# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 # Attachment '- 0P75_D2_finalized.cif' data_0P75_D2_publ #TrackingRef '- 0P75_D2_finalized.cif' _pd_block_id 2011-08-29T18:45|0P5_D2||Overall _audit_creation_method 'from EXP file using GSAS2CIF' _audit_creation_date 2011-08-29T18:45 _audit_update_record ; 2011-08-29T18:45 Initial CIF as created by GSAS2CIF ; #============================================================================= # this information describes the project, paper etc. for the CIF # # Acta Cryst. Section C papers and editorial correspondence is generated # # from the information in this section # # # # (from) CIF submission form for Rietveld refinements (Acta Cryst. C) # # Version 14 December 1998 # #============================================================================= # 1. SUBMISSION DETAILS _publ_contact_author_name ? # Name of author for correspondence _publ_contact_author_address # Address of author for correspondence ; ? ; _publ_contact_author_email ? _publ_contact_author_fax ? _publ_contact_author_phone ? _publ_contact_letter ; ? ; _publ_requested_journal ? _publ_requested_coeditor_name ? _publ_requested_category ? # Acta C: one of CI/CM/CO/FI/FM/FO #============================================================================== # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_data_validation_number ? _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_paper_category ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; ? ; _publ_section_title_footnote ; ? ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_footnote _publ_author_address #<--'Last name, first name' ; ? ; ; ? ; #============================================================================== # 4. TEXT _publ_section_synopsis ; ? ; _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_exptl_prep # Details of the preparation of the sample(s) # should be given here. ; ? ; _publ_section_exptl_refinement ; ? ; _publ_section_references ; ? ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ; ? ; #============================================================================= # 5. OVERALL REFINEMENT & COMPUTING DETAILS _refine_special_details ; ? ; _pd_proc_ls_special_details ; ? ; # The following items are used to identify the programs used. _computing_molecular_graphics ? _computing_publication_material ? _refine_ls_weighting_scheme ? _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_number_constraints ? _refine_ls_restrained_S_all ? _refine_ls_restrained_S_obs ? #============================================================================== # 6. SAMPLE PREPARATION DATA # (In the unusual case where multiple samples are used in a single # Rietveld study, this information should be moved into the phase # blocks) # The following three fields describe the preparation of the material. # The cooling rate is in K/min. The pressure at which the sample was # prepared is in kPa. The temperature of preparation is in K. _pd_prep_cool_rate ? _pd_prep_pressure ? _pd_prep_temperature ? _pd_char_colour ? # use ICDD colour descriptions _publ_author_name 'Jeffrey Long' # Information for phase 1 data_0P5_D2_phase_1 _database_code_depnum_ccdc_archive 'CCDC 853659' #TrackingRef '- 0P75_D2_finalized.cif' _pd_block_id 2011-08-29T18:45|0P5_D2_phase1||| #============================================================================== # 7. CHEMICAL, STRUCTURAL AND CRYSTAL DATA _pd_char_particle_morphology ? _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_melting_point ? _chemical_compound_source ? # for minerals and # natural products _symmetry_space_group_name_Hall ? _exptl_crystal_F_000 ? _exptl_crystal_density_diffrn ? _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _cell_measurement_temperature ? _cell_special_details ; ? ; _geom_special_details ? # The following item identifies the program(s) used (if appropriate). _computing_structure_solution ? #============================================================================== # 8. Phase information from GSAS _pd_phase_name 'from /data/people/craigy/MgMOF/BT1/1108/MOF74.xtl' _cell_length_a 26.0951(28) _cell_length_b 26.0951 _cell_length_c 6.8945(11) _cell_angle_alpha 90.0 _cell_angle_beta 90.0 _cell_angle_gamma 120.0 _cell_volume 4065.8(8) _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'R -3' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +x,+y,+z 2 -y,x-y,+z 3 y-x,-x,+z -1 -x,-y,-z -2 +y,y-x,-z -3 x-y,+x,-z 101 +x+1/3,+y+2/3,+z+2/3 102 -y+1/3,x-y+2/3,+z+2/3 103 y-x+1/3,-x+2/3,+z+2/3 -101 -x+2/3,-y+1/3,-z+1/3 -102 +y+2/3,y-x+1/3,-z+1/3 -103 x-y+2/3,+x+1/3,-z+1/3 201 +x+2/3,+y+1/3,+z+1/3 202 -y+2/3,x-y+1/3,+z+1/3 203 y-x+2/3,-x+1/3,+z+1/3 -201 -x+1/3,-y+2/3,-z+2/3 -202 +y+1/3,y-x+2/3,-z+2/3 -203 x-y+1/3,+x+2/3,-z+2/3 # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_thermal_displace_type _atom_site_U_iso_or_equiv _atom_site_symmetry_multiplicity Fe Fe 0.3820(8) 0.3514(9) 0.1416(28) 1.0 Uiso 0.035(6) 18 O O1 0.3195(11) 0.2855(12) 0.366(4) 1.0 Uiso 0.000(8) 18 O O2 0.3024(12) 0.2288(12) 0.600(4) 1.0 Uiso -0.002(8) 18 O O3 0.3570(15) 0.2700(14) 0.010(5) 1.0 Uiso 0.028(9) 18 C C1 0.3120(18) 0.2414(16) 0.442(5) 1.0 Uiso 0.094(14) 18 C C2 0.3290(11) 0.2092(12) 0.2817(35) 1.0 Uiso 0.014(8) 18 C C3 0.3428(12) 0.2210(12) 0.076(4) 1.0 Uiso 0.018(8) 18 C C4 0.3528(11) 0.1780(12) -0.0277(28) 1.0 Uiso 0.005(7) 18 H H 0.3688(23) 0.1997(19) -0.173(8) 1.0 Uiso 0.032(14) 18 D D1 0.5306(10) 0.6529(8) 0.7459(27) 1.33(5) Uiso 0.028(10) 18 loop_ _atom_type_symbol _atom_type_number_in_cell Fe 18.0 O 54.0 C 72.0 H 18.0 D 23.932 # If you change Z, be sure to change all 3 of the following _chemical_formula_sum 'C4 H D1.33 Fe O3' _chemical_formula_weight 155.57 _cell_formula_units_Z 18 # MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe Fe 3.000(21) . 103_554 N Fe Fe 3.000(21) . 202_555 N Fe O1 2.284(31) . 1_555 N Fe O1 2.233(30) . 103_554 N Fe O2 2.046(33) . 202_554 N Fe O3 2.093(33) . 1_555 N Fe O3 2.15(4) . 202_555 N Fe C1 2.83(4) . 202_554 N Fe C3 2.998(35) . 202_555 N Fe D1 2.463(27) . -1_666 N O1 Fe 2.284(31) . 1_555 N O1 Fe 2.233(30) . 202_555 N O1 O2 2.08(4) . 1_555 N O1 C1 1.19(4) . 1_555 N O1 C2 2.21(4) . 1_555 N O2 Fe 2.046(33) . 103_555 N O2 O1 2.08(4) . 1_555 N O2 C1 1.13(4) . 1_555 N O2 C2 2.43(4) . 1_555 N O3 Fe 2.093(33) . 1_555 N O3 Fe 2.15(4) . 103_554 N O3 C2 2.32(4) . 1_555 N O3 C3 1.23(4) . 1_555 N O3 C4 2.36(4) . 1_555 N O3 H 2.37(6) . 1_555 N C1 Fe 2.83(4) . 103_555 N C1 O1 1.19(4) . 1_555 N C1 O2 1.13(4) . 1_555 N C1 C2 1.58(4) . 1_555 N C1 C4 2.34(5) . -201_444 N C2 O1 2.21(4) . 1_555 N C2 O2 2.43(4) . 1_555 N C2 O3 2.32(4) . 1_555 N C2 C1 1.58(4) . 1_555 N C2 C3 1.458(30) . 1_555 N C2 C3 2.469(30) . -201_444 N C2 C4 2.470(29) . 1_555 N C2 C4 1.370(34) . -201_444 N C2 H 2.31(6) . -201_444 N C3 Fe 2.998(35) . 103_554 N C3 O3 1.23(4) . 1_555 N C3 C2 1.458(30) . 1_555 N C3 C2 2.469(30) . -201_444 N C3 C4 1.459(31) . 1_555 N C3 C4 2.466(32) . -201_444 N C3 H 2.02(6) . 1_555 N C4 O3 2.36(4) . 1_555 N C4 C1 2.34(5) . -201_444 N C4 C2 2.470(29) . 1_555 N C4 C2 1.370(34) . -201_444 N C4 C3 1.459(31) . 1_555 N C4 C3 2.466(32) . -201_444 N C4 H 1.13(7) . 1_555 N H O3 2.37(6) . 1_555 N H C2 2.31(6) . -201_444 N H C3 2.02(6) . 1_555 N H C4 1.13(7) . 1_555 N D1 Fe 2.463(27) . -1_666 N 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Fe O1 83.2(8) 1_555 . 103_554 N O1 Fe O2 177.2(17) 1_555 . 202_554 N O1 Fe O3 77.7(13) 1_555 . 1_555 N O1 Fe O3 87.3(12) 1_555 . 202_555 N O1 Fe O2 97.3(14) 103_554 . 202_554 N O1 Fe O3 90.1(13) 103_554 . 1_555 N O1 Fe O3 91.2(12) 103_554 . 202_555 N O2 Fe O3 99.5(15) 202_554 . 1_555 N O2 Fe O3 95.5(15) 202_554 . 202_555 N O3 Fe O3 164.7(18) 1_555 . 202_555 N Fe O1 Fe 83.2(9) 1_555 . 202_555 N Fe O1 C1 137.4(30) 1_555 . 1_555 N Fe O1 C1 133.1(30) 202_555 . 1_555 N Fe O2 C1 123.3(29) 103_555 . 1_555 N Fe O3 Fe 89.9(15) 1_555 . 103_554 N Fe O3 C3 132.5(28) 1_555 . 1_555 N Fe O3 C3 122.8(27) 103_554 . 1_555 N O1 C1 O2 128(4) 1_555 . 1_555 N O1 C1 C2 104.9(33) 1_555 . 1_555 N O2 C1 C2 127(4) 1_555 . 1_555 N C1 C2 C3 132.3(29) 1_555 . 1_555 N C1 C2 C4 104.6(24) 1_555 . -201_555 N C3 C2 C4 121.3(24) 1_555 . -201_555 N O3 C3 C2 119.7(30) 1_555 . 1_555 N O3 C3 C4 122.9(29) 1_555 . 1_555 N C2 C3 C4 115.7(24) 1_555 . 1_555 N C2 C4 C3 121.5(22) -201_555 . 1_555 N C2 C4 H 135.8(28) -201_555 . 1_555 N C3 C4 H 102.4(29) 1_555 . 1_555 N # Information for phase 1 data_1P5_phase_1 _database_code_depnum_ccdc_archive 'CCDC 853660' #TrackingRef '- 2P25_D2_finalized.cif' _pd_block_id 2011-08-29T18:47|1P5_phase1||| #============================================================================== # 7. CHEMICAL, STRUCTURAL AND CRYSTAL DATA _pd_char_particle_morphology ? _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_melting_point ? _chemical_compound_source ? # for minerals and # natural products _symmetry_space_group_name_Hall ? _exptl_crystal_F_000 ? _exptl_crystal_density_diffrn ? _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _cell_measurement_temperature ? _cell_special_details ; ? ; _geom_special_details ? # The following item identifies the program(s) used (if appropriate). _computing_structure_solution ? #============================================================================== # 8. Phase information from GSAS _pd_phase_name 'from /data/people/craigy/MgMOF/BT1/1108/MOF74.xtl' _cell_length_a 26.1021(28) _cell_length_b 26.1021 _cell_length_c 6.9107(12) _cell_angle_alpha 90.0 _cell_angle_beta 90.0 _cell_angle_gamma 120.0 _cell_volume 4077.6(9) _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'R -3' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +x,+y,+z 2 -y,x-y,+z 3 y-x,-x,+z -1 -x,-y,-z -2 +y,y-x,-z -3 x-y,+x,-z 101 +x+1/3,+y+2/3,+z+2/3 102 -y+1/3,x-y+2/3,+z+2/3 103 y-x+1/3,-x+2/3,+z+2/3 -101 -x+2/3,-y+1/3,-z+1/3 -102 +y+2/3,y-x+1/3,-z+1/3 -103 x-y+2/3,+x+1/3,-z+1/3 201 +x+2/3,+y+1/3,+z+1/3 202 -y+2/3,x-y+1/3,+z+1/3 203 y-x+2/3,-x+1/3,+z+1/3 -201 -x+1/3,-y+2/3,-z+2/3 -202 +y+1/3,y-x+2/3,-z+2/3 -203 x-y+1/3,+x+2/3,-z+2/3 # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_thermal_displace_type _atom_site_U_iso_or_equiv _atom_site_symmetry_multiplicity D D2 0.4521(14) 0.2954(19) 0.663(4) 1.31(8) Uani 0.11282 18 D D3 0.2348(10) 0.4864(12) 0.857(5) 1.47(6) Uani 0.11036 18 Fe Fe 0.3818(8) 0.3513(9) 0.1413(30) 1.0 Uiso 0.008(7) 18 O O1 0.3183(18) 0.2853(18) 0.353(5) 1.0 Uiso 0.005(10) 18 O O2 0.3003(15) 0.2307(16) 0.598(6) 1.0 Uiso 0.008(11) 18 O O3 0.3539(21) 0.2707(19) 0.011(7) 1.0 Uiso 0.044(14) 18 C C1 0.3121(20) 0.2435(19) 0.445(5) 1.0 Uiso 0.048(12) 18 C C2 0.3285(14) 0.2082(14) 0.279(5) 1.0 Uiso 0.007(10) 18 C C3 0.3421(13) 0.2206(14) 0.086(5) 1.0 Uiso 0.002(10) 18 C C4 0.3528(14) 0.1793(15) -0.028(4) 1.0 Uiso 0.006(10) 18 H H 0.3690(31) 0.1998(27) -0.183(12) 1.0 Uiso 0.040(16) 18 D D1 0.5339(10) 0.6540(10) 0.7473(30) 1.54(8) Uiso 0.028(10) 18 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_22 _atom_site_aniso_U_23 _atom_site_aniso_U_33 D2 0.07(4) 0.10(4) -0.058(29) 0.25(5) -0.023(31) 0.051(33) D3 0.011(25) 0.048(25) 0.047(20) 0.124(33) 0.052(27) 0.22(5) loop_ _atom_type_symbol _atom_type_number_in_cell D 77.763 Fe 18.0 O 54.0 C 72.0 H 18.0 # If you change Z, be sure to change all 3 of the following _chemical_formula_sum 'C4 H D4.32 Fe O3' _chemical_formula_weight 161.60 _cell_formula_units_Z 18 # MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe Fe 2.998(21) . 103_554 N Fe Fe 2.998(21) . 202_555 N Fe O1 2.24(4) . 1_555 N Fe O1 2.25(4) . 103_554 N Fe O2 2.00(4) . 202_554 N Fe O3 2.06(4) . 1_555 N Fe O3 2.09(6) . 202_555 N Fe C1 2.79(4) . 202_554 N Fe D1 2.400(28) . -1_666 N O1 Fe 2.24(4) . 1_555 N O1 Fe 2.25(4) . 202_555 N O1 O2 2.11(4) . 1_555 N O1 C1 1.20(5) . 1_555 N O1 C2 2.22(5) . 1_555 N O2 Fe 2.00(4) . 103_555 N O2 O1 2.11(4) . 1_555 N O2 C1 1.10(4) . 1_555 N O2 C2 2.48(5) . 1_555 N O3 Fe 2.06(4) . 1_555 N O3 Fe 2.09(6) . 103_554 N O3 C2 2.34(6) . 1_555 N O3 C3 1.29(5) . 1_555 N O3 C4 2.39(6) . 1_555 N O3 H 2.47(8) . 1_555 N C1 Fe 2.79(4) . 103_555 N C1 O1 1.20(5) . 1_555 N C1 O2 1.10(4) . 1_555 N C1 C2 1.65(5) . 1_555 N C1 C4 2.43(5) . -201_444 N C2 O1 2.22(5) . 1_555 N C2 O2 2.48(5) . 1_555 N C2 O3 2.34(6) . 1_555 N C2 C1 1.65(5) . 1_555 N C2 C3 1.38(4) . 1_555 N C2 C3 2.45(4) . -201_444 N C2 C4 2.44(4) . 1_555 N C2 C4 1.39(4) . -201_444 N C2 H 2.36(8) . -201_444 N C3 O3 1.29(5) . 1_555 N C3 C2 1.38(4) . 1_555 N C3 C2 2.45(4) . -201_444 N C3 C4 1.47(4) . 1_555 N C3 C4 2.43(4) . -201_444 N C3 H 2.15(8) . 1_555 N C4 O3 2.39(6) . 1_555 N C4 C1 2.43(5) . -201_444 N C4 C2 2.44(4) . 1_555 N C4 C2 1.39(4) . -201_444 N C4 C3 1.47(4) . 1_555 N C4 C3 2.43(4) . -201_444 N C4 H 1.18(9) . 1_555 N H O3 2.47(8) . 1_555 N H C2 2.36(8) . -201_444 N H C3 2.15(8) . 1_555 N H C4 1.18(9) . 1_555 N D1 Fe 2.400(28) . -1_666 N 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Fe O1 83.9(7) 1_555 . 103_554 N O1 Fe O2 173.6(20) 1_555 . 202_554 N O1 Fe O3 75.6(19) 1_555 . 1_555 N O1 Fe O3 87.1(17) 1_555 . 202_555 N O1 Fe O2 95.1(17) 103_554 . 202_554 N O1 Fe O3 87.5(18) 103_554 . 1_555 N O1 Fe O3 93.3(17) 103_554 . 202_555 N O2 Fe O3 98.0(20) 202_554 . 1_555 N O2 Fe O3 99.3(19) 202_554 . 202_555 N O3 Fe O3 162.5(25) 1_555 . 202_555 N Fe O1 Fe 83.8(14) 1_555 . 202_555 N Fe O1 C1 139.2(33) 1_555 . 1_555 N Fe O1 C1 125.4(34) 202_555 . 1_555 N Fe O2 C1 125(4) 103_555 . 1_555 N Fe O3 Fe 92.6(21) 1_555 . 103_554 N Fe O3 C3 130(4) 1_555 . 1_555 N Fe O3 C3 126.6(35) 103_554 . 1_555 N O1 C1 O2 132(5) 1_555 . 1_555 N O1 C1 C2 100.7(34) 1_555 . 1_555 N O2 C1 C2 127(4) 1_555 . 1_555 N C1 C2 C3 130.4(29) 1_555 . 1_555 N C1 C2 C4 105.4(28) 1_555 . -201_555 N C3 C2 C4 123.0(31) 1_555 . -201_555 N O3 C3 C2 121.8(33) 1_555 . 1_555 N O3 C3 C4 119.5(33) 1_555 . 1_555 N C2 C3 C4 117.9(29) 1_555 . 1_555 N C2 C4 C3 118.0(28) -201_555 . 1_555 N C2 C4 H 134(4) -201_555 . 1_555 N C3 C4 H 108(4) 1_555 . 1_555 N # Information for phase 1 data_OXIDIZED_phase_1 _database_code_depnum_ccdc_archive 'CCDC 853661' #TrackingRef '- OXIDIZED_0P25_D2_final.cif' _pd_block_id 2011-04-19T17:06|OXIDIZED_phase1||| #============================================================================== # 7. CHEMICAL, STRUCTURAL AND CRYSTAL DATA _pd_char_particle_morphology ? _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_melting_point ? _chemical_compound_source ? # for minerals and # natural products _symmetry_space_group_name_Hall ? _exptl_crystal_F_000 ? _exptl_crystal_density_diffrn ? _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _cell_measurement_temperature ? _cell_special_details ; ? ; _geom_special_details ? # The following item identifies the program(s) used (if appropriate). _computing_structure_solution ? #============================================================================== # 8. Phase information from GSAS _pd_phase_name 'from /data/people/craigy/MgMOF/BT1/1108/MOF74.xtl' _cell_length_a 25.9689(15) _cell_length_b 25.9689 _cell_length_c 6.8209(9) _cell_angle_alpha 90.0 _cell_angle_beta 90.0 _cell_angle_gamma 120.0 _cell_volume 3983.6(6) _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'R -3' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +x,+y,+z 2 -y,x-y,+z 3 y-x,-x,+z -1 -x,-y,-z -2 +y,y-x,-z -3 x-y,+x,-z 101 +x+1/3,+y+2/3,+z+2/3 102 -y+1/3,x-y+2/3,+z+2/3 103 y-x+1/3,-x+2/3,+z+2/3 -101 -x+2/3,-y+1/3,-z+1/3 -102 +y+2/3,y-x+1/3,-z+1/3 -103 x-y+2/3,+x+1/3,-z+1/3 201 +x+2/3,+y+1/3,+z+1/3 202 -y+2/3,x-y+1/3,+z+1/3 203 y-x+2/3,-x+1/3,+z+1/3 -201 -x+1/3,-y+2/3,-z+2/3 -202 +y+1/3,y-x+2/3,-z+2/3 -203 x-y+1/3,+x+2/3,-z+2/3 # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_thermal_displace_type _atom_site_U_iso_or_equiv _atom_site_symmetry_multiplicity Fe Fe 0.3801(5) 0.3468(6) 0.1382(15) 1.0 Uiso 0.022(4) 18 O O1 0.3273(8) 0.2982(8) 0.3592(33) 1.0 Uiso 0.048(9) 18 O O2 0.3078(10) 0.2233(11) 0.6082(27) 1.0 Uiso 0.040(7) 18 O O3 0.3510(8) 0.2706(5) 0.0014(30) 1.0 Uiso 0.032(7) 18 C C1 0.3158(12) 0.2469(8) 0.4104(25) 1.0 Uiso 0.046(7) 18 C C2 0.3365(11) 0.2120(9) 0.2843(27) 1.0 Uiso 0.053(9) 18 C C3 0.3477(9) 0.2243(8) 0.0771(29) 1.0 Uiso 0.017(5) 18 C C4 0.3576(9) 0.1790(9) -0.0157(28) 1.0 Uiso 0.029(6) 18 H H 0.3684(16) 0.1893(18) -0.198(5) 1.0 Uiso 0.026(12) 18 O O1a 0.5290(14) 0.6129(20) 0.725(5) 0.53(6) Uiso 0.027(20) 18 O O1b 0.519(4) 0.635(5) 0.927(11) 0.53(6) Uani 0.46397 18 D D1 0.5412(26) 0.6660(28) 0.686(9) 0.53(8) Uiso 0.054(30) 18 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_22 _atom_site_aniso_U_23 _atom_site_aniso_U_33 O1b 0.26(16) 0.13(14) 0.40(17) 0.32(17) 0.21(23) 0.80(32) loop_ _atom_type_symbol _atom_type_number_in_cell Fe 18.0 O 72.968 C 72.0 H 18.0 D 9.464 # If you change Z, be sure to change all 3 of the following _chemical_formula_sum 'C4 H D0.53 Fe O4.05' _chemical_formula_weight 170.81 _cell_formula_units_Z 18 # MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe O1 2.004(14) . 1_555 N Fe O1 2.032(24) . 103_554 N Fe O2 2.208(30) . 202_554 N Fe O3 1.965(14) . 1_555 N Fe O3 2.066(21) . 202_555 N Fe O1a 2.251(26) . -1_666 N Fe O1b 2.46(9) . -1_666 N Fe D1 2.53(5) . -1_666 N O1 Fe 2.004(14) . 1_555 N O1 Fe 2.032(24) . 202_555 N O1 C1 1.258(6) . 1_555 N O2 Fe 2.208(30) . 103_555 N O2 C1 1.454(6) . 1_555 N O2 H 2.02(5) . -201_444 N O3 Fe 1.965(14) . 1_555 N O3 Fe 2.066(21) . 103_554 N O3 C3 1.272(6) . 1_555 N C1 O1 1.258(6) . 1_555 N C1 O2 1.454(6) . 1_555 N C1 C2 1.530(14) . 1_555 N C2 C1 1.530(14) . 1_555 N C2 C3 1.446(6) . 1_555 N C2 C4 1.369(6) . -201_444 N C3 O3 1.272(6) . 1_555 N C3 C2 1.446(6) . 1_555 N C3 C4 1.468(6) . 1_555 N C4 C2 1.369(6) . -201_444 N C4 C3 1.468(6) . 1_555 N C4 H 1.27(4) . 1_555 N H O2 2.02(5) . -201_444 N H C4 1.27(4) . 1_555 N O1a Fe 2.251(26) . -1_666 N O1a O1b 1.563(17) . 1_555 N O1a D1 1.28(6) . 1_555 N O1b Fe 2.46(9) . -1_666 N O1b O1a 1.563(17) . 1_555 N O1b D1 1.79(8) . 1_555 N D1 Fe 2.53(5) . -1_666 N D1 O1a 1.28(6) . 1_555 N D1 O1b 1.79(8) . 1_555 N 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Fe O1 84.1(4) 1_555 . 103_554 N O1 Fe O3 85.7(12) 1_555 . 1_555 N O1 Fe O3 80.1(8) 1_555 . 202_555 N O1 Fe O3 81.8(8) 103_554 . 1_555 N O1 Fe O3 95.8(8) 103_554 . 202_555 N O3 Fe O3 165.8(12) 1_555 . 202_555 N Fe O1 Fe 93.8(6) 1_555 . 202_555 N Fe O1 C1 127.0(21) 1_555 . 1_555 N Fe O1 C1 138.1(18) 202_555 . 1_555 N Fe O3 Fe 94.0(8) 1_555 . 103_554 N Fe O3 C3 124.7(18) 1_555 . 1_555 N Fe O3 C3 134.9(16) 103_554 . 1_555 N O1 C1 O2 127.8(20) 1_555 . 1_555 N O1 C1 C2 120.2(20) 1_555 . 1_555 N O2 C1 C2 106.8(16) 1_555 . 1_555 N C1 C2 C3 120.7(19) 1_555 . 1_555 N C1 C2 C4 108.8(16) 1_555 . -201_555 N C3 C2 C4 119.6(18) 1_555 . -201_555 N O3 C3 C2 121.1(23) 1_555 . 1_555 N O3 C3 C4 128.9(20) 1_555 . 1_555 N C2 C3 C4 109.9(14) 1_555 . 1_555 N C2 C4 C3 122.2(16) -201_555 . 1_555 N C2 C4 H 119.0(20) -201_555 . 1_555 N C3 C4 H 111.1(22) 1_555 . 1_555 N O1b O1a D1 78(5) 1_555 . 1_555 N O1a O1b D1 44.1(28) 1_555 . 1_555 N O1a D1 O1b 58.3(27) 1_555 . 1_555 N # Information for phase 1 data_OXIDIZEDA_0P5_D2_phase_1 _database_code_depnum_ccdc_archive 'CCDC 853662' #TrackingRef '- OXIDIZED_0P5_D2_final.cif' _pd_block_id 2011-04-22T15:36|OXIDIZEDA_0P5_D2_phase1||| #============================================================================== # 7. CHEMICAL, STRUCTURAL AND CRYSTAL DATA _pd_char_particle_morphology ? _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_melting_point ? _chemical_compound_source ? # for minerals and # natural products _symmetry_space_group_name_Hall ? _exptl_crystal_F_000 ? _exptl_crystal_density_diffrn ? _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _cell_measurement_temperature ? _cell_special_details ; ? ; _geom_special_details ? # The following item identifies the program(s) used (if appropriate). _computing_structure_solution ? #============================================================================== # 8. Phase information from GSAS _pd_phase_name 'from /data/people/craigy/MgMOF/BT1/1108/MOF74.xtl' _cell_length_a 25.9612(14) _cell_length_b 25.9612 _cell_length_c 6.8377(7) _cell_angle_alpha 90.0 _cell_angle_beta 90.0 _cell_angle_gamma 120.0 _cell_volume 3991.1(5) _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'R -3' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +x,+y,+z 2 -y,x-y,+z 3 y-x,-x,+z -1 -x,-y,-z -2 +y,y-x,-z -3 x-y,+x,-z 101 +x+1/3,+y+2/3,+z+2/3 102 -y+1/3,x-y+2/3,+z+2/3 103 y-x+1/3,-x+2/3,+z+2/3 -101 -x+2/3,-y+1/3,-z+1/3 -102 +y+2/3,y-x+1/3,-z+1/3 -103 x-y+2/3,+x+1/3,-z+1/3 201 +x+2/3,+y+1/3,+z+1/3 202 -y+2/3,x-y+1/3,+z+1/3 203 y-x+2/3,-x+1/3,+z+1/3 -201 -x+1/3,-y+2/3,-z+2/3 -202 +y+1/3,y-x+2/3,-z+2/3 -203 x-y+1/3,+x+2/3,-z+2/3 # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_thermal_displace_type _atom_site_U_iso_or_equiv _atom_site_symmetry_multiplicity Fe Fe 0.3810(4) 0.3479(5) 0.1352(14) 1.0 Uiso 0.0225(34) 18 O O1 0.3276(8) 0.2996(7) 0.3495(28) 1.0 Uiso 0.049(9) 18 O O2 0.3032(9) 0.2203(10) 0.6025(24) 1.0 Uiso 0.032(7) 18 O O3 0.3532(7) 0.2721(4) 0.0014(27) 1.0 Uiso 0.009(5) 18 C C1 0.3144(10) 0.2468(7) 0.4087(24) 1.0 Uiso 0.037(6) 18 C C2 0.3325(10) 0.2114(8) 0.2892(24) 1.0 Uiso 0.045(8) 18 C C3 0.3444(8) 0.2236(8) 0.0831(23) 1.0 Uiso 0.009(4) 18 C C4 0.3527(9) 0.1783(9) -0.0146(22) 1.0 Uiso 0.019(5) 18 H H 0.3668(13) 0.1931(13) -0.1725(29) 1.0 Uiso 0.008(8) 18 O O1a 0.5295(17) 0.6173(25) 0.721(5) 0.54(6) Uiso 0.017(15) 18 O O1b 0.511(4) 0.618(5) 0.940(8) 0.54(6) Uani 0.53141 18 D D1 0.577(5) 0.691(5) 0.607(15) 0.39(8) Uiso 0.13(5) 18 D D2 0.5310(19) 0.6586(20) 0.721(4) 0.88(11) Uiso 0.059(20) 18 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_22 _atom_site_aniso_U_23 _atom_site_aniso_U_33 O1b 0.17(13) 0.09(13) 0.40(16) 0.51(25) 0.40(24) 0.80(30) loop_ _atom_type_symbol _atom_type_number_in_cell Fe 18.0 O 73.298 C 72.0 H 18.0 D 22.864 # If you change Z, be sure to change all 3 of the following _chemical_formula_sum 'C4 H D1.27 Fe O4.07' _chemical_formula_weight 172.61 _cell_formula_units_Z 18 # MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe Fe 2.970(10) . 103_554 N Fe Fe 2.970(10) . 202_555 N Fe O1 1.975(9) . 1_555 N Fe O1 2.031(23) . 103_554 N Fe O2 2.209(25) . 202_554 N Fe O3 1.950(9) . 1_555 N Fe O3 2.089(22) . 202_555 N Fe O1a 2.25(4) . -1_666 N Fe O1b 2.54(9) . -1_666 N Fe D1 2.54(8) . -1_666 N Fe D2 2.57(4) . -1_666 N O1 Fe 1.975(9) . 1_555 N O1 Fe 2.031(23) . 202_555 N O1 C1 1.301(9) . 1_555 N O1 C2 2.392(25) . 1_555 N O1 D1 2.39(10) . -1_666 N O2 Fe 2.209(25) . 103_555 N O2 C1 1.454(9) . 1_555 N O2 C2 2.322(24) . 1_555 N O2 H 2.14(4) . -201_444 N O2 O1b 1.94(13) . -103_435 N O3 Fe 1.950(9) . 1_555 N O3 Fe 2.089(22) . 103_554 N O3 C3 1.291(19) . 1_555 N C1 O1 1.301(9) . 1_555 N C1 O2 1.454(9) . 1_555 N C1 C2 1.472(9) . 1_555 N C1 D1 2.46(13) . -1_666 N C2 O1 2.392(25) . 1_555 N C2 O2 2.322(24) . 1_555 N C2 C1 1.472(9) . 1_555 N C2 C3 1.443(8) . 1_555 N C2 C4 1.355(21) . -201_444 N C2 H 2.183(27) . -201_444 N C3 O3 1.291(19) . 1_555 N C3 C2 1.443(8) . 1_555 N C3 C4 1.457(9) . 1_555 N C3 C4 2.380(24) . -201_444 N C3 H 2.115(26) . 1_555 N C4 C2 1.355(21) . -201_444 N C4 C3 1.457(9) . 1_555 N C4 C3 2.380(24) . -201_444 N C4 H 1.143(9) . 1_555 N H O2 2.14(4) . -201_444 N H C2 2.183(27) . -201_444 N H C3 2.115(26) . 1_555 N H C4 1.143(9) . 1_555 N O1a Fe 2.25(4) . -1_666 N O1a O1b 1.578(23) . 1_555 N O1a D1 1.85(14) . 1_555 N O1a D2 1.05(5) . 1_555 N O1b Fe 2.54(9) . -1_666 N O1b O2 1.94(13) . -102_445 N O1b O1a 1.578(23) . 1_555 N O1b D2 1.75(8) . 1_555 N D1 Fe 2.54(8) . -1_666 N D1 O1 2.39(10) . -1_666 N D1 C1 2.46(13) . -1_666 N D1 O1a 1.85(14) . 1_555 N D1 D2 1.32(12) . 1_555 N D2 Fe 2.57(4) . -1_666 N D2 O1a 1.05(5) . 1_555 N D2 O1b 1.75(8) . 1_555 N D2 D1 1.32(12) . 1_555 N 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Fe O1 83.86(34) 1_555 . 103_554 N O1 Fe O3 85.4(10) 1_555 . 1_555 N O1 Fe O3 79.3(6) 1_555 . 202_555 N O1 Fe O3 81.3(7) 103_554 . 1_555 N O1 Fe O3 96.2(7) 103_554 . 202_555 N O3 Fe O3 164.7(10) 1_555 . 202_555 N Fe O1 Fe 95.7(5) 1_555 . 202_555 N Fe O1 C1 129.1(18) 1_555 . 1_555 N Fe O1 C1 133.9(15) 202_555 . 1_555 N Fe O3 Fe 94.6(9) 1_555 . 103_554 N Fe O3 C3 125.2(16) 1_555 . 1_555 N Fe O3 C3 129.6(13) 103_554 . 1_555 N O1 C1 O2 131.9(19) 1_555 . 1_555 N O1 C1 C2 119.1(19) 1_555 . 1_555 N O2 C1 C2 105.0(15) 1_555 . 1_555 N C1 C2 C3 120.4(18) 1_555 . 1_555 N C1 C2 C4 117.3(16) 1_555 . -201_555 N C3 C2 C4 116.6(15) 1_555 . -201_555 N O3 C3 C2 123.4(20) 1_555 . 1_555 N O3 C3 C4 124.3(16) 1_555 . 1_555 N C2 C3 C4 111.9(13) 1_555 . 1_555 N C2 C4 C3 128.3(13) -201_555 . 1_555 N C2 C4 H 121.6(20) -201_555 . 1_555 N C3 C4 H 108.3(19) 1_555 . 1_555 N O1b O1a D2 81(5) 1_555 . 1_555 N O1a O1b D2 36.5(21) 1_555 . 1_555 N O1a D2 O1b 63(4) 1_555 . 1_555 N O1a D2 D1 102(6) 1_555 . 1_555 N O1b D2 D1 143(5) 1_555 . 1_555 N # Information for phase 1 data_OXIDIZEDA_1P0_D2_phase_1 _database_code_depnum_ccdc_archive 'CCDC 853663' #TrackingRef '- OXIDIZED_1P0_D2_final.cif' _pd_block_id 2011-04-21T17:34|OXIDIZEDA_1P0_D2_phase1||| #============================================================================== # 7. CHEMICAL, STRUCTURAL AND CRYSTAL DATA _pd_char_particle_morphology ? _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_melting_point ? _chemical_compound_source ? # for minerals and # natural products _symmetry_space_group_name_Hall ? _exptl_crystal_F_000 ? _exptl_crystal_density_diffrn ? _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _cell_measurement_temperature ? _cell_special_details ; ? ; _geom_special_details ? # The following item identifies the program(s) used (if appropriate). _computing_structure_solution ? #============================================================================== # 8. Phase information from GSAS _pd_phase_name 'from /data/people/craigy/MgMOF/BT1/1108/MOF74.xtl' _cell_length_a 25.9572(14) _cell_length_b 25.9572 _cell_length_c 6.8430(8) _cell_angle_alpha 90.0 _cell_angle_beta 90.0 _cell_angle_gamma 120.0 _cell_volume 3992.9(5) _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'R -3' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +x,+y,+z 2 -y,x-y,+z 3 y-x,-x,+z -1 -x,-y,-z -2 +y,y-x,-z -3 x-y,+x,-z 101 +x+1/3,+y+2/3,+z+2/3 102 -y+1/3,x-y+2/3,+z+2/3 103 y-x+1/3,-x+2/3,+z+2/3 -101 -x+2/3,-y+1/3,-z+1/3 -102 +y+2/3,y-x+1/3,-z+1/3 -103 x-y+2/3,+x+1/3,-z+1/3 201 +x+2/3,+y+1/3,+z+1/3 202 -y+2/3,x-y+1/3,+z+1/3 203 y-x+2/3,-x+1/3,+z+1/3 -201 -x+1/3,-y+2/3,-z+2/3 -202 +y+1/3,y-x+2/3,-z+2/3 -203 x-y+1/3,+x+2/3,-z+2/3 # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_thermal_displace_type _atom_site_U_iso_or_equiv _atom_site_symmetry_multiplicity Fe Fe 0.3809(4) 0.3480(5) 0.1410(15) 1.0 Uiso 0.0295(29) 18 O O1 0.3251(6) 0.2982(6) 0.3473(22) 1.0 Uiso 0.008(6) 18 O O2 0.3029(8) 0.2223(10) 0.6015(21) 1.0 Uiso 0.030(7) 18 O O3 0.3514(6) 0.2714(4) 0.0090(25) 1.0 Uiso 0.015(6) 18 C C1 0.3155(9) 0.2467(6) 0.4054(21) 1.0 Uiso 0.020(5) 18 C C2 0.3340(11) 0.2108(10) 0.2917(27) 1.0 Uiso 0.071(9) 18 C C3 0.3442(8) 0.2237(7) 0.0873(27) 1.0 Uiso 0.013(4) 18 C C4 0.3513(10) 0.1796(9) -0.0237(24) 1.0 Uiso 0.029(6) 18 H H 0.3649(13) 0.1917(12) -0.1804(31) 1.0 Uiso 0.003(8) 18 O O1a 0.5312(15) 0.6122(20) 0.714(6) 0.45(2) Uiso 0.004(6) 18 O O1b 0.515(6) 0.629(7) 0.916(16) 0.45(2) Uani 0.50382 18 D D1 0.5348(12) 0.6596(11) 0.7135(31) 1.61(6) Uani 0.19693 18 D D2 0.5361(30) 0.686(4) 0.359(13) 0.72(5) Uani 0.53931 18 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_22 _atom_site_aniso_U_23 _atom_site_aniso_U_33 O1b 0.3(2) 0.2(1) 0.1(2) 0.4(2) -0.02(2) 0.8(3) D1 0.26(4) 0.14(3) -0.050(25) 0.175(27) -0.05(2) 0.21(3) D2 0.6(2) 0.4(2) -0.1(2) 0.7(1) -0.1(1) 0.4(1) loop_ _atom_type_symbol _atom_type_number_in_cell Fe 18.0 O 70.363 C 72.0 H 18.0 D 41.957 # If you change Z, be sure to change all 3 of the following _chemical_formula_sum 'C4 H D2.33 Fe O3.91' _chemical_formula_weight 172.13 _cell_formula_units_Z 18 # MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe Fe 2.968(9) . 103_554 N Fe Fe 2.968(9) . 202_555 N Fe O1 1.973(9) . 1_555 N Fe O1 2.050(19) . 103_554 N Fe O2 2.193(24) . 202_554 N Fe O3 1.957(9) . 1_555 N Fe O3 2.071(19) . 202_555 N Fe O1a 2.214(35) . -1_666 N Fe O1b 2.48(13) . -1_666 N Fe D1 2.497(27) . -1_666 N O1 Fe 1.973(9) . 1_555 N O1 Fe 2.050(19) . 202_555 N O1 C1 1.293(9) . 1_555 N O2 Fe 2.193(24) . 103_555 N O2 C1 1.450(9) . 1_555 N O2 C2 2.341(23) . 1_555 N O2 H 2.17(4) . -201_444 N O2 O1b 2.13(16) . -103_435 N O3 Fe 1.957(9) . 1_555 N O3 Fe 2.071(19) . 103_554 N O3 C2 2.389(24) . 1_555 N O3 C3 1.273(9) . 1_555 N O3 C4 2.391(22) . 1_555 N O3 O1a 2.34(4) . -103_434 N C1 O1 1.293(9) . 1_555 N C1 O2 1.450(9) . 1_555 N C1 C2 1.467(9) . 1_555 N C2 O2 2.341(23) . 1_555 N C2 O3 2.389(24) . 1_555 N C2 C1 1.467(9) . 1_555 N C2 C3 1.432(9) . 1_555 N C2 C4 1.383(21) . -201_444 N C2 H 2.175(26) . -201_444 N C3 O3 1.273(9) . 1_555 N C3 C2 1.432(9) . 1_555 N C3 C4 1.460(9) . 1_555 N C3 H 2.186(25) . 1_555 N C3 O1a 2.32(4) . -103_434 N C4 O3 2.391(22) . 1_555 N C4 C2 1.383(21) . -201_444 N C4 C3 1.460(9) . 1_555 N C4 H 1.123(10) . 1_555 N H O2 2.17(4) . -201_444 N H C2 2.175(26) . -201_444 N H C3 2.186(25) . 1_555 N H C4 1.123(10) . 1_555 N O1a Fe 2.214(35) . -1_666 N O1a O3 2.34(4) . -102_444 N O1a C3 2.32(4) . -102_444 N O1a O1b 1.56(5) . 1_555 N O1a D1 1.19(5) . 1_555 N O1b Fe 2.48(13) . -1_666 N O1b O2 2.13(16) . -102_445 N O1b O1a 1.56(5) . 1_555 N O1b D1 1.55(13) . 1_555 N D1 Fe 2.497(27) . -1_666 N D1 O1a 1.19(5) . 1_555 N D1 O1b 1.55(13) . 1_555 N 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Fe O1 84.02(33) 1_555 . 103_554 N O1 Fe O3 83.0(9) 1_555 . 1_555 N O1 Fe O3 80.4(6) 1_555 . 202_555 N O1 Fe O3 81.3(7) 103_554 . 1_555 N O1 Fe O3 97.1(7) 103_554 . 202_555 N O3 Fe O3 163.4(10) 1_555 . 202_555 N Fe O1 Fe 95.1(5) 1_555 . 202_555 N Fe O1 C1 126.5(16) 1_555 . 1_555 N Fe O1 C1 134.8(13) 202_555 . 1_555 N Fe O3 Fe 94.9(7) 1_555 . 103_554 N Fe O3 C3 125.8(15) 1_555 . 1_555 N Fe O3 C3 131.2(13) 103_554 . 1_555 N O1 C1 O2 128.3(17) 1_555 . 1_555 N O1 C1 C2 122.6(18) 1_555 . 1_555 N O2 C1 C2 106.8(14) 1_555 . 1_555 N C1 C2 C3 116.8(18) 1_555 . 1_555 N C1 C2 C4 117.3(17) 1_555 . -201_555 N C3 C2 C4 119.4(15) 1_555 . -201_555 N O3 C3 C2 124.0(20) 1_555 . 1_555 N O3 C3 C4 121.9(18) 1_555 . 1_555 N C2 C3 C4 113.9(12) 1_555 . 1_555 N C2 C4 C3 123.9(14) -201_555 . 1_555 N C2 C4 H 120.1(18) -201_555 . 1_555 N C3 C4 H 115.0(20) 1_555 . 1_555 N O1b O1a D1 67(7) 1_555 . 1_555 N O1a O1b D1 44.8(31) 1_555 . 1_555 N O1a D1 O1b 68(5) 1_555 . 1_555 N # Information for phase 1 data_OXIDIZEDA_2P0_D2_phase_1 _database_code_depnum_ccdc_archive 'CCDC 853664' #TrackingRef '- OXIDIZED_2P0_D2_final.cif' _pd_block_id 2011-04-21T16:30|OXIDIZEDA_2P0_D2_phase1||| #============================================================================== # 7. CHEMICAL, STRUCTURAL AND CRYSTAL DATA _pd_char_particle_morphology ? _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_melting_point ? _chemical_compound_source ? # for minerals and # natural products _symmetry_space_group_name_Hall ? _exptl_crystal_F_000 ? _exptl_crystal_density_diffrn ? _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _cell_measurement_temperature ? _cell_special_details ; ? ; _geom_special_details ? # The following item identifies the program(s) used (if appropriate). _computing_structure_solution ? #============================================================================== # 8. Phase information from GSAS _pd_phase_name 'from /data/people/craigy/MgMOF/BT1/1108/MOF74.xtl' _cell_length_a 25.9538(15) _cell_length_b 25.9538 _cell_length_c 6.8539(9) _cell_angle_alpha 90.0 _cell_angle_beta 90.0 _cell_angle_gamma 120.0 _cell_volume 3998.3(6) _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'R -3' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +x,+y,+z 2 -y,x-y,+z 3 y-x,-x,+z -1 -x,-y,-z -2 +y,y-x,-z -3 x-y,+x,-z 101 +x+1/3,+y+2/3,+z+2/3 102 -y+1/3,x-y+2/3,+z+2/3 103 y-x+1/3,-x+2/3,+z+2/3 -101 -x+2/3,-y+1/3,-z+1/3 -102 +y+2/3,y-x+1/3,-z+1/3 -103 x-y+2/3,+x+1/3,-z+1/3 201 +x+2/3,+y+1/3,+z+1/3 202 -y+2/3,x-y+1/3,+z+1/3 203 y-x+2/3,-x+1/3,+z+1/3 -201 -x+1/3,-y+2/3,-z+2/3 -202 +y+1/3,y-x+2/3,-z+2/3 -203 x-y+1/3,+x+2/3,-z+2/3 # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_thermal_displace_type _atom_site_U_iso_or_equiv _atom_site_symmetry_multiplicity Fe Fe 0.3800(4) 0.3480(6) 0.1439(23) 1.0 Uiso 0.041(4) 18 O O1 0.3250(9) 0.2957(7) 0.3485(32) 1.0 Uiso 0.024(9) 18 O O2 0.3031(9) 0.2258(11) 0.6020(22) 1.0 Uiso 0.008(7) 18 O O3 0.3512(7) 0.2720(4) 0.0102(28) 1.0 Uiso 0.003(6) 18 C C1 0.3161(13) 0.2441(9) 0.4001(25) 1.0 Uiso 0.045(9) 18 C C2 0.3297(15) 0.2046(10) 0.2879(31) 1.0 Uiso 0.072(11) 18 C C3 0.3457(10) 0.2258(8) 0.0918(30) 1.0 Uiso 0.008(5) 18 C C4 0.3528(10) 0.1835(9) -0.0280(27) 1.0 Uiso 0.017(7) 18 H H 0.3679(17) 0.1938(16) -0.1851(33) 1.0 Uiso 0.001(9) 18 O O1a 0.532(1) 0.609(2) 0.716(4) 0.44(3) Uiso 0.00098 18 O O1b 0.515(5) 0.632(5) 0.902(9) 0.44(3) Uani 0.6528 18 D D1 0.5358(15) 0.6554(15) 0.734(4) 1.78(8) Uani 0.22591 18 D D2 0.5419(9) 0.6967(10) 0.315(5) 2.02(9) Uani 0.23665 18 D D3 0.232(4) 0.492(5) 0.848(21) 0.31(5) Uani 0.11626 18 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_22 _atom_site_aniso_U_23 _atom_site_aniso_U_33 O1b 0.8(4) 0.4(4) 0.2(3) 0.8(3) 0.0(3) 0.4(4) D1 0.21(4) 0.061(31) 0.011(28) 0.19(4) -0.003(26) 0.23(5) D2 0.215(34) 0.152(29) -0.017(34) 0.26(4) 0.037(31) 0.28(4) D3 0.01(8) 0.02(10) -0.09(6) 0.23(16) -0.06(9) 0.06(10) loop_ _atom_type_symbol _atom_type_number_in_cell Fe 18.0 O 69.918 C 72.0 H 18.0 D 74.13 # If you change Z, be sure to change all 3 of the following _chemical_formula_sum 'C4 H D4.12 Fe O3.88' _chemical_formula_weight 175.34 _cell_formula_units_Z 18 # MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe O1 1.977(9) . 1_555 N Fe O1 2.091(25) . 103_554 N Fe O2 2.147(27) . 202_554 N Fe O3 1.953(9) . 1_555 N Fe O3 2.047(22) . 202_555 N Fe O1a 2.205(12) . -1_666 N Fe O1b 2.530(10) . -1_666 N Fe D1 2.382(33) . -1_666 N O1 Fe 1.977(9) . 1_555 N O1 Fe 2.091(25) . 202_555 N O1 C1 1.289(9) . 1_555 N O2 Fe 2.147(27) . 103_555 N O2 C1 1.447(9) . 1_555 N O3 Fe 1.953(9) . 1_555 N O3 Fe 2.047(22) . 103_554 N O3 C3 1.264(9) . 1_555 N C1 O1 1.289(9) . 1_555 N C1 O2 1.447(9) . 1_555 N C1 C2 1.458(9) . 1_555 N C2 C1 1.458(9) . 1_555 N C2 C3 1.433(9) . 1_555 N C2 C4 1.365(9) . -201_444 N C3 O3 1.264(9) . 1_555 N C3 C2 1.433(9) . 1_555 N C3 C4 1.454(9) . 1_555 N C4 C2 1.365(9) . -201_444 N C4 C3 1.454(9) . 1_555 N C4 H 1.131(9) . 1_555 N H C4 1.131(9) . 1_555 N O1a Fe 2.205(12) . -1_666 N O1a O1b 1.55(4) . 1_555 N O1a D1 1.158(35) . 1_555 N O1b Fe 2.530(10) . -1_666 N O1b O1a 1.55(4) . 1_555 N O1b D1 1.286(26) . 1_555 N D1 Fe 2.382(33) . -1_666 N D1 O1a 1.158(35) . 1_555 N D1 O1b 1.286(26) . 1_555 N D1 D3 2.75(10) . 2_665 N D3 D1 2.75(10) . 3_565 N 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Fe O1 85.2(4) 1_555 . 103_554 N O1 Fe O2 175.5(11) 1_555 . 202_554 N O1 Fe O3 81.9(11) 1_555 . 1_555 N O1 Fe O3 82.1(7) 1_555 . 202_555 N O1 Fe O2 94.9(13) 103_554 . 202_554 N O1 Fe O3 81.5(8) 103_554 . 1_555 N O1 Fe O3 97.3(9) 103_554 . 202_555 N O2 Fe O3 102.6(4) 202_554 . 1_555 N O2 Fe O3 93.4(11) 202_554 . 202_555 N O3 Fe O3 164.0(11) 1_555 . 202_555 N Fe O1 Fe 92.7(5) 1_555 . 202_555 N Fe O1 C1 126.9(19) 1_555 . 1_555 N Fe O1 C1 137.0(15) 202_555 . 1_555 N Fe O2 C1 118.9(17) 103_555 . 1_555 N Fe O3 Fe 94.8(9) 1_555 . 103_554 N Fe O3 C3 123.7(17) 1_555 . 1_555 N Fe O3 C3 133.6(14) 103_554 . 1_555 N O1 C1 O2 119.6(19) 1_555 . 1_555 N O1 C1 C2 127.2(19) 1_555 . 1_555 N O2 C1 C2 111.9(16) 1_555 . 1_555 N C1 C2 C3 110.5(18) 1_555 . 1_555 N C1 C2 C4 119.0(19) 1_555 . -201_555 N C3 C2 C4 128.7(16) 1_555 . -201_555 N O3 C3 C2 130.7(23) 1_555 . 1_555 N O3 C3 C4 117.9(20) 1_555 . 1_555 N C2 C3 C4 111.2(14) 1_555 . 1_555 N C2 C4 C3 119.5(15) -201_555 . 1_555 N C2 C4 H 119.0(23) -201_555 . 1_555 N C3 C4 H 121.3(25) 1_555 . 1_555 N O1b O1a D1 54.3(13) 1_555 . 1_555 N O1a O1b D1 47.0(16) 1_555 . 1_555 N O1a D1 O1b 78.7(17) 1_555 . 1_555 N #--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--#