Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Barton H. Hamilton' 'Christopher J. Ziegler' _publ_contact_author_name 'Prof Christopher Ziegler' _publ_contact_author_address ; Department of Chemistry University of Akron Knight Chemical Laboratory Akron OH 44325-3601 UNITED STATES OF AMERICA ; _publ_contact_author_email 'ZIEGLER@UAKRON.EDU' _publ_section_title ; The structures of Cu(I) and Ag(I) coordination polymers using the tricyanofluoroborate anion ; data_CuBFCN3 _database_code_CSD 178955 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'copper tricyanofluoroborate' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C5 H3 B Cu F N4' _chemical_formula_weight 212.46 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' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 '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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 8.476(2) _cell_length_b 7.7715(19) _cell_length_c 12.519(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 824.6(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 781 _cell_measurement_theta_min 2.90 _cell_measurement_theta_max 25.00 _exptl_crystal_description 'needle' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.711 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 416 _exptl_absorpt_coefficient_mu 2.608 _exptl_absorpt_correction_type 'difabs' _exptl_absorpt_correction_T_min 0.231 _exptl_absorpt_correction_T_max 0.693 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'P(2)1 Syntex' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time 3/97 _diffrn_standards_decay_% ? _diffrn_reflns_number 895 _diffrn_reflns_av_R_equivalents 0.0174 _diffrn_reflns_av_sigmaI/netI 0.0455 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.90 _diffrn_reflns_theta_max 25.00 _reflns_number_total 781 _reflns_number_gt 581 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'P3' _computing_cell_refinement 'P3' _computing_data_reduction 'xdisk' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens 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^)+(0.0146P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 781 _refine_ls_number_parameters 68 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0430 _refine_ls_R_factor_gt 0.0257 _refine_ls_wR_factor_ref 0.0458 _refine_ls_wR_factor_gt 0.0447 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.000 _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 Cu Cu 0.93027(7) 0.2500 0.58867(4) 0.02155(15) Uani 1 2 d S . . F F 0.9705(2) 0.2500 0.16835(18) 0.0280(6) Uani 1 2 d S . . N1 N 1.1647(4) 0.2500 0.5962(3) 0.0258(9) Uani 1 2 d S . . N2 N 0.8640(4) 0.2500 0.4362(3) 0.0235(9) Uani 1 2 d S . . N3 N 0.8380(3) 0.0405(3) 0.65598(18) 0.0212(6) Uani 1 1 d . . . C1 C 1.2971(6) 0.2500 0.5984(4) 0.0289(11) Uani 1 2 d S . . C3 C 0.7744(3) -0.0806(4) 0.6835(2) 0.0176(7) Uani 1 1 d . . . C2 C 0.8439(4) 0.2500 0.3463(3) 0.0185(10) Uani 1 2 d S . . C4 C 1.4691(5) 0.2500 0.6021(4) 0.0615(19) Uani 1 2 d S . . H4A H 1.5065 0.3657 0.6109 0.092 Uiso 0.50 1 calc PR . . H4B H 1.5099 0.2034 0.5367 0.092 Uiso 0.50 1 calc PR . . H4C H 1.5042 0.1809 0.6610 0.092 Uiso 0.50 1 calc PR . . B B 0.8215(6) 0.2500 0.2180(3) 0.0218(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 Cu 0.0224(3) 0.0207(3) 0.0216(2) 0.000 -0.0001(3) 0.000 F 0.0185(14) 0.0382(16) 0.0272(12) 0.000 0.0019(11) 0.000 N1 0.023(2) 0.023(2) 0.032(2) 0.000 -0.001(2) 0.000 N2 0.025(2) 0.024(2) 0.0219(19) 0.000 -0.0011(16) 0.000 N3 0.0226(15) 0.0181(14) 0.0229(14) 0.0013(12) 0.0044(11) 0.0021(13) C1 0.029(3) 0.033(3) 0.025(2) 0.000 -0.002(3) 0.000 C3 0.0155(15) 0.0190(18) 0.0183(15) 0.0004(14) 0.0025(13) 0.0068(15) C2 0.008(2) 0.015(2) 0.033(3) 0.000 -0.001(2) 0.000 C4 0.019(3) 0.119(5) 0.046(3) 0.000 0.000(3) 0.000 B 0.022(3) 0.024(3) 0.020(3) 0.000 0.004(2) 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 Cu N1 1.989(4) . ? Cu N2 1.990(3) . ? Cu N3 1.993(2) 7_565 ? Cu N3 1.993(2) . ? F B 1.408(5) . ? N1 C1 1.123(5) . ? N2 C2 1.137(5) . ? N3 C3 1.138(3) . ? C1 C4 1.459(6) . ? C3 B 1.606(4) 2_655 ? C2 B 1.617(6) . ? B C3 1.606(4) 2_654 ? B C3 1.606(4) 8_765 ? 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 Cu N2 109.09(15) . . ? N1 Cu N3 111.83(9) . 7_565 ? N2 Cu N3 107.15(8) . 7_565 ? N1 Cu N3 111.83(8) . . ? N2 Cu N3 107.15(8) . . ? N3 Cu N3 109.55(13) 7_565 . ? C1 N1 Cu 178.7(4) . . ? C2 N2 Cu 172.2(4) . . ? C3 N3 Cu 171.7(2) . . ? N1 C1 C4 179.7(5) . . ? N3 C3 B 177.3(3) . 2_655 ? N2 C2 B 178.1(4) . . ? F B C3 109.6(2) . 2_654 ? F B C3 109.6(2) . 8_765 ? C3 B C3 110.1(3) 2_654 8_765 ? F B C2 109.5(4) . . ? C3 B C2 109.1(2) 2_654 . ? C3 B C2 109.1(2) 8_765 . ? 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 N2 Cu N1 C1 0.00(5) . . . . ? N3 Cu N1 C1 -118.35(10) 7_565 . . . ? N3 Cu N1 C1 118.35(10) . . . . ? N1 Cu N2 C2 0.000(4) . . . . ? N3 Cu N2 C2 121.25(8) 7_565 . . . ? N3 Cu N2 C2 -121.25(8) . . . . ? N1 Cu N3 C3 -132.5(16) . . . . ? N2 Cu N3 C3 -13.0(17) . . . . ? N3 Cu N3 C3 102.9(16) 7_565 . . . ? Cu N1 C1 C4 180.0(4) . . . . ? Cu N3 C3 B -15(8) . . . 2_655 ? Cu N2 C2 B 0.00(2) . . . . ? N2 C2 B F 0.000(18) . . . . ? N2 C2 B C3 119.9(3) . . . 2_654 ? N2 C2 B C3 -119.9(3) . . . 8_765 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.355 _refine_diff_density_min -0.267 _refine_diff_density_rms 0.071 data_AgBFCN3 _database_code_CSD 178956 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'silver tricyanofluoroborate' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C5 H3 Ag B F N4' _chemical_formula_weight 256.79 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' 'B' 'B' 0.0013 0.0007 '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' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 '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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 8.7909(18) _cell_length_b 8.1413(16) _cell_length_c 12.743(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 912.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 864 _cell_measurement_theta_min 2.97 _cell_measurement_theta_max 25.00 _exptl_crystal_description 'needle' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.870 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 488 _exptl_absorpt_coefficient_mu 2.174 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P(2)1 Syntex' _diffrn_measurement_method '/w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time 3/97 _diffrn_standards_decay_% ? _diffrn_reflns_number 1918 _diffrn_reflns_av_R_equivalents 0.0309 _diffrn_reflns_av_sigmaI/netI 0.0307 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 25.00 _reflns_number_total 864 _reflns_number_gt 736 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'P3' _computing_cell_refinement 'P3' _computing_data_reduction 'xdisk' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens 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^)+(0.0286P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 864 _refine_ls_number_parameters 74 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0346 _refine_ls_R_factor_gt 0.0247 _refine_ls_wR_factor_ref 0.0531 _refine_ls_wR_factor_gt 0.0500 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag Ag 0.97587(4) 0.2500 0.41023(3) 0.02826(14) Uani 1 2 d S . . B B 0.7996(6) 0.2500 0.7821(4) 0.0267(12) Uani 1 2 d S . . F F 0.9373(3) 0.2500 0.8377(2) 0.0400(8) Uani 1 2 d S . . C2 C 1.3568(5) 0.2500 0.4106(4) 0.0379(13) Uani 1 2 d S . . C3 C 0.8324(5) 0.2500 0.6565(4) 0.0262(11) Uani 1 2 d S . . C1 C 0.7987(3) -0.0879(4) 0.3090(2) 0.0264(7) Uani 1 1 d . . . C4 C 1.5221(8) 0.2500 0.4057(8) 0.091(4) Uani 1 2 d S . . N2 N 1.2288(5) 0.2500 0.4139(3) 0.0402(11) Uani 1 2 d S . . N3 N 0.8571(4) 0.2500 0.5698(3) 0.0326(10) Uani 1 2 d S . . N1 N 0.8662(3) 0.0278(4) 0.3291(2) 0.0360(7) Uani 1 1 d . . . H1 H 1.545(7) 0.192(10) 0.369(4) 0.13(3) Uiso 1 1 d . . . H2 H 1.571(9) 0.2500 0.470(6) 0.11(3) Uiso 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 Ag 0.0256(2) 0.0354(2) 0.0238(2) 0.000 0.00080(16) 0.000 B 0.025(3) 0.033(3) 0.022(3) 0.000 -0.002(2) 0.000 F 0.0258(16) 0.068(2) 0.0264(14) 0.000 -0.0034(12) 0.000 C2 0.022(3) 0.066(4) 0.026(3) 0.000 -0.001(2) 0.000 C3 0.019(2) 0.030(3) 0.029(3) 0.000 0.003(2) 0.000 C1 0.0270(17) 0.0296(19) 0.0226(17) 0.0001(16) -0.0032(13) 0.0101(16) C4 0.017(3) 0.207(14) 0.048(4) 0.000 0.003(3) 0.000 N2 0.030(2) 0.057(3) 0.034(2) 0.000 0.001(2) 0.000 N3 0.026(2) 0.048(3) 0.024(2) 0.000 0.0011(17) 0.000 N1 0.0418(17) 0.0311(17) 0.0350(16) -0.0059(14) -0.0110(13) 0.0034(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 Ag N2 2.224(4) . ? Ag N3 2.286(4) . ? Ag N1 2.296(3) . ? Ag N1 2.296(3) 7_565 ? B F 1.403(6) . ? B C1 1.614(5) 2_655 ? B C1 1.614(5) 8_766 ? B C3 1.626(7) . ? C2 N2 1.126(6) . ? C2 C4 1.455(9) . ? C3 N3 1.126(5) . ? C1 N1 1.142(4) . ? C1 B 1.614(5) 2_654 ? 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 N2 Ag N3 115.96(15) . . ? N2 Ag N1 115.44(9) . . ? N3 Ag N1 102.04(9) . . ? N2 Ag N1 115.44(9) . 7_565 ? N3 Ag N1 102.04(9) . 7_565 ? N1 Ag N1 103.99(14) . 7_565 ? F B C1 110.8(3) . 2_655 ? F B C1 110.8(3) . 8_766 ? C1 B C1 109.7(4) 2_655 8_766 ? F B C3 110.1(4) . . ? C1 B C3 107.7(3) 2_655 . ? C1 B C3 107.7(3) 8_766 . ? N2 C2 C4 179.7(6) . . ? N3 C3 B 179.1(5) . . ? N1 C1 B 178.7(4) . 2_654 ? C2 N2 Ag 176.6(4) . . ? C3 N3 Ag 164.0(4) . . ? C1 N1 Ag 165.7(3) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.397 _refine_diff_density_min -0.595 _refine_diff_density_rms 0.086