# om010665p.cif _publ_contact_author_name 'Prof.Ren-Gen Xiong' _publ_contact_author_address ; Prof. Xiao-Zeng You Coordination Chemistry Institue Nanjing University, Nanjing 210093, P. R. China ; _publ_contact_author_email 'xyz@netra.nju.edu.cn' _publ_contact_author_fax '86-25-3317761' _publ_contact_author_phone '86-25-3594724' _publ_requested_journal ' Organometallics' _publ_section_title ; An unprecedented luminescent two-dimensional coordination polymer with an approximately rectangular molecular grid containing copper(i)-olefin bond as bridging spacer ; _publ_section_references ; Allen, F.H., Kennard, O., Watson, D.G., Brammer, L., Orpen, A.G. & Taylor, R. (1987). Chem. Soc. Perkin Trans. II, S1-S19. Nardelli, M. (1995). J. Appl. Cryst. 28, 659. Orpen, A.G., Brammer, L., Allen, F.H., Kennard, O., Watson, D.G. & Taylor, R. (1989). J. Chem. Soc. Dalton Trans., S1-S83. Siemens (1996). SMART and SAINT. Area Detector Control and Integration Software. Siemens Analytical X-Ray Systems, Inc., Madison, Wisconsin, USA. Sheldrick, G. M. (1996). SADABS. Program for Empirical Absorption Correction of Area Detector Data, University of G\"ottingen, Germany. Sheldrick, G.M. (1997). SHELXTL V5.1 Software Reference Manual, Bruker AXS, Inc., Madison, Wisconsin, USA. Spek, A.L. (1990). Acta Cryst. A46, C-34. ; _publ_section_exptl_refinement ; The data collection covered over a hemisphere of reciprocal space by a combination of three sets of exposures; each set had a different \f angle (0, 88 and 180\%) for the crystal and each exposure of 10s covered 0.3\% in \w. The crystal-to-detector distance was 4 cm and the detector swing angle was -35\%. Coverage of the unique set is over 99% complete. Crystal decay was monitored by repeating fifty initial frames at the end of data collection and analysing the duplicate reflections, and was found to be negligible. ; #============================================================================ data_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C7 H7 Cl Cu N' _chemical_formula_weight 204.13 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c 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' _cell_length_a 7.9377(11) _cell_length_b 9.4600(12) _cell_length_c 10.7491(12) _cell_angle_alpha 90.00 _cell_angle_beta 109.494(11) _cell_angle_gamma 90.00 _cell_volume 760.89(17) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 8.34 _cell_measurement_theta_max 12.20 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.782 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 408 _exptl_absorpt_coefficient_mu 3.134 _exptl_absorpt_correction_type 'empirical used psi-scan' _exptl_absorpt_correction_T_min 0.6593 _exptl_absorpt_correction_T_max 0.7608 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf-Nonius CAD4' _diffrn_measurement_method '\w--2\q scans' _diffrn_detector_area_resol_mean 3 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 1737 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0316 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.72 _diffrn_reflns_theta_max 27.50 _reflns_number_total 1737 _reflns_number_gt 1313 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Enraf-Nonius CAD4' _computing_cell_refinement 'Enraf-Nonius CAD4' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0352P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1737 _refine_ls_number_parameters 91 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0444 _refine_ls_R_factor_gt 0.0282 _refine_ls_wR_factor_ref 0.0708 _refine_ls_wR_factor_gt 0.0664 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 0.14966(4) 0.11782(4) 0.07354(3) 0.03583(12) Uani 1 1 d . . . Cl1 Cl -0.10598(9) 0.07563(8) 0.11617(7) 0.04078(18) Uani 1 1 d . . . N1 N 0.3399(3) 0.0088(2) 0.2103(2) 0.0341(5) Uani 1 1 d . . . C1 C 0.0809(4) 0.2928(3) -0.0407(3) 0.0486(8) Uani 1 1 d . . . H1A H 0.0110 0.2776 -0.1328 0.058 Uiso 1 1 calc R . . H1B H 0.0412 0.3735 -0.0021 0.058 Uiso 1 1 calc R . . C2 C 0.2611(4) 0.2751(3) -0.0071(3) 0.0402(7) Uani 1 1 d . . . H2A H 0.3008 0.2438 -0.0797 0.048 Uiso 1 1 calc R . . C3 C 0.6032(4) -0.1457(3) 0.4026(3) 0.0327(6) Uani 1 1 d . . . C4 C 0.4265(4) -0.1451(3) 0.3969(3) 0.0365(6) Uani 1 1 d . . . H4A H 0.3921 -0.1976 0.4575 0.044 Uiso 1 1 calc R . . C5 C 0.3007(4) -0.0669(3) 0.3017(3) 0.0365(6) Uani 1 1 d . . . H5A H 0.1834 -0.0671 0.3013 0.044 Uiso 1 1 calc R . . C6 C 0.5100(4) 0.0057(3) 0.2143(3) 0.0417(7) Uani 1 1 d . . . H6A H 0.5400 0.0566 0.1507 0.050 Uiso 1 1 calc R . . C7 C 0.6430(4) -0.0677(3) 0.3064(3) 0.0396(7) Uani 1 1 d . . . H7A H 0.7592 -0.0654 0.3044 0.048 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.02791(18) 0.0333(2) 0.0422(2) 0.00473(15) 0.00619(14) -0.00168(14) Cl1 0.0305(3) 0.0476(4) 0.0465(4) -0.0065(3) 0.0159(3) 0.0002(3) N1 0.0297(11) 0.0342(12) 0.0360(12) 0.0037(10) 0.0079(9) 0.0028(10) C1 0.0492(18) 0.0375(17) 0.0433(17) 0.0113(14) -0.0057(13) -0.0070(14) C2 0.0493(17) 0.0365(15) 0.0314(14) 0.0031(12) 0.0090(12) -0.0124(13) C3 0.0386(15) 0.0258(13) 0.0323(13) -0.0038(10) 0.0100(11) 0.0023(11) C4 0.0412(15) 0.0329(15) 0.0371(15) 0.0026(11) 0.0152(12) -0.0004(12) C5 0.0277(13) 0.0377(15) 0.0432(15) 0.0002(13) 0.0104(12) -0.0017(12) C6 0.0364(15) 0.0444(17) 0.0476(17) 0.0136(14) 0.0183(13) 0.0046(13) C7 0.0285(14) 0.0440(16) 0.0479(17) 0.0082(14) 0.0149(12) 0.0075(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N1 2.006(2) . ? Cu1 C1 2.025(3) . ? Cu1 C2 2.064(3) . ? Cu1 Cl1 2.2599(8) . ? Cu1 Cl1 2.6751(8) 3 ? Cl1 Cu1 2.6751(8) 3 ? N1 C5 1.334(3) . ? N1 C6 1.337(3) . ? C1 C2 1.364(4) . ? C2 C3 1.475(4) 2_655 ? C3 C4 1.383(4) . ? C3 C7 1.391(4) . ? C3 C2 1.475(4) 2_645 ? C4 C5 1.381(4) . ? C6 C7 1.371(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 _geom_angle_publ_flag N1 Cu1 C1 148.16(11) . . ? N1 Cu1 C2 110.78(10) . . ? C1 Cu1 C2 38.97(11) . . ? N1 Cu1 Cl1 105.56(7) . . ? C1 Cu1 Cl1 100.88(10) . . ? C2 Cu1 Cl1 138.78(9) . . ? N1 Cu1 Cl1 94.66(7) . 3 ? C1 Cu1 Cl1 99.01(10) . 3 ? C2 Cu1 Cl1 97.91(8) . 3 ? Cl1 Cu1 Cl1 97.87(3) . 3 ? Cu1 Cl1 Cu1 82.13(3) . 3 ? C5 N1 C6 116.5(2) . . ? C5 N1 Cu1 120.80(18) . . ? C6 N1 Cu1 122.72(19) . . ? C2 C1 Cu1 72.08(17) . . ? C1 C2 C3 125.1(3) . 2_655 ? C1 C2 Cu1 68.95(17) . . ? C3 C2 Cu1 110.66(18) 2_655 . ? C4 C3 C7 116.3(2) . . ? C4 C3 C2 120.6(3) . 2_645 ? C7 C3 C2 123.1(3) . 2_645 ? C5 C4 C3 120.5(3) . . ? N1 C5 C4 123.0(3) . . ? N1 C6 C7 124.1(3) . . ? C6 C7 C3 119.7(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.282 _refine_diff_density_min -0.392 _refine_diff_density_rms 0.069 #===END