# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Firas Awwadi' _publ_contact_author_email fawwadi@yahoo.com loop_ _publ_author_name F.Awwadi S.Haddad B.Twamley R.Willett data_sfh11 _database_code_depnum_ccdc_archive 'CCDC 873517' #TrackingRef '- SFH11.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; '4-Bromopyridinium tetrafluoroborate' ; _chemical_name_common '4-BP BF4' _chemical_melting_point ? _chemical_formula_moiety 'C5 H5 Br N, B F4' _chemical_formula_sum 'C5 H5 B Br F4 N' _chemical_formula_weight 245.82 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 5.2238(6) _cell_length_b 22.950(3) _cell_length_c 7.4020(8) _cell_angle_alpha 90.00 _cell_angle_beta 107.640(9) _cell_angle_gamma 90.00 _cell_volume 845.68(17) _cell_formula_units_Z 4 _cell_measurement_temperature 273 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 5.74 _cell_measurement_theta_max 14.73 _exptl_crystal_description parallelpiped _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.931 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 472 _exptl_absorpt_coefficient_mu 4.868 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.2462 _exptl_absorpt_correction_T_max 0.6417 _exptl_absorpt_process_details 'Psi scans' _exptl_special_details ; ? ; _diffrn_ambient_temperature 273 _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 'Sieman P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 1129 _diffrn_reflns_av_R_equivalents 0.0332 _diffrn_reflns_av_sigmaI/netI 0.0605 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 25.49 _reflns_number_total 800 _reflns_number_gt 512 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0480P)^2^+0.5887P] 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 SHELXL _refine_ls_extinction_coef 0.0137(18) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 800 _refine_ls_number_parameters 58 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0870 _refine_ls_R_factor_gt 0.0453 _refine_ls_wR_factor_ref 0.1144 _refine_ls_wR_factor_gt 0.0995 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _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 Br1 Br 0.0000 0.23213(3) 0.7500 0.0847(6) Uani 1 2 d S . . C4 C 0.0000 0.3146(2) 0.7500 0.0497(17) Uani 1 2 d S . . F2 F 0.2267(7) 0.03289(15) 0.7968(6) 0.1094(14) Uani 1 1 d . . . C3 C 0.1317(10) 0.3439(2) 0.6441(7) 0.0546(13) Uani 1 1 d . . . H3A H 0.2219 0.3239 0.5725 0.065 Uiso 1 1 calc R . . N1 N 0.0000 0.4309(2) 0.7500 0.0490(14) Uani 1 2 d S . . H1A H 0.0000 0.4684 0.7500 0.059 Uiso 1 2 calc SR . . C2 C 0.1274(10) 0.4031(2) 0.6460(7) 0.0511(12) Uani 1 1 d . . . H2A H 0.2141 0.4240 0.5743 0.061 Uiso 1 1 calc R . . B1 B 0.0000 0.0659(3) 0.7500 0.049(2) Uani 1 2 d S . . F1 F 0.0056(7) 0.10149(15) 0.8999(5) 0.0846(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Br1 0.1213(10) 0.0335(4) 0.0893(8) 0.000 0.0169(6) 0.000 C4 0.051(4) 0.027(3) 0.063(4) 0.000 0.006(4) 0.000 F2 0.101(3) 0.080(2) 0.139(3) -0.013(2) 0.025(3) 0.044(2) C3 0.062(3) 0.047(3) 0.060(3) -0.005(2) 0.027(3) 0.005(3) N1 0.061(4) 0.036(3) 0.053(3) 0.000 0.021(3) 0.000 C2 0.055(3) 0.050(3) 0.053(3) 0.000(2) 0.024(2) -0.001(3) B1 0.050(5) 0.036(4) 0.066(5) 0.000 0.025(4) 0.000 F1 0.107(2) 0.080(2) 0.075(2) -0.0138(18) 0.0406(19) 0.009(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br1 C4 1.892(6) . ? C4 C3 1.367(6) . ? C4 C3 1.367(6) 2_556 ? F2 B1 1.359(5) . ? C3 C2 1.358(6) . ? C3 H3A 0.9300 . ? N1 C2 1.324(5) 2_556 ? N1 C2 1.324(5) . ? N1 H1A 0.8600 . ? C2 H2A 0.9300 . ? B1 F2 1.359(5) 2_556 ? B1 F1 1.371(5) . ? B1 F1 1.371(5) 2_556 ? 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 C3 C4 C3 121.0(6) . 2_556 ? C3 C4 Br1 119.5(3) . . ? C3 C4 Br1 119.5(3) 2_556 . ? C2 C3 C4 118.3(5) . . ? C2 C3 H3A 120.9 . . ? C4 C3 H3A 120.9 . . ? C2 N1 C2 122.3(6) 2_556 . ? C2 N1 H1A 118.8 2_556 . ? C2 N1 H1A 118.8 . . ? N1 C2 C3 120.1(5) . . ? N1 C2 H2A 120.0 . . ? C3 C2 H2A 120.0 . . ? F2 B1 F2 112.3(6) 2_556 . ? F2 B1 F1 110.0(2) 2_556 . ? F2 B1 F1 108.8(2) . . ? F2 B1 F1 108.8(2) 2_556 2_556 ? F2 B1 F1 110.0(2) . 2_556 ? F1 B1 F1 106.8(6) . 2_556 ? 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 C3 C4 C3 C2 -0.3(4) 2_556 . . . ? Br1 C4 C3 C2 179.7(4) . . . . ? C2 N1 C2 C3 -0.3(4) 2_556 . . . ? C4 C3 C2 N1 0.6(7) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.49 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.391 _refine_diff_density_min -0.278 _refine_diff_density_rms 0.070 data_bt814t _database_code_depnum_ccdc_archive 'CCDC 873518' #TrackingRef '- bt814t.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (3-Brpy)CuF2.2H2O _chemical_melting_point ? _chemical_formula_moiety 'C5 H8 Br Cu F2 N O2' _chemical_formula_sum 'C5 H8 Br Cu F2 N O2' _chemical_formula_weight 295.57 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/m ' _symmetry_space_group_name_Hall '-P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 7.7096(14) _cell_length_b 6.7687(12) _cell_length_c 8.5459(15) _cell_angle_alpha 90.00 _cell_angle_beta 105.241(4) _cell_angle_gamma 90.00 _cell_volume 430.27(13) _cell_formula_units_Z 2 _cell_measurement_temperature 89(2) _cell_measurement_reflns_used 5125 _cell_measurement_theta_min 2.47 _cell_measurement_theta_max 30.03 _exptl_crystal_description block _exptl_crystal_colour 'light blue' _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.281 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 286 _exptl_absorpt_coefficient_mu 7.172 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.301 _exptl_absorpt_correction_T_max 0.422 _exptl_absorpt_process_details 'TWINABS; Bruker, 2002' _exptl_special_details ; ? ; _diffrn_ambient_temperature 89(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker/Siemens SMART APEX' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.3 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10147 _diffrn_reflns_av_R_equivalents 0.0348 _diffrn_reflns_av_sigmaI/netI 0.0131 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.47 _diffrn_reflns_theta_max 25.24 _reflns_number_total 1111 _reflns_number_gt 1072 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART v. 5.630' _computing_cell_refinement 'Bruker SAINT+ v. 6.45a' _computing_data_reduction 'Bruker SAINT+ v. 6.45a' _computing_structure_solution 'XS, Bruker SHELXTL v. 6.12' _computing_structure_refinement 'XL, Bruker SHELXTL v. 6.12' _computing_molecular_graphics 'XP, Bruker SHELXTL v. 6.12' _computing_publication_material 'XCIF, Bruker SHELXTL v. 6.12' _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. Refined as a rotational twin with the second component rotated from first domain by 179.7 degrees about reciprocal axis 1.000 -0.005 -0.291 and real axis 1.000 0.001 0.001. Twin law 1.001 0.001 0.002 -0.011 -1.000 -0.004 -0.583 0.006 -1.001. Solved with Cell_Now. Refined as a HKLF5 file. ; _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^)+(0.0335P)^2^+0.8187P] 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 1111 _refine_ls_number_parameters 71 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0235 _refine_ls_R_factor_gt 0.0224 _refine_ls_wR_factor_ref 0.0648 _refine_ls_wR_factor_gt 0.0615 _refine_ls_goodness_of_fit_ref 1.152 _refine_ls_restrained_S_all 1.152 _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 Br1 Br 0.15671(5) 0.2500 -0.19170(5) 0.01814(15) Uani 1 2 d S . . C2 C 0.4620(5) 0.2500 0.0803(5) 0.0126(8) Uani 1 2 d S . . H2 H 0.3752 0.2500 0.1413 0.015 Uiso 1 2 calc SR . . C3 C 0.4047(6) 0.2500 -0.0878(5) 0.0144(9) Uani 1 2 d S . . C4 C 0.5296(6) 0.2500 -0.1800(5) 0.0155(9) Uani 1 2 d S . . H4 H 0.4926 0.2500 -0.2951 0.019 Uiso 1 2 calc SR . . C5 C 0.7090(6) 0.2500 -0.0971(5) 0.0184(10) Uani 1 2 d S . . H5 H 0.7983 0.2500 -0.1553 0.022 Uiso 1 2 calc SR . . C6 C 0.7594(6) 0.2500 0.0707(5) 0.0156(9) Uani 1 2 d S . . H6 H 0.8838 0.2500 0.1255 0.019 Uiso 1 2 calc SR . . Cu1 Cu 0.72252(6) 0.2500 0.40768(5) 0.01086(16) Uani 1 2 d S . . F1 F 0.9659(3) 0.2500 0.4055(3) 0.0128(5) Uani 1 2 d S . . F2 F 0.4811(3) 0.2500 0.4216(3) 0.0133(5) Uani 1 2 d S . . N1 N 0.6382(5) 0.2500 0.1590(4) 0.0122(7) Uani 1 2 d S . . O1 O 0.7743(2) 0.0166(3) 0.5715(2) 0.0140(4) Uani 1 1 d . . . H1A H 0.6873 -0.0692 0.5775 0.021 Uiso 1 1 d . . . H1B H 0.8656 -0.0624 0.5916 0.021 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Br1 0.0113(2) 0.0224(2) 0.0172(2) 0.000 -0.00249(17) 0.000 C2 0.012(2) 0.013(2) 0.014(2) 0.000 0.0047(16) 0.000 C3 0.011(2) 0.012(2) 0.019(2) 0.000 0.0008(17) 0.000 C4 0.018(2) 0.018(2) 0.0084(19) 0.000 0.0003(17) 0.000 C5 0.017(2) 0.022(2) 0.019(2) 0.000 0.0104(19) 0.000 C6 0.008(2) 0.019(2) 0.019(2) 0.000 0.0024(17) 0.000 Cu1 0.0067(3) 0.0141(3) 0.0116(3) 0.000 0.0021(2) 0.000 F1 0.0088(12) 0.0151(12) 0.0149(12) 0.000 0.0035(9) 0.000 F2 0.0095(12) 0.0164(12) 0.0143(11) 0.000 0.0037(9) 0.000 N1 0.0119(18) 0.0125(16) 0.0114(17) 0.000 0.0014(14) 0.000 O1 0.0097(10) 0.0119(10) 0.0202(10) 0.0045(8) 0.0037(8) 0.0021(8) _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 Br1 C3 1.884(4) . ? C2 N1 1.348(5) . ? C2 C3 1.388(6) . ? C2 H2 0.9500 . ? C3 C4 1.395(6) . ? C4 C5 1.378(6) . ? C4 H4 0.9500 . ? C5 C6 1.383(6) . ? C5 H5 0.9500 . ? C6 N1 1.347(5) . ? C6 H6 0.9500 . ? Cu1 F1 1.881(2) . ? Cu1 F2 1.896(2) . ? Cu1 N1 2.052(3) . ? Cu1 O1 2.079(2) 4_565 ? Cu1 O1 2.079(2) . ? O1 H1A 0.8996 . ? O1 H1B 0.8645 . ? 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 C2 C3 121.4(4) . . ? N1 C2 H2 119.3 . . ? C3 C2 H2 119.3 . . ? C2 C3 C4 120.3(4) . . ? C2 C3 Br1 119.7(3) . . ? C4 C3 Br1 120.0(3) . . ? C5 C4 C3 117.3(4) . . ? C5 C4 H4 121.4 . . ? C3 C4 H4 121.4 . . ? C4 C5 C6 120.2(4) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? N1 C6 C5 122.2(4) . . ? N1 C6 H6 118.9 . . ? C5 C6 H6 118.9 . . ? F1 Cu1 F2 177.07(9) . . ? F1 Cu1 N1 92.00(12) . . ? F2 Cu1 N1 90.93(12) . . ? F1 Cu1 O1 89.49(7) . 4_565 ? F2 Cu1 O1 88.61(7) . 4_565 ? N1 Cu1 O1 130.53(6) . 4_565 ? F1 Cu1 O1 89.49(7) . . ? F2 Cu1 O1 88.61(7) . . ? N1 Cu1 O1 130.53(6) . . ? O1 Cu1 O1 98.91(11) 4_565 . ? C6 N1 C2 118.5(4) . . ? C6 N1 Cu1 120.2(3) . . ? C2 N1 Cu1 121.3(3) . . ? Cu1 O1 H1A 121.0 . . ? Cu1 O1 H1B 127.3 . . ? H1A O1 H1B 99.8 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.24 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.452 _refine_diff_density_min -0.428 _refine_diff_density_rms 0.083