -1.20000
AFIX 0
C6 1 -0.376327 0.037829 -0.297685 11.00000 0.02096 0.02199 =
0.02603 -0.00227 0.00917 -0.00192
C7 1 -0.390706 -0.043323 -0.307613 11.00000 0.02715 0.02199 =
0.02530 0.00206 0.00668 0.00035
AFIX 43
H7 2 -0.317429 -0.072655 -0.177653 11.00000 -1.20000
HKLF 4
REM p21c in P2(1)/c
REM R1 = 0.0225 for 1440 Fo > 4sig(Fo) and 0.0282 for all 1753 data
REM 100 parameters refined using 0 restraints
END
WGHT 0.0362 0.0000
REM Highest difference peak 0.385, deepest hole -0.384, 1-sigma level 0.065
Q1 1 0.2702 0.3370 0.3839 11.00000 0.05 0.38
Q2 1 -0.4392 0.0583 -0.3943 11.00000 0.05 0.27
Q3 1 -0.2054 0.1104 -0.0834 11.00000 0.05 0.26
Q4 1 0.2585 0.2987 0.0674 11.00000 0.05 0.26
Q5 1 -0.5353 0.0576 -0.5827 11.00000 0.05 0.23
;
_cod_data_source_file sf3217sup1.cif
_cod_data_source_block I
_cod_original_cell_volume 730.36(13)
_cod_original_sg_symbol_H-M 'P 21/c'
_cod_database_code 2019394
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
Cu Cu1 0.16852(4) 0.271681(12) 0.06728(3) 0.03023(8) Uani d . 1 1
Cl Cl1 0.36545(8) 0.30907(3) 0.42540(7) 0.03873(13) Uani d . 1 1
N N1 -0.0301(2) 0.18754(8) 0.0991(2) 0.0272(3) Uani d . 1 1
N N2 0.0013(2) 0.16009(8) 0.3033(2) 0.0240(3) Uani d . 1 1
C C1 -0.1505(3) 0.14859(10) -0.0833(3) 0.0286(4) Uani d . 1 1
H H1 -0.1740 0.1704 -0.2224 0.034 Uiso calc R 1 1
C C2 -0.2459(3) 0.07678(9) -0.0845(3) 0.0235(3) Uani d . 1 1
C C3 -0.2049(3) 0.04779(10) 0.1263(3) 0.0272(4) Uani d . 1 1
H H3 -0.2576 -0.0006 0.1425 0.033 Uiso calc R 1 1
C C4 -0.0841(3) 0.09196(10) 0.3128(3) 0.0279(4) Uani d . 1 1
H H4 -0.0610 0.0727 0.4545 0.033 Uiso calc R 1 1
C C5 -0.4882(3) 0.08052(9) -0.4929(3) 0.0270(4) Uani d . 1 1
H H5 -0.4810 0.1348 -0.4886 0.032 Uiso calc R 1 1
C C6 -0.3763(3) 0.03783(9) -0.2977(3) 0.0233(3) Uani d . 1 1
C C7 -0.3907(3) -0.04332(9) -0.3076(3) 0.0264(3) Uani d . 1 1
H H7 -0.3174 -0.0727 -0.1777 0.032 Uiso calc R 1 1
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Cu1 0.03694(15) 0.02870(12) 0.02224(12) -0.00349(9) 0.00990(10) 0.00161(8)
Cl1 0.0461(3) 0.0450(3) 0.0262(2) -0.0212(2) 0.0164(2) -0.01082(19)
N1 0.0308(8) 0.0263(7) 0.0210(7) -0.0040(6) 0.0078(7) 0.0005(6)
N2 0.0260(8) 0.0233(6) 0.0205(7) -0.0001(5) 0.0077(6) -0.0008(5)
C1 0.0335(11) 0.0288(8) 0.0211(8) -0.0073(7) 0.0093(8) -0.0001(7)
C2 0.0219(9) 0.0237(8) 0.0236(8) 0.0000(6) 0.0083(8) -0.0015(6)
C3 0.0298(10) 0.0232(8) 0.0275(8) -0.0036(7) 0.0111(8) 0.0006(6)
C4 0.0328(11) 0.0273(8) 0.0238(8) -0.0009(7) 0.0124(8) 0.0026(7)
C5 0.0279(10) 0.0204(7) 0.0291(9) -0.0013(7) 0.0086(8) -0.0010(6)
C6 0.0210(9) 0.0220(7) 0.0260(8) -0.0019(6) 0.0092(7) -0.0023(6)
C7 0.0271(10) 0.0220(7) 0.0253(8) 0.0003(7) 0.0067(8) 0.0021(6)
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N2 Cu1 N1 4_565 . 108.75(6) y
N2 Cu1 Cl1 4_565 . 127.44(4) y
N1 Cu1 Cl1 . . 103.49(4) y
N2 Cu1 Cl1 4_565 4_565 102.96(4) y
N1 Cu1 Cl1 . 4_565 99.14(4) y
Cl1 Cu1 Cl1 . 4_565 111.63(3) y
Cu1 Cl1 Cu1 . 4_566 92.316(19) y
C1 N1 N2 . . 119.76(14) ?
C1 N1 Cu1 . . 117.38(10) ?
N2 N1 Cu1 . . 120.70(11) ?
C4 N2 N1 . . 117.98(14) ?
C4 N2 Cu1 . 4_566 125.77(11) ?
N1 N2 Cu1 . 4_566 116.24(10) ?
N1 C1 C2 . . 124.89(15) ?
N1 C1 H1 . . 117.6 ?
C2 C1 H1 . . 117.6 ?
C3 C2 C1 . . 114.63(15) ?
C3 C2 C6 . . 124.77(15) ?
C1 C2 C6 . . 120.60(14) ?
C2 C3 C4 . . 118.48(15) ?
C2 C3 H3 . . 120.8 ?
C4 C3 H3 . . 120.8 ?
N2 C4 C3 . . 124.16(15) ?
N2 C4 H4 . . 117.9 ?
C3 C4 H4 . . 117.9 ?
C7 C5 C6 3_454 . 120.55(14) ?
C7 C5 H5 3_454 . 119.7 ?
C6 C5 H5 . . 119.7 ?
C5 C6 C7 . . 118.76(15) ?
C5 C6 C2 . . 121.06(14) ?
C7 C6 C2 . . 120.18(15) ?
C5 C7 C6 3_454 . 120.68(16) ?
C5 C7 H7 3_454 . 119.7 ?
C6 C7 H7 . . 119.7 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Cu1 N2 4_565 2.0183(14) y
Cu1 N1 . 2.0936(14) y
Cu1 Cl1 . 2.2686(6) y
Cu1 Cl1 4_565 2.4241(5) y
N1 C1 . 1.325(2) ?
N1 N2 . 1.3557(19) ?
N2 C4 . 1.337(2) ?
C1 C2 . 1.411(2) ?
C1 H1 . 0.9400 ?
C2 C3 . 1.389(2) ?
C2 C6 . 1.477(2) ?
C3 C4 . 1.391(3) ?
C3 H3 . 0.9400 ?
C4 H4 . 0.9400 ?
C5 C7 3_454 1.386(2) ?
C5 C6 . 1.402(2) ?
C5 H5 . 0.9400 ?
C6 C7 . 1.406(2) ?
C7 C5 3_454 1.386(2) ?
C7 H7 . 0.9400 ?
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_site_symmetry_1
_geom_torsion_site_symmetry_4
_geom_torsion
N2 Cu1 Cl1 Cu1 4_565 4_566 122.32(5)
N1 Cu1 Cl1 Cu1 . 4_566 -4.55(5)
Cl1 Cu1 Cl1 Cu1 4_565 4_566 -110.27(3)
N2 Cu1 N1 C1 4_565 . 49.18(15)
Cl1 Cu1 N1 C1 . . -172.95(13)
Cl1 Cu1 N1 C1 4_565 . -57.96(14)
N2 Cu1 N1 N2 4_565 . -147.56(12)
Cl1 Cu1 N1 N2 . . -9.69(13)
Cl1 Cu1 N1 N2 4_565 . 105.31(12)
C1 N1 N2 C4 . . 3.1(2)
Cu1 N1 N2 C4 . . -159.80(12)
C1 N1 N2 Cu1 . 4_566 -175.36(13)
Cu1 N1 N2 Cu1 . 4_566 21.77(16)
N2 N1 C1 C2 . . -2.8(3)
Cu1 N1 C1 C2 . . 160.60(14)
N1 C1 C2 C3 . . 0.0(3)
N1 C1 C2 C6 . . -179.57(16)
C1 C2 C3 C4 . . 2.3(2)
C6 C2 C3 C4 . . -178.12(16)
N1 N2 C4 C3 . . -0.7(3)
Cu1 N2 C4 C3 4_566 . 177.57(13)
C2 C3 C4 N2 . . -2.1(3)
C7 C5 C6 C7 3_454 . -0.5(3)
C7 C5 C6 C2 3_454 . 179.68(15)
C3 C2 C6 C5 . . 150.60(17)
C1 C2 C6 C5 . . -29.8(2)
C3 C2 C6 C7 . . -29.2(2)
C1 C2 C6 C7 . . 150.37(17)
C5 C6 C7 C5 . 3_454 0.5(3)
C2 C6 C7 C5 . 3_454 -179.68(15)