# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2006 data_global #======================================================================= _audit_creation_method 'Jana2000 Version : 25/06/2004' _journal_coden_Cambridge 182 loop_ _publ_author_name 'Pascal Dietzel' 'Richard Blom' 'Hellmer Fjellvag' 'M. Hirscher' 'B. Panella' _publ_contact_author_name 'Pascal Dietzel' _publ_contact_author_address ; Department of Chemistry University of Oslo Postboks 1033, Blindern Oslo N-0315 NORWAY ; _publ_contact_author_email PASCAL.DIETZEL@KJEMI.UIO.NO _publ_requested_journal 'Chemical Communications' _publ_section_title ; Hydrogen adsorption in a nickel based coordination polymer with open metal sites in the cylindrical cavities of the desolvated frame ; _publ_section_references ; Petricek, V. & Dusek, M. (2000). Jana2000. Structure Determination Software Programs. Institute of Physics, Praha, Czech Republic. # use this reference if Diamond ver. 2 was used for visualization Brandenburg, K. (1999). DIAMOND. Version. 2.1c. Crystal Impact GbR, Bonn, Germany. # use this reference if Diamond ver. 3 was used for visualization in preparation # use this reference if SIR97 was used for solving of the structure Altomare, A., Burla, M. C., Camalli, M., Cascarano, G., Giacovazzo, C., Guagliardi, A., Moliterni, A. G. G., Polidori, G., Spagna, R. (1997). SIR97. A Package for Crystal Structure Solution by Direct Methods and Refinement, Bari, Rome, Italy. # use this reference if bond valences were calculated Brown, I. D. (1996). J. Appl. Cryst. 29, 479-480. # use this reference if Xshape wase used for crystal shape refinement Stoe & Cie (1998). X-SHAPE. Stoe & Cie, Darmstadt, Germany. ; _publ_section_figure_captions ; ? ; _publ_section_table_legends ; ? ; #======================================================================= data_Ni2(dhtp) _database_code_depnum_ccdc_archive 'CCDC 288477' #======================================================================= # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C4 H1 Ni1 O3' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_sum 'C4 H1 Ni1 O3' _chemical_formula_weight 155.7 _chemical_melting_point ? _chemical_compound_source ? #======================================================================= # 6. POWDER SPECIMEN AND CRYSTAL DATA _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'R -3' _symmetry_space_group_name_Hall '-R 3' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -y,x-y,z 3 -x+y,-x,z 4 -x,-y,-z 5 y,-x+y,-z 6 x-y,x,-z 7 2/3+x,1/3+y,1/3+z 8 2/3-y,1/3+x-y,1/3+z 9 2/3-x+y,1/3-x,1/3+z 10 2/3-x,1/3-y,1/3-z 11 2/3+y,1/3-x+y,1/3-z 12 2/3+x-y,1/3+x,1/3-z 13 1/3+x,2/3+y,2/3+z 14 1/3-y,2/3+x-y,2/3+z 15 1/3-x+y,2/3-x,2/3+z 16 1/3-x,2/3-y,2/3-z 17 1/3+y,2/3-x+y,2/3-z 18 1/3+x-y,2/3+x,2/3-z _cell_length_a 25.7856(12) _cell_length_b 25.7856(12) _cell_length_c 6.7701(10) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 3898.339 _cell_formula_units_Z 18 _cell_measurement_temperature 295 _pd_calibration_special_details ; ? ; _cell_special_details ; ? ; _exptl_crystal_density_diffrn 1.1937 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 1386 _pd_spec_size_axial 2 _pd_spec_size_equat 0.7 _pd_spec_size_thick 0.7 _pd_spec_mounting ;0.7 mm capillary of lithium borate glass ; _pd_spec_mount_mode transmission _pd_spec_shape cylinder _pd_char_particle_morphology ? _pd_char_colour green-yellow _pd_prep_cool_rate ? _pd_prep_pressure ? _pd_prep_temperature ? _exptl_absorpt_coefficient_mu 179.3 _exptl_absorpt_correction_type ? _exptl_absorpt_process_details '(Jana2000; Petricek and Dusek, 2000)' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? #======================================================================= # 7. EXPERIMENTAL DATA _exptl_special_details ; ? ; _pd_instr_location ; ? ; _diffrn_ambient_temperature 295 _diffrn_source synchrotron _diffrn_source_target ? _diffrn_source_type 'SNBL (BM01), ESRF' _diffrn_radiation_type X-ray _diffrn_radiation_wavelength 0.50134 _diffrn_radiation_monochromator ? _diffrn_measurement_device_type ? _diffrn_detector ? _diffrn_detector_type ? _pd_meas_scan_method cont _pd_meas_special_details ; ? ; _pd_meas_number_of_points 8618 _pd_meas_2theta_range_min 1.024 _pd_meas_2theta_range_max 35.492 _pd_meas_2theta_range_inc 0.004 #======================================================================= # 8. REFINEMENT DATA _pd_proc_ls_special_details ; ? ; _pd_proc_ls_profile_function Lorentzian _pd_proc_ls_background_function ? _pd_proc_ls_pref_orient_corr none _pd_proc_ls_prof_R_factor 0.0629 _pd_proc_ls_prof_wR_factor 0.0847 _pd_proc_ls_prof_wR_expected 0.0357 _refine_special_details ; ? ; _refine_ls_R_factor_gt 0.0304 _refine_ls_wR_factor_gt 0.0357 _refine_ls_R_factor_all 0.0304 _refine_ls_wR_factor_ref 0.0357 _refine_ls_number_parameters 36 _refine_ls_number_restraints ? _refine_ls_number_constraints ? _refine_ls_weighting_scheme sigma _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment ? _refine_ls_shift/su_max 0.2455 _refine_ls_shift/su_mean 0.0459 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _pd_proc_2theta_range_min 1.024 _pd_proc_2theta_range_max 27.996 _pd_proc_2theta_range_inc 0.004 _pd_proc_wavelength ? _pd_block_diffractogram_id ? _pd_proc_info_excluded_regions 'from 28 to 40.000' loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c C 0.003 0.002 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 2.31 20.843901 1.02 10.2075 1.5886 0.5687 0.865 51.651199 0.2156 H 0.000 0.000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.493002 10.5109 0.322912 26.1257 0.140191 3.14236 0.04081 57.799702 0.003038 Ni 0.344 1.121 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 12.8376 3.8785 7.292 0.2565 4.4438 12.1763 2.38 66.342102 1.0341 O 0.011 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.867 32.908901 0.2508 _computing_data_collection ? _computing_cell_refinement ? _computing_structure_solution ? _computing_structure_refinement '(Jana2000; Petricek and Dusek, 2000)' _computing_molecular_graphics ? _computing_publication_material '(Jana2000; Petricek and Dusek, 2000)' #======================================================================= # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_adp_type _atom_site_U_iso_or_equiv _atom_site_symmetry_multiplicity _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.4066(14) 0.4186(15) 0.748(3) Uiso 0.03(3) 18 1 d . . . C2 C 0.4541(15) 0.4583(10) 0.873(3) Uiso 0.004 18 1 d . . . C3 C 0.5434(10) 0.5578(6) 0.923(3) Uiso 0.00(3) 18 1 d . . . C4 C 0.4985(16) 0.5166(13) 0.798(3) Uiso 0.00(3) 18 1 d . . . H4 H 0.496(2) 0.529(3) 0.64(3) Uiso 0.00(3) 18 1 d . . . Ni1 Ni 0.6485(6) 0.6198(5) 0.6452(17) Uiso 0.0054(17) 18 1 d . . . O1 O 0.4038(15) 0.4342(14) 0.568(5) Uiso 0.00(2) 18 1 d . . . O2 O 0.3664(15) 0.3691(15) 0.813(4) Uiso 0.02(2) 18 1 d . . . O3 O 0.5838(16) 0.6122(14) 0.854(4) Uiso 0.001(16) 18 1 d . . . #======================================================================= # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag C1 C2 . . 1.42(3) yes C1 C3 . 4_667 2.49(3) yes C1 C4 . . 2.48(4) yes C1 H4 . . 2.72(8) yes C1 Ni1 . 4_666 2.95(2) yes C1 Ni1 . 18_546 2.97(3) yes C1 O1 . . 1.30(4) yes C1 O2 . . 1.25(4) yes C1 O3 . 4_667 2.85(4) yes C2 C2 . 4_667 2.85(3) yes C2 C3 . . 2.47(3) yes C2 C3 . 4_667 1.46(3) yes C2 C4 . . 1.45(3) yes C2 C4 . 4_667 2.47(3) yes C2 H4 . . 2.23(16) yes C2 O1 . . 2.35(4) yes C2 O2 . . 2.32(4) yes C2 O3 . 4_667 2.43(3) yes C3 C3 . 4_667 2.885(19) yes C3 C4 . . 1.40(3) yes C3 C4 . 4_667 2.52(3) yes C3 H4 . . 2.18(19) yes C3 Ni1 . 9_565 2.973(17) yes C3 O2 . 4_667 2.79(3) yes C3 O3 . . 1.35(3) yes C4 C4 . 4_667 2.88(3) yes C4 H4 . . 1.1(2) yes C4 O1 . . 2.78(4) yes C4 O3 . . 2.37(4) yes H4 H4 . 4_666 2.5(2) yes H4 O1 . . 2.46(7) yes H4 O1 . 4_666 2.66(13) yes H4 O3 . . 2.63(13) yes Ni1 Ni1 . 14_654 2.903(16) yes Ni1 Ni1 . 9_565 2.90(2) yes Ni1 O1 . 4_666 1.99(3) yes Ni1 O2 . 17_556 1.94(3) yes Ni1 O2 . 12_556 2.07(4) yes Ni1 O3 . . 2.12(4) yes Ni1 O3 . 14_654 1.88(4) yes O1 O2 . . 2.21(4) yes O1 O3 . 11_456 2.87(4) yes O2 O2 . 8_555 2.73(4) yes O2 O2 . 15_554 2.73(4) yes O2 O3 . 4_667 2.52(4) yes O2 O3 . 18_546 2.65(5) yes #======================================================================= # Attachment 'compound1_hydrated.cif' #======================================================================= data_Ni2(dhtp)(H2O)10 _database_code_depnum_ccdc_archive 'CCDC 288478' #======================================================================= # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C4 H11 Ni1 O4, 4 (O)' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_sum 'C4 H11 Ni1 O8' _chemical_formula_weight 245.8 _chemical_melting_point ? _chemical_compound_source ? #======================================================================= # 6. POWDER SPECIMEN AND CRYSTAL DATA _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'R -3' _symmetry_space_group_name_Hall '-R 3' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -y,x-y,z 3 -x+y,-x,z 4 -x,-y,-z 5 y,-x+y,-z 6 x-y,x,-z 7 2/3+x,1/3+y,1/3+z 8 2/3-y,1/3+x-y,1/3+z 9 2/3-x+y,1/3-x,1/3+z 10 2/3-x,1/3-y,1/3-z 11 2/3+y,1/3-x+y,1/3-z 12 2/3+x-y,1/3+x,1/3-z 13 1/3+x,2/3+y,2/3+z 14 1/3-y,2/3+x-y,2/3+z 15 1/3-x+y,2/3-x,2/3+z 16 1/3-x,2/3-y,2/3-z 17 1/3+y,2/3-x+y,2/3-z 18 1/3+x-y,2/3+x,2/3-z _cell_length_a 25.9783(7) _cell_length_b 25.9783(7) _cell_length_c 6.6883(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 3909.012 _cell_formula_units_Z 18 _cell_measurement_temperature 295 _pd_calibration_special_details ; ? ; _cell_special_details ; ? ; _exptl_crystal_density_diffrn 1.7567 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 2286 _pd_spec_size_axial 2 _pd_spec_size_equat 0.7 _pd_spec_size_thick 0.7 _pd_spec_mounting '0.7 mm capillary of lithium borate glass' _pd_spec_mount_mode transmission _pd_spec_shape cylinder _pd_char_particle_morphology ? _pd_char_colour yellow-greenish _pd_prep_cool_rate ? _pd_prep_pressure ? _pd_prep_temperature ? _exptl_absorpt_coefficient_mu 185.9 _exptl_absorpt_correction_type ? _exptl_absorpt_process_details '(Jana2000; Petricek and Dusek, 2000)' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? #======================================================================= # 7. EXPERIMENTAL DATA _exptl_special_details ; ? ; _pd_instr_location ; ? ; _diffrn_ambient_temperature 295 _diffrn_source synchrotron _diffrn_source_target ? _diffrn_source_type 'SNBL (BM01), ESRF' _diffrn_radiation_type X-ray _diffrn_radiation_wavelength 0.50134 _diffrn_radiation_monochromator ? _diffrn_measurement_device_type ? _diffrn_detector ? _diffrn_detector_type ? _pd_meas_scan_method cont _pd_meas_special_details ; ? ; _pd_meas_number_of_points 8618 _pd_meas_2theta_range_min 1.024 _pd_meas_2theta_range_max 35.492 _pd_meas_2theta_range_inc 0.004 #======================================================================= # 8. REFINEMENT DATA _pd_proc_ls_special_details ; ? ; _pd_proc_ls_profile_function Lorentzian _pd_proc_ls_background_function ? _pd_proc_ls_pref_orient_corr none _pd_proc_ls_prof_R_factor 0.0576 _pd_proc_ls_prof_wR_factor 0.0752 _pd_proc_ls_prof_wR_expected 0.0409 _refine_special_details ; ? ; _refine_ls_R_factor_gt 0.0281 _refine_ls_wR_factor_gt 0.0320 _refine_ls_R_factor_all 0.0281 _refine_ls_wR_factor_ref 0.0320 _refine_ls_number_parameters 59 _refine_ls_number_restraints ? _refine_ls_number_constraints ? _refine_ls_weighting_scheme sigma _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment ? _refine_ls_shift/su_max 0.0479 _refine_ls_shift/su_mean 0.0041 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _pd_proc_2theta_range_min 1.024 _pd_proc_2theta_range_max 35.492 _pd_proc_2theta_range_inc 0.004 _pd_proc_wavelength ? _pd_block_diffractogram_id ? _pd_proc_info_data_reduction ? loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0.001 0.001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' H 0.000 0.000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' Ni 0.291 0.594 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' O 0.004 0.003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' _computing_data_collection ? _computing_cell_refinement ? _computing_structure_solution ? _computing_structure_refinement '(Jana2000; Petricek and Dusek, 2000)' _computing_molecular_graphics ? _computing_publication_material '(Jana2000; Petricek and Dusek, 2000)' #======================================================================= # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_adp_type _atom_site_U_iso_or_equiv _atom_site_symmetry_multiplicity _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3995(15) 0.4153(16) 0.736(5) Uiso 0.004(9) 18 1 d . . . C2 C 0.4516(17) 0.4569(18) 0.889(5) Uiso 0.013(12) 18 1 d . . . C3 C 0.5452(17) 0.5533(17) 0.922(6) Uiso 0.021(12) 18 1 d . . . C4 C 0.4935(16) 0.5108(16) 0.812(5) Uiso 0.008(11) 18 1 d . . . Ni1 Ni 0.6517(2) 0.6172(2) 0.6500(7) Uiso 0.0098(7) 18 1 d . . . O1 O 0.4057(9) 0.4400(10) 0.560(3) Uiso 0.007(7) 18 1 d . . . O2 O 0.3616(9) 0.3701(10) 0.799(3) Uiso 0.010(7) 18 1 d . . . O3 O 0.5831(9) 0.6069(8) 0.829(4) Uiso 0.017(7) 18 1 d . . . O4 O 0.6516(9) 0.5456(8) 0.790(3) Uiso 0.063(9) 18 1.25 d . . . H4 H 0.494(5) 0.518(5) 0.62(2) Uiso 0.010(13) 18 1 d . . . O5 O 0.6971(11) 0.5505(10) 0.191(4) Uiso 0.104(9) 18 1.25 d . . . O6 O 0.7412(19) 0.5055(15) 0.734(8) Uiso 0.35(3) 18 1.25 d . . . O7 O 0.738(2) 0.355(5) 1.113(9) Uiso 0.69(8) 18 1.25 d . . . O8 O 0.557(2) 0.1568(15) 0.488(7) Uiso 0.30(3) 18 1.25 d . . . #======================================================================= # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag C1 C2 . . 1.60(5) yes C1 C3 . 4_667 2.60(5) yes C1 C4 . . 2.51(4) yes C1 Ni1 . 4_666 2.84(3) yes C1 Ni1 . 18_546 2.91(4) yes C1 O1 . . 1.31(4) yes C1 O2 . . 1.17(3) yes C1 H4 . . 2.68(10) yes C2 C2 . 4_667 2.82(5) yes C2 C3 . . 2.48(5) yes C2 C3 . 4_667 1.30(5) yes C2 C4 . . 1.37(5) yes C2 C4 . 4_667 2.36(5) yes C2 O1 . . 2.43(4) yes C2 O2 . . 2.37(4) yes C2 O3 . 4_667 2.37(4) yes C2 H4 . . 2.28(13) yes C3 C3 . 4_667 2.79(5) yes C3 C4 . . 1.44(5) yes C3 C4 . 4_667 2.29(5) yes C3 Ni1 . 9_565 2.98(4) yes C3 O2 . 4_667 2.91(4) yes C3 O3 . . 1.39(4) yes C3 H4 . . 2.34(13) yes C4 C4 . 4_667 2.63(5) yes C4 O1 . . 2.69(4) yes C4 O3 . . 2.42(3) yes C4 H4 . . 1.29(14) yes Ni1 Ni1 . 14_654 2.979(7) yes Ni1 Ni1 . 9_565 2.979(9) yes Ni1 O1 . 4_666 2.05(2) yes Ni1 O2 . 17_556 2.04(2) yes Ni1 O2 . 12_556 2.09(3) yes Ni1 O3 . . 2.05(3) yes Ni1 O3 . 14_654 2.00(2) yes Ni1 O4 . . 2.08(2) yes O1 O2 . . 2.25(3) yes O1 O3 . 4_666 2.95(4) yes O1 O4 . 4_666 2.90(3) yes O1 H4 . . 2.21(10) yes O1 H4 . 4_666 2.56(13) yes O2 O2 . 8_555 2.69(3) yes O2 O2 . 15_554 2.69(3) yes O2 O3 . 4_667 2.78(3) yes O2 O3 . 11_456 2.91(4) yes O2 O3 . 18_546 2.73(3) yes O2 O4 . 18_546 2.98(5) yes O3 O4 . . 2.93(4) yes O3 H4 . . 2.70(11) yes O3 O5 . 9_565 2.94(5) yes O4 O5 . 1_556 2.91(4) yes H4 H4 . 4_666 1.9(2) yes H4 O5 . 9_565 2.88(14) yes O5 O8 . 16_655 2.76(7) yes O6 O7 . 18_546 2.65(8) yes O7 O7 . 2_655 2.84(19) yes O7 O7 . 3_665 2.84(11) yes #=======================================================================