# CIF for NMe4[Cu(F4TCNQ)].H2O data_shelxl _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H14 Cu F4 N5 O' _chemical_formula_weight 431.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 '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' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P42/mmc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x, z+1/2' '-x, -y, z' 'y, -x, z+1/2' 'x, -y, -z' 'y, x, -z+1/2' '-x, y, -z' '-y, -x, -z+1/2' '-x, -y, -z' 'y, -x, -z-1/2' 'x, y, -z' '-y, x, -z-1/2' '-x, y, z' '-y, -x, z-1/2' 'x, -y, z' 'y, x, z-1/2' _cell_length_a 7.3888(2) _cell_length_b 7.3888(2) _cell_length_c 22.1438(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1208.93(6) _cell_formula_units_Z 2 _cell_measurement_temperature 250.01(10) _cell_measurement_reflns_used 1401 _cell_measurement_theta_min 3.9893 _cell_measurement_theta_max 74.5367 _exptl_crystal_description 'Gem' _exptl_crystal_colour 'Pale green' _exptl_crystal_size_max 0.4148 _exptl_crystal_size_mid 0.2029 _exptl_crystal_size_min 0.1580 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.186 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 436 _exptl_absorpt_coefficient_mu 1.667 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.86752 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET) (compiled Sep 14 2012,17:21:16) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 250.01(10) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'SuperNova (Cu) X-ray Source' _diffrn_radiation_monochromator 'mirror' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.2273 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2150 _diffrn_reflns_av_R_equivalents 0.0134 _diffrn_reflns_av_sigmaI/netI 0.0115 _diffrn_reflns_limit_h_min -2 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.99 _diffrn_reflns_theta_max 74.69 _reflns_number_total 731 _reflns_number_gt 694 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET) (compiled Sep 14 2012,17:21:16) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET) (compiled Sep 14 2012,17:21:16) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET) (compiled Sep 14 2012,17:21:16) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1242P)^2^+0.6942P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 731 _refine_ls_number_parameters 54 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0721 _refine_ls_R_factor_gt 0.0707 _refine_ls_wR_factor_ref 0.2173 _refine_ls_wR_factor_gt 0.2154 _refine_ls_goodness_of_fit_ref 1.326 _refine_ls_restrained_S_all 1.322 _refine_ls_shift/su_max 0.000 _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 1.0000 1.0000 0.7500 0.0394(5) Uani 1 8 d S . . F1 F 0.8115(5) 0.9341(7) 0.94124(14) 0.078(2) Uani 0.50 1 d P . . N1 N 0.7840(5) 1.0000 0.80295(14) 0.0545(10) Uani 1 2 d S . . C1 C 0.6588(6) 1.0000 0.83381(15) 0.0473(10) Uani 1 2 d S . . C2 C 0.5000 1.0000 0.8680(2) 0.0513(16) Uani 1 4 d S . . C3 C 0.5000 1.0000 0.9345(2) 0.0490(15) Uani 1 4 d S . . C4 C 0.6530(6) 0.9626(5) 0.96889(19) 0.0355(12) Uiso 0.50 1 d P . . N2 N 1.0000 0.5000 0.8681(5) 0.104(7) Uani 0.50 4 d SPD . . C5 C 0.835(3) 0.5000 0.8273(6) 0.108(6) Uani 0.50 2 d SP . . H5A H 0.7275 0.5000 0.8514 0.161 Uiso 0.50 2 calc SPR . . H5B H 0.8372 0.3939 0.8022 0.161 Uiso 0.25 1 calc PR . . H5C H 0.8372 0.6061 0.8022 0.161 Uiso 0.25 1 calc PR . . C6 C 1.0000 0.6736(11) 0.9054(6) 0.116(6) Uani 0.50 2 d SPD . . H6A H 1.0000 0.7764 0.8789 0.174 Uiso 0.50 2 calc SPRD . . H6B H 1.1061 0.6769 0.9304 0.174 Uiso 0.50 1 calc PRD . . H6C H 0.8939 0.6769 0.9304 0.174 Uiso 0.00 1 calc PR . . O1 O 0.457(2) 0.5000 1.0000 0.102(5) Uiso 0.50 4 d SP . . 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 0.0479(6) 0.0479(6) 0.0224(7) 0.000 0.000 0.000 F1 0.0387(15) 0.164(7) 0.0321(15) 0.0004(19) 0.0058(12) 0.014(2) N1 0.0455(18) 0.092(3) 0.0258(15) 0.000 0.0042(14) 0.000 C1 0.046(2) 0.072(3) 0.0245(16) 0.000 -0.0022(15) 0.000 C2 0.041(3) 0.090(5) 0.023(2) 0.000 0.000 0.000 C3 0.041(3) 0.081(4) 0.025(2) 0.000 0.000 0.000 N2 0.22(2) 0.053(7) 0.038(6) 0.000 0.000 0.000 C5 0.194(18) 0.072(7) 0.056(6) 0.000 0.005(10) 0.000 C6 0.21(2) 0.064(7) 0.070(8) -0.015(6) 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 1.980(3) 3_775 ? Cu1 N1 1.980(3) 12_757 ? Cu1 N1 1.980(3) 10_577 ? Cu1 N1 1.980(3) . ? F1 C4 1.338(5) . ? N1 C1 1.150(5) . ? C1 C2 1.397(5) . ? C2 C1 1.397(5) 3_675 ? C2 C3 1.471(7) . ? C3 C4 1.391(5) 15_575 ? C3 C4 1.391(5) . ? C3 C4 1.391(5) 13_655 ? C3 C4 1.391(5) 3_675 ? C4 C4 1.378(9) 11_557 ? N2 C5 1.516(19) . ? N2 C5 1.516(19) 3_765 ? N2 C6 1.526(7) . ? N2 C6 1.526(7) 3_765 ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? 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 110.52(10) 3_775 12_757 ? N1 Cu1 N1 110.52(10) 3_775 10_577 ? N1 Cu1 N1 107.39(19) 12_757 10_577 ? N1 Cu1 N1 107.39(19) 3_775 . ? N1 Cu1 N1 110.52(10) 12_757 . ? N1 Cu1 N1 110.52(10) 10_577 . ? C1 N1 Cu1 179.9(3) . . ? N1 C1 C2 176.4(4) . . ? C1 C2 C1 114.3(5) 3_675 . ? C1 C2 C3 122.9(2) 3_675 . ? C1 C2 C3 122.9(2) . . ? C4 C3 C4 22.9(3) 15_575 . ? C4 C3 C4 113.5(5) 15_575 13_655 ? C4 C3 C4 108.7(5) . 13_655 ? C4 C3 C4 108.7(5) 15_575 3_675 ? C4 C3 C4 113.5(5) . 3_675 ? C4 C3 C4 22.9(3) 13_655 3_675 ? C4 C3 C2 123.2(3) 15_575 . ? C4 C3 C2 123.2(3) . . ? C4 C3 C2 123.2(3) 13_655 . ? C4 C3 C2 123.2(3) 3_675 . ? F1 C4 C4 117.2(2) . 11_557 ? F1 C4 C3 119.4(4) . . ? C4 C4 C3 123.2(3) 11_557 . ? C5 N2 C5 106.7(13) . 3_765 ? C5 N2 C6 108.9(4) . . ? C5 N2 C6 108.9(4) 3_765 . ? C5 N2 C6 108.9(4) . 3_765 ? C5 N2 C6 108.9(4) 3_765 3_765 ? C6 N2 C6 114.4(11) . 3_765 ? N2 C5 H5A 109.5 . . ? N2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N2 C6 H6A 109.5 . . ? N2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Cu1 N1 C1 0(100) 3_775 . . . ? N1 Cu1 N1 C1 121(100) 12_757 . . . ? N1 Cu1 N1 C1 -121(100) 10_577 . . . ? Cu1 N1 C1 C2 180(100) . . . . ? N1 C1 C2 C1 0.00(3) . . . 3_675 ? N1 C1 C2 C3 180.00(3) . . . . ? C1 C2 C3 C4 -166.3(2) 3_675 . . 15_575 ? C1 C2 C3 C4 13.7(2) . . . 15_575 ? C1 C2 C3 C4 166.3(2) 3_675 . . . ? C1 C2 C3 C4 -13.7(2) . . . . ? C1 C2 C3 C4 13.7(2) 3_675 . . 13_655 ? C1 C2 C3 C4 -166.3(2) . . . 13_655 ? C1 C2 C3 C4 -13.7(2) 3_675 . . 3_675 ? C1 C2 C3 C4 166.3(2) . . . 3_675 ? C4 C3 C4 F1 -94.0(4) 15_575 . . . ? C4 C3 C4 F1 159.6(3) 13_655 . . . ? C4 C3 C4 F1 -176.4(5) 3_675 . . . ? C2 C3 C4 F1 3.6(5) . . . . ? C4 C3 C4 C4 82.37(12) 15_575 . . 11_557 ? C4 C3 C4 C4 -24.0(3) 13_655 . . 11_557 ? C4 C3 C4 C4 0.000(2) 3_675 . . 11_557 ? C2 C3 C4 C4 180.000(4) . . . 11_557 ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 74.69 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 1.021 _refine_diff_density_min -0.413 _refine_diff_density_rms 0.151 #CIF for N(CH3)2(C3H7)2[Cu(F4TCNQ)].3EtOH data_shelxl _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H38 Cu F4 N5 O3' _chemical_formula_weight 608.15 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4(2)/mmc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z+1/2' 'y, -x, z+1/2' '-x, y, -z' 'x, -y, -z' 'y, x, -z+1/2' '-y, -x, -z+1/2' '-x, -y, -z' 'x, y, -z' 'y, -x, -z-1/2' '-y, x, -z-1/2' 'x, -y, z' '-x, y, z' '-y, -x, z-1/2' 'y, x, z-1/2' _cell_length_a 7.4617(3) _cell_length_b 7.4617(3) _cell_length_c 22.0049(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1225.17(9) _cell_formula_units_Z 2 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 1489 _cell_measurement_theta_min 4.0175 _cell_measurement_theta_max 74.5122 _exptl_crystal_description 'Square Bipyramidal' _exptl_crystal_colour 'Pale Yellow' _exptl_crystal_size_max 0.3515 _exptl_crystal_size_mid 0.1320 _exptl_crystal_size_min 0.1058 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.649 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 636 _exptl_absorpt_coefficient_mu 1.894 _exptl_absorpt_correction_type 'gaussian' _exptl_absorpt_correction_T_min 0.747 _exptl_absorpt_correction_T_max 0.871 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET) (compiled Jul 11 2012,15:38:31) Numerical absorption correction based on gaussian integration over a multifaceted crystal model ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'SuperNova (Cu) X-ray Source' _diffrn_radiation_monochromator 'mirror' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.2273 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2245 _diffrn_reflns_av_R_equivalents 0.0118 _diffrn_reflns_av_sigmaI/netI 0.0099 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 4.02 _diffrn_reflns_theta_max 74.50 _reflns_number_total 742 _reflns_number_gt 699 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET) (compiled Jul 11 2012,15:38:31) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET) (compiled Jul 11 2012,15:38:31) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET) (compiled Jul 11 2012,15:38:31) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0852P)^2^+1.2552P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens . _refine_ls_hydrogen_treatment . _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 742 _refine_ls_number_parameters 35 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0522 _refine_ls_R_factor_gt 0.0508 _refine_ls_wR_factor_ref 0.1698 _refine_ls_wR_factor_gt 0.1687 _refine_ls_goodness_of_fit_ref 1.203 _refine_ls_restrained_S_all 1.203 _refine_ls_shift/su_max 0.000 _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 0.2500 0.0360(4) Uani 1 8 d S . . C3 C 0.5000 0.0000 0.0664(2) 0.0412(12) Uani 1 4 d S . . C1 C 0.5000 0.1584(5) 0.16761(17) 0.0478(10) Uani 1 2 d S . . N1 N 0.5000 0.2814(5) 0.19817(14) 0.0542(10) Uani 1 2 d S . . C2 C 0.5000 0.0000 0.1327(2) 0.0419(12) Uani 1 4 d S . . F1 F 0.5000 0.3127(4) 0.05878(12) 0.125(2) Uani 1 2 d S . . C4 C 0.5000 0.1552(5) 0.03149(18) 0.0560(12) 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 0.0433(5) 0.0433(5) 0.0215(6) 0.000 0.000 0.000 C3 0.049(3) 0.035(3) 0.041(3) 0.000 0.000 0.000 C1 0.066(3) 0.040(2) 0.0373(17) 0.0050(17) 0.000 0.000 N1 0.093(3) 0.0372(17) 0.0327(15) -0.0020(14) 0.000 0.000 C2 0.055(3) 0.032(2) 0.039(3) 0.000 0.000 0.000 F1 0.307(7) 0.0285(13) 0.0397(13) -0.0042(11) 0.000 0.000 C4 0.098(4) 0.0297(18) 0.041(2) -0.0047(16) 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 1.990(3) 2_665 ? Cu1 N1 1.990(3) . ? Cu1 N1 1.990(3) 12_656 ? Cu1 N1 1.990(3) 11_566 ? C3 C4 1.390(5) 2_655 ? C3 C4 1.390(5) . ? C3 C2 1.458(7) . ? C1 N1 1.138(5) . ? C1 C2 1.409(5) . ? C2 C1 1.409(5) 2_655 ? F1 C4 1.320(5) . ? C4 C4 1.386(8) 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 N1 Cu1 N1 110.07(18) 2_665 . ? N1 Cu1 N1 109.17(9) 2_665 12_656 ? N1 Cu1 N1 109.17(9) . 12_656 ? N1 Cu1 N1 109.17(9) 2_665 11_566 ? N1 Cu1 N1 109.17(9) . 11_566 ? N1 Cu1 N1 110.07(18) 12_656 11_566 ? C4 C3 C4 112.8(5) 2_655 . ? C4 C3 C2 123.6(2) 2_655 . ? C4 C3 C2 123.6(2) . . ? N1 C1 C2 176.8(4) . . ? C1 N1 Cu1 178.7(3) . . ? C1 C2 C1 114.0(5) . 2_655 ? C1 C2 C3 123.0(2) . . ? C1 C2 C3 123.0(2) 2_655 . ? F1 C4 C4 117.1(2) . 10 ? F1 C4 C3 119.4(3) . . ? C4 C4 C3 123.6(2) 10 . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 74.50 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.440 _refine_diff_density_min -0.479 _refine_diff_density_rms 0.075 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.020 -0.013 -0.006 768 229 ' ' _platon_squeeze_details ; ; # CIF for (N(Me)2(Bu)2)[Cu(F4TCNQ)] data_shelxl _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H36 Cu F4 N5 O2' _chemical_formula_weight 590.14 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0727 0.0534 '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' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P42/mmc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, -z' '-x, -y, z' '-x, y, -z' 'y, x, -z+1/2' 'y, -x, z+1/2' '-y, x, z+1/2' '-y, -x, -z+1/2' '-x, -y, -z' '-x, y, z' 'x, y, -z' 'x, -y, z' '-y, -x, z-1/2' '-y, x, -z-1/2' 'y, -x, -z-1/2' 'y, x, z-1/2' _cell_length_a 7.47360(10) _cell_length_b 7.47360(10) _cell_length_c 22.0963(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1234.18(3) _cell_formula_units_Z 2 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 1691 _cell_measurement_theta_min 5.9158 _cell_measurement_theta_max 74.0924 _exptl_crystal_description 'Block' _exptl_crystal_colour 'Pale yellow' _exptl_crystal_size_max 0.2581 _exptl_crystal_size_mid 0.1721 _exptl_crystal_size_min 0.0951 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.588 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 616 _exptl_absorpt_coefficient_mu 2.005 _exptl_absorpt_correction_type 'gaussian' _exptl_absorpt_correction_T_min 0.722 _exptl_absorpt_correction_T_max 0.833 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET) (compiled Jul 11 2012,15:38:31) Numerical absorption correction based on gaussian integration over a multifaceted crystal model ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'SuperNova (Cu) X-ray Source' _diffrn_radiation_monochromator 'mirror' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.2273 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2331 _diffrn_reflns_av_R_equivalents 0.0108 _diffrn_reflns_av_sigmaI/netI 0.0093 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 5.92 _diffrn_reflns_theta_max 74.26 _reflns_number_total 735 _reflns_number_gt 704 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET) (compiled Jul 11 2012,15:38:31) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET) (compiled Jul 11 2012,15:38:31) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET) (compiled Jul 11 2012,15:38:31) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0812P)^2^+1.9436P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens . _refine_ls_hydrogen_treatment . _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 735 _refine_ls_number_parameters 35 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0497 _refine_ls_R_factor_gt 0.0487 _refine_ls_wR_factor_ref 0.1549 _refine_ls_wR_factor_gt 0.1541 _refine_ls_goodness_of_fit_ref 1.138 _refine_ls_restrained_S_all 1.138 _refine_ls_shift/su_max 0.000 _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 0.2500 0.0234(4) Uani 1 8 d S . . C3 C 0.5000 0.0000 0.0662(2) 0.0241(10) Uani 1 4 d S . . C1 C 0.5000 0.1585(5) 0.16700(14) 0.0265(7) Uani 1 2 d S . . N1 N 0.5000 0.2816(4) 0.19771(12) 0.0325(7) Uani 1 2 d S . . C4 C 0.5000 0.1539(5) 0.03137(15) 0.0380(10) Uani 1 2 d S . . C2 C 0.5000 0.0000 0.1326(2) 0.0244(9) Uani 1 4 d S . . F1 F 0.5000 0.3121(4) 0.05868(10) 0.1083(19) 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 0.0278(5) 0.0278(5) 0.0146(5) 0.000 0.000 0.000 C3 0.027(2) 0.024(2) 0.021(2) 0.000 0.000 0.000 C1 0.0322(17) 0.0279(18) 0.0193(14) 0.0040(13) 0.000 0.000 N1 0.0525(19) 0.0256(15) 0.0193(13) -0.0004(12) 0.000 0.000 C4 0.071(3) 0.0207(17) 0.0227(17) -0.0025(13) 0.000 0.000 C2 0.029(2) 0.024(2) 0.020(2) 0.000 0.000 0.000 F1 0.284(6) 0.0188(12) 0.0216(11) -0.0038(9) 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 2.000(3) . ? Cu1 N1 2.000(3) 14_656 ? Cu1 N1 2.000(3) 3_665 ? Cu1 N1 2.000(3) 5 ? C3 C4 1.384(4) 3_655 ? C3 C4 1.384(4) . ? C3 C2 1.467(6) . ? C1 N1 1.143(4) . ? C1 C2 1.407(4) . ? C4 F1 1.328(4) . ? C4 C4 1.386(7) 11 ? C2 C1 1.407(4) 3_655 ? 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 109.50(8) . 14_656 ? N1 Cu1 N1 109.41(16) . 3_665 ? N1 Cu1 N1 109.50(8) 14_656 3_665 ? N1 Cu1 N1 109.50(8) . 5 ? N1 Cu1 N1 109.41(16) 14_656 5 ? N1 Cu1 N1 109.50(8) 3_665 5 ? C4 C3 C4 112.4(4) 3_655 . ? C4 C3 C2 123.8(2) 3_655 . ? C4 C3 C2 123.8(2) . . ? N1 C1 C2 176.3(3) . . ? C1 N1 Cu1 178.9(3) . . ? F1 C4 C3 119.1(3) . . ? F1 C4 C4 117.04(17) . 11 ? C3 C4 C4 123.8(2) . 11 ? C1 C2 C1 114.7(4) . 3_655 ? C1 C2 C3 122.67(19) . . ? C1 C2 C3 122.67(19) 3_655 . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 74.26 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 0.565 _refine_diff_density_min -0.487 _refine_diff_density_rms 0.072 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.020 -0.015 -0.006 781 245 ' ' _platon_squeeze_details ; ; data_shelxl _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (NEt4)[Cu(F4TCNQ)].DMSO _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H26 Cu F4 N5 O S' _chemical_formula_weight 548.08 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Orthorhombic' _symmetry_space_group_name_H-M 'Pnna' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' '-x+1/2, y+1/2, -z+1/2' 'x, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' 'x-1/2, -y-1/2, z-1/2' '-x, y-1/2, z-1/2' _cell_length_a 22.1760(4) _cell_length_b 9.6360(3) _cell_length_c 11.2931(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2413.20(11) _cell_formula_units_Z 4 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 2859 _cell_measurement_theta_min 3.9106 _cell_measurement_theta_max 74.4517 _exptl_crystal_description 'block' _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.0918 _exptl_crystal_size_mid 0.0754 _exptl_crystal_size_min 0.0526 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.509 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1128 _exptl_absorpt_coefficient_mu 2.585 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.14358 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'SuperNova (Cu) X-ray Source' _diffrn_radiation_monochromator 'mirror' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.2273 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6010 _diffrn_reflns_av_R_equivalents 0.0210 _diffrn_reflns_av_sigmaI/netI 0.0215 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.99 _diffrn_reflns_theta_max 74.59 _reflns_number_total 2417 _reflns_number_gt 2062 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0852P)^2^+3.9524P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2417 _refine_ls_number_parameters 163 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0571 _refine_ls_R_factor_gt 0.0491 _refine_ls_wR_factor_ref 0.1540 _refine_ls_wR_factor_gt 0.1456 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _refine_ls_shift/su_max 0.000 _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 S1 S 0.62344(16) 0.2992(5) 0.2898(3) 0.0981(11) Uani 0.50 1 d P . . C111 C 0.6702(3) 0.3380(8) 0.1583(6) 0.0888(19) Uani 1 1 d . . . O1 O 0.5672(5) 0.1986(12) 0.2344(13) 0.129(4) Uiso 0.50 1 d P . . Cu1 Cu 0.2500 0.0000 0.99140(4) 0.0141(2) Uani 1 2 d S . . F2 F 0.56251(7) 0.35390(18) 0.56017(13) 0.0211(4) Uani 1 1 d . . . F1 F 0.44515(7) 0.36117(17) 0.56326(13) 0.0204(4) Uani 1 1 d . . . C7 C 0.36417(15) -0.2500 1.2500 0.0146(7) Uani 1 2 d S . . N2 N 0.29969(10) -0.1180(2) 1.0998(2) 0.0187(5) Uani 1 1 d . . . N1 N 0.30517(10) 0.1098(2) 0.8902(2) 0.0199(5) Uani 1 1 d . . . C3 C 0.43775(15) 0.2500 0.7500 0.0131(7) Uani 1 2 d S . . C5 C 0.53495(11) 0.3022(3) 0.6567(2) 0.0139(5) Uani 1 1 d . . . C4 C 0.47272(11) 0.3043(3) 0.6578(2) 0.0146(5) Uani 1 1 d . . . C1 C 0.33719(11) 0.1716(3) 0.8291(2) 0.0156(5) Uani 1 1 d . . . C6 C 0.33006(11) -0.1775(2) 1.1657(2) 0.0146(5) Uani 1 1 d . . . C2 C 0.37190(16) 0.2500 0.7500 0.0159(7) Uani 1 2 d S . . C8 C 0.56982(15) 0.2500 0.7500 0.0129(7) Uani 1 2 d S . . N20 N 0.60952(15) 0.7500 -0.2500 0.0209(7) Uani 1 2 d S . . C23 C 0.64830(13) 0.7544(3) -0.1400(3) 0.0238(6) Uani 1 1 d . . . H23A H 0.6216 0.7615 -0.0699 0.029 Uiso 1 1 calc R . . H23B H 0.6734 0.8393 -0.1425 0.029 Uiso 1 1 calc R . . C21 C 0.56999(13) 0.8792(3) -0.2485(3) 0.0269(6) Uani 1 1 d . . . H21A H 0.5410 0.8709 -0.1821 0.032 Uiso 1 1 calc R . . H21B H 0.5959 0.9606 -0.2322 0.032 Uiso 1 1 calc R . . C24 C 0.68951(14) 0.6295(3) -0.1241(3) 0.0290(7) Uani 1 1 d . . . H24A H 0.7180 0.6248 -0.1903 0.044 Uiso 1 1 calc R . . H24B H 0.6652 0.5446 -0.1220 0.044 Uiso 1 1 calc R . . H24C H 0.7119 0.6387 -0.0496 0.044 Uiso 1 1 calc R . . C22 C 0.53488(16) 0.9066(4) -0.3609(4) 0.0412(9) Uani 1 1 d . . . H22A H 0.5111 0.8243 -0.3812 0.062 Uiso 1 1 calc R . . H22B H 0.5630 0.9274 -0.4255 0.062 Uiso 1 1 calc R . . H22C H 0.5079 0.9858 -0.3487 0.062 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 S1 0.0732(19) 0.130(3) 0.091(2) 0.014(2) 0.0187(17) 0.0250(19) C111 0.079(4) 0.101(5) 0.087(4) -0.008(4) 0.020(3) 0.010(3) Cu1 0.0106(3) 0.0175(3) 0.0142(3) 0.000 0.000 -0.00101(18) F2 0.0140(7) 0.0334(9) 0.0160(8) 0.0101(6) 0.0011(6) -0.0034(6) F1 0.0134(7) 0.0318(9) 0.0159(8) 0.0106(6) -0.0034(6) -0.0007(6) C7 0.0107(16) 0.0166(16) 0.0165(16) 0.0038(13) 0.000 0.000 N2 0.0110(10) 0.0232(11) 0.0218(11) 0.0049(9) 0.0001(9) 0.0001(8) N1 0.0115(10) 0.0286(12) 0.0195(11) 0.0056(9) -0.0007(8) -0.0025(9) C3 0.0111(16) 0.0159(16) 0.0124(16) 0.0007(12) 0.000 0.000 C5 0.0131(12) 0.0160(11) 0.0126(11) 0.0028(9) 0.0023(9) -0.0027(9) C4 0.0133(12) 0.0180(12) 0.0125(11) 0.0025(9) -0.0034(9) 0.0003(9) C1 0.0116(11) 0.0199(12) 0.0154(12) 0.0001(10) -0.0028(9) 0.0010(9) C6 0.0103(11) 0.0160(12) 0.0174(12) -0.0001(10) 0.0028(9) -0.0026(9) C2 0.0107(16) 0.0185(16) 0.0185(17) 0.0042(13) 0.000 0.000 C8 0.0107(16) 0.0137(15) 0.0145(16) -0.0007(12) 0.000 0.000 N20 0.0183(15) 0.0189(15) 0.0254(17) -0.0066(13) 0.000 0.000 C23 0.0215(13) 0.0253(13) 0.0245(14) -0.0066(11) 0.0005(11) -0.0025(11) C21 0.0229(13) 0.0212(14) 0.0366(16) -0.0098(12) -0.0017(12) 0.0034(11) C24 0.0278(15) 0.0287(15) 0.0306(15) -0.0008(12) -0.0035(12) 0.0011(12) C22 0.0362(18) 0.0337(17) 0.054(2) -0.0112(16) -0.0169(16) 0.0132(15) _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 S1 O1 1.276(11) 4 ? S1 S1 1.306(8) 4 ? S1 O1 1.698(11) . ? S1 C111 1.780(8) 4 ? S1 C111 1.850(7) . ? C111 S1 1.780(8) 4 ? O1 O1 1.05(2) 4 ? O1 S1 1.276(11) 4 ? Cu1 N1 1.980(2) 2 ? Cu1 N1 1.980(2) . ? Cu1 N2 2.002(2) . ? Cu1 N2 2.002(2) 2 ? F2 C5 1.345(3) . ? F1 C4 1.347(3) . ? C7 C6 1.402(3) 4_547 ? C7 C6 1.402(3) . ? C7 C8 1.464(4) 5_657 ? N2 C6 1.156(3) . ? N1 C1 1.156(3) . ? C3 C4 1.400(3) 4_556 ? C3 C4 1.400(3) . ? C3 C2 1.460(5) . ? C5 C4 1.380(4) . ? C5 C8 1.400(3) . ? C1 C2 1.400(3) . ? C2 C1 1.400(3) 4_556 ? C8 C5 1.400(3) 4_556 ? C8 C7 1.464(4) 5_657 ? N20 C23 1.512(3) . ? N20 C23 1.512(3) 4_564 ? N20 C21 1.522(3) 4_564 ? N20 C21 1.522(3) . ? C23 C24 1.522(4) . ? C21 C22 1.513(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 O1 S1 S1 82.2(6) 4 4 ? O1 S1 O1 38.2(8) 4 . ? S1 S1 O1 48.1(4) 4 . ? O1 S1 C111 130.7(7) 4 4 ? S1 S1 C111 71.8(4) 4 4 ? O1 S1 C111 97.2(5) . 4 ? O1 S1 C111 111.9(8) 4 . ? S1 S1 C111 66.1(3) 4 . ? O1 S1 C111 103.4(6) . . ? C111 S1 C111 95.0(5) 4 . ? S1 C111 S1 42.1(3) 4 . ? O1 O1 S1 93.2(6) 4 4 ? O1 O1 S1 48.6(5) 4 . ? S1 O1 S1 49.6(5) 4 . ? N1 Cu1 N1 109.50(13) 2 . ? N1 Cu1 N2 112.93(10) 2 . ? N1 Cu1 N2 108.44(9) . . ? N1 Cu1 N2 108.44(9) 2 2 ? N1 Cu1 N2 112.93(10) . 2 ? N2 Cu1 N2 104.58(13) . 2 ? C6 C7 C6 114.7(3) 4_547 . ? C6 C7 C8 122.64(15) 4_547 5_657 ? C6 C7 C8 122.64(15) . 5_657 ? C6 N2 Cu1 175.1(2) . . ? C1 N1 Cu1 178.4(2) . . ? C4 C3 C4 112.7(3) 4_556 . ? C4 C3 C2 123.64(16) 4_556 . ? C4 C3 C2 123.64(16) . . ? F2 C5 C4 117.1(2) . . ? F2 C5 C8 119.5(2) . . ? C4 C5 C8 123.4(2) . . ? F1 C4 C5 116.9(2) . . ? F1 C4 C3 119.4(2) . . ? C5 C4 C3 123.7(2) . . ? N1 C1 C2 175.4(3) . . ? N2 C6 C7 176.8(3) . . ? C1 C2 C1 113.3(3) 4_556 . ? C1 C2 C3 123.35(16) 4_556 . ? C1 C2 C3 123.35(16) . . ? C5 C8 C5 113.0(3) . 4_556 ? C5 C8 C7 123.52(15) . 5_657 ? C5 C8 C7 123.52(15) 4_556 5_657 ? C23 N20 C23 110.7(3) . 4_564 ? C23 N20 C21 111.09(17) . 4_564 ? C23 N20 C21 107.18(16) 4_564 4_564 ? C23 N20 C21 107.18(16) . . ? C23 N20 C21 111.09(17) 4_564 . ? C21 N20 C21 109.7(3) 4_564 . ? N20 C23 C24 114.6(2) . . ? C22 C21 N20 115.4(2) . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 74.59 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.842 _refine_diff_density_min -0.898 _refine_diff_density_rms 0.093 #### # CIF for P(C6H5)4[Cu(F4TCNQ)] data_shelxl _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37.50 H23.50 Cu F4 N4.50 O0.50 P' _chemical_formula_weight 715.62 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.2955 0.4335 '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/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 18.2594(6) _cell_length_b 11.8015(3) _cell_length_c 14.9782(4) _cell_angle_alpha 90.00 _cell_angle_beta 108.109(3) _cell_angle_gamma 90.00 _cell_volume 3067.75(15) _cell_formula_units_Z 4 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 6470 _cell_measurement_theta_min 3.1016 _cell_measurement_theta_max 74.2793 _exptl_crystal_description Block _exptl_crystal_colour 'Dark green' _exptl_crystal_size_max 0.3515 _exptl_crystal_size_mid 0.1320 _exptl_crystal_size_min 0.1058 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.549 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1456 _exptl_absorpt_coefficient_mu 2.042 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.88876 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_source 'SuperNova (Cu) X-ray Source' _diffrn_radiation_monochromator 'mirror' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.2273 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11902 _diffrn_reflns_av_R_equivalents 0.0241 _diffrn_reflns_av_sigmaI/netI 0.0307 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.75 _diffrn_reflns_theta_max 74.45 _reflns_number_total 6123 _reflns_number_gt 5410 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0622P)^2^+0.6998P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6123 _refine_ls_number_parameters 417 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0411 _refine_ls_R_factor_gt 0.0366 _refine_ls_wR_factor_ref 0.1030 _refine_ls_wR_factor_gt 0.0987 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.000 _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 F3 F 0.42898(7) 0.01436(15) 0.38308(8) 0.0512(4) Uani 1 1 d . . . F4 F 0.57890(7) 0.01056(16) 0.43507(8) 0.0542(4) Uani 1 1 d . . . N2 N 0.24664(8) 0.02306(14) 0.02030(10) 0.0260(3) Uani 1 1 d . . . N3 N 0.25297(9) 0.00188(14) 0.30576(11) 0.0274(3) Uani 1 1 d . . . C14 C 0.33211(10) 0.01146(16) 0.19153(12) 0.0257(3) Uani 1 1 d . . . C13 C 0.29045(10) 0.00682(15) 0.25632(12) 0.0246(3) Uani 1 1 d . . . C18 C 0.28664(9) 0.01880(15) 0.09712(12) 0.0239(3) Uani 1 1 d . . . C16 C 0.46217(11) 0.01073(18) 0.31450(12) 0.0300(4) Uani 1 1 d . . . C15 C 0.41586(10) 0.00976(16) 0.22073(12) 0.0253(3) Uani 1 1 d . . . C17 C 0.54135(10) 0.00956(18) 0.34179(12) 0.0308(4) Uani 1 1 d . . . Cu1 Cu 0.185612(13) 0.01283(2) -0.112458(16) 0.02302(9) Uani 1 1 d . . . F1 F -0.12488(6) -0.37670(9) -0.36202(7) 0.0310(2) Uani 1 1 d . . . F2 F -0.12633(6) 0.40371(10) -0.35653(8) 0.0349(2) Uani 1 1 d . . . C5 C -0.06146(9) 0.45627(16) -0.30269(11) 0.0248(3) Uani 1 1 d . . . C3 C 0.0000 -0.3611(2) -0.2500 0.0246(4) Uani 1 2 d S . . N4 N 0.11369(8) 0.14388(13) -0.15826(10) 0.0274(3) Uani 1 1 d . . . C6 C 0.0000 0.3895(2) -0.2500 0.0226(4) Uani 1 2 d S . . C4 C -0.06132(9) -0.42771(16) -0.30426(11) 0.0247(3) Uani 1 1 d . . . N1 N 0.11000(9) -0.11437(14) -0.14999(11) 0.0312(3) Uani 1 1 d . . . C8 C 0.06343(9) 0.20166(14) -0.19885(11) 0.0234(3) Uani 1 1 d . . . C2 C 0.0000 -0.2383(2) -0.2500 0.0265(5) Uani 1 2 d S . . C1 C 0.06150(9) -0.17298(15) -0.19386(12) 0.0263(3) Uani 1 1 d . . . C7 C 0.0000 0.2669(2) -0.2500 0.0241(4) Uani 1 2 d S . . P1 P 0.24996(2) 0.61265(4) 0.14103(3) 0.02789(11) Uani 1 1 d . . . C35 C 0.20850(11) 0.40168(17) 0.06358(13) 0.0330(4) Uani 1 1 d . . . H35 H 0.2080 0.4363 0.0061 0.040 Uiso 1 1 calc R . . C40 C 0.30051(10) 0.63503(18) 0.05647(12) 0.0310(4) Uani 1 1 d . . . C50 C 0.16000(10) 0.68804(17) 0.10503(12) 0.0305(4) Uani 1 1 d . . . C60 C 0.30978(10) 0.66626(16) 0.25220(13) 0.0305(4) Uani 1 1 d . . . C33 C 0.18779(11) 0.23920(17) 0.14894(14) 0.0345(4) Uani 1 1 d . . . H33 H 0.1724 0.1624 0.1497 0.041 Uiso 1 1 calc R . . C52 C 0.09013(12) 0.8636(2) 0.08840(16) 0.0406(4) Uani 1 1 d . . . H52 H 0.0888 0.9423 0.1012 0.049 Uiso 1 1 calc R . . C32 C 0.21094(12) 0.30091(18) 0.23200(14) 0.0362(4) Uani 1 1 d . . . H32 H 0.2120 0.2657 0.2894 0.043 Uiso 1 1 calc R . . C30 C 0.23098(11) 0.46394(16) 0.14698(13) 0.0301(4) Uani 1 1 d . . . C51 C 0.15829(11) 0.80363(18) 0.12372(14) 0.0359(4) Uani 1 1 d . . . H51 H 0.2037 0.8411 0.1605 0.043 Uiso 1 1 calc R . . C55 C 0.09296(11) 0.6332(2) 0.05185(14) 0.0372(4) Uani 1 1 d . . . H55 H 0.0936 0.5542 0.0398 0.045 Uiso 1 1 calc R . . C31 C 0.23243(11) 0.41341(18) 0.23174(13) 0.0337(4) Uani 1 1 d . . . H31 H 0.2479 0.4556 0.2885 0.040 Uiso 1 1 calc R . . C45 C 0.29522(12) 0.74008(19) 0.01356(14) 0.0371(4) Uani 1 1 d . . . H45 H 0.2612 0.7959 0.0239 0.045 Uiso 1 1 calc R . . C54 C 0.02543(11) 0.6948(2) 0.01673(15) 0.0422(5) Uani 1 1 d . . . H54 H -0.0202 0.6578 -0.0199 0.051 Uiso 1 1 calc R . . C41 C 0.34921(12) 0.55146(19) 0.04016(15) 0.0379(4) Uani 1 1 d . . . H41 H 0.3533 0.4797 0.0700 0.045 Uiso 1 1 calc R . . C34 C 0.18704(11) 0.28969(18) 0.06473(14) 0.0349(4) Uani 1 1 d . . . H34 H 0.1718 0.2471 0.0081 0.042 Uiso 1 1 calc R . . C53 C 0.02395(12) 0.8094(2) 0.03452(15) 0.0408(5) Uani 1 1 d . . . H53 H -0.0225 0.8510 0.0098 0.049 Uiso 1 1 calc R . . C63 C 0.40403(13) 0.7510(2) 0.42170(15) 0.0450(5) Uani 1 1 d . . . H63 H 0.4363 0.7805 0.4796 0.054 Uiso 1 1 calc R . . C61 C 0.27770(11) 0.70404(18) 0.32007(14) 0.0355(4) Uani 1 1 d . . . H61 H 0.2235 0.7009 0.3085 0.043 Uiso 1 1 calc R . . C62 C 0.32537(13) 0.7462(2) 0.40457(14) 0.0407(5) Uani 1 1 d . . . H62 H 0.3037 0.7718 0.4510 0.049 Uiso 1 1 calc R . . C65 C 0.38938(12) 0.6708(2) 0.26975(15) 0.0425(5) Uani 1 1 d . . . H65 H 0.4114 0.6451 0.2237 0.051 Uiso 1 1 calc R . . C44 C 0.33936(13) 0.7637(2) -0.04427(16) 0.0445(5) Uani 1 1 d . . . H44 H 0.3371 0.8366 -0.0719 0.053 Uiso 1 1 calc R . . C42 C 0.39158(13) 0.5751(2) -0.02040(16) 0.0466(5) Uani 1 1 d . . . H42 H 0.4238 0.5184 -0.0333 0.056 Uiso 1 1 calc R . . C43 C 0.38702(13) 0.6806(2) -0.06181(15) 0.0470(5) Uani 1 1 d . . . H43 H 0.4166 0.6963 -0.1025 0.056 Uiso 1 1 calc R . . C64 C 0.43614(13) 0.7130(3) 0.35463(16) 0.0497(6) Uani 1 1 d . . . H64 H 0.4904 0.7159 0.3669 0.060 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 F3 0.0231(5) 0.1153(13) 0.0178(5) -0.0013(6) 0.0099(4) 0.0036(6) F4 0.0220(5) 0.1260(14) 0.0139(5) -0.0008(6) 0.0045(4) 0.0026(6) N2 0.0203(6) 0.0375(8) 0.0211(7) 0.0000(6) 0.0079(6) 0.0016(5) N3 0.0222(7) 0.0392(8) 0.0216(7) 0.0001(6) 0.0081(6) -0.0012(5) C14 0.0202(8) 0.0404(10) 0.0177(7) 0.0002(6) 0.0075(6) -0.0007(6) C13 0.0200(7) 0.0336(9) 0.0190(7) 0.0003(6) 0.0041(6) 0.0002(6) C18 0.0197(7) 0.0314(8) 0.0229(9) -0.0003(6) 0.0101(7) 0.0003(6) C16 0.0237(8) 0.0525(11) 0.0160(8) 0.0008(7) 0.0093(7) 0.0018(7) C15 0.0205(8) 0.0377(9) 0.0184(8) 0.0002(6) 0.0069(6) -0.0003(6) C17 0.0236(8) 0.0547(12) 0.0140(7) -0.0007(7) 0.0054(6) 0.0010(7) Cu1 0.01935(14) 0.03046(15) 0.01899(14) 0.00018(9) 0.00558(10) 0.00042(8) F1 0.0238(5) 0.0300(5) 0.0320(5) 0.0017(4) -0.0015(4) 0.0040(4) F2 0.0243(5) 0.0298(5) 0.0386(6) -0.0024(4) -0.0075(4) -0.0019(4) C5 0.0207(7) 0.0288(8) 0.0218(7) -0.0019(6) 0.0020(6) -0.0019(6) C3 0.0231(10) 0.0284(12) 0.0224(10) 0.000 0.0072(8) 0.000 N4 0.0254(7) 0.0273(7) 0.0278(7) 0.0002(6) 0.0057(6) 0.0001(6) C6 0.0205(10) 0.0272(11) 0.0200(10) 0.000 0.0062(8) 0.000 C4 0.0196(7) 0.0295(9) 0.0223(7) 0.0012(6) 0.0027(6) 0.0029(6) N1 0.0279(7) 0.0288(8) 0.0357(8) -0.0006(6) 0.0081(6) -0.0018(6) C8 0.0238(8) 0.0247(8) 0.0219(7) -0.0005(6) 0.0074(6) -0.0016(6) C2 0.0232(10) 0.0287(12) 0.0262(11) 0.000 0.0056(9) 0.000 C1 0.0265(8) 0.0253(8) 0.0290(8) 0.0011(6) 0.0113(7) 0.0001(6) C7 0.0225(10) 0.0271(11) 0.0211(10) 0.000 0.0046(8) 0.000 P1 0.0285(2) 0.0308(2) 0.0250(2) -0.00184(16) 0.00912(17) -0.00148(16) C35 0.0341(9) 0.0363(10) 0.0275(8) -0.0004(7) 0.0080(7) -0.0003(7) C40 0.0302(8) 0.0377(10) 0.0249(8) -0.0028(7) 0.0082(7) -0.0021(7) C50 0.0293(8) 0.0374(10) 0.0265(8) 0.0007(7) 0.0115(7) -0.0011(7) C60 0.0314(8) 0.0319(9) 0.0273(8) -0.0024(7) 0.0080(7) -0.0014(7) C33 0.0314(9) 0.0306(9) 0.0418(10) 0.0014(8) 0.0119(8) 0.0011(7) C52 0.0427(11) 0.0379(11) 0.0436(11) 0.0041(9) 0.0169(9) 0.0047(9) C32 0.0401(10) 0.0372(10) 0.0328(9) 0.0048(8) 0.0135(8) 0.0040(8) C30 0.0310(8) 0.0296(9) 0.0297(9) -0.0002(7) 0.0097(7) -0.0003(7) C51 0.0338(9) 0.0381(10) 0.0355(9) 0.0001(8) 0.0104(8) -0.0006(8) C55 0.0307(9) 0.0435(11) 0.0383(10) -0.0055(8) 0.0121(8) -0.0025(8) C31 0.0380(9) 0.0376(10) 0.0263(8) -0.0001(7) 0.0109(7) 0.0010(8) C45 0.0393(10) 0.0397(11) 0.0330(9) 0.0017(8) 0.0124(8) -0.0005(8) C54 0.0282(9) 0.0593(14) 0.0392(10) -0.0051(10) 0.0108(8) -0.0021(9) C41 0.0363(9) 0.0404(11) 0.0392(10) -0.0001(8) 0.0149(8) 0.0026(8) C34 0.0329(9) 0.0358(10) 0.0331(9) -0.0053(8) 0.0062(7) 0.0001(7) C53 0.0331(9) 0.0552(13) 0.0363(10) 0.0081(9) 0.0141(8) 0.0072(9) C63 0.0451(11) 0.0512(13) 0.0325(10) -0.0096(9) 0.0029(9) 0.0005(9) C61 0.0341(9) 0.0401(10) 0.0325(9) -0.0022(8) 0.0109(7) 0.0039(8) C62 0.0468(11) 0.0449(11) 0.0301(9) -0.0055(8) 0.0115(8) 0.0084(9) C65 0.0329(9) 0.0609(14) 0.0349(10) -0.0103(9) 0.0122(8) -0.0019(9) C44 0.0456(11) 0.0525(13) 0.0366(10) 0.0082(9) 0.0144(9) -0.0040(10) C42 0.0380(10) 0.0612(14) 0.0449(11) -0.0053(11) 0.0191(9) 0.0043(10) C43 0.0398(11) 0.0703(16) 0.0353(10) 0.0031(10) 0.0181(9) -0.0050(10) C64 0.0318(10) 0.0721(17) 0.0416(11) -0.0123(11) 0.0062(9) -0.0055(10) _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 F3 C16 1.346(2) . ? F4 C17 1.352(2) . ? N2 C18 1.157(2) . ? N2 Cu1 1.9577(15) . ? N3 C13 1.155(3) . ? N3 Cu1 1.9949(15) 4_556 ? C14 C18 1.402(2) . ? C14 C13 1.408(2) . ? C14 C15 1.454(2) . ? C16 C17 1.375(3) . ? C16 C15 1.396(2) . ? C15 C17 1.394(2) 2_655 ? C17 C15 1.394(2) 2_655 ? Cu1 N3 1.9949(15) 4 ? Cu1 N1 1.9983(16) . ? Cu1 N4 2.0067(15) . ? F1 C4 1.3542(18) . ? F2 C5 1.3581(19) . ? C5 C4 1.369(3) 1_565 ? C5 C6 1.397(2) . ? C3 C4 1.402(2) . ? C3 C4 1.402(2) 2_554 ? C3 C2 1.449(4) . ? N4 C8 1.153(2) . ? C6 C5 1.397(2) 2_554 ? C6 C7 1.447(3) . ? C4 C5 1.369(3) 1_545 ? N1 C1 1.154(2) . ? C8 C7 1.403(2) . ? C2 C1 1.406(2) . ? C2 C1 1.406(2) 2_554 ? C7 C8 1.403(2) 2_554 ? P1 C30 1.796(2) . ? P1 C50 1.7972(19) . ? P1 C60 1.7987(18) . ? P1 C40 1.8034(18) . ? C35 C34 1.380(3) . ? C35 C30 1.396(3) . ? C40 C45 1.386(3) . ? C40 C41 1.399(3) . ? C50 C51 1.395(3) . ? C50 C55 1.395(3) . ? C60 C61 1.395(3) . ? C60 C65 1.395(3) . ? C33 C32 1.389(3) . ? C33 C34 1.391(3) . ? C52 C53 1.384(3) . ? C52 C51 1.386(3) . ? C32 C31 1.385(3) . ? C30 C31 1.395(3) . ? C55 C54 1.386(3) . ? C45 C44 1.383(3) . ? C54 C53 1.381(4) . ? C41 C42 1.391(3) . ? C63 C62 1.380(3) . ? C63 C64 1.386(3) . ? C61 C62 1.386(3) . ? C65 C64 1.385(3) . ? C44 C43 1.390(4) . ? C42 C43 1.382(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 C18 N2 Cu1 172.71(15) . . ? C13 N3 Cu1 177.29(15) . 4_556 ? C18 C14 C13 114.84(15) . . ? C18 C14 C15 122.80(15) . . ? C13 C14 C15 122.36(15) . . ? N3 C13 C14 176.55(18) . . ? N2 C18 C14 177.19(18) . . ? F3 C16 C17 117.05(16) . . ? F3 C16 C15 119.50(16) . . ? C17 C16 C15 123.45(16) . . ? C17 C15 C16 112.65(16) 2_655 . ? C17 C15 C14 123.70(16) 2_655 . ? C16 C15 C14 123.63(16) . . ? F4 C17 C16 117.14(16) . . ? F4 C17 C15 118.96(16) . 2_655 ? C16 C17 C15 123.89(17) . 2_655 ? N2 Cu1 N3 111.35(6) . 4 ? N2 Cu1 N1 117.22(7) . . ? N3 Cu1 N1 105.41(7) 4 . ? N2 Cu1 N4 113.90(6) . . ? N3 Cu1 N4 108.66(6) 4 . ? N1 Cu1 N4 99.28(6) . . ? F2 C5 C4 116.90(14) . 1_565 ? F2 C5 C6 118.49(16) . . ? C4 C5 C6 124.61(15) 1_565 . ? C4 C3 C4 111.8(2) . 2_554 ? C4 C3 C2 124.09(11) . . ? C4 C3 C2 124.09(11) 2_554 . ? C8 N4 Cu1 164.77(14) . . ? C5 C6 C5 111.4(2) 2_554 . ? C5 C6 C7 124.32(11) 2_554 . ? C5 C6 C7 124.32(11) . . ? F1 C4 C5 116.72(14) . 1_545 ? F1 C4 C3 119.50(16) . . ? C5 C4 C3 123.78(15) 1_545 . ? C1 N1 Cu1 161.98(15) . . ? N4 C8 C7 177.03(19) . . ? C1 C2 C1 113.5(2) . 2_554 ? C1 C2 C3 123.27(11) . . ? C1 C2 C3 123.27(11) 2_554 . ? N1 C1 C2 176.4(2) . . ? C8 C7 C8 113.4(2) 2_554 . ? C8 C7 C6 123.28(11) 2_554 . ? C8 C7 C6 123.28(11) . . ? C30 P1 C50 109.03(9) . . ? C30 P1 C60 111.64(9) . . ? C50 P1 C60 109.81(9) . . ? C30 P1 C40 109.07(9) . . ? C50 P1 C40 109.65(9) . . ? C60 P1 C40 107.61(9) . . ? C34 C35 C30 119.89(18) . . ? C45 C40 C41 120.39(18) . . ? C45 C40 P1 118.66(15) . . ? C41 C40 P1 120.74(16) . . ? C51 C50 C55 119.87(18) . . ? C51 C50 P1 119.96(14) . . ? C55 C50 P1 119.97(16) . . ? C61 C60 C65 119.95(18) . . ? C61 C60 P1 121.03(14) . . ? C65 C60 P1 119.02(14) . . ? C32 C33 C34 120.13(19) . . ? C53 C52 C51 120.3(2) . . ? C31 C32 C33 120.51(18) . . ? C31 C30 C35 120.41(19) . . ? C31 C30 P1 120.88(15) . . ? C35 C30 P1 118.51(15) . . ? C52 C51 C50 119.75(19) . . ? C54 C55 C50 119.5(2) . . ? C32 C31 C30 119.15(18) . . ? C44 C45 C40 120.0(2) . . ? C53 C54 C55 120.6(2) . . ? C42 C41 C40 119.0(2) . . ? C35 C34 C33 119.91(18) . . ? C54 C53 C52 119.97(19) . . ? C62 C63 C64 120.2(2) . . ? C62 C61 C60 119.56(19) . . ? C63 C62 C61 120.45(19) . . ? C64 C65 C60 119.71(19) . . ? C45 C44 C43 119.8(2) . . ? C43 C42 C41 120.3(2) . . ? C42 C43 C44 120.3(2) . . ? C65 C64 C63 120.2(2) . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 74.45 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.654 _refine_diff_density_min -0.559 _refine_diff_density_rms 0.062 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 0.338 0.250 107 22 ' ' 2 0.500 0.661 0.750 107 22 ' ' _platon_squeeze_details ; ; data_rweb152e_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (PPh3Me)[Cu(F4TCNQ)].DMF _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H25 Cu F4 N5 O P' _chemical_formula_weight 690.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0727 0.0534 '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 7.5735(3) _cell_length_b 11.7547(4) _cell_length_c 17.0842(5) _cell_angle_alpha 82.190(3) _cell_angle_beta 86.285(3) _cell_angle_gamma 88.218(3) _cell_volume 1503.25(9) _cell_formula_units_Z 2 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 6390 _cell_measurement_theta_min 3.7935 _cell_measurement_theta_max 74.5233 _exptl_crystal_description 'block' _exptl_crystal_colour 'yellow-green' _exptl_crystal_size_max 0.1344 _exptl_crystal_size_mid 0.0989 _exptl_crystal_size_min 0.0786 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.525 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 704 _exptl_absorpt_coefficient_mu 2.073 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.95459 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 130.01(11) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'SuperNova (Cu) X-ray Source' _diffrn_radiation_monochromator 'mirror' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.2273 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10311 _diffrn_reflns_av_R_equivalents 0.0158 _diffrn_reflns_av_sigmaI/netI 0.0239 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 3.80 _diffrn_reflns_theta_max 74.70 _reflns_number_total 5976 _reflns_number_gt 5530 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0772P)^2^+1.5330P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5976 _refine_ls_number_parameters 393 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0455 _refine_ls_R_factor_gt 0.0425 _refine_ls_wR_factor_ref 0.1277 _refine_ls_wR_factor_gt 0.1246 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.000 _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 O1 O 0.2885(6) 0.4262(4) 0.4342(3) 0.0997(12) Uiso 1 1 d . . . N100 N 0.3044(6) 0.3771(4) 0.5619(3) 0.0809(11) Uiso 1 1 d . . . C101 C 0.1032(8) 0.3771(5) 0.5802(4) 0.0855(15) Uiso 1 1 d . . . H10A H 0.0436 0.4080 0.5324 0.128 Uiso 1 1 calc R . . H10B H 0.0724 0.4250 0.6220 0.128 Uiso 1 1 calc R . . H10C H 0.0652 0.2984 0.5980 0.128 Uiso 1 1 calc R . . C102 C 0.4142(8) 0.3439(5) 0.6264(4) 0.0866(15) Uiso 1 1 d . . . H10D H 0.5311 0.3191 0.6060 0.130 Uiso 1 1 calc R . . H10E H 0.3600 0.2804 0.6621 0.130 Uiso 1 1 calc R . . H10F H 0.4271 0.4094 0.6553 0.130 Uiso 1 1 calc R . . C100 C 0.3621(8) 0.3995(5) 0.4918(4) 0.0845(14) Uiso 1 1 d . . . H100 H 0.4872 0.3940 0.4840 0.101 Uiso 1 1 calc R . . Cu1 Cu 0.58373(4) 0.94727(3) 0.194135(18) 0.01721(11) Uani 1 1 d . . . P1 P 0.10479(7) 0.32386(5) 0.23452(3) 0.01965(14) Uani 1 1 d . . . F4 F 1.30760(18) 1.05975(14) 0.41788(8) 0.0273(3) Uani 1 1 d . . . F2 F 0.62202(18) 1.37435(11) 0.13092(8) 0.0216(3) Uani 1 1 d . . . F1 F 0.38180(18) 1.40368(11) -0.12093(8) 0.0221(3) Uani 1 1 d . . . F3 F 0.74619(18) 0.88779(13) 0.43871(8) 0.0268(3) Uani 1 1 d . . . N1 N 0.7978(2) 0.92304(16) 0.25423(11) 0.0194(4) Uani 1 1 d . . . N4 N 0.5546(3) 0.85515(16) 0.10775(11) 0.0221(4) Uani 1 1 d . . . N2 N 0.5826(3) 1.10763(16) 0.13064(12) 0.0246(4) Uani 1 1 d . . . N3 N 0.3649(3) 0.93520(18) 0.26676(11) 0.0229(4) Uani 1 1 d . . . C10 C 0.8759(3) 0.94448(19) 0.46720(13) 0.0181(4) Uani 1 1 d . . . C4 C 0.4438(3) 1.44825(19) -0.05929(13) 0.0174(4) Uani 1 1 d . . . C3 C 0.5059(3) 1.37395(18) 0.00474(12) 0.0165(4) Uani 1 1 d . . . C8 C 1.0591(3) 0.94453(19) 0.33854(12) 0.0180(4) Uani 1 1 d . . . C9 C 1.0301(3) 0.97123(18) 0.41974(12) 0.0166(4) Uani 1 1 d . . . C1 C 0.5534(3) 1.17517(18) 0.07665(13) 0.0191(4) Uani 1 1 d . . . C41 C -0.1984(3) 0.20073(19) 0.28714(14) 0.0221(4) Uani 1 1 d . . . H41 H -0.1976 0.1784 0.2357 0.026 Uiso 1 1 calc R . . C11 C 0.5246(3) 0.80638(18) 0.05580(13) 0.0190(4) Uani 1 1 d . . . C25 C 0.2643(3) 0.5352(2) 0.22205(16) 0.0271(5) Uani 1 1 d . . . H25 H 0.3727 0.4930 0.2283 0.032 Uiso 1 1 calc R . . C20 C 0.1058(3) 0.47766(19) 0.22311(13) 0.0216(4) Uani 1 1 d . . . C5 C 0.5606(3) 1.43389(18) 0.06388(13) 0.0173(4) Uani 1 1 d . . . C2 C 0.5125(3) 1.24984(18) 0.00843(13) 0.0185(4) Uani 1 1 d . . . C7 C 0.9156(3) 0.93169(18) 0.29262(12) 0.0173(4) Uani 1 1 d . . . C40 C -0.0717(3) 0.2750(2) 0.30501(14) 0.0220(4) Uani 1 1 d . . . C6 C 0.2277(3) 0.93899(19) 0.30076(13) 0.0188(4) Uani 1 1 d . . . C12 C 1.1527(3) 1.02790(19) 0.45737(13) 0.0184(4) Uani 1 1 d . . . C30 C 0.0784(3) 0.2735(2) 0.14165(14) 0.0218(4) Uani 1 1 d . . . C31 C 0.0148(3) 0.3455(2) 0.07758(15) 0.0267(5) Uani 1 1 d . . . H31 H -0.0132 0.4238 0.0820 0.032 Uiso 1 1 calc R . . C35 C 0.1208(4) 0.1582(2) 0.13450(16) 0.0291(5) Uani 1 1 d . . . H35 H 0.1638 0.1084 0.1780 0.035 Uiso 1 1 calc R . . C32 C -0.0075(4) 0.3028(2) 0.00744(15) 0.0313(5) Uani 1 1 d . . . H32 H -0.0520 0.3517 -0.0361 0.038 Uiso 1 1 calc R . . C33 C 0.0348(4) 0.1888(2) 0.00053(16) 0.0325(6) Uani 1 1 d . . . H33 H 0.0192 0.1598 -0.0478 0.039 Uiso 1 1 calc R . . C23 C 0.1048(4) 0.7151(2) 0.20202(15) 0.0270(5) Uani 1 1 d . . . H23 H 0.1046 0.7967 0.1943 0.032 Uiso 1 1 calc R . . C24 C 0.2629(4) 0.6546(2) 0.21183(16) 0.0294(5) Uani 1 1 d . . . H24 H 0.3702 0.6944 0.2116 0.035 Uiso 1 1 calc R . . C45 C -0.0721(4) 0.3083(3) 0.38028(17) 0.0346(6) Uani 1 1 d . . . H45 H 0.0155 0.3584 0.3922 0.041 Uiso 1 1 calc R . . C50 C 0.3092(3) 0.2673(2) 0.27249(15) 0.0268(5) Uani 1 1 d . . . H50A H 0.3269 0.2971 0.3222 0.040 Uiso 1 1 calc R . . H50B H 0.4071 0.2906 0.2339 0.040 Uiso 1 1 calc R . . H50C H 0.3053 0.1833 0.2822 0.040 Uiso 1 1 calc R . . C21 C -0.0529(3) 0.5391(2) 0.21454(15) 0.0258(5) Uani 1 1 d . . . H21 H -0.1608 0.4995 0.2163 0.031 Uiso 1 1 calc R . . C42 C -0.3260(3) 0.1596(2) 0.34548(15) 0.0249(5) Uani 1 1 d . . . H42 H -0.4118 0.1079 0.3341 0.030 Uiso 1 1 calc R . . C34 C 0.0995(4) 0.1176(2) 0.06358(17) 0.0339(6) Uani 1 1 d . . . H34 H 0.1297 0.0399 0.0582 0.041 Uiso 1 1 calc R . . C22 C -0.0539(4) 0.6584(2) 0.20333(15) 0.0283(5) Uani 1 1 d . . . H22 H -0.1620 0.7008 0.1966 0.034 Uiso 1 1 calc R . . C44 C -0.2017(4) 0.2677(3) 0.43761(17) 0.0385(6) Uani 1 1 d . . . H44 H -0.2035 0.2906 0.4889 0.046 Uiso 1 1 calc R . . C43 C -0.3288(3) 0.1935(2) 0.42016(16) 0.0305(5) Uani 1 1 d . . . H43 H -0.4176 0.1662 0.4594 0.037 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.01800(18) 0.01760(18) 0.01677(18) -0.00449(12) -0.00163(12) -0.00136(12) P1 0.0199(3) 0.0176(3) 0.0211(3) -0.0011(2) -0.0011(2) -0.0028(2) F4 0.0185(6) 0.0440(8) 0.0208(6) -0.0097(6) 0.0063(5) -0.0147(6) F2 0.0309(7) 0.0168(6) 0.0177(6) -0.0019(5) -0.0081(5) 0.0002(5) F1 0.0314(7) 0.0172(6) 0.0201(6) -0.0067(5) -0.0103(5) -0.0012(5) F3 0.0206(7) 0.0411(8) 0.0212(6) -0.0105(6) 0.0010(5) -0.0153(6) N1 0.0190(9) 0.0230(9) 0.0168(9) -0.0051(7) -0.0012(7) 0.0006(7) N4 0.0322(10) 0.0154(9) 0.0197(9) -0.0047(7) -0.0025(8) -0.0025(7) N2 0.0359(11) 0.0149(9) 0.0240(10) -0.0040(8) -0.0062(8) -0.0015(8) N3 0.0189(9) 0.0310(10) 0.0201(9) -0.0088(8) 0.0009(7) -0.0035(7) C10 0.0154(10) 0.0224(10) 0.0174(10) -0.0040(8) -0.0029(8) -0.0052(8) C4 0.0210(10) 0.0171(10) 0.0155(9) -0.0057(8) -0.0036(8) -0.0018(8) C3 0.0179(10) 0.0150(10) 0.0170(10) -0.0038(8) -0.0007(8) -0.0014(7) C8 0.0170(10) 0.0218(10) 0.0159(10) -0.0044(8) -0.0010(8) -0.0020(8) C9 0.0152(10) 0.0192(10) 0.0156(9) -0.0026(8) -0.0008(8) -0.0012(8) C1 0.0223(10) 0.0139(9) 0.0226(11) -0.0067(8) -0.0031(8) -0.0016(8) C41 0.0211(11) 0.0196(10) 0.0258(11) -0.0033(8) -0.0032(9) -0.0002(8) C11 0.0226(10) 0.0135(9) 0.0203(10) -0.0005(8) 0.0002(8) -0.0013(8) C25 0.0234(11) 0.0230(12) 0.0345(13) -0.0037(9) 0.0026(9) -0.0028(9) C20 0.0255(11) 0.0190(10) 0.0203(10) -0.0027(8) -0.0003(8) -0.0034(9) C5 0.0200(10) 0.0165(10) 0.0157(10) -0.0013(8) -0.0034(8) -0.0007(8) C2 0.0243(11) 0.0142(10) 0.0178(10) -0.0040(8) -0.0026(8) -0.0016(8) C7 0.0194(10) 0.0167(9) 0.0157(9) -0.0027(7) 0.0019(8) 0.0002(8) C40 0.0235(11) 0.0200(10) 0.0220(11) -0.0014(8) -0.0001(9) -0.0032(8) C6 0.0216(11) 0.0191(10) 0.0166(10) -0.0038(8) -0.0039(8) -0.0021(8) C12 0.0138(9) 0.0233(10) 0.0176(10) -0.0011(8) 0.0022(8) -0.0047(8) C30 0.0204(10) 0.0215(11) 0.0238(11) -0.0040(8) 0.0009(8) -0.0029(8) C31 0.0295(12) 0.0245(12) 0.0256(12) -0.0022(9) -0.0004(9) 0.0009(9) C35 0.0358(13) 0.0219(12) 0.0292(13) -0.0018(9) -0.0014(10) -0.0016(10) C32 0.0344(13) 0.0350(14) 0.0242(12) -0.0022(10) -0.0026(10) -0.0003(11) C33 0.0355(14) 0.0364(14) 0.0273(12) -0.0111(11) 0.0029(10) -0.0089(11) C23 0.0379(13) 0.0189(11) 0.0249(11) -0.0062(9) 0.0006(10) -0.0028(9) C24 0.0299(13) 0.0243(12) 0.0342(13) -0.0058(10) 0.0046(10) -0.0083(10) C45 0.0364(14) 0.0382(14) 0.0310(13) -0.0105(11) 0.0023(11) -0.0148(12) C50 0.0244(11) 0.0243(11) 0.0308(12) 0.0009(9) -0.0044(9) -0.0010(9) C21 0.0250(12) 0.0233(11) 0.0303(12) -0.0054(9) -0.0067(9) -0.0024(9) C42 0.0190(10) 0.0217(11) 0.0334(13) -0.0014(9) -0.0019(9) -0.0024(8) C34 0.0428(15) 0.0233(12) 0.0369(14) -0.0096(10) 0.0010(12) -0.0043(11) C22 0.0309(13) 0.0238(12) 0.0318(13) -0.0078(10) -0.0058(10) 0.0015(10) C44 0.0417(16) 0.0479(17) 0.0276(13) -0.0130(12) 0.0069(11) -0.0129(13) C43 0.0270(12) 0.0310(13) 0.0316(13) -0.0004(10) 0.0059(10) -0.0044(10) _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 O1 C100 1.164(7) . ? N100 C100 1.244(7) . ? N100 C102 1.429(7) . ? N100 C101 1.536(7) . ? Cu1 N1 1.9674(19) . ? Cu1 N4 1.9726(19) . ? Cu1 N3 2.002(2) . ? Cu1 N2 2.043(2) . ? P1 C50 1.791(2) . ? P1 C20 1.792(2) . ? P1 C30 1.792(2) . ? P1 C40 1.794(2) . ? F4 C12 1.352(3) . ? F2 C5 1.360(3) . ? F1 C4 1.354(2) . ? F3 C10 1.355(2) . ? N1 C7 1.156(3) . ? N4 C11 1.158(3) . ? N2 C1 1.160(3) . ? N3 C6 1.160(3) . ? C10 C12 1.373(3) 2_776 ? C10 C9 1.397(3) . ? C4 C5 1.377(3) 2_685 ? C4 C3 1.401(3) . ? C3 C5 1.398(3) . ? C3 C2 1.451(3) . ? C8 C6 1.397(3) 1_655 ? C8 C7 1.404(3) . ? C8 C9 1.465(3) . ? C9 C12 1.397(3) . ? C1 C2 1.406(3) . ? C41 C42 1.391(3) . ? C41 C40 1.392(3) . ? C11 C2 1.403(3) 2_675 ? C25 C24 1.390(4) . ? C25 C20 1.394(3) . ? C20 C21 1.388(3) . ? C5 C4 1.377(3) 2_685 ? C2 C11 1.403(3) 2_675 ? C40 C45 1.394(4) . ? C6 C8 1.397(3) 1_455 ? C12 C10 1.373(3) 2_776 ? C30 C31 1.392(4) . ? C30 C35 1.403(3) . ? C31 C32 1.383(4) . ? C35 C34 1.381(4) . ? C32 C33 1.387(4) . ? C33 C34 1.378(4) . ? C23 C24 1.382(4) . ? C23 C22 1.390(4) . ? C45 C44 1.389(4) . ? C21 C22 1.389(3) . ? C42 C43 1.386(4) . ? C44 C43 1.391(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 C100 N100 C102 123.8(5) . . ? C100 N100 C101 118.6(5) . . ? C102 N100 C101 117.5(5) . . ? O1 C100 N100 130.8(7) . . ? N1 Cu1 N4 119.00(8) . . ? N1 Cu1 N3 111.02(8) . . ? N4 Cu1 N3 108.73(8) . . ? N1 Cu1 N2 110.07(8) . . ? N4 Cu1 N2 99.32(8) . . ? N3 Cu1 N2 107.67(9) . . ? C50 P1 C20 109.51(12) . . ? C50 P1 C30 109.00(12) . . ? C20 P1 C30 110.92(11) . . ? C50 P1 C40 108.16(11) . . ? C20 P1 C40 108.68(11) . . ? C30 P1 C40 110.52(11) . . ? C7 N1 Cu1 165.84(18) . . ? C11 N4 Cu1 174.30(19) . . ? C1 N2 Cu1 155.00(18) . . ? C6 N3 Cu1 170.4(2) . . ? F3 C10 C12 117.18(19) . 2_776 ? F3 C10 C9 119.38(19) . . ? C12 C10 C9 123.4(2) 2_776 . ? F1 C4 C5 116.64(19) . 2_685 ? F1 C4 C3 119.31(19) . . ? C5 C4 C3 124.0(2) 2_685 . ? C5 C3 C4 111.85(19) . . ? C5 C3 C2 124.5(2) . . ? C4 C3 C2 123.6(2) . . ? C6 C8 C7 116.48(19) 1_655 . ? C6 C8 C9 122.49(19) 1_655 . ? C7 C8 C9 120.86(19) . . ? C12 C9 C10 112.92(19) . . ? C12 C9 C8 123.5(2) . . ? C10 C9 C8 123.58(19) . . ? N2 C1 C2 175.4(2) . . ? C42 C41 C40 119.2(2) . . ? N4 C11 C2 178.4(2) . 2_675 ? C24 C25 C20 119.6(2) . . ? C21 C20 C25 120.3(2) . . ? C21 C20 P1 119.30(18) . . ? C25 C20 P1 120.44(19) . . ? F2 C5 C4 116.52(19) . 2_685 ? F2 C5 C3 119.38(19) . . ? C4 C5 C3 124.1(2) 2_685 . ? C11 C2 C1 113.98(19) 2_675 . ? C11 C2 C3 122.7(2) 2_675 . ? C1 C2 C3 123.32(19) . . ? N1 C7 C8 178.8(2) . . ? C41 C40 C45 120.7(2) . . ? C41 C40 P1 121.42(18) . . ? C45 C40 P1 117.73(18) . . ? N3 C6 C8 177.5(2) . 1_455 ? F4 C12 C10 117.21(19) . 2_776 ? F4 C12 C9 119.15(19) . . ? C10 C12 C9 123.6(2) 2_776 . ? C31 C30 C35 119.8(2) . . ? C31 C30 P1 121.51(18) . . ? C35 C30 P1 118.65(19) . . ? C32 C31 C30 119.8(2) . . ? C34 C35 C30 119.4(2) . . ? C31 C32 C33 120.2(2) . . ? C34 C33 C32 120.1(2) . . ? C24 C23 C22 121.0(2) . . ? C23 C24 C25 119.7(2) . . ? C44 C45 C40 119.4(2) . . ? C20 C21 C22 120.1(2) . . ? C43 C42 C41 120.4(2) . . ? C33 C34 C35 120.6(2) . . ? C21 C22 C23 119.3(2) . . ? C45 C44 C43 120.2(3) . . ? C42 C43 C44 120.1(2) . . ? _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 74.70 _diffrn_measured_fraction_theta_full 0.965 _refine_diff_density_max 0.950 _refine_diff_density_min -0.981 _refine_diff_density_rms 0.084