# 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_requested_category FM loop_ _publ_author_name D.Pinkowicz K.Kurpiewska K.Lewinski M.Balanda M.Mihalik M.Zentkova B.Sieklucka _publ_contact_author_name 'Dawid Pinkowicz' _publ_contact_author_email pinkowic@chemia.uj.edu.pl data_P_pressure _database_code_depnum_ccdc_archive 'CCDC 872123' #TrackingRef '- Ahp_pressure.cif' _audit_creation_date 2012-03-01T13:53:03-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C12 H4 Mn2 N10 Nb O6' _chemical_formula_weight 587.04 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _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 10.411(5) _cell_length_b 15.2090(18) _cell_length_c 14.1301(16) _cell_angle_alpha 90 _cell_angle_beta 109.71(3) _cell_angle_gamma 90 _cell_volume 2106.3(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.851 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1124 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.766 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_reflns_av_R_equivalents 0.104 _diffrn_reflns_av_unetI/netI 0.0731 _diffrn_reflns_number 2478 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 15 _diffrn_reflns_theta_full 15 _diffrn_measured_fraction_theta_full 0.566 _diffrn_measured_fraction_theta_max 0.566 _reflns_number_total 487 _reflns_number_gt 415 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.1249P)^2^+117.2190P] 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 none _refine_ls_extinction_method SHELXL _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_coef 0.0005(12) _refine_ls_number_reflns 487 _refine_ls_number_parameters 136 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0864 _refine_ls_R_factor_gt 0.07 _refine_ls_wR_factor_ref 0.1926 _refine_ls_wR_factor_gt 0.1748 _refine_ls_goodness_of_fit_ref 0.882 _refine_ls_restrained_S_all 0.874 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.433 _refine_diff_density_min -0.643 _refine_diff_density_rms 0.112 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 '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' Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Nb Nb 0.5976(5) 0.0221(2) 0.8055(2) 0.029(2) Uiso 1 1 d . . . Mn1 Mn 0.0985(10) -0.0512(3) 0.7949(4) 0.062(6) Uani 1 1 d . . . Mn2 Mn 0.4090(9) 0.2232(3) 0.4815(4) 0.032(5) Uani 1 1 d . . . O12 O 0.145(4) 0.0914(13) 0.8392(15) 0.047(8) Uiso 1 1 d . . . O11 O 0.037(4) -0.1908(15) 0.7698(17) 0.061(9) Uiso 1 1 d . . . O22 O 0.191(4) 0.1982(14) 0.4159(16) 0.061(9) Uiso 1 1 d . . . O21 O 0.632(4) 0.2507(12) 0.5628(15) 0.045(8) Uiso 1 1 d . . . N7 N 0.295(6) -0.061(2) 0.750(2) 0.045(11) Uiso 1 1 d . . . N3 N 0.416(4) 0.1280(15) 0.5958(19) 0.030(9) Uiso 1 1 d . . . N4 N 0.764(5) 0.206(2) 0.784(2) 0.065(12) Uiso 1 1 d . . . N1 N -0.098(7) -0.0406(19) 0.845(2) 0.040(12) Uiso 1 1 d . . . N2 N 0.559(4) -0.1227(16) 0.623(2) 0.031(9) Uiso 1 1 d . . . N6 N 0.639(4) -0.1687(17) 0.9291(18) 0.035(10) Uiso 1 1 d . . . N5 N 0.225(4) -0.0759(17) 0.955(2) 0.054(10) Uiso 1 1 d . . . N8 N 0.416(5) 0.176(2) 0.873(2) 0.053(11) Uiso 1 1 d . . . N11 N -0.011(5) 0.0079(17) 0.6387(19) 0.058(11) Uiso 1 1 d D . . N16 N -0.154(5) -0.0112(18) 0.601(2) 0.062(11) Uiso 1 1 d D . . C7 C 0.395(7) -0.031(2) 0.770(3) 0.028(13) Uiso 1 1 d . . . C3 C 0.477(5) 0.089(2) 0.668(3) 0.040(12) Uiso 1 1 d . . . C4 C 0.711(5) 0.141(2) 0.787(2) 0.018(11) Uiso 1 1 d . . . C1 C -0.191(8) -0.017(3) 0.822(3) 0.060(18) Uiso 1 1 d . . . C2 C 0.576(5) -0.075(2) 0.686(2) 0.029(11) Uiso 1 1 d . . . C6 C 0.621(6) -0.099(2) 0.886(3) 0.046(13) Uiso 1 1 d . . . C5 C 0.287(5) -0.059(2) 1.039(3) 0.035(11) Uiso 1 1 d . . . C8 C 0.486(6) 0.124(2) 0.844(2) 0.027(12) Uiso 1 1 d . . . C12 C 0.036(5) 0.076(2) 0.603(2) 0.067(15) Uiso 1 1 d D . . H12 H 0.1285 0.0882 0.6277 0.08 Uiso 1 1 calc R . . C13 C -0.050(5) 0.130(3) 0.530(3) 0.076(16) Uiso 1 1 d D . . H13 H -0.0132 0.1772 0.5065 0.091 Uiso 1 1 calc R . . C14 C -0.187(5) 0.114(2) 0.492(3) 0.069(15) Uiso 1 1 d D . . H14 H -0.2469 0.1508 0.4453 0.082 Uiso 1 1 calc R . . C15 C -0.232(5) 0.040(2) 0.528(2) 0.056(14) Uiso 1 1 d D . . H15 H -0.323 0.0249 0.4988 0.067 Uiso 1 1 calc R . . O1 O 0.176(4) 0.2521(13) 0.6873(16) 0.054(8) Uiso 1 1 d . . . O2 O 1.012(4) 0.1625(14) 0.9720(16) 0.060(8) 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 Mn1 0.096(15) 0.021(5) 0.038(5) -0.004(3) -0.018(7) -0.005(4) Mn2 0.034(13) 0.038(5) 0.030(4) 0.001(3) 0.016(5) 0.005(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Nb C8 2.11(5) . ? Nb C6 2.14(4) . ? Nb C7 2.16(6) . ? Nb C3 2.17(4) . ? Nb C5 2.19(4) 3_657 ? Nb C2 2.20(4) . ? Nb C1 2.21(8) 1_655 ? Nb C4 2.22(4) . ? Mn1 O11 2.21(3) . ? Mn1 N5 2.24(3) . ? Mn1 O12 2.26(2) . ? Mn1 N11 2.30(3) . ? Mn1 N7 2.34(7) . ? Mn1 N1 2.38(7) . ? Mn2 N3 2.15(3) . ? Mn2 O22 2.18(4) . ? Mn2 N8 2.19(3) 4_565 ? Mn2 N2 2.23(3) 3_656 ? Mn2 N6 2.23(3) 2_656 ? Mn2 O21 2.25(3) . ? N7 C7 1.08(7) . ? N3 C3 1.17(3) . ? N4 C4 1.15(4) . ? N1 C1 0.99(8) . ? N2 C2 1.12(3) . ? N2 Mn2 2.23(3) 3_656 ? N6 C6 1.20(3) . ? N6 Mn2 2.23(3) 2_646 ? N5 C5 1.17(3) . ? N8 C8 1.23(5) . ? N8 Mn2 2.19(3) 4_566 ? N11 C12 1.32(2) . ? N11 N16 1.43(5) . ? N16 C15 1.32(2) . ? C1 Nb 2.21(8) 1_455 ? C5 Nb 2.19(4) 3_657 ? C12 C13 1.38(2) . ? C13 C14 1.37(2) . ? C14 C15 1.37(2) . ? 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 C8 Nb C6 117.8(18) . . ? C8 Nb C7 75.8(18) . . ? C6 Nb C7 73.9(17) . . ? C8 Nb C3 71.9(14) . . ? C6 Nb C3 143.5(15) . . ? C7 Nb C3 75.1(16) . . ? C8 Nb C5 73.8(15) . 3_657 ? C6 Nb C5 76.3(12) . 3_657 ? C7 Nb C5 119.7(18) . 3_657 ? C3 Nb C5 137.2(11) . 3_657 ? C8 Nb C2 140.1(15) . . ? C6 Nb C2 78.0(12) . . ? C7 Nb C2 74.3(17) . . ? C3 Nb C2 75.3(12) . . ? C5 Nb C2 145.2(14) 3_657 . ? C8 Nb C1 141.7(17) . 1_655 ? C6 Nb C1 77(2) . 1_655 ? C7 Nb C1 141.3(17) . 1_655 ? C3 Nb C1 118(2) . 1_655 ? C5 Nb C1 76.9(17) 3_657 1_655 ? C2 Nb C1 74.8(16) . 1_655 ? C8 Nb C4 78.5(18) . . ? C6 Nb C4 142.8(18) . . ? C7 Nb C4 142.8(14) . . ? C3 Nb C4 71.6(14) . . ? C5 Nb C4 77.2(12) 3_657 . ? C2 Nb C4 111.8(14) . . ? C1 Nb C4 71.5(18) 1_655 . ? O11 Mn1 N5 92.4(9) . . ? O11 Mn1 O12 170.9(14) . . ? N5 Mn1 O12 83.2(9) . . ? O11 Mn1 N11 101.4(10) . . ? N5 Mn1 N11 166.2(11) . . ? O12 Mn1 N11 83.2(9) . . ? O11 Mn1 N7 97.3(13) . . ? N5 Mn1 N7 89.5(14) . . ? O12 Mn1 N7 90.6(13) . . ? N11 Mn1 N7 87.9(13) . . ? O11 Mn1 N1 83.3(13) . . ? N5 Mn1 N1 88.9(15) . . ? O12 Mn1 N1 88.7(13) . . ? N11 Mn1 N1 93.5(14) . . ? N7 Mn1 N1 178.3(11) . . ? N3 Mn2 O22 88.1(12) . . ? N3 Mn2 N8 175.8(13) . 4_565 ? O22 Mn2 N8 95.7(14) . 4_565 ? N3 Mn2 N2 93.6(9) . 3_656 ? O22 Mn2 N2 88.0(12) . 3_656 ? N8 Mn2 N2 88.4(11) 4_565 3_656 ? N3 Mn2 N6 91.5(10) . 2_656 ? O22 Mn2 N6 88.2(13) . 2_656 ? N8 Mn2 N6 86.8(12) 4_565 2_656 ? N2 Mn2 N6 173.6(9) 3_656 2_656 ? N3 Mn2 O21 88.6(11) . . ? O22 Mn2 O21 174.8(10) . . ? N8 Mn2 O21 87.5(14) 4_565 . ? N2 Mn2 O21 96.2(12) 3_656 . ? N6 Mn2 O21 87.8(12) 2_656 . ? C7 N7 Mn1 139(5) . . ? C3 N3 Mn2 150(4) . . ? C1 N1 Mn1 141(6) . . ? C2 N2 Mn2 163(4) . 3_656 ? C6 N6 Mn2 155(3) . 2_646 ? C5 N5 Mn1 157(2) . . ? C8 N8 Mn2 147(4) . 4_566 ? C12 N11 N16 119(3) . . ? C12 N11 Mn1 123(3) . . ? N16 N11 Mn1 113(2) . . ? C15 N16 N11 117(4) . . ? N7 C7 Nb 177(6) . . ? N3 C3 Nb 177(3) . . ? N4 C4 Nb 172(4) . . ? N1 C1 Nb 166(6) . 1_455 ? N2 C2 Nb 177(4) . . ? N6 C6 Nb 177(4) . . ? N5 C5 Nb 178(3) . 3_657 ? N8 C8 Nb 173(4) . . ? N11 C12 C13 122(4) . . ? C14 C13 C12 121(5) . . ? C15 C14 C13 116(4) . . ? N16 C15 C14 125(4) . . ?