# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Li Wang' _publ_contact_author_email LWANG99@JLU.EDU.CN _publ_section_title ; Synthesis, crystal structure and characterization of a new layered gallium phosphite Ga(HPO3)F3*(trans-C6N2H16) with left- and right-handed helical chains ; loop_ _publ_author_name 'Li Wang' 'Yanli Chen' 'Liangliang Huang' 'Jinhua Jiang' 'Tianyou Song' ; Li Wang ; 'Li-rong Zhang' # Attachment 'Ga-dach.cif' data_H # Attachment 'h.cif' _database_code_depnum_ccdc_archive 'CCDC 756497' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H17 F3 Ga N2 O3 P' _chemical_formula_weight 322.91 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.2635(5) _cell_length_b 9.8212(5) _cell_length_c 10.1458(3) _cell_angle_alpha 90.00 _cell_angle_beta 102.981(2) _cell_angle_gamma 90.00 _cell_volume 1093.66(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.961 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 656 _exptl_absorpt_coefficient_mu 2.699 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6876 _exptl_absorpt_correction_T_max 0.6876 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 Smart Apex CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 7705 _diffrn_reflns_av_R_equivalents 0.0379 _diffrn_reflns_av_sigmaI/netI 0.0371 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 28.25 _reflns_number_total 2686 _reflns_number_gt 2223 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0418P)^2^+0.3409P] 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 2686 _refine_ls_number_parameters 181 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0386 _refine_ls_R_factor_gt 0.0289 _refine_ls_wR_factor_ref 0.0788 _refine_ls_wR_factor_gt 0.0743 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _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 H13 H 0.262(3) 0.685(4) 0.633(4) 0.053(11) Uiso 1 1 d . . . H14 H 0.222(3) 0.638(4) 0.913(3) 0.039(9) Uiso 1 1 d . . . H7 H 0.136(3) 0.482(4) 0.587(4) 0.040(9) Uiso 1 1 d . . . H8 H 0.143(3) 0.870(4) 0.833(4) 0.032(9) Uiso 1 1 d . . . C1 C 0.2444(3) 0.6081(3) 0.7128(3) 0.0303(6) Uani 1 1 d . . . C2 C 0.2379(3) 0.7047(3) 0.8271(3) 0.0304(6) Uani 1 1 d . . . N1 N 0.1305(2) 0.5240(3) 0.6668(3) 0.0275(5) Uani 1 1 d . . . N2 N 0.1331(2) 0.7981(3) 0.7874(2) 0.0217(5) Uani 1 1 d . . . C3 C 0.3569(3) 0.7842(3) 0.8656(3) 0.0323(6) Uani 1 1 d . . . H3A H 0.3642 0.8425 0.7907 0.039 Uiso 1 1 calc R . . H3B H 0.3546 0.8422 0.9424 0.039 Uiso 1 1 calc R . . C4 C 0.4716(3) 0.5930(4) 0.7929(4) 0.0549(10) Uani 1 1 d . . . H4A H 0.5383 0.5304 0.8259 0.066 Uiso 1 1 calc R . . H4B H 0.4886 0.6404 0.7153 0.066 Uiso 1 1 calc R . . C5 C 0.4662(3) 0.6941(4) 0.9007(4) 0.0560(10) Uani 1 1 d . . . H5A H 0.5391 0.7499 0.9166 0.067 Uiso 1 1 calc R . . H5B H 0.4652 0.6460 0.9840 0.067 Uiso 1 1 calc R . . C6 C 0.3538(3) 0.5119(3) 0.7482(3) 0.0349(7) Uani 1 1 d . . . H6A H 0.3440 0.4511 0.8204 0.042 Uiso 1 1 calc R . . H6B H 0.3579 0.4570 0.6698 0.042 Uiso 1 1 calc R . . Ga1 Ga 0.09953(2) 0.11576(3) 0.55053(2) 0.01520(9) Uani 1 1 d . . . O1 O 0.15293(19) 0.4535(2) 0.41598(18) 0.0303(5) Uani 1 1 d . . . O2 O 0.20916(16) 0.20403(19) 0.45793(17) 0.0225(4) Uani 1 1 d . . . O3 O 0.12759(17) 0.28560(18) 0.22159(16) 0.0237(4) Uani 1 1 d . . . F3 F 0.02791(13) 0.00194(15) 0.39013(13) 0.0195(3) Uani 1 1 d . . . F1 F 0.21198(13) -0.01691(16) 0.61465(15) 0.0237(3) Uani 1 1 d . . . F2 F -0.02489(13) 0.24219(15) 0.48725(14) 0.0224(3) Uani 1 1 d . . . P1 P 0.20031(6) 0.32591(7) 0.36314(6) 0.01618(14) Uani 1 1 d . . . H1 H 0.316(2) 0.347(3) 0.353(3) 0.016(7) Uiso 1 1 d . . . H10 H 0.136(4) 0.827(5) 0.710(5) 0.073(15) Uiso 1 1 d . . . H11 H 0.070(4) 0.572(5) 0.643(4) 0.067(14) Uiso 1 1 d . . . H9 H 0.066(4) 0.758(4) 0.801(4) 0.060(12) Uiso 1 1 d . . . H12 H 0.127(3) 0.462(5) 0.725(4) 0.060(13) 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 C1 0.0228(13) 0.0310(16) 0.0376(16) -0.0072(13) 0.0081(12) 0.0001(11) C2 0.0242(14) 0.0260(15) 0.0378(16) -0.0015(12) 0.0001(12) 0.0006(11) N1 0.0266(13) 0.0349(15) 0.0207(12) -0.0038(11) 0.0050(10) -0.0058(11) N2 0.0240(12) 0.0239(13) 0.0176(11) 0.0000(9) 0.0055(9) 0.0027(10) C3 0.0273(14) 0.0317(16) 0.0360(15) -0.0012(13) 0.0029(12) -0.0067(12) C4 0.0231(16) 0.069(3) 0.073(3) -0.005(2) 0.0117(17) 0.0079(16) C5 0.0277(17) 0.062(3) 0.069(3) -0.004(2) -0.0087(17) -0.0020(17) C6 0.0296(15) 0.0328(17) 0.0415(17) -0.0009(13) 0.0064(13) 0.0070(13) Ga1 0.01885(15) 0.01521(15) 0.01117(14) 0.00097(10) 0.00258(10) 0.00065(10) O1 0.0507(13) 0.0201(10) 0.0223(9) -0.0033(8) 0.0129(9) 0.0003(9) O2 0.0218(9) 0.0259(10) 0.0198(8) 0.0090(7) 0.0044(7) 0.0013(7) O3 0.0358(11) 0.0191(9) 0.0137(8) 0.0007(7) 0.0004(7) -0.0022(8) F3 0.0219(7) 0.0227(7) 0.0144(6) -0.0010(6) 0.0049(6) -0.0021(6) F1 0.0226(7) 0.0237(8) 0.0238(7) 0.0074(6) 0.0031(6) 0.0050(6) F2 0.0239(8) 0.0226(8) 0.0199(7) 0.0016(6) 0.0032(6) 0.0066(6) P1 0.0186(3) 0.0169(3) 0.0129(3) 0.0012(2) 0.0031(2) -0.0018(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 C1 N1 1.509(4) . ? C1 C2 1.513(4) . ? C1 C6 1.530(4) . ? C1 H13 1.15(4) . ? C2 N2 1.477(4) . ? C2 C3 1.524(4) . ? C2 H14 1.14(3) . ? N1 H7 0.93(4) . ? N1 H11 0.82(5) . ? N1 H12 0.85(5) . ? N2 H8 0.84(4) . ? N2 H10 0.84(5) . ? N2 H9 0.89(4) . ? C3 C5 1.494(4) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.488(5) . ? C4 C6 1.527(5) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? Ga1 F1 1.8317(14) . ? Ga1 F2 1.8745(14) . ? Ga1 O2 1.9184(18) . ? Ga1 O3 1.9505(17) 4_566 ? Ga1 F3 1.9897(14) . ? Ga1 F3 2.0366(14) 3_556 ? O1 P1 1.507(2) . ? O2 P1 1.5246(18) . ? O3 P1 1.5368(17) . ? O3 Ga1 1.9505(17) 4_565 ? F3 Ga1 2.0366(14) 3_556 ? P1 H1 1.35(3) . ? 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 C1 C2 113.3(2) . . ? N1 C1 C6 108.6(2) . . ? C2 C1 C6 112.5(2) . . ? N1 C1 H13 114.0(17) . . ? C2 C1 H13 100.0(19) . . ? C6 C1 H13 108.3(19) . . ? N2 C2 C1 110.7(2) . . ? N2 C2 C3 110.7(2) . . ? C1 C2 C3 109.0(3) . . ? N2 C2 H14 108.4(17) . . ? C1 C2 H14 105.6(17) . . ? C3 C2 H14 112.2(17) . . ? C1 N1 H7 107(2) . . ? C1 N1 H11 111(3) . . ? H7 N1 H11 103(4) . . ? C1 N1 H12 110(3) . . ? H7 N1 H12 108(4) . . ? H11 N1 H12 117(4) . . ? C2 N2 H8 112(2) . . ? C2 N2 H10 105(3) . . ? H8 N2 H10 102(4) . . ? C2 N2 H9 110(3) . . ? H8 N2 H9 107(3) . . ? H10 N2 H9 121(4) . . ? C5 C3 C2 112.8(3) . . ? C5 C3 H3A 109.0 . . ? C2 C3 H3A 109.0 . . ? C5 C3 H3B 109.0 . . ? C2 C3 H3B 109.0 . . ? H3A C3 H3B 107.8 . . ? C5 C4 C6 113.0(3) . . ? C5 C4 H4A 109.0 . . ? C6 C4 H4A 109.0 . . ? C5 C4 H4B 109.0 . . ? C6 C4 H4B 109.0 . . ? H4A C4 H4B 107.8 . . ? C4 C5 C3 112.8(3) . . ? C4 C5 H5A 109.0 . . ? C3 C5 H5A 109.0 . . ? C4 C5 H5B 109.0 . . ? C3 C5 H5B 109.0 . . ? H5A C5 H5B 107.8 . . ? C4 C6 C1 110.3(3) . . ? C4 C6 H6A 109.6 . . ? C1 C6 H6A 109.6 . . ? C4 C6 H6B 109.6 . . ? C1 C6 H6B 109.6 . . ? H6A C6 H6B 108.1 . . ? F1 Ga1 F2 175.55(7) . . ? F1 Ga1 O2 91.47(7) . . ? F2 Ga1 O2 92.69(7) . . ? F1 Ga1 O3 94.38(7) . 4_566 ? F2 Ga1 O3 86.27(7) . 4_566 ? O2 Ga1 O3 102.58(8) . 4_566 ? F1 Ga1 F3 90.68(6) . . ? F2 Ga1 F3 87.56(6) . . ? O2 Ga1 F3 92.33(7) . . ? O3 Ga1 F3 164.10(7) 4_566 . ? F1 Ga1 F3 88.18(6) . 3_556 ? F2 Ga1 F3 87.41(6) . 3_556 ? O2 Ga1 F3 167.23(7) . 3_556 ? O3 Ga1 F3 90.17(7) 4_566 3_556 ? F3 Ga1 F3 74.91(6) . 3_556 ? P1 O2 Ga1 134.88(11) . . ? P1 O3 Ga1 130.50(11) . 4_565 ? Ga1 F3 Ga1 105.09(6) . 3_556 ? O1 P1 O2 113.99(11) . . ? O1 P1 O3 112.93(11) . . ? O2 P1 O3 109.44(10) . . ? O1 P1 H1 109.0(12) . . ? O2 P1 H1 103.9(11) . . ? O3 P1 H1 106.9(11) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.25 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.205 _refine_diff_density_min -0.488 _refine_diff_density_rms 0.091