Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Neil Champness' 'Sarah A. Barnett' 'Alexander J. Blake' 'Claire Wilson' _publ_contact_author_name 'Dr Neil Champness' _publ_contact_author_address ; School of Chemistry University of Nottingham University Park Nottingham NG7 2RD UNITED KINGDOM ; _publ_contact_author_email NEIL.CHAMPNESS@NOTTINGHAM.AC.UK _publ_requested_journal 'Dalton Transactions' _publ_section_title ; The Role of 4,7-phenanthroline in Coordination Polymer Construction ; data_1(COCLPH) _database_code_CSD 205821 _audit_creation_method SHELXL-97 _chemical_name_systematic ; cobalt(II) chloride 4,7-phenanthroline acetonitrile solvate ; _chemical_name_common [CoCl2(4,7-phen)].MeCN _chemical_formula_moiety 'C14 H11 Cl2 Co N3' _chemical_formula_sum 'C14 H11 Cl2 Co N3' _chemical_formula_weight 351.09 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' Co Co 0.3494 0.9721 '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 10.517(3) _cell_length_b 8.206(3) _cell_length_c 16.959(4) _cell_angle_alpha 90.00 _cell_angle_beta 99.04(2) _cell_angle_gamma 90.00 _cell_volume 1445.4(8) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 40 _cell_measurement_theta_min 11 _cell_measurement_theta_max 17.5 _exptl_crystal_description tablet _exptl_crystal_colour blue _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.613 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 708 _exptl_absorpt_coefficient_mu 1.548 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.556 _exptl_absorpt_correction_T_max 0.789 _exptl_absorpt_process_details 'XRED (Stoe & Cie, 1997b)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Stoe Stadi-4 four circle' _diffrn_measurement_method omega-theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 'random variation +/- 4.9' _diffrn_reflns_number 4985 _diffrn_reflns_av_R_equivalents 0.0457 _diffrn_reflns_av_sigmaI/netI 0.0665 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.76 _diffrn_reflns_theta_max 26.03 _reflns_number_total 2831 _reflns_number_gt 2103 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STADI-4 (Stoe & Cie, 1997a)' _computing_cell_refinement STADI-4 _computing_data_reduction 'X-RED (Stoe & Cie, 1997b)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC version 5.03 (Sheldrick, 1994)' _computing_publication_material 'SHELXL-97; PLATON (Spek, 2000)' _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 w==1/[\s^2^(Fo^2^)+(0.0265P)^2^+3.473P] where P==(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'direct methods' _atom_sites_solution_secondary 'difference Fourier synthesis' _atom_sites_solution_hydrogens 'placed geometrically' _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2831 _refine_ls_number_parameters 184 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0808 _refine_ls_R_factor_gt 0.0512 _refine_ls_wR_factor_ref 0.119 _refine_ls_wR_factor_gt 0.100 _refine_ls_goodness_of_fit_ref 1.163 _refine_ls_restrained_S_all 1.171 _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 Co1 Co 0.26228(6) 0.19591(8) 0.66790(3) 0.01864(18) Uani 1 1 d . . . Cl1 Cl 0.37392(12) 0.42723(17) 0.66495(7) 0.0313(3) Uani 1 1 d . . . Cl2 Cl 0.32656(13) -0.03640(19) 0.61826(8) 0.0382(4) Uani 1 1 d . . . C1 C -0.1282(5) 0.3450(6) 0.4905(3) 0.0204(10) Uani 1 1 d . . . H1A H -0.2007 0.3760 0.4528 0.024 Uiso 1 1 calc R . . C2 C -0.0371(4) 0.2420(6) 0.4690(3) 0.0213(11) Uani 1 1 d . . . H2A H -0.0467 0.2003 0.4162 0.026 Uiso 1 1 calc R . . C3 C 0.0698(4) 0.1980(6) 0.5246(3) 0.0197(10) Uani 1 1 d . . . H3A H 0.1319 0.1267 0.5083 0.024 Uiso 1 1 calc R . . N4 N 0.0881(4) 0.2520(5) 0.5996(2) 0.0182(8) Uani 1 1 d . . . C5 C -0.0019(4) 0.3555(6) 0.6228(3) 0.0178(10) Uani 1 1 d . . . C6 C -0.1856(4) 0.5550(6) 0.6801(3) 0.0155(9) Uani 1 1 d . . . N7 N -0.2717(3) 0.6509(5) 0.7121(2) 0.0171(8) Uani 1 1 d . . . C8 C -0.3755(4) 0.7034(6) 0.6640(3) 0.0214(10) Uani 1 1 d . . . H8A H -0.4363 0.7673 0.6863 0.026 Uiso 1 1 calc R . . C9 C -0.4000(4) 0.6699(6) 0.5826(3) 0.0229(11) Uani 1 1 d . . . H9A H -0.4738 0.7136 0.5501 0.027 Uiso 1 1 calc R . . C10 C -0.3154(4) 0.5726(6) 0.5503(3) 0.0216(10) Uani 1 1 d . . . H10A H -0.3316 0.5466 0.4950 0.026 Uiso 1 1 calc R . . C11 C -0.2051(4) 0.5113(6) 0.5985(2) 0.0166(10) Uani 1 1 d . . . C12 C -0.1127(4) 0.4046(6) 0.5694(2) 0.0163(9) Uani 1 1 d . . . C13 C 0.0162(4) 0.4078(6) 0.7037(3) 0.0188(10) Uani 1 1 d . . . H13A H 0.0916 0.3757 0.7387 0.023 Uiso 1 1 calc R . . C14 C -0.0722(4) 0.5026(6) 0.7316(3) 0.0203(10) Uani 1 1 d . . . H14A H -0.0587 0.5347 0.7861 0.024 Uiso 1 1 calc R . . N1S N 0.1687(5) 0.5024(6) 0.8785(3) 0.0354(11) Uani 1 1 d . A . C1S C 0.2546(5) 0.5746(7) 0.8630(3) 0.0380(14) Uani 1 1 d D . . C2S C 0.3533(16) 0.675(3) 0.8288(11) 0.040(7) Uiso 0.50 1 d PD A 1 C3S C 0.3787(14) 0.651(3) 0.8691(14) 0.037(7) Uiso 0.30 1 d PD A 2 C4S C 0.364(4) 0.669(6) 0.844(4) 0.026(13) Uiso 0.20 1 d PD A 3 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 Co1 0.0156(3) 0.0230(4) 0.0169(3) -0.0021(3) 0.0016(2) -0.0008(3) Cl1 0.0326(7) 0.0375(8) 0.0219(6) 0.0056(5) -0.0016(5) -0.0144(6) Cl2 0.0273(7) 0.0398(9) 0.0438(8) -0.0193(7) -0.0058(6) 0.0101(6) C1 0.024(2) 0.020(3) 0.016(2) 0.0032(19) 0.0003(18) -0.005(2) C2 0.027(2) 0.024(3) 0.012(2) -0.0016(19) 0.0010(18) -0.005(2) C3 0.020(2) 0.018(2) 0.022(2) -0.001(2) 0.0052(18) -0.004(2) N4 0.021(2) 0.016(2) 0.0169(18) -0.0001(16) 0.0022(15) -0.0023(16) C5 0.017(2) 0.018(3) 0.019(2) -0.0004(19) 0.0031(18) -0.0009(19) C6 0.013(2) 0.012(2) 0.021(2) 0.0006(19) 0.0011(17) -0.0023(18) N7 0.0156(18) 0.017(2) 0.0181(18) -0.0011(16) 0.0000(14) -0.0002(16) C8 0.018(2) 0.023(3) 0.023(2) 0.002(2) 0.0013(18) -0.002(2) C9 0.017(2) 0.028(3) 0.023(2) 0.007(2) -0.0016(18) -0.002(2) C10 0.022(2) 0.024(3) 0.017(2) 0.001(2) 0.0000(18) -0.004(2) C11 0.018(2) 0.013(2) 0.017(2) -0.0002(18) -0.0008(18) -0.0078(19) C12 0.018(2) 0.014(2) 0.017(2) -0.0003(18) 0.0030(17) -0.0036(19) C13 0.017(2) 0.020(3) 0.018(2) -0.0004(19) -0.0017(18) 0.000(2) C14 0.022(2) 0.022(3) 0.015(2) 0.0002(19) 0.0008(18) 0.000(2) N1S 0.036(3) 0.043(3) 0.027(2) 0.001(2) 0.003(2) 0.009(2) C1S 0.027(3) 0.042(4) 0.042(3) -0.018(3) -0.005(3) 0.007(3) _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 Co1 N4 2.060(4) . y Co1 N7 2.055(4) 2_546 y Co1 Cl1 2.2367(16) . y Co1 Cl2 2.2313(16) . y C1 C2 1.369(7) . ? C1 C12 1.410(6) . ? C2 C3 1.396(6) . ? C3 N4 1.332(6) . ? N4 C5 1.374(6) . ? C5 C12 1.417(6) . ? C5 C13 1.421(6) . ? C6 N7 1.375(6) . ? C6 C11 1.412(6) . ? C6 C14 1.430(6) . ? N7 C8 1.328(6) . ? N7 Co1 2.055(4) 2_556 ? C8 C9 1.390(6) . ? C9 C10 1.372(7) . ? C10 C11 1.404(6) . ? C11 C12 1.451(6) . ? C13 C14 1.354(6) . ? N1S C1S 1.145(7) . ? C1S C3S 1.436(9) . ? C1S C4S 1.464(10) . ? C1S C2S 1.512(9) . ? 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 N7 Co1 N4 119.82(15) 2_546 . y N7 Co1 Cl2 104.46(12) 2_546 . y N4 Co1 Cl2 105.92(11) . . y N7 Co1 Cl1 103.34(11) 2_546 . y N4 Co1 Cl1 102.78(12) . . y Cl2 Co1 Cl1 121.70(6) . . y C2 C1 C12 119.0(4) . . ? C1 C2 C3 120.2(4) . . ? N4 C3 C2 122.6(4) . . ? C3 N4 C5 118.4(4) . . ? C3 N4 Co1 116.4(3) . . ? C5 N4 Co1 124.7(3) . . ? N4 C5 C12 121.8(4) . . ? N4 C5 C13 118.0(4) . . ? C12 C5 C13 120.2(4) . . ? N7 C6 C11 121.9(4) . . ? N7 C6 C14 117.9(4) . . ? C11 C6 C14 120.1(4) . . ? C8 N7 C6 118.1(4) . . ? C8 N7 Co1 117.2(3) . 2_556 ? C6 N7 Co1 124.2(3) . 2_556 ? N7 C8 C9 123.5(5) . . ? C10 C9 C8 118.8(4) . . ? C9 C10 C11 120.2(4) . . ? C10 C11 C6 117.4(4) . . ? C10 C11 C12 123.6(4) . . ? C6 C11 C12 119.0(4) . . ? C1 C12 C5 118.0(4) . . ? C1 C12 C11 123.3(4) . . ? C5 C12 C11 118.8(4) . . ? C14 C13 C5 121.1(4) . . ? C13 C14 C6 120.7(4) . . ? N1S C1S C3S 161.8(11) . . ? N1S C1S C4S 179(2) . . ? C3S C1S C4S 18(3) . . ? N1S C1S C2S 170.0(9) . . ? C3S C1S C2S 28.3(13) . . ? C4S C1S C2S 10(3) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.77 _refine_diff_density_min -0.44 _refine_diff_density_rms 0.104 #======END data_2(COBRPH) _database_code_CSD 205822 _audit_creation_method SHELXL-97 _chemical_name_systematic ; cobalt(II) bromide 4,7-phenanthroline acetonitrile solvate ; _chemical_name_common [CoBr2(4,7-phen)].MeCN _chemical_formula_moiety 'C14 H11 Br2 Co N3' _chemical_formula_sum 'C14 H11 Br2 Co N3' _chemical_formula_weight 440.01 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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 10.7897(8) _cell_length_b 8.2552(7) _cell_length_c 17.0355(13) _cell_angle_alpha 90.00 _cell_angle_beta 97.4710(10) _cell_angle_gamma 90.00 _cell_volume 1504.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5407 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 28.06 _exptl_crystal_description column _exptl_crystal_colour blue _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.943 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 852 _exptl_absorpt_coefficient_mu 6.444 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.302 _exptl_absorpt_correction_T_max 0.488 _exptl_absorpt_process_details 'SADABS (Bruker, 1999b)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Bruker SMART CCD area detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 15525 _diffrn_reflns_av_R_equivalents 0.039 _diffrn_reflns_av_sigmaI/netI 0.036 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 28.91 _reflns_number_total 3615 _reflns_number_gt 2693 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART version 5.054 (Bruker, 1998)' _computing_cell_refinement 'SAINT (Bruker, 1999a)' _computing_data_reduction 'SAINT (Bruker, 1999a)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC (version 5.03)(Sheldrick, 1994)' _computing_publication_material 'SHELXL-97; PLATON (Spek, 2000)' _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 w==1/[\s^2^(Fo^2^)+(0.040P)^2^] where P==(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'direct methods' _atom_sites_solution_secondary 'difference Fourier synthesis' _atom_sites_solution_hydrogens 'placed geometrically' _refine_ls_hydrogen_treatment ; riding model for those on phenanthroline and acetonitrile treated as rigid rotor ; _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3615 _refine_ls_number_parameters 182 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0489 _refine_ls_R_factor_gt 0.0306 _refine_ls_wR_factor_ref 0.0696 _refine_ls_wR_factor_gt 0.0652 _refine_ls_goodness_of_fit_ref 0.930 _refine_ls_restrained_S_all 0.930 _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 Co1 Co 0.75814(3) 0.69274(5) 0.16834(2) 0.02060(10) Uani 1 1 d . . . Br1 Br 0.87348(3) 0.93646(4) 0.164422(18) 0.03293(10) Uani 1 1 d . . . Br2 Br 0.82949(3) 0.44832(4) 0.11662(2) 0.03897(11) Uani 1 1 d . . . C1 C 0.3845(3) 0.8398(3) -0.00592(16) 0.0225(6) Uani 1 1 d . . . H1A H 0.3152 0.8711 -0.0430 0.027 Uiso 1 1 calc R . . C2 C 0.4729(2) 0.7371(3) -0.02791(16) 0.0234(6) Uani 1 1 d . . . H2A H 0.4647 0.6949 -0.0802 0.028 Uiso 1 1 calc R . . C3 C 0.5752(3) 0.6944(3) 0.02668(16) 0.0224(6) Uani 1 1 d . . . H3A H 0.6363 0.6237 0.0102 0.027 Uiso 1 1 calc R . . N4 N 0.5909(2) 0.7483(3) 0.10091(13) 0.0195(5) Uani 1 1 d . . . C5 C 0.5025(2) 0.8502(3) 0.12425(16) 0.0192(6) Uani 1 1 d . . . C6 C 0.3229(2) 1.0510(3) 0.18153(16) 0.0189(6) Uani 1 1 d . . . N7 N 0.2375(2) 1.1458(3) 0.21314(13) 0.0209(5) Uani 1 1 d . . . C8 C 0.1379(2) 1.1972(3) 0.16547(16) 0.0224(6) Uani 1 1 d . . . H8A H 0.0783 1.2624 0.1872 0.027 Uiso 1 1 calc R . . C9 C 0.1170(3) 1.1601(4) 0.08541(17) 0.0260(6) Uani 1 1 d . . . H9A H 0.0451 1.2009 0.0533 0.031 Uiso 1 1 calc R . . C10 C 0.2007(3) 1.0641(3) 0.05286(17) 0.0231(6) Uani 1 1 d . . . H10A H 0.1874 1.0380 -0.0019 0.028 Uiso 1 1 calc R . . C11 C 0.3059(2) 1.0050(3) 0.10121(16) 0.0194(6) Uani 1 1 d . . . C12 C 0.3970(2) 0.8992(3) 0.07224(16) 0.0199(6) Uani 1 1 d . . . C13 C 0.5180(3) 0.9045(3) 0.20444(16) 0.0217(6) Uani 1 1 d . . . H13A H 0.5907 0.8739 0.2388 0.026 Uiso 1 1 calc R . . C14 C 0.4312(3) 0.9983(4) 0.23218(17) 0.0228(6) Uani 1 1 d . . . H14A H 0.4423 1.0299 0.2863 0.027 Uiso 1 1 calc R . . N1S N 0.6637(3) 1.0013(4) 0.37575(16) 0.0378(7) Uani 1 1 d . . . C1S C 0.7500(3) 1.0717(4) 0.3670(2) 0.0396(8) Uani 1 1 d . . . C2S C 0.8609(4) 1.1641(5) 0.3536(4) 0.0846(18) Uani 1 1 d . . . H2S1 H 0.8415 1.2315 0.3063 0.127 Uiso 1 1 calc R . . H2S2 H 0.9288 1.0893 0.3461 0.127 Uiso 1 1 calc R . . H2S3 H 0.8867 1.2334 0.3995 0.127 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 Co1 0.01862(19) 0.0256(2) 0.01754(19) -0.00217(16) 0.00207(14) -0.00115(16) Br1 0.03565(18) 0.0386(2) 0.02283(16) 0.00528(13) -0.00252(13) -0.01609(14) Br2 0.02909(17) 0.0404(2) 0.0447(2) -0.01999(16) -0.00532(14) 0.00937(14) C1 0.0243(14) 0.0255(16) 0.0168(14) 0.0009(11) 0.0000(11) -0.0055(12) C2 0.0260(15) 0.0272(16) 0.0166(14) -0.0029(11) 0.0018(11) -0.0039(12) C3 0.0237(14) 0.0263(16) 0.0176(13) -0.0038(12) 0.0044(11) -0.0049(12) N4 0.0182(11) 0.0224(12) 0.0181(12) -0.0005(9) 0.0027(9) -0.0029(9) C5 0.0195(13) 0.0200(14) 0.0176(13) 0.0002(11) 0.0010(11) -0.0041(11) C6 0.0179(13) 0.0203(14) 0.0184(13) 0.0009(11) 0.0023(10) -0.0023(11) N7 0.0199(11) 0.0212(12) 0.0213(12) 0.0009(10) 0.0017(9) -0.0017(9) C8 0.0187(13) 0.0240(15) 0.0240(14) 0.0002(12) 0.0006(11) 0.0011(12) C9 0.0203(14) 0.0298(17) 0.0261(16) 0.0044(13) -0.0037(12) 0.0013(12) C10 0.0231(14) 0.0273(16) 0.0178(14) 0.0003(12) -0.0013(11) -0.0021(12) C11 0.0182(13) 0.0216(14) 0.0181(13) 0.0018(11) 0.0010(11) -0.0044(11) C12 0.0210(14) 0.0193(14) 0.0190(14) 0.0019(11) 0.0014(11) -0.0042(11) C13 0.0207(14) 0.0259(15) 0.0176(14) -0.0002(12) -0.0014(11) 0.0007(11) C14 0.0259(14) 0.0259(15) 0.0157(13) -0.0019(12) -0.0004(11) 0.0006(12) N1S 0.0383(17) 0.0491(18) 0.0255(15) -0.0024(13) 0.0018(13) 0.0060(14) C1S 0.0304(18) 0.043(2) 0.044(2) -0.0201(17) -0.0023(15) 0.0108(16) C2S 0.034(2) 0.063(3) 0.160(5) -0.058(3) 0.026(3) -0.009(2) _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 Co1 N4 2.061(2) . y Co1 N7 2.050(2) 2_645 y Co1 Br1 2.3712(5) . y Co1 Br2 2.3700(5) . y C1 C2 1.364(4) . ? C1 C12 1.409(4) . ? C2 C3 1.393(4) . ? C3 N4 1.330(3) . ? N4 C5 1.369(3) . ? C5 C12 1.407(4) . ? C5 C13 1.427(4) . ? C6 N7 1.372(3) . ? C6 C11 1.409(4) . ? C6 C14 1.427(4) . ? N7 C8 1.329(3) . ? N7 Co1 2.050(2) 2_655 ? C8 C9 1.387(4) . ? C9 C10 1.372(4) . ? C10 C11 1.400(4) . ? C11 C12 1.449(4) . ? C13 C14 1.347(4) . ? N1S C1S 1.124(4) . ? C1S C2S 1.461(5) . ? 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 N7 Co1 N4 119.82(9) 2_645 . y N7 Co1 Br2 103.79(7) 2_645 . y N4 Co1 Br2 106.58(7) . . y N7 Co1 Br1 104.06(6) 2_645 . y N4 Co1 Br1 102.73(7) . . y Br2 Co1 Br1 120.99(2) . . y C2 C1 C12 119.4(3) . . ? C1 C2 C3 119.7(3) . . ? N4 C3 C2 122.8(3) . . ? C3 N4 C5 118.3(2) . . ? C3 N4 Co1 116.72(18) . . ? C5 N4 Co1 124.57(18) . . ? N4 C5 C12 122.0(2) . . ? N4 C5 C13 118.1(2) . . ? C12 C5 C13 119.8(2) . . ? N7 C6 C11 121.7(2) . . ? N7 C6 C14 118.4(2) . . ? C11 C6 C14 119.9(2) . . ? C8 N7 C6 118.3(2) . . ? C8 N7 Co1 117.04(18) . 2_655 ? C6 N7 Co1 124.32(18) . 2_655 ? N7 C8 C9 123.1(3) . . ? C10 C9 C8 119.6(3) . . ? C9 C10 C11 119.3(3) . . ? C10 C11 C6 118.1(2) . . ? C10 C11 C12 122.9(3) . . ? C6 C11 C12 119.0(2) . . ? C5 C12 C1 117.7(3) . . ? C5 C12 C11 119.2(3) . . ? C1 C12 C11 123.1(3) . . ? C14 C13 C5 121.1(3) . . ? C13 C14 C6 121.0(3) . . ? N1S C1S C2S 178.6(4) . . ? _diffrn_measured_fraction_theta_max 0.910 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.98 _refine_diff_density_min -0.72 _refine_diff_density_rms 0.11 #======END data_3(CDPHEN) _database_code_CSD 205823 _exptl_special_details ; The oxygen atoms of the nitrate anion N20 (O4, O5 and O6) showed high ADPs and were modelled isotropically over two sets of sites with the occupancy ratio 50:50. The N-O bond distances and O-N-O bond angles were constrained to be the same for each disorder component. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; Cadmium (II)-(4,7-phenanthroline)-bis-nitrate hydrate ; _chemical_name_common [Cd(NO3)2(H2O)(4,7-phen)] _chemical_formula_moiety 'C14 H13 Cd N5 O7' _chemical_formula_sum 'C14 H13 Cd N5 O7' _chemical_formula_weight 475.69 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 '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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.9304(12) _cell_length_b 7.9527(7) _cell_length_c 15.5626(14) _cell_angle_alpha 90.00 _cell_angle_beta 101.007(1) _cell_angle_gamma 90.00 _cell_volume 1692.4(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7270 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 23.68 _exptl_crystal_description column _exptl_crystal_colour 'Pale yellow' _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.867 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 944 _exptl_absorpt_coefficient_mu 1.341 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.882 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details 'SADABS v2.03 (Bruker, 2001)' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART1000 CCD area detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 14329 _diffrn_reflns_av_R_equivalents 0.049 _diffrn_reflns_av_sigmaI/netI 0.054 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 28.78 _reflns_number_total 4276 _reflns_number_gt 3408 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART version 5.624 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.02a (Bruker, 2000)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'SHELXL-97; PLATON (Spek, 2002)' _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 w==1/[\s^2^(Fo^2^)+6.951P] where P==(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'direct methods' _atom_sites_solution_secondary 'difference Fourier synthsis' _atom_sites_solution_hydrogens 'MeCN and water hydrogens found from delta-F; others geometrically placed' _refine_ls_hydrogen_treatment 'MeCN treated as rigid rotor; geometric restraints for water; others riding' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3985 _refine_ls_number_parameters 250 _refine_ls_number_restraints 33 _refine_ls_R_factor_all 0.0513 _refine_ls_R_factor_gt 0.0438 _refine_ls_wR_factor_ref 0.1049 _refine_ls_wR_factor_gt 0.1027 _refine_ls_goodness_of_fit_ref 1.142 _refine_ls_restrained_S_all 1.184 _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 Cd1 Cd 0.00097(2) -0.22890(4) 0.258904(19) 0.01943(11) Uani 1 1 d . . . N10 N -0.2006(3) -0.2557(7) 0.2539(3) 0.0369(11) Uani 1 1 d . . . O1 O -0.1432(3) -0.2160(6) 0.3212(2) 0.0400(9) Uani 1 1 d . A . O2 O -0.1659(4) -0.2726(8) 0.1861(3) 0.0734(18) Uani 1 1 d . A . O3 O -0.2882(3) -0.2757(9) 0.2541(3) 0.0752(18) Uani 1 1 d . A . N20 N 0.0193(3) -0.5911(4) 0.3137(2) 0.0285(9) Uani 1 1 d D . . O4 O 0.0388(8) -0.4544(8) 0.3512(5) 0.030(2) Uiso 0.50 1 d PD A 1 O5 O 0.0284(8) -0.7220(9) 0.3621(6) 0.036(3) Uiso 0.50 1 d PD A 1 O6 O 0.0192(7) -0.6094(11) 0.2344(4) 0.042(2) Uiso 0.50 1 d PD A 1 O4' O 0.0187(9) -0.4628(10) 0.3611(6) 0.042(3) Uiso 0.50 1 d PD A 2 O5' O 0.0314(7) -0.7353(8) 0.3405(6) 0.033(2) Uiso 0.50 1 d PD A 2 O6' O -0.0214(7) -0.5549(11) 0.2354(4) 0.043(2) Uiso 0.50 1 d PD A 2 O1W O -0.0464(3) 0.0437(4) 0.2091(2) 0.0291(8) Uani 1 1 d D A . H1W H -0.011(3) 0.127(4) 0.227(3) 0.026(15) Uiso 1 1 d D . . H2W H -0.1020(19) 0.065(7) 0.219(4) 0.06(2) Uiso 1 1 d D . . C1 C 0.2143(4) -0.0140(5) 0.5366(3) 0.0202(9) Uani 1 1 d . . . H1A H 0.2527 0.0191 0.5911 0.024 Uiso 1 1 calc R . . C2 C 0.1278(4) -0.0970(6) 0.5344(3) 0.0233(10) Uani 1 1 d . A . H2A H 0.1056 -0.1222 0.5870 0.028 Uiso 1 1 calc R . . C3 C 0.0731(4) -0.1436(6) 0.4539(3) 0.0214(9) Uani 1 1 d . . . H3A H 0.0131 -0.2012 0.4529 0.026 Uiso 1 1 calc R A . N4 N 0.0997(3) -0.1123(5) 0.3782(2) 0.0189(8) Uani 1 1 d . A . C5 C 0.2125(3) 0.0139(6) 0.2975(3) 0.0201(9) Uani 1 1 d . A . H5A H 0.1710 -0.0180 0.2442 0.024 Uiso 1 1 calc R . . C6 C 0.2959(3) 0.0961(6) 0.2947(3) 0.0202(9) Uani 1 1 d . . . H6A H 0.3122 0.1223 0.2397 0.024 Uiso 1 1 calc R . . N7 N 0.4451(3) 0.2292(5) 0.3673(2) 0.0219(8) Uani 1 1 d . . . C8 C 0.5051(3) 0.2750(6) 0.4402(3) 0.0244(9) Uani 1 1 d . . . H8A H 0.5635 0.3328 0.4355 0.029 Uiso 1 1 calc R . . C9 C 0.4866(3) 0.2426(7) 0.5232(3) 0.0276(10) Uani 1 1 d . . . H9A H 0.5314 0.2781 0.5739 0.033 Uiso 1 1 calc R . . C10 C 0.4029(4) 0.1588(6) 0.5309(3) 0.0241(10) Uani 1 1 d . . . H10A H 0.3895 0.1344 0.5872 0.029 Uiso 1 1 calc R . . C11 C 0.3366(3) 0.1090(5) 0.4553(3) 0.0188(9) Uani 1 1 d . . . C12 C 0.2462(3) 0.0223(5) 0.4578(3) 0.0185(9) Uani 1 1 d . A . C13 C 0.1846(3) -0.0267(5) 0.3789(3) 0.0187(9) Uani 1 1 d . . . C14 C 0.3607(3) 0.1449(5) 0.3735(3) 0.0189(9) Uani 1 1 d . . . N1S N 0.2915(4) 0.5672(7) 0.4206(3) 0.0421(12) Uani 1 1 d . . . C2S C 0.2473(5) 0.5252(7) 0.4710(4) 0.0362(13) Uani 1 1 d . . . C3S C 0.1914(5) 0.4678(8) 0.5357(4) 0.0484(16) Uani 1 1 d . . . H3S1 H 0.2204 0.3641 0.5631 0.073 Uiso 1 1 calc R . . H3S2 H 0.1236 0.4461 0.5068 0.073 Uiso 1 1 calc R . . H3S3 H 0.1924 0.5545 0.5805 0.073 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 Cd1 0.01797(17) 0.02184(17) 0.01850(17) -0.00139(12) 0.00351(11) -0.00018(13) N10 0.025(2) 0.052(3) 0.034(2) 0.003(2) 0.0065(18) -0.009(2) O1 0.028(2) 0.066(3) 0.0269(18) -0.0036(18) 0.0075(15) -0.002(2) O2 0.053(3) 0.136(5) 0.036(2) -0.035(3) 0.019(2) -0.051(3) O3 0.024(2) 0.138(5) 0.063(3) 0.020(3) 0.006(2) -0.023(3) N20 0.026(2) 0.029(2) 0.031(2) -0.0021(17) 0.0081(18) -0.0076(18) O1W 0.029(2) 0.0244(19) 0.0345(19) -0.0026(14) 0.0082(16) 0.0025(16) C1 0.025(3) 0.018(2) 0.017(2) -0.0014(15) 0.0032(17) 0.0032(18) C2 0.028(3) 0.025(2) 0.019(2) 0.0013(17) 0.0079(18) -0.001(2) C3 0.022(2) 0.020(2) 0.023(2) -0.0013(16) 0.0061(18) -0.0012(18) N4 0.0158(19) 0.0207(19) 0.0208(18) -0.0002(14) 0.0049(14) 0.0001(15) C5 0.020(2) 0.023(2) 0.016(2) -0.0008(16) 0.0010(17) 0.0002(18) C6 0.020(2) 0.024(2) 0.017(2) 0.0008(16) 0.0042(17) -0.0009(18) N7 0.0208(19) 0.025(2) 0.0196(17) -0.0014(15) 0.0033(14) -0.0030(16) C8 0.019(2) 0.029(2) 0.025(2) -0.0031(18) 0.0024(17) 0.000(2) C9 0.023(2) 0.038(3) 0.020(2) -0.0052(19) -0.0004(17) -0.002(2) C10 0.027(3) 0.029(2) 0.017(2) -0.0009(17) 0.0032(18) 0.001(2) C11 0.019(2) 0.019(2) 0.017(2) 0.0001(15) 0.0024(17) 0.0015(17) C12 0.019(2) 0.017(2) 0.019(2) -0.0001(15) 0.0031(17) -0.0010(17) C13 0.020(2) 0.017(2) 0.019(2) -0.0005(15) 0.0019(17) 0.0015(17) C14 0.020(2) 0.019(2) 0.018(2) -0.0017(15) 0.0032(17) 0.0010(17) N1S 0.036(3) 0.053(3) 0.036(3) 0.001(2) 0.002(2) -0.004(2) C2S 0.043(4) 0.033(3) 0.028(3) 0.003(2) -0.004(2) 0.006(2) C3S 0.063(5) 0.047(4) 0.035(3) 0.013(3) 0.009(3) 0.001(3) _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 Cd1 N4 2.286(4) . y Cd1 N7 2.257(4) 2_545 y Cd1 O1W 2.354(4) . y Cd1 O1 2.394(4) . y Cd1 O2 2.408(5) . y Cd1 O4 2.295(9) . y Cd1 O4' 2.429(10) . y Cd1 O6' 2.629(9) . y N10 O3 1.231(6) . ? N10 O1 1.232(6) . ? N10 O2 1.249(6) . ? N20 O5' 1.221(6) . ? N20 O4 1.239(6) . ? N20 O6 1.243(6) . ? N20 O4' 1.260(6) . ? N20 O6' 1.276(6) . ? N20 O5 1.277(6) . ? C1 C2 1.368(7) . ? C1 C12 1.412(6) . ? C2 C3 1.387(6) . ? C3 N4 1.324(6) . ? N4 C13 1.362(6) . ? C5 C6 1.341(6) . ? C5 C13 1.431(6) . ? C6 C14 1.431(6) . ? N7 C8 1.325(6) . ? N7 C14 1.373(6) . ? N7 Cd1 2.257(4) 2 ? C8 C9 1.389(6) . ? C9 C10 1.368(7) . ? C10 C11 1.407(6) . ? C11 C14 1.407(6) . ? C11 C12 1.443(6) . ? C12 C13 1.412(6) . ? N1S C2S 1.136(7) . ? C2S C3S 1.459(9) . ? 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 N7 Cd1 N4 121.19(13) 2_545 . y N7 Cd1 O4 110.7(2) 2_545 . y N4 Cd1 O4 77.17(19) . . y N7 Cd1 O1W 88.20(13) 2_545 . y N4 Cd1 O1W 88.93(13) . . y O4 Cd1 O1W 160.4(2) . . y N7 Cd1 O1 143.44(13) 2_545 . y N4 Cd1 O1 94.31(13) . . y O4 Cd1 O1 83.7(3) . . y O1W Cd1 O1 83.67(14) . . y N7 Cd1 O2 91.21(14) 2_545 . y N4 Cd1 O2 144.86(15) . . y O4 Cd1 O2 105.5(3) . . y O1W Cd1 O2 78.07(18) . . y O1 Cd1 O2 52.24(13) . . y N7 Cd1 O4' 116.6(2) 2_545 . y N4 Cd1 O4' 79.0(2) . . y O4 Cd1 O4' 7.9(4) . . y O1W Cd1 O4' 155.2(2) . . y O1 Cd1 O4' 75.9(3) . . y O2 Cd1 O4' 99.5(3) . . y N7 Cd1 O6' 77.5(2) 2_545 . y N4 Cd1 O6' 123.38(17) . . y O4 Cd1 O6' 47.4(2) . . y O1W Cd1 O6' 147.59(17) . . y O1 Cd1 O6' 90.7(2) . . y O2 Cd1 O6' 73.4(2) . . y O4' Cd1 O6' 48.0(2) . . y O3 N10 O1 120.9(5) . . ? O3 N10 O2 122.2(5) . . ? O1 N10 O2 116.9(4) . . ? N10 O1 Cd1 95.9(3) . . ? N10 O2 Cd1 94.7(3) . . ? O5' N20 O4 131.3(7) . . ? O5' N20 O6 101.8(6) . . ? O4 N20 O6 121.9(6) . . ? O5' N20 O4' 125.2(7) . . ? O4 N20 O4' 16.1(7) . . ? O6 N20 O4' 132.6(7) . . ? O5' N20 O6' 123.1(6) . . ? O4 N20 O6' 105.6(6) . . ? O6 N20 O6' 32.9(5) . . ? O4' N20 O6' 109.0(6) . . ? O5' N20 O5 16.5(6) . . ? O4 N20 O5 116.7(6) . . ? O6 N20 O5 118.2(6) . . ? O4' N20 O5 109.0(7) . . ? O6' N20 O5 136.4(7) . . ? N20 O4 Cd1 112.8(5) . . ? N20 O4' Cd1 104.4(6) . . ? N20 O6' Cd1 94.0(4) . . ? C2 C1 C12 119.9(4) . . ? C1 C2 C3 118.8(4) . . ? N4 C3 C2 123.6(4) . . ? C3 N4 C13 118.5(4) . . ? C3 N4 Cd1 114.7(3) . . ? C13 N4 Cd1 126.6(3) . . ? C6 C5 C13 121.4(4) . . ? C5 C6 C14 120.9(4) . . ? C8 N7 C14 118.8(4) . . ? C8 N7 Cd1 116.4(3) . 2 ? C14 N7 Cd1 124.4(3) . 2 ? N7 C8 C9 123.2(4) . . ? C10 C9 C8 119.0(4) . . ? C9 C10 C11 119.9(4) . . ? C14 C11 C10 117.9(4) . . ? C14 C11 C12 118.8(4) . . ? C10 C11 C12 123.3(4) . . ? C1 C12 C13 117.4(4) . . ? C1 C12 C11 122.8(4) . . ? C13 C12 C11 119.8(4) . . ? N4 C13 C12 121.8(4) . . ? N4 C13 C5 119.2(4) . . ? C12 C13 C5 119.0(4) . . ? N7 C14 C11 121.3(4) . . ? N7 C14 C6 118.7(4) . . ? C11 C14 C6 120.0(4) . . ? N1S C2S C3S 178.8(7) . . ? _diffrn_measured_fraction_theta_max 0.903 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 1.40 _refine_diff_density_min -1.80 _refine_diff_density_rms 0.13 #======END data_4(PHENZN) _database_code_CSD 205824 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Zinc(II)-(4,7-phenanthroline)-bis-nitrate hydrate.acetonitrile ; _chemical_name_common [Zn(NO3)2(4,7-phen)(H2O)].MeCN _chemical_formula_moiety 'C12 H10 N4 O7 Zn, C2 H3 N' _chemical_formula_sum 'C14 H13 N5 O7 Zn' _chemical_formula_weight 428.66 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 '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 22.3308(11) _cell_length_b 7.8991(4) _cell_length_c 18.5781(9) _cell_angle_alpha 90.00 _cell_angle_beta 96.296(1) _cell_angle_gamma 90.00 _cell_volume 3257.3(3) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7018 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 27.9 _exptl_crystal_description 'block cut from lath' _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.748 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1744 _exptl_absorpt_coefficient_mu 1.561 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.921 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'SADABS version 2.03 (Bruker, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Bruker SMART1000 CCD area detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 29503 _diffrn_reflns_av_R_equivalents 0.033 _diffrn_reflns_av_sigmaI/netI 0.032 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 28.85 _reflns_number_total 8392 _reflns_number_gt 6045 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART version 5.624 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.02a (Bruker, 2000)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material 'SHELXL-97; PLATON (Spek, 2001)' _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 w==1/[\s^2^(Fo^2^)+(0.04P)^2^+2.884P] where P==(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'direct methods' _atom_sites_solution_secondary 'difference Fourier synthesis' _atom_sites_solution_hydrogens 'those on MeCN and H2O found from delta-F; others geometrically placed' _refine_ls_hydrogen_treatment ; MeCN treated as ridid rotor model; geometric restraints applied to H2O; others riding model ; _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7835 _refine_ls_number_parameters 505 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0536 _refine_ls_R_factor_gt 0.0341 _refine_ls_wR_factor_ref 0.0912 _refine_ls_wR_factor_gt 0.0791 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _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 Zn1 Zn 0.125106(11) 0.21461(3) 0.372791(13) 0.01542(8) Uani 1 1 d . . . Zn2 Zn 0.369982(11) 0.81047(3) 0.132378(13) 0.01492(7) Uani 1 1 d . . . N10 N 0.14344(9) 0.5949(2) 0.33743(11) 0.0214(4) Uani 1 1 d . . . O1 O 0.15466(8) 0.4404(2) 0.32326(9) 0.0244(4) Uani 1 1 d . . . O2 O 0.10411(8) 0.6295(2) 0.37729(10) 0.0321(4) Uani 1 1 d . . . O3 O 0.17207(9) 0.7070(2) 0.31005(11) 0.0352(5) Uani 1 1 d . . . N20 N 0.22073(9) 0.2814(3) 0.47004(11) 0.0219(4) Uani 1 1 d . . . O4 O 0.16480(7) 0.3095(2) 0.47310(10) 0.0269(4) Uani 1 1 d . . . O5 O 0.23428(9) 0.1943(2) 0.41817(10) 0.0319(4) Uani 1 1 d . . . O6 O 0.25785(8) 0.3407(3) 0.51668(11) 0.0393(5) Uani 1 1 d . . . N30 N 0.35207(9) 0.4423(3) 0.14802(11) 0.0241(4) Uani 1 1 d . . . O7 O 0.35343(8) 0.5750(2) 0.18536(9) 0.0213(4) Uani 1 1 d . . . O8 O 0.35512(11) 0.4549(3) 0.08161(11) 0.0451(6) Uani 1 1 d . . . O9 O 0.34428(10) 0.3034(2) 0.17769(11) 0.0346(5) Uani 1 1 d . . . N40 N 0.27220(9) 0.7753(3) 0.02590(11) 0.0244(5) Uani 1 1 d . . . O10 O 0.28013(8) 0.7911(2) 0.09463(9) 0.0241(4) Uani 1 1 d . . . O11 O 0.31591(9) 0.7944(3) -0.00926(11) 0.0399(5) Uani 1 1 d . . . O12 O 0.22119(9) 0.7480(3) -0.00372(11) 0.0379(5) Uani 1 1 d . . . O1W O 0.12947(8) -0.0319(2) 0.42231(9) 0.0211(4) Uani 1 1 d D . . H1W H 0.1210(13) -0.120(3) 0.3988(15) 0.048(10) Uiso 1 1 d D . . H2W H 0.1626(8) -0.053(4) 0.4463(14) 0.039(9) Uiso 1 1 d D . . O2W O 0.37247(8) 1.0550(2) 0.08557(9) 0.0205(3) Uani 1 1 d D . . H3W H 0.3467(11) 1.068(4) 0.0494(10) 0.042(9) Uiso 1 1 d D . . H4W H 0.3650(13) 1.133(3) 0.1143(12) 0.047(10) Uiso 1 1 d D . . C1 C -0.06513(10) 0.3459(3) 0.46116(12) 0.0189(5) Uani 1 1 d . . . H1A H -0.1007 0.3746 0.4821 0.023 Uiso 1 1 calc R . . C2 C -0.01892(11) 0.2617(3) 0.50133(12) 0.0211(5) Uani 1 1 d . . . H2A H -0.0222 0.2311 0.5502 0.025 Uiso 1 1 calc R . . C3 C 0.03274(11) 0.2220(3) 0.46912(12) 0.0196(5) Uani 1 1 d . . . H3A H 0.0642 0.1624 0.4970 0.023 Uiso 1 1 calc R . . N4 N 0.04032(8) 0.2635(2) 0.40117(10) 0.0160(4) Uani 1 1 d . . . C5 C 0.00309(10) 0.3919(3) 0.28747(12) 0.0172(4) Uani 1 1 d . . . H5A H 0.0394 0.3615 0.2685 0.021 Uiso 1 1 calc R . . C6 C -0.04006(10) 0.4765(3) 0.24511(12) 0.0164(4) Uani 1 1 d . . . H6A H -0.0335 0.5056 0.1970 0.020 Uiso 1 1 calc R . . N7 N -0.13753(8) 0.6109(2) 0.22727(10) 0.0154(4) Uani 1 1 d . . . C8 C -0.19038(10) 0.6468(3) 0.25126(12) 0.0178(5) Uani 1 1 d . . . H8A H -0.2196 0.7070 0.2202 0.021 Uiso 1 1 calc R . . C9 C -0.20457(10) 0.6000(3) 0.31959(12) 0.0190(5) Uani 1 1 d . . . H9A H -0.2431 0.6251 0.3340 0.023 Uiso 1 1 calc R . . C10 C -0.16225(10) 0.5173(3) 0.36590(12) 0.0184(5) Uani 1 1 d . . . H10A H -0.1708 0.4877 0.4133 0.022 Uiso 1 1 calc R . . C11 C -0.10625(10) 0.4768(3) 0.34285(12) 0.0160(4) Uani 1 1 d . . . C12 C -0.05918(10) 0.3893(3) 0.38882(11) 0.0154(4) Uani 1 1 d . . . C13 C -0.00497(10) 0.3477(3) 0.36037(12) 0.0158(4) Uani 1 1 d . . . C14 C -0.09558(10) 0.5226(3) 0.27184(12) 0.0152(4) Uani 1 1 d . . . C21 C 0.34687(10) 0.9860(3) 0.37830(12) 0.0182(5) Uani 1 1 d . . . H21A H 0.3409 1.0110 0.4270 0.022 Uiso 1 1 calc R . . C22 C 0.30307(10) 0.9030(3) 0.33429(12) 0.0193(5) Uani 1 1 d . . . H22A H 0.2661 0.8725 0.3517 0.023 Uiso 1 1 calc R . . C23 C 0.31352(10) 0.8641(3) 0.26374(12) 0.0183(5) Uani 1 1 d . . . H23A H 0.2832 0.8047 0.2340 0.022 Uiso 1 1 calc R . . N24 N 0.36415(8) 0.9061(2) 0.23574(10) 0.0152(4) Uani 1 1 d . . . C25 C 0.46152(10) 1.0412(3) 0.24860(12) 0.0159(4) Uani 1 1 d . . . H25A H 0.4657 1.0154 0.1995 0.019 Uiso 1 1 calc R . . C26 C 0.50650(10) 1.1235(3) 0.28921(12) 0.0167(4) Uani 1 1 d . . . H26A H 0.5418 1.1541 0.2681 0.020 Uiso 1 1 calc R . . N27 N 0.54830(8) 1.2491(2) 0.40231(10) 0.0169(4) Uani 1 1 d . . . C28 C 0.54238(11) 1.2917(3) 0.47078(12) 0.0204(5) Uani 1 1 d . . . H28A H 0.5747 1.3498 0.4978 0.024 Uiso 1 1 calc R . . C29 C 0.49128(11) 1.2551(3) 0.50453(13) 0.0221(5) Uani 1 1 d . . . H29A H 0.4889 1.2887 0.5532 0.026 Uiso 1 1 calc R . . C30 C 0.44458(11) 1.1704(3) 0.46676(12) 0.0205(5) Uani 1 1 d . . . H30A H 0.4095 1.1438 0.4892 0.025 Uiso 1 1 calc R . . C31 C 0.44869(10) 1.1225(3) 0.39452(12) 0.0159(4) Uani 1 1 d . . . C32 C 0.40061(10) 1.0338(3) 0.35104(12) 0.0155(4) Uani 1 1 d . . . C33 C 0.40778(10) 0.9925(3) 0.27860(12) 0.0148(4) Uani 1 1 d . . . C34 C 0.50172(10) 1.1653(3) 0.36337(12) 0.0156(4) Uani 1 1 d . . . N1S N 0.07014(11) 0.4270(3) 0.13859(12) 0.0361(6) Uani 1 1 d . . . C1S C 0.11874(13) 0.4717(3) 0.14137(14) 0.0284(6) Uani 1 1 d . . . C2S C 0.18097(13) 0.5305(4) 0.14373(17) 0.0404(7) Uani 1 1 d . . . H2S1 H 0.1821 0.6355 0.1158 0.061 Uiso 1 1 calc R . . H2S2 H 0.2053 0.4439 0.1229 0.061 Uiso 1 1 calc R . . H2S3 H 0.1972 0.5517 0.1941 0.061 Uiso 1 1 calc R . . N1T N 0.57129(11) 1.0686(3) 0.14054(12) 0.0348(6) Uani 1 1 d . . . C1T C 0.61919(12) 1.0193(3) 0.14662(13) 0.0252(5) Uani 1 1 d . . . C2T C 0.68044(13) 0.9525(4) 0.15448(16) 0.0343(6) Uani 1 1 d . . . H2T1 H 0.6921 0.9218 0.2052 0.051 Uiso 1 1 calc R . . H2T2 H 0.7081 1.0389 0.1397 0.051 Uiso 1 1 calc R . . H2T3 H 0.6823 0.8520 0.1239 0.051 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 Zn1 0.01428(13) 0.01717(14) 0.01454(14) -0.00170(10) 0.00042(10) 0.00002(10) Zn2 0.01379(13) 0.01601(13) 0.01473(13) -0.00005(10) 0.00059(10) -0.00020(10) N10 0.0226(10) 0.0197(10) 0.0210(10) -0.0037(8) -0.0012(8) -0.0002(8) O1 0.0307(10) 0.0142(8) 0.0298(9) -0.0004(7) 0.0093(8) -0.0001(7) O2 0.0292(10) 0.0325(10) 0.0357(10) -0.0114(8) 0.0090(8) 0.0040(8) O3 0.0441(12) 0.0201(9) 0.0417(11) 0.0036(8) 0.0065(9) -0.0100(8) N20 0.0196(10) 0.0250(11) 0.0204(10) -0.0016(8) -0.0005(8) -0.0046(8) O4 0.0160(8) 0.0349(10) 0.0297(10) -0.0069(8) 0.0018(7) -0.0016(7) O5 0.0368(11) 0.0277(10) 0.0338(10) -0.0088(8) 0.0155(9) -0.0026(8) O6 0.0244(10) 0.0578(14) 0.0332(11) -0.0082(10) -0.0088(8) -0.0113(9) N30 0.0265(11) 0.0212(10) 0.0256(11) -0.0057(9) 0.0081(9) -0.0023(9) O7 0.0276(9) 0.0155(8) 0.0211(8) -0.0023(7) 0.0042(7) -0.0001(7) O8 0.0774(16) 0.0317(11) 0.0303(11) -0.0052(9) 0.0237(11) -0.0058(11) O9 0.0541(13) 0.0152(9) 0.0353(11) 0.0007(8) 0.0087(9) -0.0024(8) N40 0.0209(11) 0.0256(11) 0.0258(11) -0.0053(9) -0.0013(9) -0.0023(8) O10 0.0231(9) 0.0305(10) 0.0178(8) 0.0008(7) -0.0020(7) -0.0047(7) O11 0.0332(11) 0.0519(13) 0.0368(11) -0.0144(10) 0.0144(9) -0.0062(9) O12 0.0281(10) 0.0485(12) 0.0335(11) -0.0054(9) -0.0132(9) -0.0098(9) O1W 0.0226(9) 0.0171(8) 0.0226(9) 0.0007(7) -0.0019(7) 0.0014(7) O2W 0.0227(9) 0.0170(8) 0.0212(9) 0.0010(7) 0.0001(7) 0.0021(7) C1 0.0151(11) 0.0241(12) 0.0179(11) -0.0001(9) 0.0038(9) 0.0009(9) C2 0.0217(12) 0.0270(12) 0.0145(11) 0.0049(9) 0.0021(9) 0.0000(10) C3 0.0193(12) 0.0231(12) 0.0160(11) 0.0021(9) 0.0006(9) 0.0012(9) N4 0.0155(9) 0.0170(9) 0.0154(9) 0.0006(7) 0.0013(7) 0.0008(7) C5 0.0159(11) 0.0201(11) 0.0159(11) 0.0003(9) 0.0030(9) 0.0002(9) C6 0.0179(11) 0.0181(11) 0.0139(10) 0.0019(8) 0.0041(9) 0.0005(9) N7 0.0156(9) 0.0148(9) 0.0157(9) 0.0001(7) 0.0017(7) -0.0011(7) C8 0.0144(11) 0.0172(11) 0.0213(11) 0.0020(9) -0.0002(9) 0.0014(8) C9 0.0150(11) 0.0196(11) 0.0234(12) -0.0003(9) 0.0063(9) -0.0004(9) C10 0.0184(11) 0.0195(11) 0.0179(11) 0.0003(9) 0.0047(9) -0.0006(9) C11 0.0158(11) 0.0147(10) 0.0175(11) -0.0020(9) 0.0011(9) -0.0006(8) C12 0.0161(11) 0.0150(10) 0.0152(10) -0.0005(8) 0.0018(8) -0.0007(8) C13 0.0163(11) 0.0145(10) 0.0164(10) 0.0006(8) 0.0004(9) 0.0009(8) C14 0.0155(11) 0.0146(10) 0.0152(11) -0.0003(8) 0.0004(8) -0.0006(8) C21 0.0212(12) 0.0177(11) 0.0163(11) -0.0001(9) 0.0046(9) 0.0000(9) C22 0.0182(11) 0.0192(11) 0.0211(11) -0.0009(9) 0.0047(9) -0.0013(9) C23 0.0156(11) 0.0166(11) 0.0225(12) -0.0008(9) 0.0007(9) -0.0007(9) N24 0.0137(9) 0.0143(9) 0.0177(9) 0.0002(7) 0.0020(7) 0.0003(7) C25 0.0169(11) 0.0175(11) 0.0133(10) -0.0009(8) 0.0023(9) -0.0005(9) C26 0.0142(11) 0.0189(11) 0.0173(11) 0.0007(9) 0.0034(9) -0.0013(9) N27 0.0163(9) 0.0185(9) 0.0157(9) -0.0013(7) 0.0017(7) -0.0022(7) C28 0.0227(12) 0.0200(12) 0.0179(11) -0.0032(9) 0.0001(9) -0.0040(9) C29 0.0234(12) 0.0280(13) 0.0155(11) -0.0048(10) 0.0049(9) -0.0034(10) C30 0.0211(12) 0.0231(12) 0.0182(11) -0.0013(9) 0.0061(9) -0.0049(9) C31 0.0175(11) 0.0152(10) 0.0152(10) -0.0003(8) 0.0030(9) 0.0013(8) C32 0.0164(11) 0.0132(10) 0.0167(11) -0.0002(8) 0.0016(9) 0.0006(8) C33 0.0148(10) 0.0132(10) 0.0162(11) 0.0010(8) 0.0008(9) 0.0005(8) C34 0.0172(11) 0.0144(10) 0.0150(10) 0.0003(8) 0.0001(9) -0.0004(8) N1S 0.0355(14) 0.0455(15) 0.0274(12) -0.0003(11) 0.0036(10) -0.0026(11) C1S 0.0395(16) 0.0253(13) 0.0207(13) 0.0009(10) 0.0049(11) 0.0029(11) C2S 0.0373(17) 0.0376(17) 0.0467(18) 0.0084(14) 0.0068(14) -0.0089(13) N1T 0.0325(13) 0.0496(15) 0.0223(11) 0.0043(11) 0.0028(10) 0.0021(11) C1T 0.0324(15) 0.0249(13) 0.0186(12) 0.0013(10) 0.0039(11) -0.0030(11) C2T 0.0365(16) 0.0324(15) 0.0355(15) -0.0037(12) 0.0107(13) 0.0077(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 Zn1 N4 2.0569(18) . y Zn1 N7 2.0777(18) 2_545 y Zn1 O4 2.1115(17) . y Zn1 O1 2.1437(16) . y Zn1 O1W 2.1509(17) . y Zn2 O10 2.0573(17) . y Zn2 N27 2.0587(19) 2_645 y Zn2 N24 2.0810(18) . y Zn2 O2W 2.1216(17) . y Zn2 O7 2.1550(16) . y N10 O3 1.234(3) . ? N10 O2 1.240(3) . ? N10 O1 1.279(2) . ? N20 O6 1.225(3) . ? N20 O5 1.248(3) . ? N20 O4 1.276(3) . ? N30 O8 1.247(3) . ? N30 O9 1.249(3) . ? N30 O7 1.256(2) . ? N40 O12 1.228(3) . ? N40 O11 1.242(3) . ? N40 O10 1.276(3) . ? C1 C2 1.377(3) . ? C1 C12 1.407(3) . ? C2 C3 1.392(3) . ? C3 N4 1.333(3) . ? N4 C13 1.368(3) . ? C5 C6 1.352(3) . ? C5 C13 1.429(3) . ? C6 C14 1.432(3) . ? N7 C8 1.337(3) . ? N7 C14 1.371(3) . ? N7 Zn1 2.0777(18) 2 ? C8 C9 1.392(3) . ? C9 C10 1.372(3) . ? C10 C11 1.403(3) . ? C11 C14 1.413(3) . ? C11 C12 1.454(3) . ? C12 C13 1.412(3) . ? C21 C22 1.371(3) . ? C21 C32 1.404(3) . ? C22 C23 1.391(3) . ? C23 N24 1.337(3) . ? N24 C33 1.370(3) . ? C25 C26 1.355(3) . ? C25 C33 1.430(3) . ? C26 C34 1.432(3) . ? N27 C28 1.336(3) . ? N27 C34 1.371(3) . ? N27 Zn2 2.0587(19) 2_655 ? C28 C29 1.391(3) . ? C29 C30 1.367(3) . ? C30 C31 1.407(3) . ? C31 C34 1.415(3) . ? C31 C32 1.451(3) . ? C32 C33 1.411(3) . ? N1S C1S 1.137(4) . ? C1S C2S 1.461(4) . ? N1T C1T 1.132(3) . ? C1T C2T 1.458(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 N4 Zn1 N7 121.36(7) . 2_545 y N4 Zn1 O4 90.92(7) . . y N7 Zn1 O4 147.71(7) 2_545 . y N4 Zn1 O1 106.81(7) . . y N7 Zn1 O1 82.32(7) 2_545 . y O4 Zn1 O1 87.95(7) . . y N4 Zn1 O1W 93.45(7) . . y N7 Zn1 O1W 91.23(7) 2_545 . y O4 Zn1 O1W 87.08(7) . . y O1 Zn1 O1W 159.21(7) . . y O10 Zn2 N27 137.79(7) . 2_645 y O10 Zn2 N24 100.61(7) . . y N27 Zn2 N24 121.45(7) 2_645 . y O10 Zn2 O2W 89.78(7) . . y N27 Zn2 O2W 91.27(7) 2_645 . y N24 Zn2 O2W 93.13(7) . . y O10 Zn2 O7 83.22(7) . . y N27 Zn2 O7 98.17(7) 2_645 . y N24 Zn2 O7 81.99(7) . . y O2W Zn2 O7 170.56(7) . . y O3 N10 O2 121.4(2) . . ? O3 N10 O1 118.6(2) . . ? O2 N10 O1 120.1(2) . . ? N10 O1 Zn1 128.97(14) . . ? O6 N20 O5 123.7(2) . . ? O6 N20 O4 119.5(2) . . ? O5 N20 O4 116.9(2) . . ? N20 O4 Zn1 102.53(13) . . ? O8 N30 O9 122.2(2) . . ? O8 N30 O7 118.6(2) . . ? O9 N30 O7 119.1(2) . . ? N30 O7 Zn2 117.59(14) . . ? O12 N40 O11 122.0(2) . . ? O12 N40 O10 119.1(2) . . ? O11 N40 O10 118.9(2) . . ? N40 O10 Zn2 111.82(14) . . ? C2 C1 C12 119.4(2) . . ? C1 C2 C3 118.9(2) . . ? N4 C3 C2 123.3(2) . . ? C3 N4 C13 118.77(19) . . ? C3 N4 Zn1 114.38(15) . . ? C13 N4 Zn1 126.48(15) . . ? C6 C5 C13 121.1(2) . . ? C5 C6 C14 120.8(2) . . ? C8 N7 C14 118.43(19) . . ? C8 N7 Zn1 115.09(15) . 2 ? C14 N7 Zn1 126.27(14) . 2 ? N7 C8 C9 123.1(2) . . ? C10 C9 C8 119.2(2) . . ? C9 C10 C11 119.5(2) . . ? C10 C11 C14 118.3(2) . . ? C10 C11 C12 122.7(2) . . ? C14 C11 C12 119.00(19) . . ? C1 C12 C13 118.4(2) . . ? C1 C12 C11 122.6(2) . . ? C13 C12 C11 119.01(19) . . ? N4 C13 C12 121.2(2) . . ? N4 C13 C5 118.80(19) . . ? C12 C13 C5 120.0(2) . . ? N7 C14 C11 121.34(19) . . ? N7 C14 C6 118.68(19) . . ? C11 C14 C6 120.0(2) . . ? C22 C21 C32 119.7(2) . . ? C21 C22 C23 119.0(2) . . ? N24 C23 C22 123.2(2) . . ? C23 N24 C33 118.37(19) . . ? C23 N24 Zn2 114.19(15) . . ? C33 N24 Zn2 127.18(14) . . ? C26 C25 C33 121.0(2) . . ? C25 C26 C34 121.2(2) . . ? C28 N27 C34 118.38(19) . . ? C28 N27 Zn2 114.99(15) . 2_655 ? C34 N27 Zn2 126.58(15) . 2_655 ? N27 C28 C29 123.3(2) . . ? C30 C29 C28 119.2(2) . . ? C29 C30 C31 119.7(2) . . ? C30 C31 C34 118.1(2) . . ? C30 C31 C32 122.6(2) . . ? C34 C31 C32 119.28(19) . . ? C21 C32 C33 118.2(2) . . ? C21 C32 C31 122.6(2) . . ? C33 C32 C31 119.21(19) . . ? N24 C33 C32 121.43(19) . . ? N24 C33 C25 118.74(19) . . ? C32 C33 C25 119.8(2) . . ? N27 C34 C31 121.4(2) . . ? N27 C34 C26 119.12(19) . . ? C31 C34 C26 119.5(2) . . ? N1S C1S C2S 179.0(3) . . ? N1T C1T C2T 178.9(3) . . ? _diffrn_measured_fraction_theta_max 0.917 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.04 _refine_diff_density_min -0.43 _refine_diff_density_rms 0.08 #======END data_5(NIPHEN) _database_code_CSD 205825 _refine_special_details ; The free 4,7-phenanthroline shows high ADPs and part of it has been modelled over two sets of sites with the occupancy ratio 55:45. The chains of solvent molecules running through channels in the structure do not model convincingly as dichloromethane, as the bond lenghs and peak height ratios are not ideal. Instead they been modelled as two sets of water molecules, (O2W + O2WA) and (O3W and O3WA): hydrogen atoms in this region were not located. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; Aquabis(nitrato)(4,7-phenanthroline)nickel(II) 4,7-phenanthroline water 1/1/0.9 ; _chemical_name_common [Ni(NO3)2(H2O)(4,7-phen)].(4,7-phen) _chemical_formula_moiety 'C12 H10 N4 Ni O7, C12 H8 N2, 0.9(H2 O)' _chemical_formula_sum 'C24 H19.80 N6 Ni O7.90' _chemical_formula_weight 577.37 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/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 15.3438(13) _cell_length_b 7.9690(7) _cell_length_c 21.943(2) _cell_angle_alpha 90.00 _cell_angle_beta 110.107(2) _cell_angle_gamma 90.00 _cell_volume 2519.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1844 _cell_measurement_theta_min 2.75 _cell_measurement_theta_max 25.0 _exptl_crystal_description lath _exptl_crystal_colour 'pale green' _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.522 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1188 _exptl_absorpt_coefficient_mu 0.831 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.896 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'SADABS version 2.03 (Bruker, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Bruker SMART1000 CCD area detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 12631 _diffrn_reflns_av_R_equivalents 0.049 _diffrn_reflns_av_sigmaI/netI 0.078 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.74 _diffrn_reflns_theta_max 28.81 _reflns_number_total 6217 _reflns_number_gt 3615 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART version 5.624 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.02a (Bruker, 2000)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'SHELXL-97; PLATON (Spek, 2001)' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w==1/[\s^2^(Fo^2^)+(0.064P)^2^+2.416P] where P==(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'Patterson map' _atom_sites_solution_secondary 'difference Fourier synthesis' _atom_sites_solution_hydrogens 'those on water molecule, found from delta-F; others placed geometrically' _refine_ls_hydrogen_treatment 'geometric restraints applied to water; others riding' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5816 _refine_ls_number_parameters 363 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.106 _refine_ls_R_factor_gt 0.0530 _refine_ls_wR_factor_ref 0.149 _refine_ls_wR_factor_gt 0.121 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.002 _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 Ni1 Ni 0.67281(3) 0.84624(6) 0.67680(2) 0.01972(15) Uani 1 1 d . . . N10 N 0.7908(3) 0.8803(5) 0.62203(17) 0.0355(9) Uani 1 1 d . . . O1 O 0.81394(19) 0.8235(4) 0.67920(14) 0.0350(7) Uani 1 1 d . . . O2 O 0.70555(18) 0.9187(4) 0.59571(13) 0.0288(7) Uani 1 1 d . . . O3 O 0.8457(2) 0.8962(6) 0.59290(17) 0.0623(11) Uani 1 1 d . . . N20 N 0.6817(2) 1.2171(4) 0.69350(16) 0.0289(8) Uani 1 1 d . . . O4 O 0.70699(19) 1.0748(3) 0.72217(13) 0.0267(6) Uani 1 1 d . . . O5 O 0.6288(2) 1.2238(4) 0.63697(13) 0.0351(7) Uani 1 1 d . . . O6 O 0.7127(3) 1.3459(4) 0.72535(16) 0.0605(11) Uani 1 1 d . . . O10 O 0.6487(2) 0.6086(4) 0.64003(14) 0.0290(7) Uani 1 1 d D . . H11W H 0.651(4) 0.582(6) 0.6035(11) 0.073(19) Uiso 1 1 d D . . H12W H 0.675(3) 0.529(5) 0.6646(19) 0.069(19) Uiso 1 1 d D . . C1 C 0.7769(3) 0.6419(5) 0.89972(19) 0.0283(9) Uani 1 1 d . . . H1A H 0.8018 0.6049 0.9435 0.034 Uiso 1 1 calc R . . C2 C 0.8308(3) 0.7340(5) 0.87330(19) 0.0287(9) Uani 1 1 d . . . H2A H 0.8935 0.7600 0.8980 0.034 Uiso 1 1 calc R . . C3 C 0.7911(3) 0.7883(5) 0.80909(19) 0.0260(9) Uani 1 1 d . . . H3A H 0.8283 0.8540 0.7914 0.031 Uiso 1 1 calc R . . N4 N 0.7045(2) 0.7542(4) 0.77110(14) 0.0208(7) Uani 1 1 d . . . C5 C 0.5584(2) 0.6179(5) 0.75709(17) 0.0197(8) Uani 1 1 d . . . H5A H 0.5362 0.6529 0.7130 0.024 Uiso 1 1 calc R . . C6 C 0.5019(3) 0.5302(5) 0.78112(17) 0.0216(8) Uani 1 1 d . . . H6A H 0.4409 0.5029 0.7533 0.026 Uiso 1 1 calc R . . N7 N 0.4699(2) 0.3949(4) 0.86888(14) 0.0205(7) Uani 1 1 d . . . C8 C 0.4979(3) 0.3504(5) 0.93151(17) 0.0227(8) Uani 1 1 d . . . H8A H 0.4552 0.2940 0.9471 0.027 Uiso 1 1 calc R . . C9 C 0.5869(3) 0.3830(5) 0.97507(18) 0.0235(8) Uani 1 1 d . . . H9A H 0.6036 0.3497 1.0192 0.028 Uiso 1 1 calc R . . C10 C 0.6500(3) 0.4634(5) 0.95368(17) 0.0235(8) Uani 1 1 d . . . H10A H 0.7109 0.4860 0.9827 0.028 Uiso 1 1 calc R . . C11 C 0.6514(3) 0.6584(5) 0.79748(17) 0.0210(8) Uani 1 1 d . . . C12 C 0.6850(3) 0.6026(5) 0.86185(18) 0.0227(8) Uani 1 1 d . . . C13 C 0.6235(3) 0.5120(5) 0.88823(17) 0.0206(8) Uani 1 1 d . . . C14 C 0.5319(3) 0.4780(5) 0.84722(17) 0.0194(8) Uani 1 1 d . . . C21 C 0.3446(3) 0.9715(5) 1.10891(19) 0.0292(9) Uani 1 1 d . . . H21A H 0.3430 0.9464 1.1509 0.035 Uiso 1 1 calc R . . C22 C 0.4209(3) 1.0481(5) 1.10242(19) 0.0281(9) Uani 1 1 d . . . H22A H 0.4722 1.0787 1.1396 0.034 Uiso 1 1 calc R . . C23 C 0.4218(3) 1.0801(5) 1.0403(2) 0.0287(9) Uani 1 1 d . . . H23A H 0.4756 1.1305 1.0363 0.034 Uiso 1 1 calc R . . N24 N 0.3521(2) 1.0445(5) 0.98631(16) 0.0316(8) Uani 1 1 d . A . C25 C 0.2063(5) 0.9008(13) 0.9343(4) 0.027(2) Uiso 0.560(14) 1 d P A 1 H25A H 0.2158 0.9109 0.8939 0.033 Uiso 0.560(14) 1 calc PR A 1 C26 C 0.1297(6) 0.8234(13) 0.9367(4) 0.032(2) Uiso 0.560(14) 1 d P A 1 H26A H 0.0820 0.7938 0.8973 0.039 Uiso 0.560(14) 1 calc PR A 1 N27 N 0.0378(5) 0.7025(13) 0.9963(4) 0.039(2) Uiso 0.560(14) 1 d P A 1 C28 C 0.0297(7) 0.6671(16) 1.0530(5) 0.041(2) Uiso 0.560(14) 1 d P A 1 H28A H -0.0210 0.5994 1.0536 0.049 Uiso 0.560(14) 1 calc PR A 1 C25' C 0.1939(8) 0.9702(18) 0.9351(5) 0.034(3) Uiso 0.440(14) 1 d P A 2 H25B H 0.1957 1.0165 0.8956 0.041 Uiso 0.440(14) 1 calc PR A 2 C26' C 0.1144(9) 0.902(2) 0.9388(6) 0.045(3) Uiso 0.440(14) 1 d P A 2 H26B H 0.0618 0.8908 0.9004 0.054 Uiso 0.440(14) 1 calc PR A 2 N27' N 0.0261(7) 0.7804(17) 0.9964(5) 0.038(3) Uiso 0.440(14) 1 d P A 2 C28' C 0.0179(8) 0.7329(19) 1.0511(6) 0.036(3) Uiso 0.440(14) 1 d P A 2 H28B H -0.0421 0.7012 1.0503 0.043 Uiso 0.440(14) 1 calc PR A 2 C29 C 0.0921(3) 0.7246(8) 1.1121(2) 0.0518(14) Uani 1 1 d . . . H29A H 0.0783 0.7098 1.1507 0.062 Uiso 1 1 calc R A 1 C30 C 0.1726(3) 0.8015(6) 1.1147(2) 0.0374(11) Uani 1 1 d . A . H30A H 0.2193 0.8236 1.1554 0.045 Uiso 1 1 calc R . . C31 C 0.2750(3) 0.9695(6) 0.99269(19) 0.0324(10) Uani 1 1 d . . . C32 C 0.2688(3) 0.9303(5) 1.05352(18) 0.0256(9) Uani 1 1 d . A . C33 C 0.1858(3) 0.8482(6) 1.0566(2) 0.0324(10) Uani 1 1 d . . . C34 C 0.1185(6) 0.7838(15) 0.9988(4) 0.033(2) Uiso 0.560(14) 1 d P A 1 C34' C 0.1085(8) 0.8491(18) 0.9984(5) 0.033(3) Uiso 0.440(14) 1 d P A 2 O1W O 1.0549(12) 0.757(3) 0.7708(9) 0.073(5) Uiso 0.25 1 d P B 1 O2W O 1.0194(13) 1.021(3) 0.7591(9) 0.079(5) Uiso 0.25 1 d P C 1 O1WA O 1.0267(15) 0.658(3) 0.7609(10) 0.063(5) Uiso 0.20 1 d P D 2 O2WA O 1.0381(14) 0.915(3) 0.7634(10) 0.059(5) Uiso 0.20 1 d P E 2 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 Ni1 0.0236(3) 0.0197(3) 0.0175(2) 0.0021(2) 0.00927(19) 0.0019(2) N10 0.035(2) 0.047(3) 0.031(2) 0.0064(17) 0.0187(17) 0.0040(18) O1 0.0290(15) 0.049(2) 0.0282(15) 0.0097(14) 0.0116(13) 0.0073(14) O2 0.0286(15) 0.0356(17) 0.0249(14) 0.0089(13) 0.0128(13) 0.0051(13) O3 0.046(2) 0.105(3) 0.053(2) 0.012(2) 0.0395(19) 0.006(2) N20 0.037(2) 0.0197(18) 0.0280(19) 0.0018(14) 0.0086(17) -0.0016(16) O4 0.0339(15) 0.0176(15) 0.0257(14) 0.0041(12) 0.0064(12) 0.0024(12) O5 0.0451(18) 0.0310(17) 0.0200(14) 0.0030(13) -0.0007(13) 0.0035(14) O6 0.100(3) 0.0206(18) 0.0355(19) -0.0044(15) -0.0087(19) -0.0079(19) O10 0.0432(18) 0.0235(16) 0.0228(15) -0.0003(12) 0.0145(14) 0.0068(13) C1 0.025(2) 0.037(3) 0.0208(19) 0.0050(18) 0.0050(16) 0.0017(19) C2 0.025(2) 0.034(2) 0.026(2) 0.0018(18) 0.0065(17) -0.0037(18) C3 0.026(2) 0.029(2) 0.024(2) 0.0020(17) 0.0094(17) -0.0037(17) N4 0.0226(16) 0.0216(18) 0.0197(16) 0.0019(13) 0.0092(14) -0.0012(13) C5 0.0246(19) 0.020(2) 0.0133(17) -0.0001(14) 0.0045(15) -0.0003(15) C6 0.025(2) 0.024(2) 0.0146(17) -0.0006(15) 0.0061(15) -0.0014(16) N7 0.0246(16) 0.0205(17) 0.0176(15) -0.0015(12) 0.0089(13) -0.0019(13) C8 0.030(2) 0.022(2) 0.0197(18) 0.0002(17) 0.0126(16) -0.0003(17) C9 0.033(2) 0.023(2) 0.0153(18) 0.0010(15) 0.0081(16) -0.0004(17) C10 0.027(2) 0.025(2) 0.0170(18) 0.0004(16) 0.0057(16) -0.0014(17) C11 0.0266(19) 0.0176(19) 0.0213(18) -0.0016(16) 0.0116(16) 0.0012(16) C12 0.027(2) 0.022(2) 0.0191(18) -0.0014(15) 0.0079(16) 0.0006(16) C13 0.024(2) 0.019(2) 0.0193(18) -0.0024(15) 0.0080(16) -0.0014(15) C14 0.025(2) 0.0158(19) 0.0196(18) -0.0007(15) 0.0107(16) -0.0004(15) C21 0.037(2) 0.031(2) 0.0186(19) 0.0030(17) 0.0076(18) 0.0041(19) C22 0.032(2) 0.028(2) 0.021(2) 0.0015(17) 0.0046(17) 0.0009(18) C23 0.032(2) 0.024(2) 0.029(2) 0.0019(18) 0.0100(19) -0.0019(18) N24 0.034(2) 0.038(2) 0.0245(18) 0.0040(16) 0.0123(16) -0.0026(17) C29 0.045(3) 0.080(4) 0.038(3) 0.002(3) 0.025(2) -0.010(3) C30 0.037(3) 0.050(3) 0.027(2) -0.002(2) 0.013(2) -0.006(2) C31 0.027(2) 0.051(3) 0.019(2) -0.0015(19) 0.0075(17) -0.001(2) C32 0.026(2) 0.030(2) 0.0214(19) 0.0004(17) 0.0089(17) 0.0040(18) C33 0.027(2) 0.046(3) 0.027(2) -0.002(2) 0.0120(18) -0.002(2) _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 Ni1 O10 2.042(3) . y Ni1 O4 2.055(3) . y Ni1 N4 2.089(3) . y Ni1 O2 2.090(3) . y Ni1 N7 2.107(3) 2_656 y Ni1 O1 2.156(3) . y N10 O3 1.227(4) . ? N10 O1 1.264(4) . ? N10 O2 1.272(4) . ? N20 O5 1.228(4) . ? N20 O6 1.241(4) . ? N20 O4 1.290(4) . ? C1 C2 1.374(5) . ? C1 C12 1.404(5) . ? C2 C3 1.398(5) . ? C3 N4 1.331(5) . ? N4 C11 1.380(5) . ? C5 C6 1.354(5) . ? C5 C11 1.434(5) . ? C6 C14 1.425(5) . ? N7 C8 1.339(5) . ? N7 C14 1.372(4) . ? N7 Ni1 2.107(3) 2_646 ? C8 C9 1.395(5) . ? C9 C10 1.372(5) . ? C10 C13 1.406(5) . ? C11 C12 1.399(5) . ? C12 C13 1.458(5) . ? C13 C14 1.410(5) . ? C21 C22 1.371(6) . ? C21 C32 1.402(6) . ? C22 C23 1.392(5) . ? C23 N24 1.325(5) . ? N24 C31 1.374(5) . ? C25 C26 1.343(11) . ? C25 C31 1.458(9) . ? C26 C34 1.465(11) . ? N27 C28 1.322(12) . ? N27 C34 1.383(11) . ? C28 C29 1.398(11) . ? C25' C26' 1.363(15) . ? C25' C31 1.437(12) . ? C26' C34' 1.407(16) . ? N27' C28' 1.304(14) . ? N27' C34' 1.365(14) . ? C28' C29 1.430(13) . ? C29 C30 1.362(6) . ? C30 C33 1.408(6) . ? C31 C32 1.406(5) . ? C32 C33 1.453(6) . ? C33 C34' 1.413(12) . ? C33 C34 1.428(10) . ? 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 O10 Ni1 O4 174.10(12) . . y O10 Ni1 N4 90.84(12) . . y O4 Ni1 N4 84.13(12) . . y O10 Ni1 O2 89.07(12) . . y O4 Ni1 O2 94.10(11) . . y N4 Ni1 O2 153.91(11) . . y O10 Ni1 N7 88.00(12) . 2_656 y O4 Ni1 N7 96.77(12) . 2_656 y N4 Ni1 N7 112.71(11) . 2_656 y O2 Ni1 N7 93.36(11) . 2_656 y O10 Ni1 O1 88.60(12) . . y O4 Ni1 O1 88.61(12) . . y N4 Ni1 O1 93.23(11) . . y O2 Ni1 O1 60.69(10) . . y N7 Ni1 O1 153.88(11) 2_656 . y O3 N10 O1 123.0(4) . . ? O3 N10 O2 121.4(4) . . ? O1 N10 O2 115.5(3) . . ? N10 O1 Ni1 90.5(2) . . ? N10 O2 Ni1 93.3(2) . . ? O5 N20 O6 121.6(3) . . ? O5 N20 O4 121.0(3) . . ? O6 N20 O4 117.4(3) . . ? N20 O4 Ni1 124.0(2) . . ? C2 C1 C12 119.8(4) . . ? C1 C2 C3 118.2(4) . . ? N4 C3 C2 124.3(4) . . ? C3 N4 C11 117.1(3) . . ? C3 N4 Ni1 113.0(2) . . ? C11 N4 Ni1 129.7(2) . . ? C6 C5 C11 120.7(3) . . ? C5 C6 C14 121.4(3) . . ? C8 N7 C14 117.8(3) . . ? C8 N7 Ni1 110.8(2) . 2_646 ? C14 N7 Ni1 130.9(2) . 2_646 ? N7 C8 C9 123.2(3) . . ? C10 C9 C8 119.5(3) . . ? C9 C10 C13 119.2(3) . . ? N4 C11 C12 122.2(3) . . ? N4 C11 C5 118.1(3) . . ? C12 C11 C5 119.7(3) . . ? C11 C12 C1 118.3(3) . . ? C11 C12 C13 119.6(3) . . ? C1 C12 C13 122.1(3) . . ? C10 C13 C14 118.3(3) . . ? C10 C13 C12 122.8(3) . . ? C14 C13 C12 118.8(3) . . ? N7 C14 C13 122.0(3) . . ? N7 C14 C6 118.3(3) . . ? C13 C14 C6 119.7(3) . . ? C22 C21 C32 119.8(4) . . ? C21 C22 C23 118.7(4) . . ? N24 C23 C22 124.0(4) . . ? C23 N24 C31 117.4(3) . . ? C26 C25 C31 121.2(7) . . ? C25 C26 C34 121.2(8) . . ? C28 N27 C34 115.9(8) . . ? N27 C28 C29 123.1(9) . . ? C26' C25' C31 117.9(10) . . ? C25' C26' C34' 121.3(11) . . ? C28' N27' C34' 117.9(10) . . ? N27' C28' C29 125.2(10) . . ? C30 C29 C28 120.6(6) . . ? C30 C29 C28' 115.9(6) . . ? C28 C29 C28' 22.4(6) . . ? C29 C30 C33 119.5(4) . . ? N24 C31 C32 122.4(4) . . ? N24 C31 C25' 115.1(6) . . ? C32 C31 C25' 121.0(6) . . ? N24 C31 C25 117.5(4) . . ? C32 C31 C25 119.1(5) . . ? C25' C31 C25 23.4(5) . . ? C21 C32 C31 117.7(4) . . ? C21 C32 C33 122.9(4) . . ? C31 C32 C33 119.4(4) . . ? C30 C33 C34' 118.8(6) . . ? C30 C33 C34 115.1(5) . . ? C34' C33 C34 22.0(5) . . ? C30 C33 C32 124.2(4) . . ? C34' C33 C32 115.6(6) . . ? C34 C33 C32 119.9(5) . . ? N27 C34 C33 124.6(7) . . ? N27 C34 C26 117.1(8) . . ? C33 C34 C26 117.9(7) . . ? N27' C34' C26' 116.5(10) . . ? N27' C34' C33 120.5(9) . . ? C26' C34' C33 122.7(10) . . ? _diffrn_measured_fraction_theta_max 0.885 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 0.79 _refine_diff_density_min -0.45 _refine_diff_density_rms 0.10 #======END data_6(CUCLPH) _database_code_CSD 205826 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Dichloro-bis(4,7-phenanthroline)copper(II) ; _chemical_name_common [Cu(Cl)2(4,7-phen)2] _chemical_formula_moiety 'C24 H16 Cl2 Cu N4' _chemical_formula_sum 'C24 H16 Cl2 Cu N4' _chemical_formula_weight 494.85 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 5.1490(15) _cell_length_b 18.613(6) _cell_length_c 10.889(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.242(5) _cell_angle_gamma 90.00 _cell_volume 1015.8(5) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 1577 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 24.12 _exptl_crystal_description Lath _exptl_crystal_colour Orange/brown _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.618 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 502 _exptl_absorpt_coefficient_mu 1.359 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.866 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'SADABS version 2.03 (Bruker, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'Bruker SMART APEX CCD area detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 6147 _diffrn_reflns_av_R_equivalents 0.026 _diffrn_reflns_av_sigmaI/netI 0.033 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 28.14 _reflns_number_total 2365 _reflns_number_gt 1902 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART version 5.625 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.02a (Bruker, 2000)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'SHELXL-97; PLATON (Spek, 2001)' _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 w==1/[\s^2^(Fo^2^)+(0.0511P)^2^+0.499P] where P==(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'direct methods' _atom_sites_solution_secondary 'difference Fourier synthesis' _atom_sites_solution_hydrogens 'geometrically placed' _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2285 _refine_ls_number_parameters 142 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0657 _refine_ls_R_factor_gt 0.0531 _refine_ls_wR_factor_ref 0.1203 _refine_ls_wR_factor_gt 0.1136 _refine_ls_goodness_of_fit_ref 1.139 _refine_ls_restrained_S_all 1.139 _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 0.5000 0.5000 0.0000 0.04185(19) Uani 1 2 d S . . Cl1 Cl 0.20902(18) 0.46012(5) -0.17402(8) 0.0566(3) Uani 1 1 d . . . C1 C 0.3433(6) 0.28163(19) 0.1959(3) 0.0477(8) Uani 1 1 d . . . H1A H 0.3007 0.2395 0.2327 0.057 Uiso 1 1 calc R . . C2 C 0.2512(7) 0.3455(2) 0.2278(3) 0.0542(9) Uani 1 1 d . . . H2A H 0.1473 0.3476 0.2872 0.065 Uiso 1 1 calc R . . C3 C 0.3136(7) 0.4074(2) 0.1712(3) 0.0543(9) Uani 1 1 d . . . H3A H 0.2485 0.4509 0.1936 0.065 Uiso 1 1 calc R . . N4 N 0.4623(5) 0.40790(14) 0.0862(2) 0.0429(6) Uani 1 1 d . . . C5 C 0.7278(6) 0.34568(16) -0.0333(3) 0.0412(7) Uani 1 1 d . . . H5A H 0.7662 0.3892 -0.0671 0.049 Uiso 1 1 calc R . . C6 C 0.8292(6) 0.28433(17) -0.0675(3) 0.0438(7) Uani 1 1 d . . . H6A H 0.9396 0.2862 -0.1241 0.053 Uiso 1 1 calc R . . N7 N 0.8748(6) 0.15688(16) -0.0628(3) 0.0569(8) Uani 1 1 d . . . C8 C 0.8179(9) 0.0944(2) -0.0197(4) 0.0671(11) Uani 1 1 d . . . H8A H 0.8868 0.0535 -0.0495 0.081 Uiso 1 1 calc R . . C9 C 0.6624(9) 0.0857(2) 0.0669(4) 0.0643(11) Uani 1 1 d . . . H9A H 0.6299 0.0400 0.0946 0.077 Uiso 1 1 calc R . . C10 C 0.5572(8) 0.14446(19) 0.1113(3) 0.0523(9) Uani 1 1 d . . . H10A H 0.4520 0.1394 0.1697 0.063 Uiso 1 1 calc R . . C11 C 0.6084(6) 0.21308(16) 0.0683(3) 0.0399(7) Uani 1 1 d . . . C12 C 0.5032(6) 0.27896(16) 0.1072(3) 0.0385(7) Uani 1 1 d . . . C13 C 0.5614(6) 0.34414(15) 0.0549(3) 0.0373(6) Uani 1 1 d . . . C14 C 0.7720(6) 0.21633(17) -0.0193(3) 0.0418(7) Uani 1 1 d . . . 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 0.0480(3) 0.0339(3) 0.0428(3) -0.0048(2) 0.0087(2) 0.0063(2) Cl1 0.0610(6) 0.0523(5) 0.0505(5) -0.0066(4) 0.0005(4) 0.0015(4) C1 0.0457(19) 0.057(2) 0.0422(18) 0.0066(15) 0.0146(14) -0.0028(15) C2 0.051(2) 0.075(3) 0.0413(19) -0.0025(17) 0.0200(15) 0.0048(18) C3 0.058(2) 0.058(2) 0.049(2) -0.0100(17) 0.0177(16) 0.0116(17) N4 0.0467(15) 0.0405(14) 0.0421(15) -0.0046(11) 0.0112(12) 0.0033(12) C5 0.0454(18) 0.0392(16) 0.0406(17) 0.0047(13) 0.0136(13) -0.0021(13) C6 0.0424(17) 0.0513(19) 0.0413(17) 0.0020(14) 0.0167(14) 0.0029(14) N7 0.0619(19) 0.0494(17) 0.0619(19) -0.0005(14) 0.0196(15) 0.0156(14) C8 0.083(3) 0.043(2) 0.073(3) 0.0037(18) 0.015(2) 0.0218(19) C9 0.085(3) 0.0380(19) 0.065(3) 0.0079(17) 0.006(2) 0.0005(19) C10 0.063(2) 0.048(2) 0.0435(19) 0.0088(15) 0.0069(16) -0.0040(16) C11 0.0394(17) 0.0412(16) 0.0364(16) 0.0039(13) 0.0032(13) -0.0012(13) C12 0.0367(16) 0.0442(17) 0.0336(15) 0.0046(12) 0.0061(12) 0.0010(13) C13 0.0395(16) 0.0367(15) 0.0347(15) -0.0007(12) 0.0063(12) 0.0004(12) C14 0.0395(17) 0.0417(17) 0.0431(17) 0.0005(13) 0.0072(13) 0.0044(13) _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 N4 1.985(3) 3_665 ? Cu1 N4 1.985(3) . y Cu1 Cl1 2.2552(9) . y Cu1 Cl1 2.2552(9) 3_665 ? C1 C2 1.354(5) . ? C1 C12 1.406(4) . ? C2 C3 1.378(5) . ? C3 N4 1.330(4) . ? N4 C13 1.365(4) . ? C5 C6 1.343(4) . ? C5 C13 1.426(4) . ? C6 C14 1.427(4) . ? N7 C8 1.311(5) . ? N7 C14 1.358(4) . ? C8 C9 1.380(6) . ? C9 C10 1.358(5) . ? C10 C11 1.406(4) . ? C11 C14 1.411(4) . ? C11 C12 1.443(4) . ? C12 C13 1.401(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 N4 Cu1 N4 180 3_665 . ? N4 Cu1 Cl1 90.30(8) 3_665 . ? N4 Cu1 Cl1 89.70(8) . . y N4 Cu1 Cl1 89.70(8) 3_665 3_665 ? N4 Cu1 Cl1 90.30(8) . 3_665 ? Cl1 Cu1 Cl1 180 . 3_665 ? C2 C1 C12 120.1(3) . . ? C1 C2 C3 119.2(3) . . ? N4 C3 C2 123.2(3) . . ? C3 N4 C13 118.3(3) . . ? C3 N4 Cu1 118.0(2) . . ? C13 N4 Cu1 123.4(2) . . ? C6 C5 C13 120.1(3) . . ? C5 C6 C14 121.7(3) . . ? C8 N7 C14 117.4(3) . . ? N7 C8 C9 124.2(4) . . ? C10 C9 C8 119.3(4) . . ? C9 C10 C11 119.6(4) . . ? C10 C11 C14 116.8(3) . . ? C10 C11 C12 124.3(3) . . ? C14 C11 C12 119.0(3) . . ? C13 C12 C1 117.5(3) . . ? C13 C12 C11 119.2(3) . . ? C1 C12 C11 123.3(3) . . ? N4 C13 C12 121.6(3) . . ? N4 C13 C5 117.8(3) . . ? C12 C13 C5 120.5(3) . . ? N7 C14 C11 122.8(3) . . ? N7 C14 C6 117.7(3) . . ? C11 C14 C6 119.5(3) . . ? _diffrn_measured_fraction_theta_max 0.919 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 0.45 _refine_diff_density_min -0.46 _refine_diff_density_rms 0.07 #======END data_7(CUBRPH) _database_code_CSD 205827 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Dibromo-bis(4,7-phenanthroline)copper(II) ; _chemical_name_common [Cu(Cl)2(4,7-phen)2] _chemical_formula_moiety 'C24 H16 Br2 Cu N4' _chemical_formula_sum 'C24 H16 Br2 Cu N4' _chemical_formula_weight 583.77 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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 5.4065(6) _cell_length_b 18.709(2) _cell_length_c 10.7551(12) _cell_angle_alpha 90.00 _cell_angle_beta 103.348(2) _cell_angle_gamma 90.00 _cell_volume 1058.5(2) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 4136 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 25.79 _exptl_crystal_description Lath _exptl_crystal_colour Orange/brown _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.832 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 574 _exptl_absorpt_coefficient_mu 4.827 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.720 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'SADABS version 2.03 (Bruker, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'Bruker SMART APEX CCD area detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 12246 _diffrn_reflns_av_R_equivalents 0.024 _diffrn_reflns_av_sigmaI/netI 0.021 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 28.18 _reflns_number_total 2541 _reflns_number_gt 2045 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART version 5.625 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.02a (Bruker, 2000)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'SHELXL-97; PLATON (Spek, 2001)' _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 w==1/[\s^2^(Fo^2^)+(0.0346P)^2^+0.730P] where P==(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'direct methods' _atom_sites_solution_secondary 'difference Fourier synthesis' _atom_sites_solution_hydrogens 'geometrically placed' _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2454 _refine_ls_number_parameters 142 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0395 _refine_ls_R_factor_gt 0.0291 _refine_ls_wR_factor_ref 0.0739 _refine_ls_wR_factor_gt 0.0679 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _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 0.0000 0.5000 0.5000 0.03810(12) Uani 1 2 d S . . Br1 Br 0.30534(5) 0.458541(15) 0.68683(3) 0.05002(11) Uani 1 1 d . . . C1 C 0.1461(5) 0.27957(15) 0.3098(2) 0.0437(6) Uani 1 1 d . . . H1A H 0.1872 0.2369 0.2752 0.052 Uiso 1 1 calc R . . C2 C 0.2381(5) 0.34271(17) 0.2754(3) 0.0498(7) Uani 1 1 d . . . H2A H 0.3395 0.3434 0.2163 0.060 Uiso 1 1 calc R . . C3 C 0.1781(5) 0.40573(16) 0.3297(3) 0.0481(6) Uani 1 1 d . . . H3A H 0.2421 0.4485 0.3059 0.058 Uiso 1 1 calc R . . N4 N 0.0332(4) 0.40783(11) 0.4143(2) 0.0398(5) Uani 1 1 d . . . C5 C -0.2321(5) 0.34866(13) 0.5337(2) 0.0398(5) Uani 1 1 d . . . H5A H -0.2695 0.3926 0.5653 0.048 Uiso 1 1 calc R . . C6 C -0.3339(5) 0.28858(14) 0.5691(3) 0.0426(6) Uani 1 1 d . . . H6A H -0.4429 0.2918 0.6243 0.051 Uiso 1 1 calc R . . N7 N -0.3854(5) 0.16177(13) 0.5675(2) 0.0547(6) Uani 1 1 d . . . C8 C -0.3296(7) 0.09825(16) 0.5279(3) 0.0614(8) Uani 1 1 d . . . H8A H -0.3992 0.0582 0.5580 0.074 Uiso 1 1 calc R . . C9 C -0.1727(7) 0.08792(15) 0.4437(3) 0.0591(8) Uani 1 1 d . . . H9A H -0.1413 0.0420 0.4180 0.071 Uiso 1 1 calc R . . C10 C -0.0652(6) 0.14526(14) 0.3991(3) 0.0491(6) Uani 1 1 d . . . H10A H 0.0411 0.1389 0.3433 0.059 Uiso 1 1 calc R . . C11 C -0.1167(5) 0.21458(13) 0.4384(2) 0.0367(5) Uani 1 1 d . . . C12 C -0.0109(4) 0.27901(13) 0.3977(2) 0.0351(5) Uani 1 1 d . . . C13 C -0.0662(4) 0.34533(12) 0.4474(2) 0.0343(5) Uani 1 1 d . . . C14 C -0.2785(5) 0.21974(14) 0.5239(2) 0.0398(5) Uani 1 1 d . . . 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 0.0459(2) 0.0307(2) 0.0384(2) 0.00169(17) 0.01100(19) -0.00438(17) Br1 0.05366(18) 0.04834(17) 0.04506(17) 0.00292(12) 0.00522(12) 0.00070(12) C1 0.0456(14) 0.0496(15) 0.0376(14) -0.0071(11) 0.0133(11) 0.0023(12) C2 0.0495(15) 0.0647(18) 0.0402(15) 0.0006(13) 0.0204(12) -0.0022(13) C3 0.0536(16) 0.0492(15) 0.0442(15) 0.0039(12) 0.0171(13) -0.0084(12) N4 0.0446(11) 0.0376(11) 0.0381(11) 0.0016(9) 0.0116(9) -0.0038(9) C5 0.0450(14) 0.0369(12) 0.0400(14) -0.0061(10) 0.0150(11) 0.0001(10) C6 0.0429(14) 0.0478(14) 0.0418(14) -0.0025(11) 0.0193(11) -0.0043(12) N7 0.0624(15) 0.0475(13) 0.0567(15) 0.0040(11) 0.0189(12) -0.0157(12) C8 0.078(2) 0.0429(16) 0.062(2) 0.0037(14) 0.0130(17) -0.0170(15) C9 0.080(2) 0.0334(13) 0.0588(18) -0.0026(13) 0.0059(16) -0.0026(14) C10 0.0606(17) 0.0422(14) 0.0435(15) -0.0042(12) 0.0103(13) 0.0053(12) C11 0.0400(12) 0.0361(12) 0.0320(12) -0.0013(10) 0.0040(10) 0.0013(10) C12 0.0347(12) 0.0391(12) 0.0311(12) -0.0015(10) 0.0070(9) 0.0012(10) C13 0.0367(12) 0.0336(11) 0.0325(12) 0.0009(9) 0.0079(10) -0.0009(9) C14 0.0414(13) 0.0407(13) 0.0365(13) -0.0003(10) 0.0077(10) -0.0049(11) _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 N4 1.983(2) 3_566 ? Cu1 N4 1.983(2) . y Cu1 Br1 2.4151(3) 3_566 ? Cu1 Br1 2.4151(3) . y C1 C2 1.366(4) . ? C1 C12 1.409(3) . ? C2 C3 1.387(4) . ? C3 N4 1.332(3) . ? N4 C13 1.368(3) . ? C5 C6 1.345(4) . ? C5 C13 1.433(3) . ? C6 C14 1.433(4) . ? N7 C8 1.321(4) . ? N7 C14 1.362(3) . ? C8 C9 1.389(5) . ? C9 C10 1.359(4) . ? C10 C11 1.411(4) . ? C11 C14 1.411(4) . ? C11 C12 1.445(3) . ? C12 C13 1.410(3) . ? 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 N4 Cu1 N4 180 3_566 . ? N4 Cu1 Br1 89.40(6) 3_566 3_566 ? N4 Cu1 Br1 90.60(6) . 3_566 ? N4 Cu1 Br1 90.60(6) 3_566 . ? N4 Cu1 Br1 89.40(6) . . y Br1 Cu1 Br1 180 3_566 . ? C2 C1 C12 120.2(2) . . ? C1 C2 C3 119.0(2) . . ? N4 C3 C2 123.0(3) . . ? C3 N4 C13 118.8(2) . . ? C3 N4 Cu1 118.28(18) . . ? C13 N4 Cu1 122.66(17) . . ? C6 C5 C13 120.4(2) . . ? C5 C6 C14 121.6(2) . . ? C8 N7 C14 117.3(3) . . ? N7 C8 C9 123.7(3) . . ? C10 C9 C8 119.7(3) . . ? C9 C10 C11 119.3(3) . . ? C14 C11 C10 116.9(2) . . ? C14 C11 C12 119.2(2) . . ? C10 C11 C12 123.8(2) . . ? C1 C12 C13 117.4(2) . . ? C1 C12 C11 123.5(2) . . ? C13 C12 C11 119.1(2) . . ? N4 C13 C12 121.6(2) . . ? N4 C13 C5 118.2(2) . . ? C12 C13 C5 120.2(2) . . ? N7 C14 C11 123.1(2) . . ? N7 C14 C6 117.4(2) . . ? C11 C14 C6 119.5(2) . . ? _diffrn_measured_fraction_theta_max 0.943 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.63 _refine_diff_density_min -0.35 _refine_diff_density_rms 0.07 #======END data_8(CUPHEN) _database_code_CSD 205828 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Copper(II) nitrate bis-(4,7-phenanthroline) ; _chemical_name_common [Cu(NO3)2(4,7-phen)2] _chemical_formula_moiety Cu0.5(NO3)(C12H8N2) _chemical_formula_sum 'C12 H8 Cu0.5 N3 O3' _chemical_formula_weight 273.98 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' O O 0.0106 0.0060 '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 6.6182(6) _cell_length_b 24.671(2) _cell_length_c 7.1845(6) _cell_angle_alpha 90.00 _cell_angle_beta 107.596(1) _cell_angle_gamma 90.00 _cell_volume 1118.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2426 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 28.0 _exptl_crystal_description Plate _exptl_crystal_colour Purple _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.628 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 558 _exptl_absorpt_coefficient_mu 1.034 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.616 _exptl_absorpt_correction_T_max 0.819 _exptl_absorpt_process_details 'SADABS (Bruker, 1996)' _exptl_special_details ; The oxygen atoms of the nitrate anion were found to be disordered and were modelled over 2 sets of alternative sites. Occupancies within each set were constrained to be equal and the linked occupancies refined to 0.67 for the major and 0.33 for the minor componant. The disordered oxygen atoms were refined with individual isotropic displacement parameters and no distance or angle restraints were applied. ; _diffrn_ambient_temperature 150(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 'Bruker SMART1000 CCD area detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 5970 _diffrn_reflns_av_R_equivalents 0.025 _diffrn_reflns_av_sigmaI/netI 0.040 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 28.65 _reflns_number_total 2662 _reflns_number_gt 1997 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART version 5.054 (Bruker, 1998)' _computing_cell_refinement 'Bruker SAINT version 6.02a (Bruker, 2000)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'SHELXL-97; PLATON (Spek, 2001)' _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 w==1/[\s^2^(Fo^2^)+(0.053P)^2^] where P==(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'direct methods' _atom_sites_solution_secondary 'difference Fourier synthesis' _atom_sites_solution_hydrogens 'geometrically placed' _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2591 _refine_ls_number_parameters 166 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0515 _refine_ls_R_factor_gt 0.0363 _refine_ls_wR_factor_ref 0.0958 _refine_ls_wR_factor_gt 0.0906 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _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 0.0000 0.5000 0.0000 0.01699(12) Uani 1 2 d S . . N10 N -0.1020(4) 0.53779(8) 0.2986(3) 0.0290(5) Uani 1 1 d . . . C1 C 0.4465(4) 0.35682(9) 0.3267(3) 0.0248(5) Uani 1 1 d . . . H1A H 0.5437 0.3288 0.3840 0.030 Uiso 1 1 calc R . . C2 C 0.5131(4) 0.40950(9) 0.3401(3) 0.0257(5) Uani 1 1 d . . . H2A H 0.6554 0.4186 0.4098 0.031 Uiso 1 1 calc R . . C3 C 0.3680(4) 0.44993(9) 0.2493(3) 0.0217(5) Uani 1 1 d . . . H3A H 0.4162 0.4863 0.2551 0.026 Uiso 1 1 calc R A . N4 N 0.1667(3) 0.43953(7) 0.1558(3) 0.0181(4) Uani 1 1 d . . . C5 C -0.1261(4) 0.37709(9) 0.0631(3) 0.0239(5) Uani 1 1 d . . . H5A H -0.2200 0.4065 0.0158 0.029 Uiso 1 1 calc R . . C6 C -0.2032(4) 0.32584(9) 0.0482(4) 0.0269(5) Uani 1 1 d . . . H6A H -0.3514 0.3200 -0.0055 0.032 Uiso 1 1 calc R . . N7 N -0.1541(3) 0.22991(8) 0.0788(3) 0.0297(5) Uani 1 1 d . . . C8 C -0.0248(4) 0.18799(9) 0.1326(4) 0.0320(6) Uani 1 1 d . . . H8A H -0.0843 0.1527 0.1103 0.038 Uiso 1 1 calc R . . C9 C 0.1926(4) 0.19247(9) 0.2198(4) 0.0311(6) Uani 1 1 d . . . H9A H 0.2780 0.1609 0.2539 0.037 Uiso 1 1 calc R . . C10 C 0.2830(4) 0.24299(9) 0.2562(3) 0.0276(5) Uani 1 1 d . . . H10A H 0.4310 0.2469 0.3174 0.033 Uiso 1 1 calc R . . C11 C 0.1528(4) 0.28876(8) 0.2016(3) 0.0209(5) Uani 1 1 d . . . C12 C 0.2339(3) 0.34422(8) 0.2279(3) 0.0195(5) Uani 1 1 d . . . C13 C 0.0943(3) 0.38719(8) 0.1488(3) 0.0180(4) Uani 1 1 d . . . C14 C -0.0653(4) 0.28055(8) 0.1121(3) 0.0232(5) Uani 1 1 d . . . O1 O -0.2366(5) 0.50784(11) 0.2074(5) 0.0282(7) Uiso 0.67 1 d P A 1 O2 O 0.0686(4) 0.54599(11) 0.2365(4) 0.0204(7) Uiso 0.67 1 d P A 1 O3 O -0.0964(5) 0.56221(11) 0.4520(4) 0.0323(6) Uiso 0.67 1 d P A 1 O1' O -0.2111(9) 0.5000(2) 0.1560(9) 0.0248(12) Uiso 0.33 1 d P A 2 O2' O 0.0554(10) 0.5527(2) 0.2882(10) 0.0300(16) Uiso 0.33 1 d P A 2 O3' O -0.2099(11) 0.5503(2) 0.4061(9) 0.0447(15) Uiso 0.33 1 d P A 2 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 0.0166(2) 0.01242(19) 0.02083(19) -0.00130(14) 0.00402(14) -0.00008(15) N10 0.0450(14) 0.0224(10) 0.0233(10) 0.0020(8) 0.0158(10) 0.0104(10) C1 0.0220(12) 0.0212(11) 0.0284(12) 0.0044(9) 0.0035(10) 0.0045(10) C2 0.0162(11) 0.0231(12) 0.0335(13) -0.0001(9) 0.0008(10) -0.0021(9) C3 0.0200(11) 0.0166(11) 0.0271(12) 0.0001(8) 0.0053(9) -0.0033(9) N4 0.0179(9) 0.0147(9) 0.0221(9) -0.0011(7) 0.0065(7) 0.0009(7) C5 0.0197(12) 0.0178(11) 0.0327(13) -0.0002(9) 0.0055(10) 0.0022(9) C6 0.0190(12) 0.0197(12) 0.0396(14) -0.0036(10) 0.0050(10) -0.0022(10) N7 0.0318(12) 0.0162(10) 0.0378(12) -0.0018(8) 0.0054(10) -0.0052(9) C8 0.0424(16) 0.0148(11) 0.0347(14) 0.0001(9) 0.0057(12) -0.0071(11) C9 0.0392(15) 0.0156(11) 0.0337(13) 0.0033(9) 0.0035(11) 0.0038(11) C10 0.0298(13) 0.0197(12) 0.0292(13) 0.0026(9) 0.0027(10) 0.0023(10) C11 0.0247(12) 0.0158(10) 0.0214(11) 0.0007(8) 0.0058(9) 0.0003(9) C12 0.0216(12) 0.0155(10) 0.0206(11) 0.0003(8) 0.0052(9) 0.0005(9) C13 0.0182(11) 0.0147(10) 0.0212(10) -0.0022(8) 0.0060(9) -0.0006(8) C14 0.0252(12) 0.0164(11) 0.0272(12) -0.0002(8) 0.0067(10) -0.0044(9) _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 O2 1.979(3) . y Cu1 O2 1.979(3) 3_565 ? Cu1 N4 1.9873(17) 3_565 ? Cu1 N4 1.9873(17) . y Cu1 O1' 2.038(6) . y Cu1 O1' 2.038(6) 3_565 ? Cu1 O2' 2.377(7) . ? Cu1 O2' 2.377(7) 3_565 ? N10 O2' 1.128(7) . ? N10 O1 1.190(3) . ? N10 O3' 1.239(6) . ? N10 O3 1.247(3) . ? N10 O2 1.348(4) . ? N10 O1' 1.412(6) . ? C1 C2 1.366(3) . ? C1 C12 1.406(3) . ? C2 C3 1.401(3) . ? C3 N4 1.323(3) . ? N4 C13 1.373(3) . ? C5 C6 1.356(3) . ? C5 C13 1.423(3) . ? C6 C14 1.428(3) . ? N7 C8 1.323(3) . ? N7 C14 1.371(3) . ? C8 C9 1.389(4) . ? C9 C10 1.373(3) . ? C10 C11 1.402(3) . ? C11 C14 1.406(3) . ? C11 C12 1.461(3) . ? C12 C13 1.408(3) . ? 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 O2 Cu1 O2 180.00(12) . 3_565 ? O2 Cu1 N4 89.85(9) . 3_565 y O2 Cu1 N4 90.15(9) 3_565 3_565 ? O2 Cu1 N4 90.15(9) . . y O2 Cu1 N4 89.85(9) 3_565 . ? N4 Cu1 N4 180.00(6) 3_565 . ? O2 Cu1 O1' 62.96(18) . . y O2 Cu1 O1' 117.04(18) 3_565 . ? N4 Cu1 O1' 87.36(16) 3_565 . ? N4 Cu1 O1' 92.64(16) . . y O2 Cu1 O1' 117.04(18) . 3_565 y O2 Cu1 O1' 62.96(18) 3_565 3_565 ? N4 Cu1 O1' 92.64(16) 3_565 3_565 ? N4 Cu1 O1' 87.36(16) . 3_565 y O1' Cu1 O1' 180.000(1) . 3_565 ? O2 Cu1 O2' 4.8(2) . . ? O2 Cu1 O2' 175.2(2) 3_565 . ? N4 Cu1 O2' 89.60(16) 3_565 . ? N4 Cu1 O2' 90.40(16) . . ? O1' Cu1 O2' 58.1(2) . . ? O1' Cu1 O2' 121.9(2) 3_565 . ? O2 Cu1 O2' 175.2(2) . 3_565 ? O2 Cu1 O2' 4.8(2) 3_565 3_565 ? N4 Cu1 O2' 90.40(16) 3_565 3_565 ? N4 Cu1 O2' 89.60(16) . 3_565 ? O1' Cu1 O2' 121.9(2) . 3_565 ? O1' Cu1 O2' 58.1(2) 3_565 3_565 ? O2' Cu1 O2' 180.0(2) . 3_565 ? O2' N10 O1 135.9(4) . . ? O2' N10 O3' 132.7(5) . . ? O1 N10 O3' 91.2(4) . . ? O2' N10 O3 96.9(4) . . ? O1 N10 O3 127.1(3) . . ? O3' N10 O3 36.6(3) . . ? O2' N10 O2 17.7(3) . . ? O1 N10 O2 118.3(2) . . ? O3' N10 O2 150.1(4) . . ? O3 N10 O2 114.6(3) . . ? O2' N10 O1' 116.6(4) . . ? O1 N10 O1' 19.4(3) . . ? O3' N10 O1' 110.6(4) . . ? O3 N10 O1' 146.3(4) . . ? O2 N10 O1' 98.9(3) . . ? C2 C1 C12 119.9(2) . . ? C1 C2 C3 118.9(2) . . ? N4 C3 C2 122.8(2) . . ? C3 N4 C13 119.18(18) . . ? C3 N4 Cu1 116.27(14) . . ? C13 N4 Cu1 123.87(15) . . ? C6 C5 C13 120.6(2) . . ? C5 C6 C14 121.0(2) . . ? C8 N7 C14 117.1(2) . . ? N7 C8 C9 124.0(2) . . ? C10 C9 C8 119.4(2) . . ? C9 C10 C11 118.9(2) . . ? C10 C11 C14 118.1(2) . . ? C10 C11 C12 123.2(2) . . ? C14 C11 C12 118.71(19) . . ? C1 C12 C13 118.14(19) . . ? C1 C12 C11 123.0(2) . . ? C13 C12 C11 118.8(2) . . ? N4 C13 C12 121.0(2) . . ? N4 C13 C5 118.76(19) . . ? C12 C13 C5 120.28(19) . . ? N7 C14 C11 122.5(2) . . ? N7 C14 C6 117.3(2) . . ? C11 C14 C6 120.15(19) . . ? N10 O2 Cu1 101.55(18) . . ? N10 O1' Cu1 96.5(3) . . ? N10 O2' Cu1 88.7(4) . . ? _diffrn_measured_fraction_theta_max 0.905 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 0.62 _refine_diff_density_min -0.44 _refine_diff_density_rms 0.08 #======END