#------------------------------------------------------------------------------ #$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $ #$Revision: 176760 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/01/87/2018794.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2018794 loop_ _publ_author_name 'Huang, Wenjiang' 'Zhang, Jinfang' 'Li, Jianghua' 'Zhang, Chi' _publ_section_title ; A twofold interwoven two-dimensional\\rightarrow two-dimensional (2-D\\rightarrow 2-D) cluster--organic network based on the [Cu~2~I~2~] cluster and the 4,4'-(diazenediyl)dipyridine ligand: poly[[\m~2~-4,4'-(diazenediyl)dipyridine]-\m~2~-iodido-copper(I)] ; _journal_coeditor_code SK3470 _journal_issue 2 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 123 _journal_page_last 126 _journal_paper_doi 10.1107/S0108270113000942 _journal_volume 69 _journal_year 2013 _chemical_formula_iupac '[Cu I (C10 H8 N4)]' _chemical_formula_moiety 'C10 H8 Cu I N4' _chemical_formula_sum 'C10 H8 Cu I N4' _chemical_formula_weight 374.65 _chemical_name_systematic ; poly[[\m-4,4'-(diazenediyl)dipyridine]-\m~2~-iodido-copper(I)] ; _space_group_IT_number 13 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yc' _symmetry_space_group_name_H-M 'P 1 2/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method 'SHELXTL (Sheldrick, 2008)' _cell_angle_alpha 90.00 _cell_angle_beta 98.73(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 9.7137(19) _cell_length_b 8.0745(16) _cell_length_c 15.396(3) _cell_measurement_reflns_used 3410 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 28.8928 _cell_measurement_theta_min 2.5225 _cell_volume 1193.6(4) _computing_cell_refinement 'CrystalClear (Rigaku, 2008)' _computing_data_collection 'CrystalClear (Rigaku, 2008)' _computing_data_reduction 'CrystalClear (Rigaku, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _computing_structure_refinement 'SHELXTL (Sheldrick, 2008)' _computing_structure_solution 'SHELXTL (Sheldrick, 2008)' _diffrn_ambient_temperature 150(2) _diffrn_measured_fraction_theta_full 0.989 _diffrn_measured_fraction_theta_max 0.989 _diffrn_measurement_device_type 'Rigaku Saturn724+ (2x2 bin mode)' _diffrn_measurement_method '\w 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 0.0526 _diffrn_reflns_av_sigmaI/netI 0.0613 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 6682 _diffrn_reflns_theta_full 25.34 _diffrn_reflns_theta_max 25.34 _diffrn_reflns_theta_min 2.86 _diffrn_standards_decay_% 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 4.393 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.7945 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(CrystalClear; Rigaku, 2008)' _exptl_crystal_colour brown _exptl_crystal_density_diffrn 2.085 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 712 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _refine_diff_density_max 0.796 _refine_diff_density_min -0.632 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.169 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 145 _refine_ls_number_reflns 2171 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.169 _refine_ls_R_factor_all 0.0876 _refine_ls_R_factor_gt 0.0603 _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/[\s^2^(Fo^2^)+(0.0198P)^2^+2.6592P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0838 _refine_ls_wR_factor_ref 0.0934 _reflns_number_gt 1674 _reflns_number_total 2171 _reflns_threshold_expression I>2sigma(I) _iucr_refine_instructions_details ; TITL s in P2/c CELL 0.71073 9.7137 8.0745 15.3960 90.000 98.730 90.000 ZERR 4 0.0019 0.0016 0.0030 0.000 0.030 0.000 LATT 1 SYMM - X , Y , 0.50000 - Z SFAC C 2.31000 20.84392 1.02000 10.20751 1.58860 0.56870 0.86500 = 51.65125 0.21560 0.00330 0.00160 11.500 0.68000 12.01000 SFAC H 0.49300 10.51091 0.32291 26.12573 0.14019 3.14236 0.04081 = 57.79977 0.00304 0.00000 0.00000 0.624 0.35000 1.00800 SFAC Cu 13.33801 3.58280 7.16761 0.24700 5.61581 11.39661 1.67350 = 64.81267 1.19100 0.32010 1.26510 5180.000 1.52000 63.55000 SFAC I 20.14722 4.34700 18.99492 0.38140 7.51381 27.76604 2.27350 = 66.87767 4.07120 -0.47420 1.81190 7730.000 1.40000 126.90000 SFAC N 12.21261 0.00570 3.13220 9.89331 2.01250 28.99754 1.16630 = 0.58260 -11.52901 0.00610 0.00330 19.600 0.68000 14.01000 UNIT 40 32 4 4 16 L.S. 5 FMAP 2 PLAN -20 ACTA BOND $H CONF omit 0 1 0 WGHT 0.019800 2.659200 FVAR 2.20169 I1 4 0.100630 0.312522 0.415935 11.00000 0.05694 0.03382 = 0.05879 -0.00192 0.00065 0.00231 CU1 3 0.052596 0.623728 0.451621 11.00000 0.04467 0.03864 = 0.05792 0.00301 -0.01635 -0.00234 N1 5 -0.074520 0.721329 0.346671 11.00000 0.04054 0.03139 = 0.04695 -0.00092 -0.00064 -0.00040 N2 5 0.239823 0.725010 0.504151 11.00000 0.03910 0.03538 = 0.05240 0.00082 -0.00988 0.00039 N3 5 0.586774 0.927929 0.666061 11.00000 0.04104 0.06153 = 0.06253 -0.00832 -0.00493 -0.00985 N4 5 0.600616 1.080388 0.663288 11.00000 0.04262 0.06148 = 0.04977 -0.00491 -0.00455 -0.01045 C1 1 -0.087606 0.884339 0.336159 11.00000 0.04458 0.04413 = 0.04582 -0.00385 -0.00847 -0.00284 AFIX 43 H1A 2 -0.024653 0.951956 0.371343 11.00000 -1.20000 AFIX 0 C2 1 -0.188768 0.959725 0.276295 11.00000 0.05407 0.03967 = 0.05228 0.00865 0.00007 0.01117 AFIX 43 H2A 2 -0.193099 1.074374 0.270772 11.00000 -1.20000 AFIX 0 C3 1 -0.283349 0.858824 0.224879 11.00000 0.04356 0.04239 = 0.03566 0.00151 -0.00421 0.00924 C4 1 -0.270788 0.691287 0.233989 11.00000 0.05840 0.05658 = 0.07418 -0.00319 -0.03494 0.00365 AFIX 43 H4A 2 -0.333626 0.621256 0.200326 11.00000 -1.20000 AFIX 0 C5 1 -0.163958 0.626717 0.293627 11.00000 0.06129 0.03677 = 0.07224 -0.00094 -0.02023 0.00313 AFIX 43 H5A 2 -0.153636 0.512295 0.297121 11.00000 -1.20000 AFIX 0 C6 1 0.254044 0.888368 0.512339 11.00000 0.04782 0.04150 = 0.04880 0.00156 -0.00820 -0.00269 AFIX 43 H6A 2 0.184530 0.954988 0.482255 11.00000 -1.20000 AFIX 0 C7 1 0.365208 0.964792 0.562550 11.00000 0.05133 0.04714 = 0.04765 -0.00347 -0.00517 -0.01621 AFIX 43 H7A 2 0.369885 1.079646 0.566459 11.00000 -1.20000 AFIX 0 C8 1 0.468928 0.868232 0.606698 11.00000 0.02987 0.06031 = 0.04351 -0.00213 -0.00096 -0.00032 C9 1 0.458597 0.698359 0.597597 11.00000 0.05846 0.04258 = 0.10199 -0.01815 -0.03488 0.00950 AFIX 43 H9A 2 0.527956 0.629429 0.625945 11.00000 -1.20000 AFIX 0 C10 1 0.342431 0.632603 0.545213 11.00000 0.05333 0.04078 = 0.10067 -0.01559 -0.03237 0.00013 AFIX 43 H10A 2 0.336317 0.518228 0.538616 11.00000 -1.20000 HKLF 4 REM s R = New: P2/c REM R1 = 0.0603 for 1674 Fo > 4sig(Fo) and 0.0876 for all 2171 data REM 145 parameters refined using 0 restraints END WGHT 0.0199 2.6483 REM Highest difference peak 0.796, deepest hole -0.632, 1-sigma level 0.125 Q1 1 -0.4195 0.5833 0.2070 11.00000 0.05 0.80 Q2 1 0.5269 0.5858 0.6842 11.00000 0.05 0.55 Q3 1 0.0747 0.3063 0.3923 11.00000 0.05 0.52 Q4 1 0.1736 0.3269 0.3713 11.00000 0.05 0.51 Q5 1 0.0200 0.3136 0.4546 11.00000 0.05 0.51 Q6 1 0.0249 0.3159 0.5147 11.00000 0.05 0.49 Q7 1 0.0944 0.2781 0.5241 11.00000 0.05 0.48 Q8 1 -0.1575 0.5214 0.3440 11.00000 0.05 0.46 Q9 1 0.3382 0.3227 0.4199 11.00000 0.05 0.46 Q10 1 0.1367 0.3056 0.4440 11.00000 0.05 0.44 Q11 1 0.1330 0.7454 0.5286 11.00000 0.05 0.43 Q12 1 0.2474 0.3067 0.4507 11.00000 0.05 0.42 Q13 1 0.2374 0.4468 0.4433 11.00000 0.05 0.40 Q14 1 0.0777 0.6175 0.4763 11.00000 0.05 0.39 Q15 1 -0.0886 0.3820 0.4521 11.00000 0.05 0.38 Q16 1 0.0837 0.1096 0.4177 11.00000 0.05 0.37 Q17 1 -0.1201 0.8983 0.2896 11.00000 0.05 0.37 Q18 1 0.4834 0.8486 0.5621 11.00000 0.05 0.36 Q19 1 -0.1927 0.6828 0.1987 11.00000 0.05 0.36 Q20 1 0.0020 0.1485 0.2835 11.00000 0.05 0.36 ; _cod_data_source_file sk3470.cif _cod_data_source_block I _cod_original_sg_symbol_H-M 'P 2/c' _cod_database_code 2018794 _cod_database_fobs_code 2018794 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, 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 I I1 0.10063(6) 0.31252(6) 0.41593(4) 0.0507(2) Uani d . 1 1 Cu Cu1 0.05260(10) 0.62373(12) 0.45162(7) 0.0496(3) Uani d . 1 1 N N1 -0.0745(6) 0.7213(8) 0.3467(4) 0.0404(16) Uani d . 1 1 N N2 0.2398(6) 0.7250(8) 0.5042(4) 0.0440(17) Uani d . 1 1 N N3 0.5868(7) 0.9279(10) 0.6661(4) 0.056(2) Uani d . 1 1 N N4 0.6006(7) 1.0804(10) 0.6633(4) 0.0525(19) Uani d . 1 1 C C1 -0.0876(8) 0.8843(10) 0.3362(5) 0.046(2) Uani d . 1 1 H H1A -0.0247 0.9520 0.3713 0.056 Uiso calc R 1 1 C C2 -0.1888(8) 0.9597(10) 0.2763(5) 0.050(2) Uani d . 1 1 H H2A -0.1931 1.0744 0.2708 0.059 Uiso calc R 1 1 C C3 -0.2833(8) 0.8588(10) 0.2249(5) 0.042(2) Uani d . 1 1 C C4 -0.2708(9) 0.6913(11) 0.2340(6) 0.068(3) Uani d . 1 1 H H4A -0.3336 0.6213 0.2003 0.081 Uiso calc R 1 1 C C5 -0.1640(8) 0.6267(11) 0.2936(5) 0.060(3) Uani d . 1 1 H H5A -0.1536 0.5123 0.2971 0.072 Uiso calc R 1 1 C C6 0.2540(8) 0.8884(10) 0.5123(5) 0.048(2) Uani d . 1 1 H H6A 0.1845 0.9550 0.4823 0.057 Uiso calc R 1 1 C C7 0.3652(8) 0.9648(10) 0.5625(5) 0.050(2) Uani d . 1 1 H H7A 0.3699 1.0796 0.5665 0.060 Uiso calc R 1 1 C C8 0.4689(7) 0.8682(11) 0.6067(5) 0.045(2) Uani d . 1 1 C C9 0.4586(9) 0.6984(11) 0.5976(6) 0.073(3) Uani d . 1 1 H H9A 0.5280 0.6294 0.6259 0.087 Uiso calc R 1 1 C C10 0.3424(8) 0.6326(11) 0.5452(6) 0.069(3) Uani d . 1 1 H H10A 0.3363 0.5182 0.5386 0.083 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 I1 0.0569(4) 0.0338(3) 0.0588(4) 0.0023(3) 0.0007(3) -0.0019(3) Cu1 0.0447(6) 0.0386(6) 0.0579(7) -0.0023(5) -0.0164(5) 0.0030(5) N1 0.041(4) 0.031(4) 0.047(4) 0.000(3) -0.001(3) -0.001(3) N2 0.039(4) 0.035(4) 0.052(4) 0.000(3) -0.010(3) 0.001(3) N3 0.041(4) 0.062(5) 0.063(5) -0.010(4) -0.005(4) -0.008(4) N4 0.043(4) 0.061(5) 0.050(4) -0.010(4) -0.005(3) -0.005(4) C1 0.045(5) 0.044(6) 0.046(5) -0.003(4) -0.008(4) -0.004(4) C2 0.054(5) 0.040(5) 0.052(5) 0.011(4) 0.000(4) 0.009(4) C3 0.044(5) 0.042(5) 0.036(4) 0.009(4) -0.004(4) 0.002(4) C4 0.058(6) 0.057(6) 0.074(6) 0.004(5) -0.035(5) -0.003(5) C5 0.061(6) 0.037(5) 0.072(6) 0.003(4) -0.020(5) -0.001(4) C6 0.048(5) 0.041(6) 0.049(5) -0.003(4) -0.008(4) 0.002(4) C7 0.051(5) 0.047(6) 0.048(5) -0.016(4) -0.005(4) -0.003(4) C8 0.030(4) 0.060(6) 0.044(5) 0.000(4) -0.001(4) -0.002(4) C9 0.058(6) 0.043(6) 0.102(8) 0.009(5) -0.035(6) -0.018(5) C10 0.053(6) 0.041(6) 0.101(7) 0.000(4) -0.032(5) -0.016(5) 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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./trash8 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 Cu1 I1 Cu1 . 3_566 62.15(4) N1 Cu1 N2 . . 123.7(3) N1 Cu1 I1 . . 108.02(18) N2 Cu1 I1 . . 106.82(19) N1 Cu1 I1 . 3_566 100.64(19) N2 Cu1 I1 . 3_566 100.42(19) I1 Cu1 I1 . 3_566 117.85(4) N1 Cu1 Cu1 . 3_566 118.39(18) N2 Cu1 Cu1 . 3_566 116.93(18) I1 Cu1 Cu1 . 3_566 61.05(4) I1 Cu1 Cu1 3_566 3_566 56.80(4) C1 N1 C5 . . 116.7(6) C1 N1 Cu1 . . 121.0(5) C5 N1 Cu1 . . 121.5(5) C10 N2 C6 . . 116.9(6) C10 N2 Cu1 . . 121.5(5) C6 N2 Cu1 . . 120.5(5) N4 N3 C8 . . 113.1(7) N3 N4 C3 . 4_676 113.1(7) N1 C1 C2 . . 124.2(7) N1 C1 H1A . . 117.9 C2 C1 H1A . . 117.9 C1 C2 C3 . . 117.7(7) C1 C2 H2A . . 121.1 C3 C2 H2A . . 121.1 C4 C3 C2 . . 119.0(7) C4 C3 N4 . 4_475 117.0(7) C2 C3 N4 . 4_475 124.0(7) C3 C4 C5 . . 119.3(7) C3 C4 H4A . . 120.3 C5 C4 H4A . . 120.3 N1 C5 C4 . . 122.9(8) N1 C5 H5A . . 118.5 C4 C5 H5A . . 118.5 N2 C6 C7 . . 124.0(7) N2 C6 H6A . . 118.0 C7 C6 H6A . . 118.0 C8 C7 C6 . . 118.6(8) C8 C7 H7A . . 120.7 C6 C7 H7A . . 120.7 C7 C8 C9 . . 118.6(7) C7 C8 N3 . . 125.5(8) C9 C8 N3 . . 115.9(7) C8 C9 C10 . . 118.6(7) C8 C9 H9A . . 120.7 C10 C9 H9A . . 120.7 N2 C10 C9 . . 123.2(8) N2 C10 H10A . . 118.4 C9 C10 H10A . . 118.4 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance I1 Cu1 . 2.6290(13) I1 Cu1 3_566 2.7495(15) Cu1 N1 . 2.037(6) Cu1 N2 . 2.045(6) N1 C1 . 1.330(9) N1 C5 . 1.338(9) N2 C10 . 1.326(9) N2 C6 . 1.330(9) N3 N4 . 1.240(9) N3 C8 . 1.435(9) N4 C3 4_676 1.444(9) C1 C2 . 1.382(9) C1 H1A . 0.9300 C2 C3 . 1.383(10) C2 H2A . 0.9300 C3 C4 . 1.364(11) C3 N4 4_475 1.444(9) C4 C5 . 1.379(10) C4 H4A . 0.9300 C5 H5A . 0.9300 C6 C7 . 1.375(9) C6 H6A . 0.9300 C7 C8 . 1.370(10) C7 H7A . 0.9300 C8 C9 . 1.381(11) C9 C10 . 1.389(10) C9 H9A . 0.9300 C10 H10A . 0.9300 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 Cu1 I1 Cu1 N1 3_566 . -113.0(2) Cu1 I1 Cu1 N2 3_566 . 111.9(2) Cu1 I1 Cu1 I1 3_566 3_566 0.0 N2 Cu1 N1 C1 . . -37.0(7) I1 Cu1 N1 C1 . . -162.6(6) I1 Cu1 N1 C1 3_566 . 73.3(6) Cu1 Cu1 N1 C1 3_566 . 131.1(6) N2 Cu1 N1 C5 . . 153.7(6) I1 Cu1 N1 C5 . . 28.0(7) I1 Cu1 N1 C5 3_566 . -96.1(6) Cu1 Cu1 N1 C5 3_566 . -38.2(7) N1 Cu1 N2 C10 . . -152.1(7) I1 Cu1 N2 C10 . . -26.0(7) I1 Cu1 N2 C10 3_566 . 97.5(7) Cu1 Cu1 N2 C10 3_566 . 39.6(8) N1 Cu1 N2 C6 . . 40.2(7) I1 Cu1 N2 C6 . . 166.3(6) I1 Cu1 N2 C6 3_566 . -70.2(6) Cu1 Cu1 N2 C6 3_566 . -128.1(6) C8 N3 N4 C3 . 4_676 178.2(6) C5 N1 C1 C2 . . 1.8(12) Cu1 N1 C1 C2 . . -168.1(6) N1 C1 C2 C3 . . 0.8(13) C1 C2 C3 C4 . . -1.5(13) C1 C2 C3 N4 . 4_475 176.3(7) C2 C3 C4 C5 . . -0.4(14) N4 C3 C4 C5 4_475 . -178.3(8) C1 N1 C5 C4 . . -3.8(13) Cu1 N1 C5 C4 . . 166.0(7) C3 C4 C5 N1 . . 3.2(15) C10 N2 C6 C7 . . -2.2(13) Cu1 N2 C6 C7 . . 166.0(6) N2 C6 C7 C8 . . 0.5(13) C6 C7 C8 C9 . . 1.2(13) C6 C7 C8 N3 . . -175.7(8) N4 N3 C8 C7 . . -11.7(12) N4 N3 C8 C9 . . 171.4(9) C7 C8 C9 C10 . . -1.0(14) N3 C8 C9 C10 . . 176.2(9) C6 N2 C10 C9 . . 2.4(14) Cu1 N2 C10 C9 . . -165.7(8) C8 C9 C10 N2 . . -0.8(16)