# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_MOZIF-1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common MOZIF-1 _chemical_melting_point ? _chemical_formula_moiety 'C6 H4 Mo N6 O8 Zn2' _chemical_formula_sum 'C6 H4 Mo N6 O8 Zn2' _chemical_formula_weight 514.87 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' Mo Mo -1.6832 0.6857 '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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I-42m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'y, -x, -z' '-x, -y, z' '-y, x, -z' 'x, -y, -z' '-y, -x, z' '-x, y, -z' 'y, x, z' 'x+1/2, y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-x+1/2, -y+1/2, z+1/2' '-y+1/2, x+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-y+1/2, -x+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'y+1/2, x+1/2, z+1/2' _cell_length_a 13.6272(2) _cell_length_b 13.6272(2) _cell_length_c 10.0246(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1861.57(7) _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 Octahedral _exptl_crystal_colour colourless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.29 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.837 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 992 _exptl_absorpt_coefficient_mu 3.259 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.301 _exptl_absorpt_correction_T_max 0.389 _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-58' _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 '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_% ? _diffrn_reflns_number 2361 _diffrn_reflns_av_R_equivalents 0.0324 _diffrn_reflns_av_sigmaI/netI 0.0462 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 29.05 _reflns_number_total 1041 _reflns_number_gt 875 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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. _platon_squeeze_details Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 0.500 0.000 282 55 ' ' 2 0.000 0.000 0.500 282 55 ' ' ; _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^)+(0.0390P)^2^+2.9719P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.11(5) _refine_ls_number_reflns 1041 _refine_ls_number_parameters 57 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0511 _refine_ls_R_factor_gt 0.0408 _refine_ls_wR_factor_ref 0.0984 _refine_ls_wR_factor_gt 0.0938 _refine_ls_goodness_of_fit_ref 1.162 _refine_ls_restrained_S_all 1.162 _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 Mo1 Mo 0.5000 0.0000 0.2500 0.0210(2) Uani 1 4 d S . . Zn1 Zn 0.5000 0.18884(5) 0.0000 0.0264(2) Uani 1 2 d S . . O1 O 0.4527(4) 0.3411(4) -0.1759(6) 0.0626(18) Uani 1 1 d . . . O2 O 0.5195(4) 0.1049(3) 0.1530(5) 0.0449(15) Uani 1 1 d . . . N1 N 0.3801(5) 0.3801(5) -0.1309(8) 0.038(2) Uani 1 2 d S . . N2 N 0.3734(4) 0.2564(4) 0.0403(5) 0.0324(14) Uani 1 1 d . . . C1 C 0.3361(4) 0.3361(4) -0.0109(19) 0.027(2) Uani 1 2 d S . . C2 C 0.3113(5) 0.2401(6) 0.1428(9) 0.055(2) Uani 1 1 d . . . H2 H 0.3160 0.1888 0.2037 0.066 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 Mo1 0.0214(3) 0.0214(3) 0.0204(4) 0.000 0.000 0.000 Zn1 0.0287(4) 0.0203(4) 0.0300(5) 0.000 0.0020(9) 0.000 O1 0.060(3) 0.063(4) 0.064(4) 0.024(3) 0.039(3) 0.028(3) O2 0.054(5) 0.031(2) 0.050(3) 0.021(2) 0.002(3) 0.002(2) N1 0.042(3) 0.042(3) 0.030(4) 0.011(3) 0.011(3) 0.007(4) N2 0.033(3) 0.028(3) 0.037(4) 0.008(2) 0.006(2) 0.004(2) C1 0.024(2) 0.024(2) 0.035(6) 0.004(4) 0.004(4) 0.000(3) C2 0.056(5) 0.046(5) 0.064(5) 0.030(4) 0.033(4) 0.014(4) _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 Mo1 O2 1.749(4) 10 ? Mo1 O2 1.749(4) 12_545 ? Mo1 O2 1.749(4) . ? Mo1 O2 1.749(4) 3_655 ? Zn1 O2 1.932(4) . ? Zn1 O2 1.932(4) 7_655 ? Zn1 N2 1.997(5) . ? Zn1 N2 1.997(5) 7_655 ? O1 N1 1.211(6) . ? N1 O1 1.211(6) 8 ? N1 C1 1.472(18) . ? N2 C1 1.304(9) . ? N2 C2 1.350(9) . ? C1 N2 1.304(9) 8 ? C2 C2 1.372(13) 8 ? C2 H2 0.9300 . ? 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 O2 Mo1 O2 112.4(3) 10 12_545 ? O2 Mo1 O2 108.01(15) 10 . ? O2 Mo1 O2 108.02(15) 12_545 . ? O2 Mo1 O2 108.02(15) 10 3_655 ? O2 Mo1 O2 108.01(16) 12_545 3_655 ? O2 Mo1 O2 112.4(3) . 3_655 ? O2 Zn1 O2 107.4(3) . 7_655 ? O2 Zn1 N2 103.4(2) . . ? O2 Zn1 N2 108.3(2) 7_655 . ? O2 Zn1 N2 108.3(2) . 7_655 ? O2 Zn1 N2 103.4(2) 7_655 7_655 ? N2 Zn1 N2 125.1(3) . 7_655 ? Mo1 O2 Zn1 154.8(3) . . ? O1 N1 O1 125.4(8) 8 . ? O1 N1 C1 117.3(4) 8 . ? O1 N1 C1 117.3(4) . . ? C1 N2 C2 101.1(8) . . ? C1 N2 Zn1 129.9(6) . . ? C2 N2 Zn1 128.3(5) . . ? N2 C1 N2 119.6(13) 8 . ? N2 C1 N1 120.1(7) 8 . ? N2 C1 N1 120.1(7) . . ? N2 C2 C2 109.0(4) . 8 ? N2 C2 H2 125.5 . . ? C2 C2 H2 125.5 8 . ? 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 Mo1 O2 Zn1 153.9(7) 10 . . . ? O2 Mo1 O2 Zn1 -84.2(6) 12_545 . . . ? O2 Mo1 O2 Zn1 34.9(6) 3_655 . . . ? O2 Zn1 O2 Mo1 -35.0(6) 7_655 . . . ? N2 Zn1 O2 Mo1 79.4(8) . . . . ? N2 Zn1 O2 Mo1 -146.1(7) 7_655 . . . ? O2 Zn1 N2 C1 162.1(9) . . . . ? O2 Zn1 N2 C1 -84.2(9) 7_655 . . . ? N2 Zn1 N2 C1 37.9(9) 7_655 . . . ? O2 Zn1 N2 C2 -6.1(7) . . . . ? O2 Zn1 N2 C2 107.6(7) 7_655 . . . ? N2 Zn1 N2 C2 -130.3(7) 7_655 . . . ? C2 N2 C1 N2 -2.1(14) . . . 8 ? Zn1 N2 C1 N2 -172.8(5) . . . 8 ? C2 N2 C1 N1 -178.2(10) . . . . ? Zn1 N2 C1 N1 11.2(15) . . . . ? O1 N1 C1 N2 2.3(15) 8 . . 8 ? O1 N1 C1 N2 -178.3(10) . . . 8 ? O1 N1 C1 N2 178.3(10) 8 . . . ? O1 N1 C1 N2 -2.3(15) . . . . ? C1 N2 C2 C2 1.1(7) . . . 8 ? Zn1 N2 C2 C2 172.0(3) . . . 8 ? _diffrn_measured_fraction_theta_max 0.894 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.597 _refine_diff_density_min -0.989 _refine_diff_density_rms 0.115 _database_code_depnum_ccdc_archive 'CCDC 934758'