Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Zheng, Li-Min' 'Gao, Song' 'Jacobson, Allan J.' 'Korp, James D.' 'Song, Hui-Hua' 'Xin, Xin-Quan' 'Yin, Ping' _publ_contact_author_name 'Dr Li-Min Zheng' _publ_contact_author_address ; Department of Chemistry Coordination Chemistry Institute Nanjing University Nanjing 210093 CHINA ; _publ_contact_author_email 'LMZHENG@NETRA.NJU.EDU.CN' _publ_section_title ; Syntheses, crystal structures and magnetic properties of manganese(II)-hedp compounds involving alkylenediamine templates (hedp = 1-hydroxyethylidene-diphosphonate) ; <> data_[NH3(CH2)4NH3][Mn(hedpH2)2] _database_code_CSD 178161 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? 'C4 H14 N2 2+, C4 H12 O14 P4 Mn 2-' _chemical_formula_sum 'C8 H26 Mn N2 O14 P4' _chemical_formula_weight 553.13 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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mn' 'Mn' 0.3368 0.7283 '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 5.3984(6) _cell_length_b 9.4004(10) _cell_length_c 10.4042(11) _cell_angle_alpha 65.237(2) _cell_angle_beta 80.868(2) _cell_angle_gamma 88.957(2) _cell_volume 472.67(9) _cell_formula_units_Z 1 _cell_measurement_temperature 566(2) _cell_measurement_reflns_used 1254 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 23.5 _exptl_crystal_description 'Plate' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.943 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 285 _exptl_absorpt_coefficient_mu 1.113 _exptl_absorpt_correction_type 'Empirical' _exptl_absorpt_correction_T_min 0.860 _exptl_absorpt_correction_T_max 0.975 _exptl_absorpt_process_details ? _exptl_special_details ; All measurements were made with a Siemens SMART platform diffractometer equipped with a 1K CCD area detector. A hemisphere of data (1271 frames at 5 cm detector distance) was collected using a narrow-frame method with scan widths of 0.30\% in omega and an exposure time of 35 s/frame. The first 50 frames were re-measured at the end of data collection to monitor instrument and crystal stability, and the maximum correction on I was <1%. The data were integrated using the Siemens SAINT program, with the intensities corrected for Lorentz factor, polarization, air absorption, and absorption due to variation in the path length through the detector faceplate. A psi scan absorption correction was applied based on the entire data set. Redundant reflections were averaged. Final cell constants were refined using 1254 reflections having I>10\s(I), and these, along with other information pertinent to data collection and refinement, are listed in Table 1. The Laue symmetry was determined to be -1, and from the systematic absences noted the space group was unambiguously P-1. Acknowledgment for use of MRSEC/TCSUH Facilities: This work made use of MRSEC/TCSUH Shared Experimental Facilities supported by the National Science Foundation under Award Number DMR-9632667 and the Texas Center for Superconductivity at the University of Houston. ; _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 'Siemens SMART CCD' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 1K _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 2168 _diffrn_reflns_av_R_equivalents 0.0279 _diffrn_reflns_av_sigmaI/netI 0.0319 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 23.50 _reflns_number_total 1380 _reflns_number_gt 1148 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART software (Siemens, 1996)' _computing_cell_refinement 'Bruker SAINT software (Bruker, 1999)' _computing_data_reduction 'Bruker SAINT software (Bruker, 1999)' _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^)+(0.0573P)^2^+0.0315P] 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 SHELXL _refine_ls_extinction_coef 0.011(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1380 _refine_ls_number_parameters 135 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0414 _refine_ls_R_factor_gt 0.0310 _refine_ls_wR_factor_ref 0.0858 _refine_ls_wR_factor_gt 0.0825 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _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 Mn1 Mn 0.0000 0.0000 0.0000 0.0168(3) Uani 1 2 d S . . P1 P 0.48287(15) 0.22298(9) 0.02341(9) 0.0140(3) Uani 1 1 d . . . P2 P 0.21324(16) -0.05179(10) 0.29945(9) 0.0166(3) Uani 1 1 d . . . O1 O 0.3412(4) 0.1570(2) -0.0559(2) 0.0172(5) Uani 1 1 d . . . O2 O 0.7540(4) 0.1802(2) 0.0288(2) 0.0190(5) Uani 1 1 d . . . O3 O 0.4693(4) 0.4045(2) -0.0492(2) 0.0213(6) Uani 1 1 d . . . H3 H 0.5000 0.5000 0.0000 0.026 Uiso 1 2 d S . . O4 O 0.0411(4) -0.0894(3) 0.2178(2) 0.0233(6) Uani 1 1 d . . . O5 O 0.1087(4) -0.0896(3) 0.4543(2) 0.0259(6) Uani 1 1 d . . . H5 H 0.0000 0.0000 0.5000 0.031 Uiso 1 2 d S . . O6 O 0.4597(4) -0.1430(3) 0.3053(2) 0.0252(6) Uani 1 1 d . . . H6 H 0.5093 -0.1432 0.2267 0.030 Uiso 1 1 calc R . . O7 O 0.0730(4) 0.2412(3) 0.1947(2) 0.0241(6) Uani 1 1 d . . . H7 H -0.0166 0.2073 0.1560 0.029 Uiso 1 1 calc R . . C1 C 0.3062(6) 0.1594(4) 0.2077(3) 0.0165(8) Uani 1 1 d . . . C2 C 0.4486(6) 0.2073(4) 0.2994(3) 0.0227(8) Uani 1 1 d . . . H2A H 0.3430 0.1863 0.3895 0.034 Uiso 1 1 calc R . . H2B H 0.4962 0.3173 0.2504 0.034 Uiso 1 1 calc R . . H2C H 0.5965 0.1484 0.3164 0.034 Uiso 1 1 calc R . . C3 C 0.8392(7) -0.4794(5) 0.3428(4) 0.0333(10) Uani 1 1 d . . . H3A H 0.7152 -0.5666 0.3917 0.050 Uiso 1 1 calc R . . H3B H 0.7572 -0.3843 0.3355 0.050 Uiso 1 1 calc R . . C4 C 1.0481(7) -0.5039(4) 0.4295(4) 0.0350(10) Uani 1 1 d . . . H4A H 1.1819 -0.4238 0.3755 0.052 Uiso 1 1 calc R . . H4B H 1.1165 -0.6054 0.4473 0.052 Uiso 1 1 calc R . . N1 N 0.9368(6) -0.4671(4) 0.1959(3) 0.0322(8) Uani 1 1 d . . . H1N H 0.8108 -0.4499 0.1464 0.048 Uiso 1 1 calc R . . H2N H 1.0058 -0.5560 0.2024 0.048 Uiso 1 1 calc R . . H3N H 1.0520 -0.3879 0.1514 0.048 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 Mn1 0.0148(4) 0.0177(4) 0.0207(4) -0.0105(3) -0.0037(3) 0.0010(3) P1 0.0139(5) 0.0129(5) 0.0160(5) -0.0071(4) -0.0019(3) 0.0007(4) P2 0.0169(5) 0.0166(5) 0.0158(5) -0.0066(4) -0.0016(4) 0.0021(4) O1 0.0145(12) 0.0209(12) 0.0187(12) -0.0111(10) -0.0016(9) -0.0011(10) O2 0.0145(12) 0.0220(13) 0.0242(13) -0.0135(10) -0.0030(10) 0.0024(10) O3 0.0302(14) 0.0131(12) 0.0218(13) -0.0078(10) -0.0065(10) 0.0016(10) O4 0.0232(14) 0.0219(13) 0.0212(13) -0.0053(10) -0.0034(10) -0.0055(11) O5 0.0347(15) 0.0235(13) 0.0159(13) -0.0078(11) 0.0052(11) -0.0002(11) O6 0.0242(14) 0.0247(14) 0.0253(14) -0.0100(11) -0.0029(11) 0.0074(11) O7 0.0176(13) 0.0277(14) 0.0318(14) -0.0172(11) -0.0044(10) 0.0054(11) C1 0.0149(18) 0.0177(18) 0.0190(18) -0.0101(14) -0.0028(14) 0.0058(14) C2 0.029(2) 0.0221(19) 0.0172(19) -0.0086(15) -0.0026(15) -0.0042(16) C3 0.032(2) 0.037(2) 0.035(2) -0.0168(19) -0.0122(18) 0.0078(19) C4 0.037(2) 0.027(2) 0.040(2) -0.0120(19) -0.0083(19) 0.0032(18) N1 0.0293(18) 0.0310(18) 0.0317(19) -0.0069(15) -0.0106(14) 0.0026(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 Mn1 O4 2.109(2) . ? Mn1 O4 2.109(2) 2 ? Mn1 O2 2.223(2) 2_655 ? Mn1 O2 2.223(2) 1_455 ? Mn1 O1 2.225(2) 2 ? Mn1 O1 2.225(2) . ? P1 O2 1.514(2) . ? P1 O1 1.516(2) . ? P1 O3 1.556(2) . ? P1 C1 1.850(3) . ? P2 O4 1.491(2) . ? P2 O5 1.510(2) . ? P2 O6 1.565(2) . ? P2 C1 1.844(3) . ? O2 Mn1 2.223(2) 1_655 ? O7 C1 1.458(4) . ? C1 C2 1.520(4) . ? C3 N1 1.492(5) . ? C3 C4 1.509(5) . ? C4 C4 1.509(8) 2_746 ? 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 O4 Mn1 O4 180.00(16) . 2 ? O4 Mn1 O2 90.29(8) . 2_655 ? O4 Mn1 O2 89.71(8) 2 2_655 ? O4 Mn1 O2 89.71(8) . 1_455 ? O4 Mn1 O2 90.29(8) 2 1_455 ? O2 Mn1 O2 180.00(11) 2_655 1_455 ? O4 Mn1 O1 90.92(8) . 2 ? O4 Mn1 O1 89.08(8) 2 2 ? O2 Mn1 O1 91.37(8) 2_655 2 ? O2 Mn1 O1 88.63(8) 1_455 2 ? O4 Mn1 O1 89.08(8) . . ? O4 Mn1 O1 90.92(8) 2 . ? O2 Mn1 O1 88.63(8) 2_655 . ? O2 Mn1 O1 91.37(8) 1_455 . ? O1 Mn1 O1 180.00(12) 2 . ? O2 P1 O1 115.86(12) . . ? O2 P1 O3 109.84(13) . . ? O1 P1 O3 107.10(12) . . ? O2 P1 C1 109.96(13) . . ? O1 P1 C1 107.92(13) . . ? O3 P1 C1 105.64(13) . . ? O4 P2 O5 115.87(14) . . ? O4 P2 O6 111.90(14) . . ? O5 P2 O6 104.73(13) . . ? O4 P2 C1 108.80(14) . . ? O5 P2 C1 107.86(14) . . ? O6 P2 C1 107.26(13) . . ? P1 O1 Mn1 135.73(12) . . ? P1 O2 Mn1 138.14(13) . 1_655 ? P2 O4 Mn1 134.94(13) . . ? O7 C1 C2 107.8(2) . . ? O7 C1 P2 106.1(2) . . ? C2 C1 P2 110.3(2) . . ? O7 C1 P1 106.60(19) . . ? C2 C1 P1 111.4(2) . . ? P2 C1 P1 114.30(17) . . ? N1 C3 C4 111.3(3) . . ? C3 C4 C4 110.5(4) . 2_746 ? 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 O2 P1 O1 Mn1 119.97(17) . . . . ? O3 P1 O1 Mn1 -117.09(18) . . . . ? C1 P1 O1 Mn1 -3.8(2) . . . . ? O4 Mn1 O1 P1 -21.53(18) . . . . ? O4 Mn1 O1 P1 158.47(18) 2 . . . ? O2 Mn1 O1 P1 -111.84(18) 2_655 . . . ? O2 Mn1 O1 P1 68.16(18) 1_455 . . . ? O1 Mn1 O1 P1 121(100) 2 . . . ? O1 P1 O2 Mn1 -19.1(2) . . . 1_655 ? O3 P1 O2 Mn1 -140.59(18) . . . 1_655 ? C1 P1 O2 Mn1 103.6(2) . . . 1_655 ? O5 P2 O4 Mn1 152.52(17) . . . . ? O6 P2 O4 Mn1 -87.5(2) . . . . ? C1 P2 O4 Mn1 30.8(2) . . . . ? O4 Mn1 O4 P2 165(100) 2 . . . ? O2 Mn1 O4 P2 93.4(2) 2_655 . . . ? O2 Mn1 O4 P2 -86.6(2) 1_455 . . . ? O1 Mn1 O4 P2 -175.2(2) 2 . . . ? O1 Mn1 O4 P2 4.8(2) . . . . ? O4 P2 C1 O7 54.9(2) . . . . ? O5 P2 C1 O7 -71.6(2) . . . . ? O6 P2 C1 O7 176.08(18) . . . . ? O4 P2 C1 C2 171.3(2) . . . . ? O5 P2 C1 C2 44.9(2) . . . . ? O6 P2 C1 C2 -67.5(2) . . . . ? O4 P2 C1 P1 -62.30(19) . . . . ? O5 P2 C1 P1 171.25(16) . . . . ? O6 P2 C1 P1 58.9(2) . . . . ? O2 P1 C1 O7 164.49(19) . . . . ? O1 P1 C1 O7 -68.3(2) . . . . ? O3 P1 C1 O7 46.0(2) . . . . ? O2 P1 C1 C2 47.2(2) . . . . ? O1 P1 C1 C2 174.4(2) . . . . ? O3 P1 C1 C2 -71.3(2) . . . . ? O2 P1 C1 P2 -78.64(19) . . . . ? O1 P1 C1 P2 48.60(19) . . . . ? O3 P1 C1 P2 162.90(16) . . . . ? N1 C3 C4 C4 173.0(4) . . . 2_746 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H3 O3 1.230(2) 1.230(2) 2.461(4) 180.00(15) 2_665 O5 H5 O5 1.228(2) 1.228(2) 2.456(4) 180.00(18) 2_556 O6 H6 O1 0.82 1.89 2.702(3) 172.7 2_655 O7 H7 O2 0.82 2.04 2.843(3) 165.9 1_455 N1 H1N O3 0.89 1.89 2.783(4) 175.4 2_655 N1 H2N O7 0.89 1.97 2.831(4) 163.6 1_645 N1 H3N O2 0.89 2.19 3.028(4) 156.1 2_755 _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 23.50 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.375 _refine_diff_density_min -0.481 _refine_diff_density_rms 0.074 #===END data_[NH3(CH2)4NH3]Mn2(hedpH)2.2H2O _database_code_CSD 178162 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C4 H14 N2 2+, C4 H10 O14 P4 Mn2 2-, 2 H2 O' _chemical_formula_sum 'C8 H28 Mn2 N2 O16 P4' _chemical_formula_weight 642.08 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mn' 'Mn' 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 5.6315(5) _cell_length_b 12.2419(10) _cell_length_c 16.4002(14) _cell_angle_alpha 90.00 _cell_angle_beta 99.309(2) _cell_angle_gamma 90.00 _cell_volume 1115.74(16) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 2998 _cell_measurement_theta_min 2.09 _cell_measurement_theta_max 25.05 _exptl_crystal_description 'diamond-shaped column' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_diffrn 1.911 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 656 _exptl_absorpt_coefficient_mu 1.497 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.7237 _exptl_absorpt_correction_T_max 0.8770 _exptl_absorpt_process_details ? _publ_section_experimental ; All measurements were made with a Siemens SMART platform diffractometer equipped with a 1K CCD area detector. A hemisphere of data (1271 frames at 5 cm detector distance) was collected using a narrow-frame method with scan widths of 0.30\% in omega and an exposure time of 35 s/frame. The first 50 frames were re-measured at the end of data collection to monitor instrument and crystal stability, and the maximum correction on I was <1%. The data were integrated using the Siemens SAINT program, with the intensities corrected for Lorentz factor, polarization, air absorption, and absorption due to variation in the path length through the detector faceplate. A psi scan absorption correction was applied based on the entire data set. Redundant reflections were averaged. Final cell constants were refined using 2998 reflections having I>10\s(I), and these, along with other information pertinent to data collection and refinement, are listed in Table 1. The Laue symmetry was determined to be 2/m, and from the systematic absences noted the space group was unambiguously P2(1)/n. Acknowledgment for use of MRSEC/TCSUH Facilities: This work made use of MRSEC/TCSUH Shared Experimental Facilities supported by the National Science Foundation under Award Number DMR-9632667 and the Texas Center for Superconductivity at the University of Houston. ; _diffrn_ambient_temperature 223(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' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 1K _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 5868 _diffrn_reflns_av_R_equivalents 0.0382 _diffrn_reflns_av_sigmaI/netI 0.0273 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 25.05 _reflns_number_total 2081 _reflns_number_gt 1644 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART software (Siemens, 1996)' _computing_cell_refinement 'Bruker SAINT software (Bruker, 1999)' _computing_data_reduction 'Bruker SAINT software (Bruker, 1999)' _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^)+(0.0421P)^2^+0.5948P] 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 SHELXL _refine_ls_extinction_coef 0.0014(6) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1973 _refine_ls_number_parameters 153 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0395 _refine_ls_R_factor_gt 0.0284 _refine_ls_wR_factor_ref 0.0731 _refine_ls_wR_factor_gt 0.0689 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.033 _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 Mn1 Mn 0.79270(7) 0.44645(3) 0.41811(3) 0.01243(14) Uani 1 1 d . . . P1 P 0.27530(12) 0.58529(6) 0.38008(4) 0.01119(18) Uani 1 1 d . . . P2 P 0.23663(12) 0.34108(6) 0.34823(4) 0.01215(18) Uani 1 1 d . . . O1 O 0.5474(3) 0.57858(15) 0.40074(12) 0.0167(4) Uani 1 1 d . . . O1W O -0.2621(4) 0.14914(17) 0.30980(15) 0.0276(5) Uani 1 1 d G . . H1WA H -0.3568 0.1984 0.3301 0.033 Uiso 1 1 d G . . H1WB H -0.1305 0.1796 0.2946 0.033 Uiso 1 1 d G . . O2 O 0.1372(3) 0.56355(15) 0.45114(11) 0.0138(4) Uani 1 1 d . . . O3 O 0.1948(3) 0.69832(15) 0.34304(12) 0.0171(4) Uani 1 1 d . . . O4 O 0.5065(3) 0.33208(15) 0.37637(12) 0.0173(4) Uani 1 1 d . . . O5 O 0.0788(3) 0.32797(15) 0.41439(11) 0.0145(4) Uani 1 1 d . . . O6 O 0.1456(3) 0.25877(16) 0.27849(12) 0.0184(4) Uani 1 1 d D . . H6 H 0.223(5) 0.235(2) 0.2239(12) 0.026 Uiso 1 1 d D . . O7 O -0.0937(3) 0.48372(15) 0.29075(12) 0.0156(4) Uani 1 1 d . . . H7 H -0.1397 0.5401 0.2648 0.022 Uiso 1 1 calc R . . C1 C 0.1691(5) 0.4786(2) 0.30343(16) 0.0120(6) Uani 1 1 d . . . C2 C 0.2657(5) 0.4894(2) 0.22173(17) 0.0159(6) Uani 1 1 d . . . H2A H 0.2318 0.5622 0.1994 0.024 Uiso 1 1 calc R . . H2B H 0.1883 0.4358 0.1827 0.024 Uiso 1 1 calc R . . H2C H 0.4381 0.4772 0.2313 0.024 Uiso 1 1 calc R . . N1 N 0.1733(4) 0.23097(18) 0.56861(15) 0.0183(5) Uani 1 1 d . . . H1A H 0.3120 0.2612 0.5935 0.027 Uiso 1 1 calc R . . H1B H 0.0584 0.2414 0.6001 0.027 Uiso 1 1 calc R . . H1C H 0.1279 0.2625 0.5190 0.027 Uiso 1 1 calc R . . C3 C 0.2092(5) 0.1112(2) 0.5574(2) 0.0236(7) Uani 1 1 d . . . H3A H 0.2479 0.0760 0.6116 0.028 Uiso 1 1 calc R . . H3B H 0.3446 0.0996 0.5277 0.028 Uiso 1 1 calc R . . C4 C -0.0173(5) 0.0600(2) 0.5091(2) 0.0217(7) Uani 1 1 d . . . H4A H -0.1494 0.0675 0.5410 0.026 Uiso 1 1 calc R . . H4B H -0.0626 0.0995 0.4570 0.026 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 Mn1 0.0106(2) 0.0153(2) 0.0112(2) -0.00038(17) 0.00127(16) 0.00034(16) P1 0.0112(4) 0.0116(3) 0.0107(4) 0.0000(3) 0.0016(3) -0.0003(3) P2 0.0115(4) 0.0118(4) 0.0133(4) -0.0019(3) 0.0025(3) -0.0001(3) O1 0.0122(10) 0.0167(10) 0.0202(11) -0.0033(8) 0.0001(8) -0.0015(8) O1W 0.0172(11) 0.0279(12) 0.0381(14) -0.0128(11) 0.0054(10) -0.0040(9) O2 0.0148(10) 0.0161(10) 0.0102(10) -0.0002(8) 0.0012(8) -0.0018(7) O3 0.0215(11) 0.0143(10) 0.0165(10) 0.0036(8) 0.0059(9) 0.0032(8) O4 0.0129(10) 0.0146(10) 0.0243(11) -0.0014(9) 0.0027(8) 0.0014(8) O5 0.0158(10) 0.0148(10) 0.0131(10) 0.0012(8) 0.0028(8) 0.0012(7) O6 0.0201(10) 0.0183(10) 0.0179(10) -0.0083(9) 0.0062(8) -0.0046(8) O7 0.0114(10) 0.0179(10) 0.0169(10) 0.0026(8) 0.0004(8) 0.0016(7) C1 0.0091(13) 0.0156(14) 0.0108(14) 0.0003(11) -0.0002(11) 0.0009(10) C2 0.0169(14) 0.0185(14) 0.0131(15) -0.0017(12) 0.0045(12) -0.0022(11) N1 0.0192(13) 0.0155(12) 0.0200(13) -0.0019(10) 0.0029(10) -0.0009(9) C3 0.0258(17) 0.0150(15) 0.0283(18) -0.0028(13) -0.0005(14) 0.0027(12) C4 0.0215(15) 0.0179(16) 0.0248(16) -0.0013(13) 0.0009(13) -0.0002(12) _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 Mn1 O1 2.1162(19) . ? Mn1 O2 2.1201(19) 3_666 ? Mn1 O4 2.1611(19) . ? Mn1 O5 2.1762(18) 1_655 ? Mn1 O7 2.3265(19) 1_655 ? Mn1 O2 2.4026(18) 1_655 ? P1 O1 1.5171(19) . ? P1 O2 1.525(2) . ? P1 O3 1.5492(19) . ? P1 C1 1.844(3) . ? P2 O5 1.518(2) . ? P2 O4 1.5191(19) . ? P2 O6 1.548(2) . ? P2 C1 1.852(3) . ? O2 Mn1 2.1201(19) 3_666 ? O2 Mn1 2.4026(18) 1_455 ? O5 Mn1 2.1762(18) 1_455 ? O7 C1 1.462(3) . ? O7 Mn1 2.3265(19) 1_455 ? C1 C2 1.531(4) . ? N1 C3 1.495(4) . ? C3 C4 1.524(4) . ? C4 C4 1.518(5) 3_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 O1 Mn1 O2 101.01(7) . 3_666 ? O1 Mn1 O4 90.88(7) . . ? O2 Mn1 O4 106.88(7) 3_666 . ? O1 Mn1 O5 167.37(7) . 1_655 ? O2 Mn1 O5 88.42(7) 3_666 1_655 ? O4 Mn1 O5 94.42(7) . 1_655 ? O1 Mn1 O7 89.86(7) . 1_655 ? O2 Mn1 O7 152.39(7) 3_666 1_655 ? O4 Mn1 O7 98.16(7) . 1_655 ? O5 Mn1 O7 78.06(7) 1_655 1_655 ? O1 Mn1 O2 93.44(7) . 1_655 ? O2 Mn1 O2 78.17(7) 3_666 1_655 ? O4 Mn1 O2 172.61(7) . 1_655 ? O5 Mn1 O2 80.17(7) 1_655 1_655 ? O7 Mn1 O2 75.88(6) 1_655 1_655 ? O1 P1 O2 116.18(11) . . ? O1 P1 O3 110.91(11) . . ? O2 P1 O3 107.60(11) . . ? O1 P1 C1 108.57(11) . . ? O2 P1 C1 104.36(11) . . ? O3 P1 C1 108.86(11) . . ? O5 P2 O4 116.59(11) . . ? O5 P2 O6 107.27(11) . . ? O4 P2 O6 111.89(11) . . ? O5 P2 C1 105.86(11) . . ? O4 P2 C1 108.53(11) . . ? O6 P2 C1 106.04(12) . . ? P1 O1 Mn1 133.25(11) . . ? P1 O2 Mn1 138.44(11) . 3_666 ? P1 O2 Mn1 115.13(10) . 1_455 ? Mn1 O2 Mn1 101.83(7) 3_666 1_455 ? P2 O4 Mn1 135.03(11) . . ? P2 O5 Mn1 118.12(10) . 1_455 ? C1 O7 Mn1 106.43(14) . 1_455 ? O7 C1 C2 111.5(2) . . ? O7 C1 P1 106.01(17) . . ? C2 C1 P1 114.40(19) . . ? O7 C1 P2 103.51(17) . . ? C2 C1 P2 110.29(19) . . ? P1 C1 P2 110.50(13) . . ? N1 C3 C4 110.4(2) . . ? C4 C4 C3 112.2(3) 3_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 O2 P1 O1 Mn1 77.97(18) . . . . ? O3 P1 O1 Mn1 -158.77(14) . . . . ? C1 P1 O1 Mn1 -39.21(19) . . . . ? O2 Mn1 O1 P1 -99.19(16) 3_666 . . . ? O4 Mn1 O1 P1 8.20(17) . . . . ? O5 Mn1 O1 P1 123.1(3) 1_655 . . . ? O7 Mn1 O1 P1 106.35(16) 1_655 . . . ? O2 Mn1 O1 P1 -177.80(16) 1_655 . . . ? O1 P1 O2 Mn1 14.9(2) . . . 3_666 ? O3 P1 O2 Mn1 -110.03(17) . . . 3_666 ? C1 P1 O2 Mn1 134.42(16) . . . 3_666 ? O1 P1 O2 Mn1 -135.58(10) . . . 1_455 ? O3 P1 O2 Mn1 99.45(11) . . . 1_455 ? C1 P1 O2 Mn1 -16.10(13) . . . 1_455 ? O5 P2 O4 Mn1 -91.64(18) . . . . ? O6 P2 O4 Mn1 144.37(15) . . . . ? C1 P2 O4 Mn1 27.7(2) . . . . ? O1 Mn1 O4 P2 -1.62(18) . . . . ? O2 Mn1 O4 P2 100.17(17) 3_666 . . . ? O5 Mn1 O4 P2 -170.14(17) 1_655 . . . ? O7 Mn1 O4 P2 -91.60(17) 1_655 . . . ? O2 Mn1 O4 P2 -127.5(5) 1_655 . . . ? O4 P2 O5 Mn1 132.99(11) . . . 1_455 ? O6 P2 O5 Mn1 -100.69(12) . . . 1_455 ? C1 P2 O5 Mn1 12.21(15) . . . 1_455 ? Mn1 O7 C1 C2 173.78(17) 1_455 . . . ? Mn1 O7 C1 P1 -61.12(16) 1_455 . . . ? Mn1 O7 C1 P2 55.22(16) 1_455 . . . ? O1 P1 C1 O7 175.85(16) . . . . ? O2 P1 C1 O7 51.35(18) . . . . ? O3 P1 C1 O7 -63.32(19) . . . . ? O1 P1 C1 C2 -60.9(2) . . . . ? O2 P1 C1 C2 174.64(19) . . . . ? O3 P1 C1 C2 60.0(2) . . . . ? O1 P1 C1 P2 64.33(16) . . . . ? O2 P1 C1 P2 -60.18(15) . . . . ? O3 P1 C1 P2 -174.84(12) . . . . ? O5 P2 C1 O7 -45.66(18) . . . . ? O4 P2 C1 O7 -171.53(15) . . . . ? O6 P2 C1 O7 68.10(18) . . . . ? O5 P2 C1 C2 -165.05(17) . . . . ? O4 P2 C1 C2 69.1(2) . . . . ? O6 P2 C1 C2 -51.3(2) . . . . ? O5 P2 C1 P1 67.47(15) . . . . ? O4 P2 C1 P1 -58.41(16) . . . . ? O6 P2 C1 P1 -178.77(12) . . . . ? N1 C3 C4 C4 175.8(3) . . . 3_556 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1WA O4 0.90 2.01 2.892(3) 165.5 1_455 O1W H1WB O6 0.90 1.89 2.778(3) 170.3 . O6 H6 O3 1.098(10) 1.334(11) 2.431(3) 175(3) 2_545 O7 H7 O1W 0.83 1.83 2.655(3) 169.2 2_455 N1 H1A O1 0.90 2.11 2.812(3) 133.9 3_666 N1 H1C O5 0.90 1.87 2.767(3) 172.0 . N1 H1B O3 0.90 1.97 2.849(3) 165.4 3_566 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.410 _refine_diff_density_min -0.354 _refine_diff_density_rms 0.077 #===END data_[NH3(CH2)5NH3]Mn2(hedpH)2.2H2O _database_code_CSD 178163 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C5 H16 N2 2+, C4 H10 O14 P4 Mn2 2-, 2 H2 O' _chemical_formula_sum 'C9 H30 Mn2 N2 O16 P4' _chemical_formula_weight 656.11 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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mn' 'Mn' 0.3368 0.7283 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 5.6141(3) _cell_length_b 12.4252(6) _cell_length_c 16.4117(8) _cell_angle_alpha 90.00 _cell_angle_beta 98.9250(10) _cell_angle_gamma 90.00 _cell_volume 1130.96(10) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 5044 _cell_measurement_theta_min 1.26 _cell_measurement_theta_max 24.99 _exptl_crystal_description 'diamond-shaped column' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 1.927 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 672 _exptl_absorpt_coefficient_mu 1.479 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.7004 _exptl_absorpt_correction_T_max 0.8682 _exptl_absorpt_process_details ? _publ_section_experimental ; All measurements were made with a Siemens SMART platform diffractometer equipped with a 1K CCD area detector. A hemisphere of data (1271 frames at 5 cm detector distance) was collected using a narrow-frame method with scan widths of 0.30\% in omega and an exposure time of 25 s/frame. The first 50 frames were re-measured at the end of data collection to monitor instrument and crystal stability, and the maximum correction on I was <1%. The data were integrated using the Siemens SAINT program, with the intensities corrected for Lorentz factor, polarization, air absorption, and absorption due to variation in the path length through the detector faceplate. A psi scan absorption correction was applied based on the entire data set. Redundant reflections were averaged. Final cell constants were refined using 5044 reflections having I>10\s(I), and these, along with other information pertinent to data collection and refinement, are listed in Table 1. The Laue symmetry was determined to be 2/m, and from the systematic absences found the space group was shown to be either P2(1) or P2(1)/m. Although the polymeric anion chain contains an inversion center, the diamine does not and thus the correct space group is P2(1). Acknowledgment for use of MRSEC/TCSUH Facilities: This work made use of MRSEC/TCSUH Shared Experimental Facilities supported by the National Science Foundation under Award Number DMR-9632667 and the Texas Center for Superconductivity at the University of Houston. ; _diffrn_ambient_temperature 223(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' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 1K _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 5938 _diffrn_reflns_av_R_equivalents 0.0186 _diffrn_reflns_av_sigmaI/netI 0.0145 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.26 _diffrn_reflns_theta_max 24.99 _reflns_number_total 3916 _reflns_number_gt 3793 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART software (Siemens, 1996)' _computing_cell_refinement 'Bruker SAINT software (Bruker, 1999)' _computing_data_reduction 'Bruker SAINT software (Bruker, 1999)' _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^)+(0.0264P)^2^+1.6158P] 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 SHELXL _refine_ls_extinction_coef 0.0015(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.539(17) _refine_ls_number_reflns 3916 _refine_ls_number_parameters 307 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0258 _refine_ls_R_factor_gt 0.0246 _refine_ls_wR_factor_ref 0.0617 _refine_ls_wR_factor_gt 0.0612 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _refine_ls_shift/su_max 0.002 _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 Mn1 Mn 1.02711(8) 0.30859(4) 0.16690(3) 0.01305(14) Uani 1 1 d . . . Mn2 Mn 0.43830(8) 0.18626(4) 0.32722(3) 0.01337(14) Uani 1 1 d . . . P1 P 0.47191(16) 0.41307(7) 0.09662(6) 0.0131(2) Uani 1 1 d . . . P2 P 0.50921(14) 0.17260(8) 0.12669(5) 0.0121(2) Uani 1 1 d . . . P3 P 0.99371(15) 0.08322(7) 0.39567(6) 0.0124(2) Uani 1 1 d . . . P4 P 0.95563(15) 0.32519(7) 0.36935(5) 0.0113(2) Uani 1 1 d . . . O1 O 0.7400(4) 0.4222(2) 0.12597(16) 0.0183(6) Uani 1 1 d . . . O1W O -0.0111(5) 0.6107(3) 0.0692(2) 0.0322(7) Uani 1 1 d G . . H1WA H 0.1293 0.5794 0.0627 0.032 Uiso 1 1 d G . . H1WB H -0.1300 0.5627 0.0716 0.045 Uiso 1 1 d G . . O2W O 1.5160(5) -0.1087(3) 0.4455(2) 0.0337(8) Uani 1 1 d G . . H2WA H 1.4030 -0.0724 0.4677 0.047 Uiso 1 1 d G . . H2WB H 1.6061 -0.0656 0.4183 0.047 Uiso 1 1 d G . . O2 O 0.3080(4) 0.4256(2) 0.16130(15) 0.0150(5) Uani 1 1 d . . . O3 O 0.3843(4) 0.4948(2) 0.02717(16) 0.0198(6) Uani 1 1 d . . . H3 H 0.4907 0.5247 -0.0209 0.028 Uiso 1 1 d . . . O4 O 0.7800(4) 0.1804(2) 0.14868(15) 0.0181(6) Uani 1 1 d . . . O5 O 0.3664(4) 0.1914(2) 0.19697(15) 0.0157(5) Uani 1 1 d . . . O6 O 0.4318(4) 0.0624(2) 0.08761(15) 0.0180(6) Uani 1 1 d . . . O7 O 0.1436(4) 0.2725(2) 0.03710(15) 0.0156(6) Uani 1 1 d . . . H7 H 0.0994 0.2200 0.0072 0.022 Uiso 1 1 calc R . . O8 O 0.7240(4) 0.0749(2) 0.36916(16) 0.0182(6) Uani 1 1 d . . . O9 O 1.1476(4) 0.0744(2) 0.32808(15) 0.0147(5) Uani 1 1 d . . . O10 O 1.0873(4) -0.0011(2) 0.46217(16) 0.0195(6) Uani 1 1 d . . . H10 H 1.0225 -0.0234 0.5203 0.027 Uiso 1 1 d . . . O12 O 1.0951(4) 0.3092(2) 0.29723(14) 0.0154(5) Uani 1 1 d . . . O11 O 0.6844(4) 0.3161(2) 0.34812(15) 0.0175(6) Uani 1 1 d . . . O13 O 1.0337(4) 0.4335(2) 0.41044(15) 0.0168(6) Uani 1 1 d . . . O14 O 1.3236(4) 0.2228(2) 0.45554(15) 0.0159(6) Uani 1 1 d . . . H14 H 1.3678 0.2811 0.4775 0.022 Uiso 1 1 calc R . . C1 C 0.4057(5) 0.2781(3) 0.0511(2) 0.0105(7) Uani 1 1 d . . . C2 C 0.5102(6) 0.2671(3) -0.0288(2) 0.0184(8) Uani 1 1 d . . . H2A H 0.4506 0.3252 -0.0659 0.028 Uiso 1 1 calc R . . H2B H 0.4617 0.1986 -0.0545 0.028 Uiso 1 1 calc R . . H2C H 0.6847 0.2706 -0.0168 0.028 Uiso 1 1 calc R . . C3 C 1.0612(6) 0.2170(3) 0.4427(2) 0.0146(8) Uani 1 1 d . . . C4 C 0.9587(6) 0.2271(3) 0.5233(2) 0.0173(8) Uani 1 1 d . . . H4A H 0.9963 0.2977 0.5470 0.026 Uiso 1 1 calc R . . H4B H 1.0296 0.1722 0.5617 0.026 Uiso 1 1 calc R . . H4C H 0.7852 0.2176 0.5125 0.026 Uiso 1 1 calc R . . N1 N 0.0412(6) 0.9915(3) 0.1657(2) 0.0299(9) Uani 1 1 d . . . H1A H -0.1039 1.0130 0.1396 0.045 Uiso 1 1 calc R . . H1B H 0.1525 1.0012 0.1324 0.045 Uiso 1 1 calc R . . H1C H 0.0815 1.0304 0.2120 0.045 Uiso 1 1 calc R . . C11 C 0.0305(8) 0.8768(3) 0.1871(3) 0.0335(10) Uani 1 1 d . . . H11A H -0.0225 0.8345 0.1372 0.040 Uiso 1 1 calc R . . H11B H -0.0861 0.8662 0.2251 0.040 Uiso 1 1 calc R . . C12 C 0.2759(7) 0.8398(3) 0.2270(2) 0.0319(9) Uani 1 1 d . . . H12A H 0.3402 0.8913 0.2701 0.038 Uiso 1 1 calc R . . H12B H 0.3842 0.8394 0.1856 0.038 Uiso 1 1 calc R . . C13 C 0.2743(8) 0.7282(3) 0.2651(3) 0.0380(10) Uani 1 1 d . . . H13A H 0.1948 0.7313 0.3141 0.046 Uiso 1 1 calc R . . H13B H 0.1825 0.6789 0.2254 0.046 Uiso 1 1 calc R . . C14 C 0.5270(7) 0.6863(3) 0.2888(3) 0.0398(10) Uani 1 1 d . . . H14A H 0.5873 0.6647 0.2383 0.048 Uiso 1 1 calc R . . H14B H 0.6287 0.7456 0.3133 0.048 Uiso 1 1 calc R . . C15 C 0.5583(8) 0.5942(3) 0.3471(3) 0.0399(11) Uani 1 1 d . . . H15A H 0.7283 0.5726 0.3553 0.048 Uiso 1 1 calc R . . H15B H 0.5213 0.6188 0.4005 0.048 Uiso 1 1 calc R . . N2 N 0.4099(5) 0.4988(3) 0.32175(19) 0.0192(7) Uani 1 1 d . . . H2D H 0.3703 0.4981 0.2665 0.029 Uiso 1 1 calc R . . H2E H 0.2748 0.5010 0.3449 0.029 Uiso 1 1 calc R . . H2F H 0.4938 0.4389 0.3384 0.029 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 Mn1 0.0120(2) 0.0144(3) 0.0131(3) 0.0007(2) 0.00325(18) -0.0009(2) Mn2 0.0129(2) 0.0145(3) 0.0132(3) 0.0005(2) 0.00342(19) -0.0010(2) P1 0.0116(4) 0.0120(5) 0.0165(5) 0.0022(4) 0.0044(3) -0.0001(3) P2 0.0134(4) 0.0112(5) 0.0124(4) -0.0003(4) 0.0043(3) 0.0004(3) P3 0.0130(4) 0.0108(5) 0.0144(4) 0.0012(4) 0.0050(3) 0.0001(3) P4 0.0128(4) 0.0107(5) 0.0111(4) 0.0007(4) 0.0039(3) 0.0001(3) O1 0.0128(12) 0.0152(14) 0.0270(14) 0.0001(12) 0.0032(10) -0.0004(10) O1W 0.0207(14) 0.0282(18) 0.0479(18) 0.0123(15) 0.0055(13) 0.0042(12) O2W 0.0203(14) 0.0325(18) 0.049(2) 0.0225(15) 0.0085(13) 0.0042(12) O2 0.0144(11) 0.0148(13) 0.0168(12) -0.0002(11) 0.0060(9) -0.0015(10) O3 0.0192(13) 0.0201(15) 0.0217(13) 0.0080(12) 0.0085(10) 0.0049(11) O4 0.0151(11) 0.0157(15) 0.0231(14) 0.0028(12) 0.0021(10) 0.0005(11) O5 0.0177(11) 0.0163(13) 0.0137(12) 0.0024(11) 0.0039(9) 0.0002(10) O6 0.0232(13) 0.0142(15) 0.0185(13) -0.0015(11) 0.0089(10) -0.0030(10) O7 0.0114(11) 0.0172(14) 0.0179(12) -0.0038(11) 0.0013(9) -0.0011(9) O8 0.0156(12) 0.0134(14) 0.0256(14) 0.0005(12) 0.0037(10) -0.0010(10) O9 0.0166(11) 0.0127(13) 0.0161(12) 0.0006(10) 0.0068(9) -0.0011(9) O10 0.0217(13) 0.0191(15) 0.0193(13) 0.0066(12) 0.0086(10) 0.0035(10) O12 0.0184(11) 0.0168(14) 0.0123(11) -0.0003(11) 0.0066(9) -0.0004(10) O11 0.0146(11) 0.0147(15) 0.0229(14) 0.0026(11) 0.0026(9) -0.0001(10) O13 0.0198(12) 0.0147(15) 0.0166(12) -0.0038(11) 0.0055(9) -0.0021(10) O14 0.0115(11) 0.0176(14) 0.0185(13) -0.0025(11) 0.0022(9) -0.0008(9) C1 0.0113(14) 0.0098(19) 0.0109(16) -0.0011(14) 0.0036(12) 0.0007(12) C2 0.0192(17) 0.022(2) 0.0151(19) 0.0028(16) 0.0061(14) 0.0015(15) C3 0.0097(15) 0.019(2) 0.0148(18) 0.0011(15) 0.0009(13) -0.0005(14) C4 0.0181(16) 0.019(2) 0.0158(19) 0.0004(15) 0.0045(14) 0.0027(14) N1 0.0255(18) 0.021(2) 0.044(2) 0.0059(16) 0.0068(16) 0.0030(13) C11 0.043(2) 0.020(2) 0.036(2) 0.0018(18) 0.0000(19) -0.0068(17) C12 0.037(2) 0.029(2) 0.031(2) 0.0003(17) 0.0080(17) 0.0053(18) C13 0.040(2) 0.032(3) 0.040(3) 0.007(2) 0.001(2) -0.005(2) C14 0.040(2) 0.023(2) 0.056(3) 0.003(2) 0.005(2) -0.0026(18) C15 0.041(2) 0.023(2) 0.050(3) 0.002(2) -0.007(2) -0.0046(19) N2 0.0225(15) 0.0151(18) 0.0201(17) -0.0012(13) 0.0031(12) 0.0032(13) _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 Mn1 O4 2.103(3) . ? Mn1 O12 2.114(2) . ? Mn1 O2 2.157(3) 1_655 ? Mn1 O1 2.169(3) . ? Mn1 O7 2.366(3) 1_655 ? Mn1 O5 2.388(3) 1_655 ? Mn2 O5 2.114(2) . ? Mn2 O11 2.117(3) . ? Mn2 O9 2.145(3) 1_455 ? Mn2 O8 2.149(3) . ? Mn2 O14 2.340(3) 1_455 ? Mn2 O12 2.448(3) 1_455 ? P1 O1 1.512(2) . ? P1 O2 1.517(3) . ? P1 O3 1.549(3) . ? P1 C1 1.850(4) . ? P2 O4 1.510(2) . ? P2 O5 1.521(3) . ? P2 O6 1.546(3) . ? P2 C1 1.836(3) . ? P3 O9 1.512(3) . ? P3 O8 1.512(2) . ? P3 O10 1.545(3) . ? P3 C3 1.848(4) . ? P4 O11 1.513(2) . ? P4 O12 1.530(2) . ? P4 O13 1.538(3) . ? P4 C3 1.840(4) . ? O2 Mn1 2.157(3) 1_455 ? O5 Mn1 2.388(3) 1_455 ? O7 C1 1.455(4) . ? O7 Mn1 2.366(3) 1_455 ? O9 Mn2 2.145(2) 1_655 ? O12 Mn2 2.448(3) 1_655 ? O14 C3 1.457(4) . ? O14 Mn2 2.340(3) 1_655 ? C1 C2 1.523(5) . ? C3 C4 1.527(5) . ? N1 C11 1.471(5) . ? C11 C12 1.503(6) . ? C12 C13 1.522(6) . ? C13 C14 1.504(6) . ? C14 C15 1.485(6) . ? C15 N2 1.471(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 O4 Mn1 O12 99.10(10) . . ? O4 Mn1 O2 167.13(10) . 1_655 ? O12 Mn1 O2 91.27(10) . 1_655 ? O4 Mn1 O1 90.39(9) . . ? O12 Mn1 O1 108.65(10) . . ? O2 Mn1 O1 93.51(10) 1_655 . ? O4 Mn1 O7 89.81(9) . 1_655 ? O12 Mn1 O7 151.64(9) . 1_655 ? O2 Mn1 O7 77.50(9) 1_655 1_655 ? O1 Mn1 O7 98.08(9) . 1_655 ? O4 Mn1 O5 93.15(10) . 1_655 ? O12 Mn1 O5 77.30(8) . 1_655 ? O2 Mn1 O5 81.66(9) 1_655 1_655 ? O1 Mn1 O5 172.52(10) . 1_655 ? O7 Mn1 O5 75.36(8) 1_655 1_655 ? O5 Mn2 O11 99.11(10) . . ? O5 Mn2 O9 90.00(10) . 1_455 ? O11 Mn2 O9 166.07(10) . 1_455 ? O5 Mn2 O8 111.05(10) . . ? O11 Mn2 O8 90.15(9) . . ? O9 Mn2 O8 96.42(10) 1_455 . ? O5 Mn2 O14 150.24(9) . 1_455 ? O11 Mn2 O14 88.30(10) . 1_455 ? O9 Mn2 O14 78.68(9) 1_455 1_455 ? O8 Mn2 O14 97.62(10) . 1_455 ? O5 Mn2 O12 75.94(8) . 1_455 ? O11 Mn2 O12 91.74(9) . 1_455 ? O9 Mn2 O12 80.20(9) 1_455 1_455 ? O8 Mn2 O12 172.36(10) . 1_455 ? O14 Mn2 O12 75.05(8) 1_455 1_455 ? O1 P1 O2 116.85(15) . . ? O1 P1 O3 111.85(15) . . ? O2 P1 O3 106.85(14) . . ? O1 P1 C1 108.93(15) . . ? O2 P1 C1 105.64(15) . . ? O3 P1 C1 106.05(15) . . ? O4 P2 O5 116.00(14) . . ? O4 P2 O6 111.33(16) . . ? O5 P2 O6 107.65(15) . . ? O4 P2 C1 108.48(15) . . ? O5 P2 C1 104.71(15) . . ? O6 P2 C1 108.23(15) . . ? O9 P3 O8 116.39(15) . . ? O9 P3 O10 107.39(14) . . ? O8 P3 O10 111.87(15) . . ? O9 P3 C3 105.56(16) . . ? O8 P3 C3 108.22(15) . . ? O10 P3 C3 106.86(15) . . ? O11 P4 O12 115.46(13) . . ? O11 P4 O13 111.98(16) . . ? O12 P4 O13 107.91(15) . . ? O11 P4 C3 107.86(15) . . ? O12 P4 C3 105.08(15) . . ? O13 P4 C3 108.12(16) . . ? P1 O1 Mn1 134.82(17) . . ? P1 O2 Mn1 119.18(15) . 1_455 ? P2 O4 Mn1 134.44(17) . . ? P2 O5 Mn2 136.18(14) . . ? P2 O5 Mn1 115.73(13) . 1_455 ? Mn2 O5 Mn1 104.39(10) . 1_455 ? C1 O7 Mn1 105.22(19) . 1_455 ? P3 O8 Mn2 135.44(17) . . ? P3 O9 Mn2 118.68(15) . 1_655 ? P4 O12 Mn1 138.56(14) . . ? P4 O12 Mn2 113.99(13) . 1_655 ? Mn1 O12 Mn2 102.36(10) . 1_655 ? P4 O11 Mn2 134.62(17) . . ? C3 O14 Mn2 105.9(2) . 1_655 ? O7 C1 C2 112.0(3) . . ? O7 C1 P2 106.2(2) . . ? C2 C1 P2 113.2(2) . . ? O7 C1 P1 104.0(2) . . ? C2 C1 P1 110.4(3) . . ? P2 C1 P1 110.59(17) . . ? O14 C3 C4 112.3(3) . . ? O14 C3 P4 105.9(2) . . ? C4 C3 P4 112.4(2) . . ? O14 C3 P3 104.0(2) . . ? C4 C3 P3 110.8(3) . . ? P4 C3 P3 111.06(18) . . ? N1 C11 C12 109.4(3) . . ? C11 C12 C13 113.3(4) . . ? C14 C13 C12 110.9(4) . . ? C15 C14 C13 116.5(4) . . ? N2 C15 C14 115.7(3) . . ? 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 O2 P1 O1 Mn1 93.1(2) . . . . ? O3 P1 O1 Mn1 -143.4(2) . . . . ? C1 P1 O1 Mn1 -26.5(3) . . . . ? O4 Mn1 O1 P1 0.2(2) . . . . ? O12 Mn1 O1 P1 -99.6(2) . . . . ? O2 Mn1 O1 P1 167.9(2) 1_655 . . . ? O7 Mn1 O1 P1 90.0(2) 1_655 . . . ? O5 Mn1 O1 P1 118.4(7) 1_655 . . . ? O1 P1 O2 Mn1 -131.40(16) . . . 1_455 ? O3 P1 O2 Mn1 102.51(17) . . . 1_455 ? C1 P1 O2 Mn1 -10.11(19) . . . 1_455 ? O5 P2 O4 Mn1 -79.5(2) . . . . ? O6 P2 O4 Mn1 156.97(19) . . . . ? C1 P2 O4 Mn1 38.0(3) . . . . ? O12 Mn1 O4 P2 102.1(2) . . . . ? O2 Mn1 O4 P2 -114.5(4) 1_655 . . . ? O1 Mn1 O4 P2 -6.8(2) . . . . ? O7 Mn1 O4 P2 -104.9(2) 1_655 . . . ? O5 Mn1 O4 P2 179.8(2) 1_655 . . . ? O4 P2 O5 Mn2 -20.4(3) . . . . ? O6 P2 O5 Mn2 105.1(2) . . . . ? C1 P2 O5 Mn2 -139.9(2) . . . . ? O4 P2 O5 Mn1 133.86(15) . . . 1_455 ? O6 P2 O5 Mn1 -100.69(17) . . . 1_455 ? C1 P2 O5 Mn1 14.34(19) . . . 1_455 ? O11 Mn2 O5 P2 65.6(3) . . . . ? O9 Mn2 O5 P2 -125.0(2) 1_455 . . . ? O8 Mn2 O5 P2 -28.1(3) . . . . ? O14 Mn2 O5 P2 168.33(19) 1_455 . . . ? O12 Mn2 O5 P2 155.2(2) 1_455 . . . ? O11 Mn2 O5 Mn1 -90.53(11) . . . 1_455 ? O9 Mn2 O5 Mn1 78.88(12) 1_455 . . 1_455 ? O8 Mn2 O5 Mn1 175.76(9) . . . 1_455 ? O14 Mn2 O5 Mn1 12.2(3) 1_455 . . 1_455 ? O12 Mn2 O5 Mn1 -1.01(11) 1_455 . . 1_455 ? O9 P3 O8 Mn2 -88.0(3) . . . . ? O10 P3 O8 Mn2 148.1(2) . . . . ? C3 P3 O8 Mn2 30.6(3) . . . . ? O5 Mn2 O8 P3 95.1(2) . . . . ? O11 Mn2 O8 P3 -4.7(2) . . . . ? O9 Mn2 O8 P3 -172.4(2) 1_455 . . . ? O14 Mn2 O8 P3 -93.0(2) 1_455 . . . ? O12 Mn2 O8 P3 -109.1(7) 1_455 . . . ? O8 P3 O9 Mn2 135.18(16) . . . 1_655 ? O10 P3 O9 Mn2 -98.59(17) . . . 1_655 ? C3 P3 O9 Mn2 15.15(19) . . . 1_655 ? O11 P4 O12 Mn1 16.6(3) . . . . ? O13 P4 O12 Mn1 -109.6(3) . . . . ? C3 P4 O12 Mn1 135.2(3) . . . . ? O11 P4 O12 Mn2 -132.54(15) . . . 1_655 ? O13 P4 O12 Mn2 101.34(16) . . . 1_655 ? C3 P4 O12 Mn2 -13.84(18) . . . 1_655 ? O4 Mn1 O12 P4 -61.1(3) . . . . ? O2 Mn1 O12 P4 126.6(3) 1_655 . . . ? O1 Mn1 O12 P4 32.4(3) . . . . ? O7 Mn1 O12 P4 -167.94(19) 1_655 . . . ? O5 Mn1 O12 P4 -152.3(2) 1_655 . . . ? O4 Mn1 O12 Mn2 90.20(10) . . . 1_655 ? O2 Mn1 O12 Mn2 -82.15(11) 1_655 . . 1_655 ? O1 Mn1 O12 Mn2 -176.28(9) . . . 1_655 ? O7 Mn1 O12 Mn2 -16.6(3) 1_655 . . 1_655 ? O5 Mn1 O12 Mn2 -1.00(11) 1_655 . . 1_655 ? O12 P4 O11 Mn2 78.6(2) . . . . ? O13 P4 O11 Mn2 -157.34(19) . . . . ? C3 P4 O11 Mn2 -38.5(3) . . . . ? O5 Mn2 O11 P4 -102.1(2) . . . . ? O9 Mn2 O11 P4 127.7(4) 1_455 . . . ? O8 Mn2 O11 P4 9.3(2) . . . . ? O14 Mn2 O11 P4 106.9(2) 1_455 . . . ? O12 Mn2 O11 P4 -178.1(2) 1_455 . . . ? Mn1 O7 C1 C2 -174.5(2) 1_455 . . . ? Mn1 O7 C1 P2 61.4(2) 1_455 . . . ? Mn1 O7 C1 P1 -55.3(2) 1_455 . . . ? O4 P2 C1 O7 -175.6(2) . . . . ? O5 P2 C1 O7 -51.2(3) . . . . ? O6 P2 C1 O7 63.5(2) . . . . ? O4 P2 C1 C2 61.1(3) . . . . ? O5 P2 C1 C2 -174.5(2) . . . . ? O6 P2 C1 C2 -59.8(3) . . . . ? O4 P2 C1 P1 -63.4(2) . . . . ? O5 P2 C1 P1 61.08(19) . . . . ? O6 P2 C1 P1 175.71(16) . . . . ? O1 P1 C1 O7 171.5(2) . . . . ? O2 P1 C1 O7 45.2(2) . . . . ? O3 P1 C1 O7 -68.0(2) . . . . ? O1 P1 C1 C2 -68.2(3) . . . . ? O2 P1 C1 C2 165.5(2) . . . . ? O3 P1 C1 C2 52.3(2) . . . . ? O1 P1 C1 P2 57.9(2) . . . . ? O2 P1 C1 P2 -68.41(19) . . . . ? O3 P1 C1 P2 178.40(16) . . . . ? Mn2 O14 C3 C4 173.8(2) 1_655 . . . ? Mn2 O14 C3 P4 -63.2(2) 1_655 . . . ? Mn2 O14 C3 P3 53.9(2) 1_655 . . . ? O11 P4 C3 O14 175.0(2) . . . . ? O12 P4 C3 O14 51.3(3) . . . . ? O13 P4 C3 O14 -63.7(3) . . . . ? O11 P4 C3 C4 -62.1(3) . . . . ? O12 P4 C3 C4 174.3(2) . . . . ? O13 P4 C3 C4 59.2(3) . . . . ? O11 P4 C3 P3 62.7(2) . . . . ? O12 P4 C3 P3 -61.0(2) . . . . ? O13 P4 C3 P3 -176.01(17) . . . . ? O9 P3 C3 O14 -47.2(2) . . . . ? O8 P3 C3 O14 -172.4(2) . . . . ? O10 P3 C3 O14 66.9(2) . . . . ? O9 P3 C3 C4 -168.0(2) . . . . ? O8 P3 C3 C4 66.7(3) . . . . ? O10 P3 C3 C4 -53.9(3) . . . . ? O9 P3 C3 P4 66.32(19) . . . . ? O8 P3 C3 P4 -58.9(2) . . . . ? O10 P3 C3 P4 -179.57(16) . . . . ? N1 C11 C12 C13 169.7(4) . . . . ? C11 C12 C13 C14 168.7(4) . . . . ? C12 C13 C14 C15 163.2(4) . . . . ? C13 C14 C15 N2 55.4(6) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1WA O3 0.90 1.94 2.820(4) 166.3 . O1W H1WB O1 0.90 2.14 2.951(4) 149.5 1_455 O2W H2WA O10 0.90 1.97 2.803(4) 153.1 . O2W H2WB O8 0.90 2.07 2.931(4) 158.5 1_655 O3 H3 O6 1.124(2) 1.325(3) 2.434(4) 167.23(16) 2_655 O7 H7 O1W 0.83 1.86 2.689(4) 173.8 2_545 O10 H10 O13 1.108(3) 1.338(3) 2.436(4) 169.78(18) 2_746 O14 H14 O2W 0.83 1.91 2.717(4) 164.2 2_856 N1 H1A O4 0.90 2.19 2.759(5) 120.4 1_465 N1 H1B O6 0.90 1.98 2.846(4) 160.1 1_565 N1 H1C O9 0.90 1.96 2.833(5) 162.8 1_465 N2 H2D O2 0.90 1.93 2.761(4) 152.6 . N2 H2E O13 0.90 2.04 2.862(4) 152.1 1_455 N2 H2F O11 0.90 1.86 2.740(4) 166.8 . _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.367 _refine_diff_density_min -0.266 _refine_diff_density_rms 0.056 #===END data_[NH3(CH2)6NH3]MN2(hedpH)2.2H2O _database_code_CSD 178164 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H18 N2 2+, C4 H10 O14 P4 Mn2 2-, 2 H2 O' _chemical_formula_sum 'C10 H32 Mn2 N2 O16 P4' _chemical_formula_weight 670.14 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mn' 'Mn' 0.3368 0.7283 '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/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 5.6597(2) _cell_length_b 12.8273(6) _cell_length_c 16.4012(7) _cell_angle_alpha 90.00 _cell_angle_beta 98.4850(10) _cell_angle_gamma 90.00 _cell_volume 1177.67(9) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 4866 _cell_measurement_theta_min 2.02 _cell_measurement_theta_max 25.0 _exptl_crystal_description 'diamond-shaped column' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.16 _exptl_crystal_density_diffrn 1.890 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 688 _exptl_absorpt_coefficient_mu 1.422 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.7431 _exptl_absorpt_correction_T_max 0.9325 _exptl_absorpt_process_details ? _publ_section_experimental ; All measurements were made with a Siemens SMART platform diffractometer equipped with a 1K CCD area detector. A hemisphere of data (1271 frames at 5 cm detector distance) was collected using a narrow-frame method with scan widths of 0.30\% in omega and an exposure time of 25 s/frame. The first 50 frames were re-measured at the end of data collection to monitor instrument and crystal stability, and the maximum correction on I was <1%. The data were integrated using the Siemens SAINT program, with the intensities corrected for Lorentz factor, polarization, air absorption, and absorption due to variation in the path length through the detector faceplate. A psi scan absorption correction was applied based on the entire data set. Redundant reflections were averaged. Final cell constants were refined using 4866 reflections having I>10\s(I), and these, along with other information pertinent to data collection and refinement, are listed in Table 1. The Laue symmetry was determined to be 2/m, and from the systematic absences noted the space group was unambiguously P2(1)/n. Acknowledgment for use of MRSEC/TCSUH Facilities: This work made use of MRSEC/TCSUH Shared Experimental Facilities supported by the National Science Foundation under Award Number DMR-9632667 and the Texas Center for Superconductivity at the University of Houston. ; _diffrn_ambient_temperature 223(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' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 1K _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 6207 _diffrn_reflns_av_R_equivalents 0.0204 _diffrn_reflns_av_sigmaI/netI 0.0090 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2185 _reflns_number_gt 1967 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART software (Siemens, 1996)' _computing_cell_refinement 'Bruker SAINT software (Bruker, 1999)' _computing_data_reduction 'Bruker SAINT software (Bruker, 1999)' _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^)+(0.0365P)^2^+2.0541P] 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 SHELXL _refine_ls_extinction_coef 0.0037(6) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2076 _refine_ls_number_parameters 197 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.0280 _refine_ls_R_factor_gt 0.0267 _refine_ls_wR_factor_ref 0.0766 _refine_ls_wR_factor_gt 0.0760 _refine_ls_goodness_of_fit_ref 1.113 _refine_ls_restrained_S_all 1.122 _refine_ls_shift/su_max 0.024 _refine_ls_shift/su_mean 0.001 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 Mn1 Mn 0.78515(6) 0.43986(3) 0.41626(2) 0.01450(14) Uani 1 1 d . . . P1 P 0.27486(11) 0.57786(5) 0.38100(4) 0.01266(17) Uani 1 1 d . . . P2 P 0.22905(11) 0.34582(5) 0.34174(4) 0.01387(17) Uani 1 1 d . . . O1 O 0.5439(3) 0.56687(13) 0.39979(11) 0.0175(4) Uani 1 1 d . . . O1W O -0.2654(4) 0.16010(18) 0.29829(17) 0.0417(6) Uani 1 1 d GD . . H1WA H -0.3613 0.2078 0.3172 0.050 Uiso 1 1 d GD . . H1WB H -0.1255 0.1874 0.2882 0.050 Uiso 1 1 d GD . . O2 O 0.1395(3) 0.55888(13) 0.45303(11) 0.0170(4) Uani 1 1 d . . . O3 O 0.2019(3) 0.68684(14) 0.34546(11) 0.0180(4) Uani 1 1 d . . . H3 H 0.261(5) 0.723(2) 0.292(2) 0.025 Uiso 1 1 d . . . O4 O 0.4939(3) 0.33673(14) 0.37241(12) 0.0209(4) Uani 1 1 d . . . O5 O 0.0652(3) 0.33152(13) 0.40691(10) 0.0163(4) Uani 1 1 d . . . O6 O 0.1464(3) 0.27099(15) 0.27008(11) 0.0221(4) Uani 1 1 d . . . O7 O -0.0952(3) 0.48729(14) 0.29128(11) 0.0173(4) Uani 1 1 d . . . H7 H -0.1380 0.5419 0.2663 0.024 Uiso 1 1 calc R . . C1 C 0.1647(4) 0.48009(19) 0.30284(15) 0.0138(5) Uani 1 1 d . . . C2 C 0.2644(5) 0.4988(2) 0.22263(15) 0.0200(6) Uani 1 1 d . . . H2A H 0.2278 0.5694 0.2038 0.030 Uiso 1 1 calc R . . H2B H 0.1926 0.4498 0.1811 0.030 Uiso 1 1 calc R . . H2C H 0.4362 0.4890 0.2320 0.030 Uiso 1 1 calc R . . N1 N 0.201(4) 1.2609(11) 0.5601(17) 0.017(4) Uani 0.50 1 d PD A -1 H1A H 0.2895 1.3173 0.5772 0.025 Uiso 0.50 1 calc PR A -1 H1B H 0.0956 1.2486 0.5950 0.025 Uiso 0.50 1 calc PR A -1 H1C H 0.1219 1.2726 0.5092 0.025 Uiso 0.50 1 calc PR A -1 C11 C 0.3590(17) 1.1696(7) 0.5583(7) 0.040(3) Uani 0.50 1 d PD A -1 H11A H 0.4236 1.1496 0.6149 0.048 Uiso 0.50 1 calc PR A -1 H11B H 0.4934 1.1882 0.5298 0.048 Uiso 0.50 1 calc PR A -1 C12 C 0.2255(12) 1.0770(5) 0.5146(6) 0.0409(17) Uani 0.50 1 d PD A -1 C13 C -0.016(2) 1.0613(12) 0.5457(10) 0.034(4) Uiso 0.20 1 d PD A -1 C14 C -0.125(3) 0.9538(12) 0.5270(7) 0.037(5) Uiso 0.20 1 d PD A -1 C13' C 0.042(2) 1.0338(9) 0.5626(7) 0.038(3) Uiso 0.30 1 d PD A -1 C14' C -0.052(2) 0.9293(8) 0.5277(5) 0.032(3) Uiso 0.30 1 d PD A -1 C15 C -0.1645(13) 0.9349(5) 0.4360(4) 0.0323(14) Uani 0.50 1 d PD A -1 C16 C -0.3137(17) 0.8387(7) 0.4091(6) 0.030(2) Uani 0.50 1 d PD A -1 H16A H -0.4550 0.8379 0.4371 0.037 Uiso 0.50 1 calc PR A -1 H16B H -0.3686 0.8425 0.3496 0.037 Uiso 0.50 1 calc PR A -1 N2 N -0.178(4) 0.7412(11) 0.4279(18) 0.019(4) Uani 0.50 1 d PD A -1 H2D H -0.2679 0.6865 0.4080 0.028 Uiso 0.50 1 calc PR A -1 H2E H -0.1382 0.7346 0.4829 0.028 Uiso 0.50 1 calc PR A -1 H2F H -0.0439 0.7430 0.4043 0.028 Uiso 0.50 1 calc PR A -1 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 Mn1 0.0136(2) 0.0160(2) 0.0143(2) -0.00039(14) 0.00337(15) 0.00168(14) P1 0.0133(3) 0.0124(3) 0.0128(3) 0.0000(2) 0.0035(2) -0.0003(2) P2 0.0131(3) 0.0130(3) 0.0162(3) -0.0024(2) 0.0046(2) -0.0003(2) O1 0.0147(9) 0.0155(9) 0.0219(9) -0.0028(7) 0.0011(7) -0.0008(7) O1W 0.0214(11) 0.0340(13) 0.0699(17) -0.0257(12) 0.0075(11) -0.0054(9) O2 0.0212(9) 0.0164(9) 0.0146(9) 0.0005(7) 0.0066(7) 0.0004(7) O3 0.0204(9) 0.0152(9) 0.0197(9) 0.0035(7) 0.0068(7) 0.0017(7) O4 0.0149(9) 0.0168(9) 0.0313(10) -0.0001(8) 0.0040(8) 0.0015(7) O5 0.0175(9) 0.0151(9) 0.0174(9) 0.0005(7) 0.0059(7) 0.0016(7) O6 0.0242(10) 0.0207(10) 0.0226(10) -0.0096(8) 0.0081(8) -0.0038(8) O7 0.0118(8) 0.0183(9) 0.0215(9) 0.0047(7) 0.0011(7) 0.0006(7) C1 0.0115(11) 0.0156(12) 0.0144(12) 0.0000(9) 0.0026(9) -0.0013(9) C2 0.0203(13) 0.0246(14) 0.0159(13) -0.0023(11) 0.0053(10) -0.0052(11) N1 0.014(4) 0.019(5) 0.016(7) -0.001(3) 0.002(5) -0.002(3) C11 0.025(4) 0.020(4) 0.071(8) -0.009(5) -0.007(5) 0.003(3) C12 0.035(4) 0.023(3) 0.065(6) -0.007(4) 0.009(4) 0.002(3) C15 0.041(4) 0.024(3) 0.033(4) 0.000(3) 0.008(3) 0.005(3) C16 0.025(4) 0.020(4) 0.043(5) 0.000(4) -0.005(4) 0.003(3) N2 0.025(6) 0.013(4) 0.019(7) 0.003(3) 0.006(4) -0.002(3) _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 Mn1 O1 2.1173(18) . ? Mn1 O2 2.1233(18) 3_666 ? Mn1 O5 2.1303(17) 1_655 ? Mn1 O4 2.1527(18) . ? Mn1 O7 2.3323(18) 1_655 ? Mn1 O2 2.5219(18) 1_655 ? P1 O1 1.5147(18) . ? P1 O2 1.5194(18) . ? P1 O3 1.5471(18) . ? P1 C1 1.835(2) . ? P2 O4 1.5138(18) . ? P2 O5 1.5261(17) . ? P2 O6 1.5359(19) . ? P2 C1 1.854(3) . ? O2 Mn1 2.1233(18) 3_666 ? O2 Mn1 2.5219(18) 1_455 ? O5 Mn1 2.1303(17) 1_455 ? O7 C1 1.458(3) . ? O7 Mn1 2.3323(18) 1_455 ? C1 C2 1.525(3) . ? N1 C11 1.477(9) . ? C11 C12 1.528(8) . ? C12 C13' 1.499(9) . ? C12 C13 1.541(9) . ? C13 C14 1.524(9) . ? C14 C15 1.497(9) . ? C13' C14' 1.522(9) . ? C14' C15 1.545(8) . ? C15 C16 1.523(8) . ? C16 N2 1.478(9) . ? 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 Mn1 O2 98.78(7) . 3_666 ? O1 Mn1 O5 164.89(7) . 1_655 ? O2 Mn1 O5 92.12(7) 3_666 1_655 ? O1 Mn1 O4 89.01(7) . . ? O2 Mn1 O4 111.82(7) 3_666 . ? O5 Mn1 O4 96.67(7) 1_655 . ? O1 Mn1 O7 87.29(7) . 1_655 ? O2 Mn1 O7 147.59(7) 3_666 1_655 ? O5 Mn1 O7 77.96(6) 1_655 1_655 ? O4 Mn1 O7 100.02(7) . 1_655 ? O1 Mn1 O2 92.29(6) . 1_655 ? O2 Mn1 O2 73.73(7) 3_666 1_655 ? O5 Mn1 O2 80.69(6) 1_655 1_655 ? O4 Mn1 O2 174.04(7) . 1_655 ? O7 Mn1 O2 74.24(6) 1_655 1_655 ? O1 P1 O2 115.71(10) . . ? O1 P1 O3 111.42(10) . . ? O2 P1 O3 107.48(10) . . ? O1 P1 C1 107.83(10) . . ? O2 P1 C1 105.98(10) . . ? O3 P1 C1 108.05(11) . . ? O4 P2 O5 115.62(10) . . ? O4 P2 O6 112.38(11) . . ? O5 P2 O6 108.24(10) . . ? O4 P2 C1 108.70(11) . . ? O5 P2 C1 104.11(10) . . ? O6 P2 C1 107.16(11) . . ? P1 O1 Mn1 135.03(11) . . ? P1 O2 Mn1 137.28(11) . 3_666 ? P1 O2 Mn1 112.67(9) . 1_455 ? Mn1 O2 Mn1 106.27(7) 3_666 1_455 ? P2 O4 Mn1 137.35(11) . . ? P2 O5 Mn1 120.49(10) . 1_455 ? C1 O7 Mn1 106.70(13) . 1_455 ? O7 C1 C2 111.86(19) . . ? O7 C1 P1 106.25(15) . . ? C2 C1 P1 111.37(17) . . ? O7 C1 P2 104.29(15) . . ? C2 C1 P2 111.34(17) . . ? P1 C1 P2 111.42(13) . . ? N1 C11 C12 111.5(10) . . ? C13' C12 C11 111.9(7) . . ? C13' C12 C13 20.1(7) . . ? C11 C12 C13 110.3(7) . . ? C14 C13 C12 113.8(10) . . ? C15 C14 C13 110.1(10) . . ? C12 C13' C14' 111.1(8) . . ? C13' C14' C15 113.4(8) . . ? C14 C15 C16 114.5(8) . . ? C14 C15 C14' 19.4(8) . . ? C16 C15 C14' 112.0(7) . . ? N2 C16 C15 112.1(10) . . ? 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 O2 P1 O1 Mn1 77.32(17) . . . . ? O3 P1 O1 Mn1 -159.51(13) . . . . ? C1 P1 O1 Mn1 -41.09(18) . . . . ? O2 Mn1 O1 P1 -101.80(15) 3_666 . . . ? O5 Mn1 O1 P1 122.5(2) 1_655 . . . ? O4 Mn1 O1 P1 10.14(16) . . . . ? O7 Mn1 O1 P1 110.22(16) 1_655 . . . ? O2 Mn1 O1 P1 -175.68(15) 1_655 . . . ? O1 P1 O2 Mn1 21.31(19) . . . 3_666 ? O3 P1 O2 Mn1 -103.91(16) . . . 3_666 ? C1 P1 O2 Mn1 140.74(15) . . . 3_666 ? O1 P1 O2 Mn1 -132.82(10) . . . 1_455 ? O3 P1 O2 Mn1 101.96(10) . . . 1_455 ? C1 P1 O2 Mn1 -13.39(12) . . . 1_455 ? O5 P2 O4 Mn1 -93.41(18) . . . . ? O6 P2 O4 Mn1 141.63(15) . . . . ? C1 P2 O4 Mn1 23.2(2) . . . . ? O1 Mn1 O4 P2 0.36(17) . . . . ? O2 Mn1 O4 P2 99.42(17) 3_666 . . . ? O5 Mn1 O4 P2 -165.59(17) 1_655 . . . ? O7 Mn1 O4 P2 -86.70(17) 1_655 . . . ? O2 Mn1 O4 P2 -102.2(6) 1_655 . . . ? O4 P2 O5 Mn1 131.79(11) . . . 1_455 ? O6 P2 O5 Mn1 -101.15(12) . . . 1_455 ? C1 P2 O5 Mn1 12.63(14) . . . 1_455 ? Mn1 O7 C1 C2 174.27(16) 1_455 . . . ? Mn1 O7 C1 P1 -63.99(15) 1_455 . . . ? Mn1 O7 C1 P2 53.83(14) 1_455 . . . ? O1 P1 C1 O7 175.51(14) . . . . ? O2 P1 C1 O7 51.03(17) . . . . ? O3 P1 C1 O7 -63.93(17) . . . . ? O1 P1 C1 C2 -62.44(19) . . . . ? O2 P1 C1 C2 173.08(17) . . . . ? O3 P1 C1 C2 58.1(2) . . . . ? O1 P1 C1 P2 62.53(14) . . . . ? O2 P1 C1 P2 -61.95(14) . . . . ? O3 P1 C1 P2 -176.91(11) . . . . ? O4 P2 C1 O7 -168.54(14) . . . . ? O5 P2 C1 O7 -44.77(16) . . . . ? O6 P2 C1 O7 69.78(16) . . . . ? O4 P2 C1 C2 70.66(19) . . . . ? O5 P2 C1 C2 -165.57(16) . . . . ? O6 P2 C1 C2 -51.03(19) . . . . ? O4 P2 C1 P1 -54.33(15) . . . . ? O5 P2 C1 P1 69.44(14) . . . . ? O6 P2 C1 P1 -176.02(11) . . . . ? N1 C11 C12 C13' -68.1(16) . . . . ? N1 C11 C12 C13 -46.6(17) . . . . ? C13' C12 C13 C14 -63.3(17) . . . . ? C11 C12 C13 C14 -161.9(11) . . . . ? C12 C13 C14 C15 -59.2(18) . . . . ? C11 C12 C13' C14' -168.4(9) . . . . ? C13 C12 C13' C14' 102(2) . . . . ? C12 C13' C14' C15 -58.0(13) . . . . ? C13 C14 C15 C16 -169.4(11) . . . . ? C13 C14 C15 C14' 104(2) . . . . ? C13' C14' C15 C14 -63.5(18) . . . . ? C13' C14' C15 C16 -164.9(9) . . . . ? C14 C15 C16 N2 -74.6(18) . . . . ? C14' C15 C16 N2 -53.5(16) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1WA O4 0.90 2.11 2.993(3) 166.1 1_455 O1W H1WB O6 0.90 1.93 2.827(3) 169.2 . O3 H3 O6 1.09(3) 1.36(3) 2.444(2) 174(3) 2 O7 H7 O1W 0.83 1.88 2.711(3) 175.5 2_455 N1 H1A O1 0.90 1.77 2.67(2) 174.0 3_676 N1 H1B O3 0.90 2.23 3.02(3) 146.0 3_576 N1 H1C O5 0.90 1.82 2.67(3) 156.6 1_565 N2 H2D O1 0.90 1.86 2.74(2) 163.1 1_455 N2 H2E O5 0.90 1.98 2.85(3) 160.1 3_566 N2 H2F O3 0.90 1.94 2.79(3) 155.8 . _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.477 _refine_diff_density_min -0.338 _refine_diff_density_rms 0.073