# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Dominic S. Wright' 'Andrew D. Bond' 'Emma L. Doyle' 'Felipe Garcia' 'Richard A. Kowenicki' 'M. McPartlin' 'Lucia Riera' _publ_contact_author_name 'Dr Dominic S. Wright' _publ_contact_author_address ; Department of Chemistry Cambridge University Lensfield Road Cambridge CB2 1EW UNITED KINGDOM ; _publ_contact_author_email DSW1000@CUS.CAM.AC.UK _publ_requested_journal 'Chemical Communications' _publ_section_title ; Exo-Metal Coordination by a Cyclic [{P(µ-N-2-NC5H4)}2(µ-O)]2 Dimer in [{P(µ-N-2-NC5H4)}2(µ-O)]2{CuCl. (C5H5N)2}4 {2-NC5H4= 2-pyridyl, C5H5N= pyridine) ; data_dw0240 _database_code_CSD 217696 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H30 Cl2 Cu N6' _chemical_formula_weight 609.04 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 orthorhombic _symmetry_space_group_name_H-M Ccca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, z+1/2' 'x+1/2, -y+1/2, z+1/2' '-x, -y+1/2, z' 'x+1/2, y+1/2, z' '-x+1, y+1/2, z+1/2' 'x+1, -y+1, z+1/2' '-x+1/2, -y+1, z' '-x, -y, -z' 'x-1/2, -y, -z-1/2' '-x-1/2, y-1/2, -z-1/2' 'x, y-1/2, -z' '-x+1/2, -y+1/2, -z' 'x, -y+1/2, -z-1/2' '-x, y, -z-1/2' 'x+1/2, y, -z' _cell_length_a 11.8453(3) _cell_length_b 14.2813(3) _cell_length_c 16.8855(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2856.46(13) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 6968 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.416 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1260 _exptl_absorpt_coefficient_mu 0.983 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.830 _exptl_absorpt_correction_T_max 0.891 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_method CCD _diffrn_reflns_number 15146 _diffrn_reflns_av_R_equivalents 0.0617 _diffrn_reflns_av_sigmaI/netI 0.0353 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.74 _diffrn_reflns_theta_max 27.46 _reflns_number_total 1635 _reflns_number_gt 1082 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution teXsan _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0560P)^2^+5.8840P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1635 _refine_ls_number_parameters 93 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0886 _refine_ls_R_factor_gt 0.0517 _refine_ls_wR_factor_ref 0.1396 _refine_ls_wR_factor_gt 0.1185 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.001 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 0.2500 0.7500 0.0655(4) Uani 1 4 d S . . N1 N 0.0000 0.3920(2) 0.7500 0.0343(7) Uani 1 2 d S . . N2 N 0.0000 0.2500 0.8722(2) 0.0427(9) Uani 1 2 d S . . N3 N 0.2500 0.5000 0.9452(2) 0.0438(9) Uani 1 2 d S . . C1 C 0.0824(3) 0.44033(19) 0.78610(17) 0.0359(6) Uani 1 1 d . . . H1 H 0.1412 0.4068 0.8117 0.043 Uiso 1 1 calc R . . C2 C 0.0850(3) 0.53671(19) 0.78744(17) 0.0361(7) Uani 1 1 d . . . H2 H 0.1444 0.5688 0.8137 0.043 Uiso 1 1 calc R . . C3 C 0.0000 0.5862(3) 0.7500 0.0356(9) Uani 1 2 d S . . H3 H 0.0000 0.6527 0.7500 0.043 Uiso 1 2 calc SR . . C4 C 0.0875(3) 0.2155(2) 0.9131(2) 0.0489(8) Uani 1 1 d . . . H4 H 0.1499 0.1907 0.8846 0.059 Uiso 1 1 calc R . . C5 C 0.0907(4) 0.2143(2) 0.9945(2) 0.0586(10) Uani 1 1 d . . . H5 H 0.1542 0.1895 1.0217 0.070 Uiso 1 1 calc R . . C6 C 0.0000 0.2500 1.0358(3) 0.0604(15) Uani 1 2 d S . . H6 H 0.0000 0.2500 1.0921 0.072 Uiso 1 2 calc SR . . C7 C 0.1650(3) 0.4643(2) 0.98682(18) 0.0459(8) Uani 1 1 d . . . H7 H 0.1030 0.4384 0.9586 0.055 Uiso 1 1 calc R . . C8 C 0.1613(3) 0.4627(2) 1.06832(19) 0.0506(8) Uani 1 1 d . . . H8 H 0.0985 0.4363 1.0953 0.061 Uiso 1 1 calc R . . C9 C 0.2500 0.5000 1.1098(3) 0.0531(12) Uani 1 2 d S . . H9 H 0.2500 0.5000 1.1660 0.064 Uiso 1 2 calc SR . . Cl1 Cl 0.24963(10) 0.2500 0.7500 0.0526(3) Uani 1 2 d S . . 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 0.1331(10) 0.0204(4) 0.0431(5) 0.000 0.000 0.000 N1 0.0427(19) 0.0233(14) 0.0369(16) 0.000 0.0016(17) 0.000 N2 0.060(2) 0.0217(15) 0.0467(19) 0.000 0.000 0.0020(17) N3 0.042(2) 0.055(2) 0.0345(19) 0.000 0.000 -0.0026(19) C1 0.0347(16) 0.0373(15) 0.0358(14) 0.0002(12) -0.0006(14) 0.0067(13) C2 0.0388(17) 0.0361(15) 0.0335(14) -0.0046(11) 0.0022(13) -0.0061(13) C3 0.049(2) 0.0240(17) 0.0340(19) 0.000 0.006(2) 0.000 C4 0.055(2) 0.0311(14) 0.060(2) 0.0023(14) 0.0029(18) 0.0056(15) C5 0.070(3) 0.0406(18) 0.065(2) 0.0069(17) -0.017(2) -0.0011(19) C6 0.098(5) 0.037(2) 0.046(3) 0.000 0.000 -0.012(3) C7 0.0451(19) 0.0530(19) 0.0395(18) -0.0051(13) 0.0013(15) -0.0040(16) C8 0.049(2) 0.061(2) 0.0418(18) 0.0012(15) 0.0097(16) -0.0022(17) C9 0.056(3) 0.072(3) 0.031(2) 0.000 0.000 0.010(3) Cl1 0.0478(7) 0.0326(5) 0.0775(8) -0.0060(5) 0.000 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N1 2.028(3) . ? Cu1 N1 2.028(3) 14_557 ? Cu1 N2 2.064(4) 14_557 ? Cu1 N2 2.064(4) . ? N1 C1 1.342(4) . ? N1 C1 1.342(3) 15_557 ? N2 C4 1.338(4) 4 ? N2 C4 1.338(4) . ? N3 C7 1.330(4) 8 ? N3 C7 1.330(4) . ? C1 C2 1.377(4) . ? C2 C3 1.383(4) . ? C3 C2 1.383(4) 15_557 ? C4 C5 1.376(5) . ? C5 C6 1.379(5) . ? C6 C5 1.379(5) 4 ? C7 C8 1.377(4) . ? C8 C9 1.370(4) . ? C9 C8 1.370(4) 8 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu1 N1 180.0 . 14_557 ? N1 Cu1 N2 90.0 . 14_557 ? N1 Cu1 N2 90.0 14_557 14_557 ? N1 Cu1 N2 90.0 . . ? N1 Cu1 N2 90.0 14_557 . ? N2 Cu1 N2 180.0 14_557 . ? C1 N1 C1 118.1(3) . 15_557 ? C1 N1 Cu1 120.96(17) . . ? C1 N1 Cu1 120.96(17) 15_557 . ? C4 N2 C4 118.0(4) 4 . ? C4 N2 Cu1 121.0(2) 4 . ? C4 N2 Cu1 121.0(2) . . ? C7 N3 C7 116.1(4) 8 . ? N1 C1 C2 122.5(3) . . ? C1 C2 C3 119.2(3) . . ? C2 C3 C2 118.5(4) 15_557 . ? N2 C4 C5 122.7(4) . . ? C6 C5 C4 118.7(4) . . ? C5 C6 C5 119.2(5) 4 . ? N3 C7 C8 124.0(3) . . ? C9 C8 C7 118.7(4) . . ? C8 C9 C8 118.6(4) . 8 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.299 _refine_diff_density_min -1.401 _refine_diff_density_rms 0.076 data_dw0239 _database_code_CSD 217697 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C90 H86 Cl4 Cu4 N22 O2 P4' _chemical_formula_weight 2027.65 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' P P 0.1023 0.0942 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.7629(3) _cell_length_b 13.9287(2) _cell_length_c 14.1546(3) _cell_angle_alpha 61.079(7) _cell_angle_beta 87.902(7) _cell_angle_gamma 82.493(9) _cell_volume 2353.57(8) _cell_formula_units_Z 1 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 17982 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 27.48 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.431 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1040 _exptl_absorpt_coefficient_mu 1.133 #_exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.7421 _exptl_absorpt_correction_T_max 0.8952 # Absorption correction _exptl_absorpt_correction_type multi-scan #_exptl_absorpt_correction_T_min 0.806 #_exptl_absorpt_correction_T_max 0.895 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' #_diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_method CCD _diffrn_reflns_number 23631 _diffrn_reflns_av_R_equivalents 0.0491 _diffrn_reflns_av_sigmaI/netI 0.0488 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.56 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8249 _reflns_number_gt 6670 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution teXsan _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0496P)^2^+2.3181P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8249 _refine_ls_number_parameters 546 _refine_ls_number_restraints 126 _refine_ls_R_factor_all 0.0607 _refine_ls_R_factor_gt 0.0439 _refine_ls_wR_factor_ref 0.1135 _refine_ls_wR_factor_gt 0.1039 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.201 _refine_ls_shift/su_mean 0.010 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 -0.15879(3) 0.97270(3) 0.26513(3) 0.03237(12) Uani 1 1 d . . . Cu2 Cu 0.03263(3) 0.65791(3) 0.17166(3) 0.03407(12) Uani 1 1 d . . . P1 P -0.08023(5) 0.98911(6) 0.12519(6) 0.02650(18) Uani 1 1 d . . . P2 P 0.01601(5) 0.83408(6) 0.09109(6) 0.02688(18) Uani 1 1 d . . . Cl2 Cl -0.10725(6) 0.58281(7) 0.25465(7) 0.0455(2) Uani 1 1 d . . . Cl1 Cl -0.20762(8) 1.12567(8) 0.28463(8) 0.0538(3) Uani 1 1 d . . . O1 O -0.06990(14) 1.11304(16) 0.02608(16) 0.0288(5) Uani 1 1 d . . . N1 N 0.03503(17) 0.9160(2) 0.14520(19) 0.0277(6) Uani 1 1 d . . . N11 N 0.1839(2) 0.8217(3) 0.2338(3) 0.0535(8) Uani 1 1 d . . . C12 C 0.1130(2) 0.9063(3) 0.2119(2) 0.0318(7) Uani 1 1 d . . . C13 C 0.1124(3) 0.9805(3) 0.2491(3) 0.0418(8) Uani 1 1 d . . . H13 H 0.0617 1.0408 0.2289 0.050 Uiso 1 1 calc R . . C14 C 0.1901(4) 0.9629(5) 0.3184(4) 0.0723(14) Uani 1 1 d . . . H14 H 0.1923 1.0108 0.3482 0.087 Uiso 1 1 calc R . . C15 C 0.2637(3) 0.8766(6) 0.3438(4) 0.0861(18) Uani 1 1 d . . . H15 H 0.3174 0.8646 0.3902 0.103 Uiso 1 1 calc R . . C16 C 0.2577(3) 0.8091(4) 0.3010(4) 0.0737(15) Uani 1 1 d . . . H16 H 0.3085 0.7493 0.3193 0.088 Uiso 1 1 calc R . . N2 N -0.09745(17) 0.9103(2) 0.06653(19) 0.0269(5) Uani 1 1 d . . . N21 N -0.25820(19) 0.9822(2) 0.0134(2) 0.0362(6) Uani 1 1 d . . . C22 C -0.1862(2) 0.9019(2) 0.0271(2) 0.0288(7) Uani 1 1 d . . . C23 C -0.1968(2) 0.8174(3) 0.0049(3) 0.0403(8) Uani 1 1 d . . . H23 H -0.1431 0.7629 0.0144 0.048 Uiso 1 1 calc R . . C24 C -0.2874(3) 0.8144(3) -0.0313(3) 0.0538(10) Uani 1 1 d . . . H24 H -0.2973 0.7570 -0.0467 0.065 Uiso 1 1 calc R . . C25 C -0.3633(3) 0.8951(3) -0.0450(3) 0.0566(11) Uani 1 1 d . . . H25 H -0.4263 0.8946 -0.0698 0.068 Uiso 1 1 calc R . . C26 C -0.3459(3) 0.9763(3) -0.0218(3) 0.0500(10) Uani 1 1 d . . . H26 H -0.3986 1.0317 -0.0311 0.060 Uiso 1 1 calc R . . N31 N -0.07334(19) 0.8666(2) 0.4058(2) 0.0379(7) Uani 1 1 d . . . C32 C -0.0232(3) 0.7712(3) 0.4224(3) 0.0504(10) Uani 1 1 d . . . H32 H -0.0296 0.7479 0.3702 0.061 Uiso 1 1 calc R . . C33 C 0.0379(3) 0.7039(4) 0.5124(4) 0.0711(13) Uani 1 1 d . . . H33 H 0.0724 0.6362 0.5214 0.085 Uiso 1 1 calc R . . C34 C 0.0475(3) 0.7370(4) 0.5884(4) 0.0732(14) Uani 1 1 d . . . H34 H 0.0879 0.6921 0.6513 0.088 Uiso 1 1 calc R . . C35 C -0.0022(3) 0.8357(4) 0.5715(4) 0.0666(12) Uani 1 1 d . . . H35 H 0.0041 0.8612 0.6220 0.080 Uiso 1 1 calc R . . C36 C -0.0617(3) 0.8977(3) 0.4804(3) 0.0490(9) Uani 1 1 d . . . H36 H -0.0962 0.9660 0.4698 0.059 Uiso 1 1 calc R . . N41 N 0.0814(2) 0.5862(2) 0.0761(2) 0.0413(7) Uani 1 1 d . . . C42 C 0.1205(3) 0.6398(3) -0.0204(3) 0.0525(10) Uani 1 1 d . . . H42 H 0.1216 0.7172 -0.0511 0.063 Uiso 1 1 calc R . . C43 C 0.1597(3) 0.5876(4) -0.0776(4) 0.0637(12) Uani 1 1 d . . . H43 H 0.1867 0.6287 -0.1464 0.076 Uiso 1 1 calc R . . C44 C 0.1590(3) 0.4758(4) -0.0339(4) 0.0615(11) Uani 1 1 d . . . H44 H 0.1855 0.4381 -0.0718 0.074 Uiso 1 1 calc R . . C45 C 0.1191(3) 0.4191(3) 0.0660(4) 0.0579(11) Uani 1 1 d . . . H45 H 0.1180 0.3415 0.0987 0.069 Uiso 1 1 calc R . . C46 C 0.0811(3) 0.4772(3) 0.1170(3) 0.0469(9) Uani 1 1 d . . . H46 H 0.0530 0.4378 0.1854 0.056 Uiso 1 1 calc R . . N51 N -0.28243(19) 0.8977(2) 0.2774(2) 0.0346(6) Uani 1 1 d . . . C52 C -0.3725(2) 0.9470(3) 0.2785(3) 0.0452(9) Uani 1 1 d . . . H52 H -0.3786 1.0125 0.2845 0.054 Uiso 1 1 calc R . . C53 C -0.4564(3) 0.9069(4) 0.2714(3) 0.0585(11) Uani 1 1 d . . . H53 H -0.5190 0.9437 0.2735 0.070 Uiso 1 1 calc R . . C54 C -0.4484(3) 0.8129(4) 0.2613(4) 0.0633(12) Uani 1 1 d . . . H54 H -0.5053 0.7843 0.2550 0.076 Uiso 1 1 calc R . . C55 C -0.3567(3) 0.7614(3) 0.2605(3) 0.0509(10) Uani 1 1 d . . . H55 H -0.3490 0.6958 0.2546 0.061 Uiso 1 1 calc R . . C56 C -0.2763(3) 0.8059(3) 0.2684(3) 0.0390(8) Uani 1 1 d . . . H56 H -0.2130 0.7697 0.2675 0.047 Uiso 1 1 calc R . . N61 N 0.1366(2) 0.5658(2) 0.2929(2) 0.0379(7) Uani 1 1 d . . . C62 C 0.2308(3) 0.5570(4) 0.2708(3) 0.0620(12) Uani 1 1 d . . . H62 H 0.2487 0.5967 0.1976 0.074 Uiso 1 1 calc R . . C63 C 0.3041(3) 0.4940(4) 0.3470(4) 0.0676(13) Uani 1 1 d . . . H63 H 0.3705 0.4905 0.3269 0.081 Uiso 1 1 calc R . . C64 C 0.2793(3) 0.4367(3) 0.4524(3) 0.0550(10) Uani 1 1 d . . . H64 H 0.3280 0.3910 0.5070 0.066 Uiso 1 1 calc R . . C65 C 0.1839(3) 0.4460(4) 0.4779(3) 0.0601(11) Uani 1 1 d . . . H65 H 0.1648 0.4087 0.5509 0.072 Uiso 1 1 calc R . . C66 C 0.1144(3) 0.5109(3) 0.3956(3) 0.0515(10) Uani 1 1 d . . . H66 H 0.0476 0.5162 0.4141 0.062 Uiso 1 1 calc R . . N1S N 0.4758(3) 0.6336(4) 0.5304(3) 0.0695(11) Uani 1 1 d D . . C2S C 0.4708(3) 0.7110(4) 0.5585(4) 0.0635(12) Uani 1 1 d D . . H2S H 0.5211 0.7576 0.5356 0.076 Uiso 1 1 calc R . . C3S C 0.3990(3) 0.7289(4) 0.6177(4) 0.0693(13) Uani 1 1 d D . . H3S H 0.3994 0.7860 0.6360 0.083 Uiso 1 1 calc R . . C4S C 0.3265(4) 0.6640(5) 0.6505(4) 0.0772(15) Uani 1 1 d D . . H4S H 0.2745 0.6755 0.6914 0.093 Uiso 1 1 calc R . . C5S C 0.3293(3) 0.5816(4) 0.6240(4) 0.0748(14) Uani 1 1 d D . . H5S H 0.2796 0.5342 0.6466 0.090 Uiso 1 1 calc R . . C6S C 0.4046(3) 0.5687(4) 0.5643(4) 0.0658(12) Uani 1 1 d D . . H6S H 0.4066 0.5112 0.5461 0.079 Uiso 1 1 calc R . . N1T N 0.4437(6) 0.6722(9) 0.1421(6) 0.0811(19) Uiso 0.569(5) 1 d PD A 1 C2T C 0.5083(6) 0.6254(8) 0.0987(8) 0.075(2) Uiso 0.569(5) 1 d PD A 1 H2T H 0.5614 0.5739 0.1430 0.090 Uiso 0.569(5) 1 calc PR A 1 C3T C 0.5014(8) 0.6480(9) -0.0063(9) 0.096(3) Uiso 0.569(5) 1 d PD A 1 H3T H 0.5487 0.6154 -0.0365 0.115 Uiso 0.569(5) 1 calc PR A 1 C4T C 0.4224(10) 0.7202(11) -0.0651(11) 0.104(3) Uiso 0.569(5) 1 d P A 1 H4T H 0.4139 0.7371 -0.1380 0.124 Uiso 0.569(5) 1 calc PR A 1 C5T C 0.3576(7) 0.7676(8) -0.0247(8) 0.073(2) Uiso 0.569(5) 1 d PD A 1 H5T H 0.3031 0.8170 -0.0678 0.088 Uiso 0.569(5) 1 calc PR A 1 C6T C 0.3692(7) 0.7456(8) 0.0763(9) 0.075(2) Uiso 0.569(5) 1 d PD A 1 H6T H 0.3236 0.7825 0.1039 0.090 Uiso 0.569(5) 1 calc PR A 1 N1U N 0.4215(9) 0.7250(10) 0.1070(9) 0.0811(19) Uiso 0.431(5) 1 d PD A 2 C2U C 0.4841(10) 0.6326(10) 0.1357(10) 0.075(2) Uiso 0.431(5) 1 d PD A 2 H2U H 0.5221 0.6017 0.2008 0.090 Uiso 0.431(5) 1 calc PR A 2 C3U C 0.4943(10) 0.5827(11) 0.0745(12) 0.096(3) Uiso 0.431(5) 1 d PD A 2 H3U H 0.5393 0.5174 0.0959 0.115 Uiso 0.431(5) 1 calc PR A 2 C4U C 0.4414(12) 0.6251(14) -0.0153(13) 0.104(3) Uiso 0.431(5) 1 d P A 2 H4U H 0.4522 0.5926 -0.0610 0.124 Uiso 0.431(5) 1 calc PR A 2 C5U C 0.3712(9) 0.7147(10) -0.0453(9) 0.073(2) Uiso 0.431(5) 1 d PD A 2 H5U H 0.3280 0.7402 -0.1059 0.088 Uiso 0.431(5) 1 calc PR A 2 C6U C 0.3671(9) 0.7654(11) 0.0177(13) 0.075(2) Uiso 0.431(5) 1 d PD A 2 H6U H 0.3237 0.8318 -0.0038 0.090 Uiso 0.431(5) 1 calc PR A 2 N1Q N -0.4141(7) 0.8525(10) 0.7150(9) 0.0754(17) Uiso 0.466(5) 1 d PD B 1 C2Q C -0.4088(9) 0.9341(8) 0.6171(11) 0.0664(19) Uiso 0.466(5) 1 d PD B 1 H2Q H -0.4476 1.0032 0.5968 0.080 Uiso 0.466(5) 1 calc PR B 1 C3Q C -0.3484(11) 0.9225(9) 0.5427(8) 0.066(2) Uiso 0.466(5) 1 d PD B 1 H3Q H -0.3483 0.9815 0.4707 0.079 Uiso 0.466(5) 1 calc PR B 1 C4Q C -0.2893(8) 0.8262(13) 0.5732(11) 0.064(2) Uiso 0.466(5) 1 d P B 1 H4Q H -0.2466 0.8170 0.5230 0.077 Uiso 0.466(5) 1 calc PR B 1 C5Q C -0.2915(9) 0.7406(9) 0.6786(12) 0.069(2) Uiso 0.466(5) 1 d PD B 1 H5Q H -0.2501 0.6724 0.7024 0.083 Uiso 0.466(5) 1 calc PR B 1 C6Q C -0.3547(12) 0.7579(9) 0.7463(10) 0.076(2) Uiso 0.466(5) 1 d PD B 1 H6Q H -0.3568 0.7006 0.8188 0.091 Uiso 0.466(5) 1 calc PR B 1 N1R N -0.4338(6) 0.8915(8) 0.6638(9) 0.0754(17) Uiso 0.534(5) 1 d PD B 2 C2R C -0.3864(8) 0.9341(7) 0.5740(9) 0.0664(19) Uiso 0.534(5) 1 d PD B 2 H2R H -0.4107 1.0066 0.5196 0.080 Uiso 0.534(5) 1 calc PR B 2 C3R C -0.3031(8) 0.8810(11) 0.5523(7) 0.066(2) Uiso 0.534(5) 1 d PD B 2 H3R H -0.2711 0.9148 0.4855 0.079 Uiso 0.534(5) 1 calc PR B 2 C4R C -0.2699(7) 0.7768(10) 0.6332(11) 0.064(2) Uiso 0.534(5) 1 d P B 2 H4R H -0.2140 0.7356 0.6227 0.077 Uiso 0.534(5) 1 calc PR B 2 C5R C -0.3176(8) 0.7318(7) 0.7296(9) 0.069(2) Uiso 0.534(5) 1 d PD B 2 H5R H -0.2928 0.6615 0.7873 0.083 Uiso 0.534(5) 1 calc PR B 2 C6R C -0.3997(9) 0.7889(11) 0.7410(8) 0.076(2) Uiso 0.534(5) 1 d PD B 2 H6R H -0.4348 0.7555 0.8057 0.091 Uiso 0.534(5) 1 calc PR B 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 0.0326(2) 0.0339(2) 0.0313(2) -0.01710(18) 0.00342(16) -0.00175(16) Cu2 0.0399(2) 0.0251(2) 0.0326(2) -0.01148(18) 0.00135(17) 0.00043(16) P1 0.0261(4) 0.0261(4) 0.0257(4) -0.0116(3) 0.0004(3) -0.0013(3) P2 0.0266(4) 0.0239(4) 0.0268(4) -0.0103(3) -0.0009(3) 0.0001(3) Cl2 0.0422(5) 0.0396(5) 0.0432(5) -0.0112(4) 0.0074(4) -0.0057(4) Cl1 0.0685(6) 0.0431(5) 0.0568(6) -0.0326(5) -0.0062(5) 0.0071(4) O1 0.0300(11) 0.0257(11) 0.0284(11) -0.0118(9) 0.0021(8) -0.0020(8) N1 0.0285(13) 0.0269(14) 0.0270(13) -0.0133(11) -0.0026(10) 0.0017(10) N11 0.0376(17) 0.0469(19) 0.060(2) -0.0154(16) -0.0050(15) 0.0051(14) C12 0.0253(15) 0.0364(18) 0.0268(16) -0.0092(14) 0.0004(12) -0.0065(13) C13 0.0393(19) 0.053(2) 0.047(2) -0.0343(19) 0.0033(16) -0.0108(16) C14 0.078(3) 0.104(4) 0.068(3) -0.060(3) 0.013(3) -0.045(3) C15 0.046(3) 0.134(5) 0.061(3) -0.030(3) -0.019(2) -0.024(3) C16 0.039(2) 0.072(3) 0.077(3) -0.012(3) -0.020(2) 0.009(2) N2 0.0237(12) 0.0272(13) 0.0288(14) -0.0131(11) -0.0005(10) -0.0011(10) N21 0.0319(14) 0.0355(16) 0.0375(16) -0.0156(13) -0.0024(12) 0.0002(12) C22 0.0291(16) 0.0289(17) 0.0239(16) -0.0090(13) 0.0027(12) -0.0050(13) C23 0.0383(18) 0.038(2) 0.047(2) -0.0238(17) -0.0085(15) 0.0009(15) C24 0.055(2) 0.051(2) 0.062(3) -0.032(2) -0.0152(19) -0.0073(19) C25 0.043(2) 0.060(3) 0.065(3) -0.026(2) -0.0199(19) -0.0071(19) C26 0.0322(19) 0.051(2) 0.057(2) -0.020(2) -0.0109(16) 0.0058(16) N31 0.0356(15) 0.0389(17) 0.0332(15) -0.0125(13) 0.0015(12) -0.0061(12) C32 0.054(2) 0.040(2) 0.048(2) -0.0143(18) -0.0063(18) -0.0021(18) C33 0.066(3) 0.048(3) 0.073(3) -0.011(2) -0.020(2) 0.010(2) C34 0.066(3) 0.077(3) 0.059(3) -0.018(3) -0.024(2) -0.006(2) C35 0.067(3) 0.080(3) 0.052(3) -0.029(2) -0.012(2) -0.014(2) C36 0.048(2) 0.057(2) 0.043(2) -0.0239(19) -0.0018(17) -0.0083(18) N41 0.0509(17) 0.0339(16) 0.0391(17) -0.0184(14) 0.0048(13) -0.0028(13) C42 0.068(3) 0.042(2) 0.051(2) -0.0245(19) 0.015(2) -0.0111(19) C43 0.081(3) 0.062(3) 0.059(3) -0.039(2) 0.020(2) -0.011(2) C44 0.075(3) 0.057(3) 0.071(3) -0.047(2) 0.008(2) -0.003(2) C45 0.074(3) 0.040(2) 0.066(3) -0.031(2) -0.006(2) 0.002(2) C46 0.056(2) 0.034(2) 0.046(2) -0.0167(17) 0.0016(17) -0.0026(16) N51 0.0331(14) 0.0398(16) 0.0305(15) -0.0165(13) 0.0027(11) -0.0059(12) C52 0.039(2) 0.053(2) 0.046(2) -0.0272(19) 0.0035(16) -0.0026(16) C53 0.031(2) 0.079(3) 0.065(3) -0.035(2) -0.0004(17) -0.0045(19) C54 0.049(2) 0.083(3) 0.062(3) -0.033(3) 0.003(2) -0.030(2) C55 0.064(3) 0.045(2) 0.044(2) -0.0185(18) 0.0046(18) -0.0222(19) C56 0.0450(19) 0.0329(19) 0.0328(18) -0.0107(15) 0.0041(15) -0.0067(15) N61 0.0431(16) 0.0301(15) 0.0348(16) -0.0118(13) -0.0008(12) -0.0017(12) C62 0.045(2) 0.072(3) 0.039(2) -0.005(2) 0.0038(17) -0.003(2) C63 0.044(2) 0.079(3) 0.055(3) -0.015(2) -0.0048(19) 0.002(2) C64 0.052(2) 0.052(2) 0.050(2) -0.017(2) -0.0167(19) 0.0008(18) C65 0.065(3) 0.068(3) 0.034(2) -0.015(2) -0.0049(18) -0.002(2) C66 0.050(2) 0.061(3) 0.037(2) -0.0207(19) -0.0021(17) 0.0035(18) N1S 0.047(2) 0.090(3) 0.081(3) -0.051(2) 0.0054(18) -0.002(2) C2S 0.049(2) 0.064(3) 0.077(3) -0.033(3) -0.005(2) -0.012(2) C3S 0.072(3) 0.071(3) 0.081(3) -0.053(3) -0.013(3) 0.006(3) C4S 0.068(3) 0.096(4) 0.075(3) -0.052(3) 0.015(2) 0.007(3) C5S 0.052(3) 0.073(3) 0.090(4) -0.030(3) 0.008(2) -0.019(2) C6S 0.058(3) 0.067(3) 0.090(4) -0.054(3) -0.012(2) 0.004(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 Cu1 N51 2.070(3) . ? Cu1 N31 2.098(3) . ? Cu1 P1 2.1482(8) . ? Cu1 Cl1 2.2909(10) . ? Cu2 N61 2.051(3) . ? Cu2 N41 2.084(3) . ? Cu2 P2 2.1308(9) . ? Cu2 Cl2 2.3135(10) . ? P1 O1 1.636(2) . ? P1 N2 1.708(3) . ? P1 N1 1.722(2) . ? P2 O1 1.648(2) 2_575 ? P2 N1 1.702(3) . ? P2 N2 1.713(2) . ? O1 P2 1.648(2) 2_575 ? N1 C12 1.405(4) . ? N11 C16 1.354(6) . ? N11 C12 1.343(4) . ? C12 C13 1.368(5) . ? C13 C14 1.393(6) . ? C14 C15 1.375(8) . ? C15 C16 1.353(8) . ? N2 C22 1.403(4) . ? N21 C26 1.349(4) . ? N21 C22 1.336(4) . ? C22 C23 1.382(5) . ? C23 C24 1.379(5) . ? C24 C25 1.375(5) . ? C25 C26 1.371(6) . ? N31 C32 1.330(5) . ? N31 C36 1.342(5) . ? C32 C33 1.388(6) . ? C33 C34 1.375(7) . ? C34 C35 1.365(7) . ? C35 C36 1.376(6) . ? N41 C42 1.333(5) . ? N41 C46 1.339(4) . ? C42 C43 1.383(5) . ? C43 C44 1.371(6) . ? C44 C45 1.378(6) . ? C45 C46 1.371(5) . ? N51 C56 1.336(4) . ? N51 C52 1.340(4) . ? C52 C53 1.372(5) . ? C53 C54 1.375(6) . ? C54 C55 1.371(6) . ? C55 C56 1.370(5) . ? N61 C66 1.321(5) . ? N61 C62 1.327(5) . ? C62 C63 1.373(6) . ? C63 C64 1.365(6) . ? C64 C65 1.356(6) . ? C65 C66 1.387(5) . ? N1S C2S 1.311(5) . ? N1S C6S 1.335(5) . ? C2S C3S 1.349(6) . ? C3S C4S 1.350(6) . ? C4S C5S 1.366(6) . ? C5S C6S 1.361(6) . ? N1T C6T 1.356(10) . ? N1T C2T 1.338(9) . ? C2T C3T 1.368(13) . ? C3T C4T 1.362(15) . ? C4T C5T 1.315(15) . ? C5T C6T 1.321(13) . ? N1U C6U 1.322(11) . ? N1U C2U 1.339(11) . ? C2U C3U 1.343(17) . ? C3U C4U 1.31(2) . ? C4U C5U 1.368(19) . ? C5U C6U 1.376(17) . ? N1Q C2Q 1.307(11) . ? N1Q C6Q 1.335(11) . ? C2Q C3Q 1.376(14) . ? C3Q C4Q 1.353(16) . ? C4Q C5Q 1.391(17) . ? C5Q C6Q 1.357(16) . ? N1R C2R 1.305(10) . ? N1R C6R 1.346(10) . ? C2R C3R 1.388(13) . ? C3R C4R 1.373(14) . ? C4R C5R 1.379(14) . ? C5R C6R 1.345(14) . ? 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 N51 Cu1 N31 105.91(11) . . ? N51 Cu1 P1 109.30(8) . . ? N31 Cu1 P1 110.18(8) . . ? N51 Cu1 Cl1 107.16(8) . . ? N31 Cu1 Cl1 103.40(9) . . ? P1 Cu1 Cl1 119.94(4) . . ? N61 Cu2 N41 95.33(11) . . ? N61 Cu2 P2 121.22(9) . . ? N41 Cu2 P2 115.15(8) . . ? N61 Cu2 Cl2 101.25(8) . . ? N41 Cu2 Cl2 107.33(9) . . ? P2 Cu2 Cl2 114.07(3) . . ? O1 P1 N2 106.18(12) . . ? O1 P1 N1 105.29(12) . . ? N2 P1 N1 79.85(12) . . ? O1 P1 Cu1 118.95(8) . . ? N2 P1 Cu1 121.56(9) . . ? N1 P1 Cu1 117.84(9) . . ? O1 P2 N1 105.25(12) 2_575 . ? O1 P2 N2 105.13(11) 2_575 . ? N1 P2 N2 80.25(12) . . ? O1 P2 Cu2 112.68(8) 2_575 . ? N1 P2 Cu2 126.95(9) . . ? N2 P2 Cu2 121.28(9) . . ? P2 O1 P1 136.46(13) 2_575 . ? C12 N1 P2 129.3(2) . . ? C12 N1 P1 128.9(2) . . ? P2 N1 P1 99.85(13) . . ? C16 N11 C12 115.8(4) . . ? N11 C12 C13 125.1(3) . . ? N11 C12 N1 115.2(3) . . ? C13 C12 N1 119.7(3) . . ? C12 C13 C14 116.4(4) . . ? C15 C14 C13 120.4(4) . . ? C14 C15 C16 118.3(4) . . ? N11 C16 C15 124.0(4) . . ? C22 N2 P1 127.1(2) . . ? C22 N2 P2 132.1(2) . . ? P1 N2 P2 99.96(13) . . ? C26 N21 C22 116.3(3) . . ? N21 C22 C23 123.8(3) . . ? N21 C22 N2 114.0(3) . . ? C23 C22 N2 122.2(3) . . ? C22 C23 C24 118.2(3) . . ? C25 C24 C23 119.4(4) . . ? C24 C25 C26 118.4(3) . . ? N21 C26 C25 123.9(3) . . ? C32 N31 C36 116.8(3) . . ? C32 N31 Cu1 123.0(3) . . ? C36 N31 Cu1 120.0(2) . . ? N31 C32 C33 123.2(4) . . ? C34 C33 C32 118.7(4) . . ? C35 C34 C33 118.8(4) . . ? C34 C35 C36 119.0(4) . . ? N31 C36 C35 123.4(4) . . ? C42 N41 C46 117.0(3) . . ? C42 N41 Cu2 124.4(3) . . ? C46 N41 Cu2 118.4(2) . . ? N41 C42 C43 122.9(4) . . ? C44 C43 C42 119.1(4) . . ? C43 C44 C45 118.8(4) . . ? C46 C45 C44 118.5(4) . . ? C45 C46 N41 123.8(4) . . ? C56 N51 C52 117.1(3) . . ? C56 N51 Cu1 120.6(2) . . ? C52 N51 Cu1 121.6(2) . . ? N51 C52 C53 122.9(4) . . ? C52 C53 C54 119.0(4) . . ? C53 C54 C55 118.7(4) . . ? C56 C55 C54 119.1(4) . . ? N51 C56 C55 123.2(3) . . ? C66 N61 C62 116.4(3) . . ? C66 N61 Cu2 122.8(2) . . ? C62 N61 Cu2 120.8(2) . . ? N61 C62 C63 124.1(4) . . ? C64 C63 C62 118.5(4) . . ? C65 C64 C63 118.8(4) . . ? C64 C65 C66 118.9(4) . . ? N61 C66 C65 123.3(4) . . ? C2S N1S C6S 116.6(4) . . ? N1S C2S C3S 124.3(4) . . ? C4S C3S C2S 118.8(4) . . ? C3S C4S C5S 118.9(4) . . ? C4S C5S C6S 118.6(4) . . ? N1S C6S C5S 122.8(4) . . ? C6T N1T C2T 116.8(7) . . ? C3T C2T N1T 123.1(8) . . ? C2T C3T C4T 115.8(9) . . ? C3T C4T C5T 122.6(11) . . ? C6T C5T C4T 119.3(9) . . ? C5T C6T N1T 122.4(8) . . ? C6U N1U C2U 118.6(9) . . ? C3U C2U N1U 121.5(9) . . ? C2U C3U C4U 119.3(12) . . ? C3U C4U C5U 122.1(15) . . ? C6U C5U C4U 115.9(10) . . ? N1U C6U C5U 122.3(11) . . ? C2Q N1Q C6Q 119.5(9) . . ? N1Q C2Q C3Q 121.6(8) . . ? C2Q C3Q C4Q 119.2(9) . . ? C5Q C4Q C3Q 119.5(10) . . ? C4Q C5Q C6Q 117.6(9) . . ? N1Q C6Q C5Q 122.5(10) . . ? C2R N1R C6R 117.8(8) . . ? N1R C2R C3R 124.7(8) . . ? C4R C3R C2R 115.9(8) . . ? C3R C4R C5R 120.1(9) . . ? C6R C5R C4R 119.1(8) . . ? N1R C6R C5R 122.2(8) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.811 _refine_diff_density_min -0.472 _refine_diff_density_rms 0.088