# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2006 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Dr. Jamie L. Manson' _publ_contact_author_address ; Department of Chemistry and Biochemistry Eastern Washington University Cheney, WA 99004 ; _publ_contact_author_email JManson@ewu.edu _publ_contact_author_fax '(509) 359-6973' _publ_contact_author_phone '(509) 359-2878' _publ_section_title ; [Cu(HF~2~)(pyz)~2~]BF~4~ {pyz = pyrazine}: Long-range magnetic ordering in a pseudo-cubic coordination polymer comprised of bridging HF~2~^-^ and pyrazine ligands ; loop_ _publ_author_name _publ_author_address 'Jamie L. Manson' ; Department of Chemistry and Biochemistry Eastern Washington University Cheney, WA 99004 ; 'Marianne M. Connor' ; Department of Chemistry and Biochemistry Eastern Washington University Cheney, WA 99004 ; 'John A. Schlueter' ; Materials Science Division Argonne National Laboratory 9700 South Cass Avenue Argonne, IL 60439, USA ; 'Tom Lancaster' ; Claredon Laboratory Physics Department Oxford University Oxford, OX1 3PU, UK ; 'Stephen Blundell' ; Claredon Laboratory Physics Department Oxford University Oxford, OX1 3PU, UK ; ; M.L.Brooks ; ; Claredon Laboratory Physics Department Oxford University Oxford, OX1 3PU, UK ; 'Francis L. Pratt' ; ISIS Facility Rutherford-Appleton Laboratory Chilton, Didcot OX11 0QX, UK ; 'Thomas Papageorgiou' ; Hochfeld-Magnetlabor Dresden (HLD) Forschungszentrum Rossendorf D-01314 Dresden, Germany ; 'Andreas D. Bianchi' ; Hochfeld-Magnetlabor Dresden (HLD) Forschungszentrum Rossendorf D-01314 Dresden, Germany ; 'Jochen Wosnitza' ; Hochfeld-Magnetlabor Dresden (HLD) Forschungszentrum Rossendorf D-01314 Dresden, Germany ; 'Myung-Hwan Whangbo' ; Department of Chemistry North Carolina State University Raleigh, NC 27695 ; data_CuPyzHF2BF4 _database_code_depnum_ccdc_archive 'CCDC 611880' _audit_creation_method 'manual editing of SHELXL-97 cif file' _chemical_name_systematic ; ? ; _chemical_name_common 'Bis(pyrazine) copper(ii) bifloride tetrafluoroborate' _chemical_melting_point ? _chemical_formula_moiety 'Cu 2+, (C4 H4 N2)2, H F2 1-, B F4 1-' _chemical_formula_sum 'C8 H9 B Cu F6 N4' _chemical_formula_weight 349.54 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' 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' F F 0.0171 0.0103 '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 tetragonal _symmetry_space_group_name_H-M 'P 4/n b m' _symmetry_space_group_name_Hall '-P 4a 2b' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y+1/2, x, z' 'y, -x+1/2, z' '-x+1/2, y, -z' 'x, -y+1/2, -z' 'y, x, -z' '-y+1/2, -x+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y-1/2, -x, -z' '-y, x-1/2, -z' 'x-1/2, -y, z' '-x, y-1/2, z' '-y, -x, z' 'y-1/2, x-1/2, z' _cell_length_a 9.6901(4) _cell_length_b 9.6901(4) _cell_length_c 6.6193(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 621.54(5) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 1858 _cell_measurement_theta_min 2.973 _cell_measurement_theta_max 28.209 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max .38 _exptl_crystal_size_mid .32 _exptl_crystal_size_min .26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.868 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 346 _exptl_absorpt_coefficient_mu 1.825 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.544 _exptl_absorpt_correction_T_max 0.664 _exptl_absorpt_process_details ; (Sheldrick, 2001) ; _exptl_special_details ; The data collection nominally covered over a hemisphere of reciprocal space, by a combination of four sets of exposures; each set had a different \f angle for the crystal and each exposure covered 0.3\% in \w. The crystal-to-detector distance was 4.975 cm. Coverage of the unique set was over 99% complete to at least 28\% in \q. Crystal decay was monitored by repeating the initial 50 frames at the end of data collection and analyzing the duplicate reflections. Decay was found to be less than 1%, and no decay correction was therefore applied. ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART CCD area detector' _diffrn_measurement_method 'area detector \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 5131 _diffrn_reflns_av_R_equivalents 0.0238 _diffrn_reflns_av_sigmaI/netI 0.0117 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 28.21 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 28.21 _diffrn_measured_fraction_theta_full 0.995 _reflns_number_total 423 _reflns_number_gt 369 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995)' _computing_cell_refinement 'SAINT (Bruker, 2001)' _computing_data_reduction 'SAINT (Bruker, 2001)' _computing_structure_solution 'SHELXTL (Sheldrick, 2001)' _computing_structure_refinement 'SHELXTL (Sheldrick, 2001)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2001)' _computing_publication_material 'SHELXTL (Sheldrick, 2001)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0887P)^2^+0.6494P] 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 423 _refine_ls_number_parameters 28 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0479 _refine_ls_R_factor_gt 0.0440 _refine_ls_wR_factor_ref 0.1296 _refine_ls_wR_factor_gt 0.1220 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.001 _refine_diff_density_max 1.952 _refine_diff_density_min -0.798 _refine_diff_density_rms 0.123 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 0.2500 0.2500 0.5000 0.0261(4) Uani 1 8 d S . . N N 0.1012(3) 0.3988(3) 0.5000 0.0296(7) Uani 1 2 d S . . C C 0.0930(3) 0.4916(3) 0.3522(4) 0.0409(7) Uani 1 1 d . . . H1 H 0.1564 0.4885 0.2469 0.049 Uiso 1 1 calc R . . B B 0.2500 0.7500 0.0000 0.059(3) Uani 1 8 d S . . F1 F 0.3340(4) 0.6660(4) 0.1056(10) 0.127(2) Uani 1 2 d S . . F2 F 0.2500 0.2500 0.1665(6) 0.0622(15) Uani 1 4 d S . . H2 H 0.2500 0.2500 0.0000 0.056 Uiso 1 8 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 0.0178(4) 0.0178(4) 0.0427(6) 0.000 0.000 0.000 N 0.0223(9) 0.0223(9) 0.0443(15) 0.0032(7) 0.0032(7) 0.0018(11) C 0.0328(13) 0.0342(13) 0.0556(15) 0.0109(11) 0.0127(11) 0.0088(11) B 0.055(5) 0.055(5) 0.066(7) 0.000 0.000 0.000 F1 0.109(3) 0.109(3) 0.165(5) 0.057(3) -0.057(3) -0.016(3) F2 0.073(2) 0.073(2) 0.040(2) 0.000 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 Cu N 2.040(4) . ? Cu F2 2.207(4) . ? N C 1.331(3) . ? C C 1.390(5) 16_565 ? C H1 0.9300 . ? B F1 1.347(4) . ? F2 H2 1.102(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 N Cu N 90.0 . 3 ? N Cu N 180.0 . 2 ? N Cu F2 90.0 . 5_556 ? N Cu F2 90.0 . . ? F2 Cu F2 180.0 5_556 . ? C N C 117.4(3) 8_556 . ? C N Cu 121.30(17) . . ? N C C 121.30(17) . 16_565 ? N C H1 119.3 . . ? C C H1 119.3 16_565 . ? F1 B F1 105.6(3) 11_565 . ? F1 B F1 117.5(7) 2_565 . ? Cu F2 H2 180.0 . . ? 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 F2 Cu N C 149.35(16) 5_556 . . . ? F2 Cu N C -30.65(16) . . . . ? C N C C -0.003(1) 8_556 . . 16_565 ? Cu N C C 180.0 . . . 16_565 ? #===End