# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name _publ_author_address _publ_author_footnote A.Churchard ;ICM, University of Warsaw Zwiriki i Wigury 93 02-089 Warsaw Poland ; ; ; M.Derzsi ;ICM, University of Warsaw Zwiriki i Wigury 93 02-089 Warsaw Poland ; ; ; Z.Jaglicic ;Institute of Mathematics Physics and Mechanics Jadranska 19 Ljubljana Slovenia ; ;and University of Ljubljana Faculty of Civil and Geodetic Engineering, Jamova 2 Ljubljana Slovenia ; A.Remhof ;Empa ? Swiss Federal Laboratories for Materials Science and Technology Hydrogen and Energy \"Uberlandstrasse 129 CH-8600 D\"ubendorf Switzerland ; ; ; W.Grochala ;ICM, University of Warsaw Zwiriki i Wigury 93 02-089 Warsaw Poland ; ;and Faculty of Chemistry, University of Warsaw Pasteura 1 02-093 Warsaw Poland ; _publ_contact_author_name 'Mr Andrew Churchard' _publ_contact_author_address ;ICM, University of Warsaw Zwiriki i Wigury 93 02-089 Warsaw Poland ; _publ_contact_author_email achurch@icm.edu.pl _publ_section_title ; Chemo-switched chromatic, magnetic and structural changes with retention of molecular crystallinity, Ni(12aneS4)(BF4)2 ; # Attachment '- blue_from_theoretical_ring_NiO2_sep_mols.cif' #======================================================================= #TrackingRef '- blue_from_theoretical_ring_NiO2_sep_mols.cif' #======================================================================= #======================================================================= data_I _database_code_depnum_ccdc_archive 'CCDC 846503' #TrackingRef '- blue_from_theoretical_ring_NiO2_sep_mols.cif' #======================================================================= _audit_creation_method 'Jana2006 Version : 23/10/2010' # 5. CHEMICAL DATA _chemical_formula_moiety 'C8 H20 Ni O2 S4 2+, 2(B F4 -)' _chemical_formula_structural '(Ni (C8 H16 S4) (H2 O)2) (B F4)2' _chemical_formula_sum 'C8 H20 B2 F8 Ni O2 S4' _chemical_formula_weight 508.78 #======================================================================= # 6. POWDER SPECIMEN AND CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P -2xab;-2ybc;-2zac' _symmetry_Int_Tables_number 61 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x+1/2,-y,z+1/2 3 -x,y+1/2,-z+1/2 4 x+1/2,-y+1/2,-z 5 -x,-y,-z 6 x+1/2,y,-z+1/2 7 x,-y+1/2,z+1/2 8 -x+1/2,y+1/2,z _cell_length_a 18.5287(5) _cell_length_b 15.2433(4) _cell_length_c 13.3682(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3775.69(17) _cell_formula_units_Z 8 _cell_measurement_temperature 100 _cell_special_details ; ? ; _exptl_crystal_density_diffrn 1.7895 _exptl_crystal_F_000 2064 _pd_char_colour light_blue _exptl_absorpt_coefficient_mu 2.14 #======================================================================= # 7. EXPERIMENTAL DATA _exptl_special_details ? _pd_instr_location ; MS - X04SA: Materials Science Beamline Paul Scherrer Institute 5232 Villigen PSI Switzerland ; _pd_calibration_special_details ; Wavelength calibrated with NIST 640C Si standard ; _diffrn_ambient_temperature 100 _diffrn_source synchrotron _diffrn_source_type 'PSI SLS MS - X04SA Beamline' _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.80035 _diffrn_measurement_device_type ;three coaxial heavy-duty rotation tables mounted on a lifting table see Gozzo et al., J. Alloys Compounds, 2004, 362, 206-217 ; _diffrn_detector 'solid-state silicon microstrip' _diffrn_detector_type MythenII _pd_meas_scan_method fixed _pd_meas_special_details ; correction for flatfield, rate and bad channels applied ; _pd_meas_number_of_points 30823 _pd_meas_2theta_range_min 2.089 _pd_meas_2theta_range_max 117.881 _pd_meas_2theta_range_inc 0.004 #======================================================================= # 8. REFINEMENT DATA _pd_proc_ls_profile_function Pseudo-Voigt _pd_proc_ls_background_function '20 Legendre polynoms' _pd_proc_ls_pref_orient_corr none _pd_proc_ls_prof_R_factor 0.0281 _pd_proc_ls_prof_wR_factor 0.0352 _pd_proc_ls_prof_wR_expected 0.0081 _refine_ls_goodness_of_fit_all 0.0435 _refine_ls_number_parameters 54 _refine_ls_number_restraints 20 _refine_ls_number_constraints 0 _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment mixed _refine_ls_shift/su_max 0.0113 _refine_ls_shift/su_mean 0.0025 _pd_proc_2theta_range_min 4.001 _pd_proc_2theta_range_max 60 _pd_proc_2theta_range_inc 0.004 _pd_proc_wavelength 0.80035 _refine_special_details ;H positions are not refined ; loop_ _pd_proc_info_excluded_regions 'from 1.085 to 4.000 remove peak related to sample environment' 'from 47.09 to 47.115 count spikes to 0' 'from 48.09 to 48.115 count spikes to 0' loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0.005 0.002 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' S 0.152 0.159 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' Ni 0.314 1.381 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' F 0.023 0.014 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' B 0.002 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' _computing_cell_refinement 'Expo2009 (Altomare et al., 2009)' _computing_data_reduction 'Jana2006 (Petricek, Dusek & Palatinus, 2006)' _computing_structure_solution 'FOX (Favre-Nicolin & Cerny, 2002)' _computing_structure_refinement 'Jana2006 (Petricek, Dusek & Palatinus, 2006)' _computing_molecular_graphics ; Vesta (Momma & Izumi, 2008) Mercury (Macrae et al., 2008) ; #======================================================================= # 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 B1 B 0.40200(15) 0.7523(3) 0.4782(3) Uiso 0.0127 8 1 d . . . F1 F 0.36111(15) 0.8178(3) 0.5187(3) Uiso 0.0127 8 1 d . . . F2 F 0.41017(15) 0.7667(3) 0.3782(3) Uiso 0.0127 8 1 d . . . F3 F 0.36849(15) 0.6735(3) 0.4929(3) Uiso 0.0127 8 1 d . . . F4 F 0.46791(15) 0.7511(3) 0.5229(3) Uiso 0.0127 8 1 d . . . B2 B 0.36469(18) 0.45821(19) 0.7087(2) Uiso 0.0127 8 1 d . . . F5 F 0.36188(18) 0.42042(19) 0.8010(2) Uiso 0.0127 8 1 d . . . F6 F 0.40860(18) 0.40925(19) 0.6473(2) Uiso 0.0127 8 1 d . . . F7 F 0.29531(18) 0.46178(19) 0.6681(2) Uiso 0.0127 8 1 d . . . F8 F 0.39204(18) 0.54201(19) 0.7169(2) Uiso 0.0127 8 1 d . . . C8 C 0.65675(8) 0.54143(11) 0.57504(15) Uiso 0.0127 8 1 d . . . C1 C 0.70029(8) 0.62355(11) 0.55914(15) Uiso 0.0127 8 1 d . . . C2 C 0.58000(8) 0.44521(11) 0.72146(15) Uiso 0.0127 8 1 d . . . C3 C 0.55572(8) 0.44743(11) 0.82909(15) Uiso 0.0127 8 1 d . . . C4 C 0.60042(8) 0.56902(11) 0.97594(15) Uiso 0.0127 8 1 d . . . C5 C 0.67681(8) 0.58885(11) 0.94492(15) Uiso 0.0127 8 1 d . . . C6 C 0.74393(8) 0.74352(11) 0.70781(15) Uiso 0.0127 8 1 d . . . C7 C 0.75562(8) 0.68342(11) 0.79595(15) Uiso 0.0127 8 1 d . . . S1 S 0.65343(8) 0.52084(11) 0.70713(15) Uiso 0.0127 8 1 d . . . S2 S 0.53668(8) 0.55783(11) 0.87410(15) Uiso 0.0127 8 1 d . . . S3 S 0.67457(8) 0.68679(11) 0.86971(15) Uiso 0.0127 8 1 d . . . S4 S 0.66635(8) 0.71605(11) 0.63133(15) Uiso 0.0127 8 1 d . . . H1c1 H 0.70032(8) 0.63836(11) 0.48934(15) Uiso 0.0152 8 1 d . . . H2c1 H 0.74972(8) 0.61268(11) 0.57674(15) Uiso 0.0152 8 1 d . . . H1c2 H 0.54079(8) 0.46260(11) 0.67891(15) Uiso 0.0152 8 1 d . . . H2c2 H 0.59605(8) 0.38712(11) 0.70488(15) Uiso 0.0152 8 1 d . . . H1c3 H 0.59195(8) 0.42092(11) 0.87058(15) Uiso 0.0152 8 1 d . . . H2c3 H 0.51353(8) 0.41152(11) 0.83685(15) Uiso 0.0152 8 1 d . . . H1c4 H 0.58384(8) 0.61345(11) 1.02136(15) Uiso 0.0152 8 1 d . . . H2c4 H 0.59971(8) 0.51681(11) 1.01609(15) Uiso 0.0152 8 1 d . . . H1c5 H 0.69531(8) 0.54106(11) 0.90581(15) Uiso 0.0152 8 1 d . . . H2c5 H 0.70575(8) 0.59903(11) 1.00336(15) Uiso 0.0152 8 1 d . . . H1c6 H 0.78653(8) 0.74421(11) 0.66694(15) Uiso 0.0152 8 1 d . . . H2c6 H 0.73961(8) 0.80291(11) 0.73093(15) Uiso 0.0152 8 1 d . . . H1c7 H 0.79544(8) 0.70448(11) 0.83512(15) Uiso 0.0152 8 1 d . . . H2c7 H 0.76352(8) 0.62468(11) 0.77249(15) Uiso 0.0152 8 1 d . . . H1c8 H 0.67995(8) 0.49312(11) 0.54205(15) Uiso 0.0152 8 1 d . . . H2c8 H 0.60868(8) 0.55015(11) 0.55016(15) Uiso 0.0152 8 1 d . . . Ni1 Ni 0.58958(9) 0.64810(10) 0.7499(2) Uiso 0.0127 8 1 d . . . O1 O 0.50646(9) 0.62273(10) 0.6516(2) Uiso 0.0127 8 1 d . . . O2 O 0.53493(9) 0.76358(10) 0.7733(2) Uiso 0.0127 8 1 d . . . H1o1 H 0.50574(9) 0.57655(10) 0.6202(2) Uiso 0.0152 8 1 d . . . H2o1 H 0.47410(9) 0.65880(10) 0.6440(2) Uiso 0.0152 8 1 d . . . H1o2 H 0.55075(9) 0.79985(10) 0.8129(2) Uiso 0.0152 8 1 d . . . H2o2 H 0.49730(9) 0.77339(10) 0.7430(2) Uiso 0.0152 8 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 B1 F1 . . 1.366(5) ? B1 F2 . . 1.362(5) ? B1 F3 . . 1.367(5) ? B1 F4 . . 1.360(4) ? B2 F5 . . 1.363(4) ? B2 F6 . . 1.375(4) ? B2 F7 . . 1.397(5) ? B2 F8 . . 1.379(4) ? C8 C1 . . 1.504(2) ? C8 H1c8 . . 0.960(2) ? C8 H2c8 . . 0.960(2) ? C1 H1c1 . . 0.960(3) ? C1 H2c1 . . 0.960(2) ? C2 C3 . . 1.508(3) ? C2 H1c2 . . 0.960(2) ? C2 H2c2 . . 0.960(2) ? C3 H1c3 . . 0.960(2) ? C3 H2c3 . . 0.960(2) ? C4 C5 . . 1.506(2) ? C4 H1c4 . . 0.960(3) ? C4 H2c4 . . 0.960(3) ? C5 H1c5 . . 0.960(2) ? C5 H2c5 . . 0.960(3) ? C6 C7 . . 1.508(3) ? C6 H1c6 . . 0.960(2) ? C6 H2c6 . . 0.960(2) ? C7 H1c7 . . 0.960(2) ? C7 H2c7 . . 0.960(2) ? S1 Ni1 . . 2.343(2) ? S2 Ni1 . . 2.369(3) ? S3 Ni1 . . 2.323(3) ? S4 Ni1 . . 2.368(3) ? Ni1 O1 . . 2.060(3) ? Ni1 O2 . . 2.055(2) ? O1 H1o1 . . 0.820(3) ? O1 H2o1 . . 0.820(2) ? O2 H1o2 . . 0.820(3) ? O2 H2o2 . . 0.820(3) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag F1 B1 F2 . . . 109.5(3) ? F1 B1 F3 . . . 109.5(3) ? F1 B1 F4 . . . 109.5(3) ? F2 B1 F3 . . . 109.5(3) ? F2 B1 F4 . . . 109.5(3) ? F3 B1 F4 . . . 109.4(3) ? F5 B2 F6 . . . 109.5(3) ? F5 B2 F7 . . . 109.5(3) ? F5 B2 F8 . . . 109.5(3) ? F6 B2 F7 . . . 109.5(3) ? F6 B2 F8 . . . 109.5(3) ? F7 B2 F8 . . . 109.5(3) ? C1 C8 H1c8 . . . 109.47(18) ? C1 C8 H2c8 . . . 109.47(18) ? H1c8 C8 H2c8 . . . 111.2(2) ? C8 C1 H1c1 . . . 109.47(19) ? C8 C1 H2c1 . . . 109.47(18) ? H1c1 C1 H2c1 . . . 106.1(2) ? C3 C2 H1c2 . . . 109.47(18) ? C3 C2 H2c2 . . . 109.5(2) ? H1c2 C2 H2c2 . . . 110.6(2) ? C2 C3 H1c3 . . . 109.47(18) ? C2 C3 H2c3 . . . 109.5(2) ? H1c3 C3 H2c3 . . . 105.5(2) ? C5 C4 H1c4 . . . 109.47(17) ? C5 C4 H2c4 . . . 109.47(17) ? H1c4 C4 H2c4 . . . 103.1(2) ? C4 C5 H1c5 . . . 109.47(17) ? C4 C5 H2c5 . . . 109.5(2) ? H1c5 C5 H2c5 . . . 111.5(2) ? C7 C6 H1c6 . . . 109.47(18) ? C7 C6 H2c6 . . . 109.5(2) ? H1c6 C6 H2c6 . . . 104.0(2) ? C6 C7 H1c7 . . . 109.47(18) ? C6 C7 H2c7 . . . 109.5(2) ? H1c7 C7 H2c7 . . . 111.9(2) ? S1 Ni1 S2 . . . 84.20(8) ? S1 Ni1 S3 . . . 92.07(9) ? S1 Ni1 S4 . . . 84.01(9) ? S1 Ni1 O1 . . . 93.82(10) ? S1 Ni1 O2 . . . 174.47(17) ? S2 Ni1 S3 . . . 86.81(11) ? S2 Ni1 S4 . . . 166.34(10) ? S2 Ni1 O1 . . . 91.63(10) ? S2 Ni1 O2 . . . 100.76(12) ? S3 Ni1 S4 . . . 86.75(8) ? S3 Ni1 O1 . . . 173.72(12) ? S3 Ni1 O2 . . . 90.65(11) ? S4 Ni1 O1 . . . 96.01(13) ? S4 Ni1 O2 . . . 91.34(10) ? O1 Ni1 O2 . . . 83.66(10) ? Ni1 O1 H1o1 . . . 120.0(2) ? Ni1 O1 H2o1 . . . 120.0(2) ? H1o1 O1 H2o1 . . . 120.0(3) ? Ni1 O2 H1o2 . . . 120.0(2) ? Ni1 O2 H2o2 . . . 120.0(2) ? H1o2 O2 H2o2 . . . 120.0(3) ? #======================================================================= # Attachment '- purple_from_theoretical_ring_inc_Ni_adjusts_publish.cif' #======================================================================= data_II _database_code_depnum_ccdc_archive 'CCDC 846504' #TrackingRef '- purple_from_theoretical_ring_inc_Ni_adjusts_publish.cif' #======================================================================= _audit_creation_method 'Jana2006 Version : 23/10/2010' # 5. CHEMICAL DATA _chemical_formula_moiety 'C8 H16 Ni S4 2+, 2(B F4 -)' _chemical_formula_structural '(Ni (C8 H16 S4)) (B F4)2' _chemical_formula_sum 'C8 H16 B2 F8 Ni S4' _chemical_formula_weight 472.78 #======================================================================= # 6. POWDER SPECIMEN AND CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P -2xab;-2ybc;-2zac' _symmetry_Int_Tables_number 61 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x+1/2,-y,z+1/2 3 -x,y+1/2,-z+1/2 4 x+1/2,-y+1/2,-z 5 -x,-y,-z 6 x+1/2,y,-z+1/2 7 x,-y+1/2,z+1/2 8 -x+1/2,y+1/2,z _cell_length_a 16.1254(3) _cell_length_b 15.2621(3) _cell_length_c 13.2577(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3262.83(10) _cell_formula_units_Z 8 _cell_measurement_temperature 100 _cell_special_details ; ? ; _exptl_crystal_density_diffrn 1.9241 _exptl_crystal_F_000 1904 _pd_char_colour dark_violet _exptl_absorpt_coefficient_mu 2.455 #======================================================================= # 7. EXPERIMENTAL DATA _exptl_special_details ? _pd_instr_location ; MS - X04SA: Materials Science Beamline Paul Scherrer Institute 5232 Villigen PSI Switzerland ; _pd_calibration_special_details ; Wavelength calibrated with NIST 640C Si standard ; _diffrn_ambient_temperature 100 _diffrn_source synchrotron _diffrn_source_type 'PSI SLS MS - X04SA Beamline' _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.80035 _diffrn_measurement_device_type ;three coaxial heavy-duty rotation tables mounted on a lifting table see Gozzo et al., J. Alloys Compounds, 2004, 362, 206-217 ; _diffrn_detector 'solid-state silicon microstrip' _diffrn_detector_type MythenII _pd_meas_scan_method fixed _pd_meas_special_details ; correction for flatfield, rate and bad channels applied ; _pd_meas_number_of_points 30823 _pd_meas_2theta_range_min 2.089 _pd_meas_2theta_range_max 117.881 _pd_meas_2theta_range_inc 0.004 #======================================================================= # 8. REFINEMENT DATA _pd_proc_ls_profile_function Pseudo-Voigt _pd_proc_ls_background_function '20 Chebyshev polynoms' _pd_proc_ls_pref_orient_corr none _pd_proc_ls_prof_R_factor 0.0168 _pd_proc_ls_prof_wR_factor 0.0203 _pd_proc_ls_prof_wR_expected 0.0124 _refine_ls_goodness_of_fit_all 0.0136 _refine_ls_number_parameters 48 _refine_ls_number_restraints 20 _refine_ls_number_constraints 0 _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment mixed _refine_ls_shift/su_max 0.0145 _refine_ls_shift/su_mean 0.0016 _pd_proc_2theta_range_min 4.001 _pd_proc_2theta_range_max 60 _pd_proc_2theta_range_inc 0.004 _pd_proc_wavelength 0.80035 loop_ _pd_proc_info_excluded_regions 'from 1.085 to 4.000 remove peak related to sample environment' 'from 47.09 to 47.115 count spikes to 0' 'from 48.09 to 48.115 count spikes to 0' loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0.005 0.002 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' S 0.152 0.159 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' Ni 0.314 1.381 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' F 0.023 0.014 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' B 0.002 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' _computing_cell_refinement 'Expo2009 (Altomare et al., 2009)' _computing_data_reduction 'Jana2006 (Petricek, Dusek & Palatinus, 2006)' _computing_structure_solution 'FOX (Favre-Nicolin & Cerny, 2002)' _computing_structure_refinement 'Jana2006 (Petricek, Dusek & Palatinus, 2006)' _computing_molecular_graphics ; Vesta (Momma & Izumi, 2008) Mercury (Macrae et al., 2008) ; #======================================================================= # 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 F1a F 0.54284(18) 0.2642(2) 0.36078(18) Uiso 0.0127 8 1 d . . . F2a F 0.62525(18) 0.3055(2) 0.48893(18) Uiso 0.0127 8 1 d . . . F3a F 0.49625(18) 0.2554(2) 0.52090(18) Uiso 0.0127 8 1 d . . . F4a F 0.59597(18) 0.1619(2) 0.46599(18) Uiso 0.0127 8 1 d . . . B1a B 0.56511(18) 0.2470(2) 0.45902(18) Uiso 0.0127 8 1 d . . . F5a F 0.26011(15) 0.57810(16) 0.2617(2) Uiso 0.0127 8 1 d . . . F6a F 0.15349(15) 0.49493(16) 0.2076(2) Uiso 0.0127 8 1 d . . . F7a F 0.13107(15) 0.63299(16) 0.2598(2) Uiso 0.0127 8 1 d . . . F8a F 0.16504(15) 0.52960(16) 0.3716(2) Uiso 0.0127 8 1 d . . . B2a B 0.17736(15) 0.55903(16) 0.2754(2) Uiso 0.0127 8 1 d . . . C1a C 0.32435(7) 0.40362(7) 0.09527(9) Uiso 0.0127 8 1 d . . . C3a C 0.41051(7) 0.43408(7) 0.07033(9) Uiso 0.0127 8 1 d . . . C4a C 0.44479(7) 0.54619(7) 0.23283(9) Uiso 0.0127 8 1 d . . . C5a C 0.47310(7) 0.54889(7) 0.34054(9) Uiso 0.0127 8 1 d . . . C6a C 0.31299(7) 0.38420(7) 0.49371(9) Uiso 0.0127 8 1 d . . . C7a C 0.34643(7) 0.47128(7) 0.45976(9) Uiso 0.0127 8 1 d . . . C8a C 0.23622(7) 0.28411(7) 0.22134(9) Uiso 0.0127 8 1 d . . . C9a C 0.22666(7) 0.32690(7) 0.32283(9) Uiso 0.0127 8 1 d . . . H1a H 0.34929(7) 0.35593(7) 0.55682(9) Uiso 0.0127 8 1 d . . . H2a H 0.24725(7) 0.38800(7) 0.51714(9) Uiso 0.0127 8 1 d . . . H3a H 0.30673(7) 0.50253(7) 0.40189(9) Uiso 0.0127 8 1 d . . . H4a H 0.35480(7) 0.51719(7) 0.52383(9) Uiso 0.0127 8 1 d . . . H5a H 0.23192(7) 0.21190(7) 0.22680(9) Uiso 0.0127 8 1 d . . . H6a H 0.18907(7) 0.30709(7) 0.16643(9) Uiso 0.0127 8 1 d . . . H7a H 0.21815(7) 0.39852(7) 0.31722(9) Uiso 0.0127 8 1 d . . . H8a H 0.17381(7) 0.29919(7) 0.36603(9) Uiso 0.0127 8 1 d . . . H9a H 0.28880(7) 0.45174(7) 0.14033(9) Uiso 0.0127 8 1 d . . . H10a H 0.28934(7) 0.38712(7) 0.02589(9) Uiso 0.0127 8 1 d . . . H11a H 0.44341(7) 0.38727(7) 0.02063(9) Uiso 0.0127 8 1 d . . . H12a H 0.41124(7) 0.49949(7) 0.03417(9) Uiso 0.0127 8 1 d . . . H13a H 0.37684(7) 0.55357(7) 0.22621(9) Uiso 0.0127 8 1 d . . . H14a H 0.47570(7) 0.59725(7) 0.18681(9) Uiso 0.0127 8 1 d . . . H15a H 0.54145(7) 0.55309(7) 0.34458(9) Uiso 0.0127 8 1 d . . . H16a H 0.44678(7) 0.60456(7) 0.38364(9) Uiso 0.0127 8 1 d . . . Ni1a Ni 0.40665(7) 0.36139(7) 0.28972(9) Uiso 0.0127 8 1 d . . . S1a S 0.47373(7) 0.43994(7) 0.18301(9) Uiso 0.0127 8 1 d . . . S2a S 0.44753(7) 0.44854(7) 0.40627(9) Uiso 0.0127 8 1 d . . . S3a S 0.32028(7) 0.30344(7) 0.39366(9) Uiso 0.0127 8 1 d . . . S4a S 0.33804(7) 0.30376(7) 0.16765(9) Uiso 0.0127 8 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 F1a B1a . . 1.376(3) yes F2a B1a . . 1.376(4) yes F3a B1a . . 1.387(4) yes F4a B1a . . 1.393(4) yes F5a B2a . . 1.378(3) yes F6a B2a . . 1.383(4) yes F7a B2a . . 1.369(4) yes F8a B2a . . 1.367(4) yes C1a C3a . . 1.5018(17) yes C1a H9a . . 1.1068(16) yes C1a H10a . . 1.1083(16) yes C1a S4a . . 1.8144(16) yes C3a H11a . . 1.1072(16) yes C3a H12a . . 1.1075(16) yes C3a S1a . . 1.8108(16) yes C4a C5a . . 1.4997(16) yes C4a H13a . . 1.1050(17) yes C4a H14a . . 1.1081(16) yes C4a S1a . . 1.8121(16) yes C5a H15a . . 1.1052(17) yes C5a H16a . . 1.1084(16) yes C5a S2a . . 1.8097(16) yes C6a C7a . . 1.5033(16) yes C6a H1a . . 1.1086(16) yes C6a H2a . . 1.1061(17) yes C6a S3a . . 1.8145(16) yes C7a H3a . . 1.1073(16) yes C7a H4a . . 1.1094(16) yes C7a S2a . . 1.8114(17) yes C8a C9a . . 1.5036(16) yes C8a H5a . . 1.1066(16) yes C8a H6a . . 1.1094(16) yes C8a S4a . . 1.8145(17) yes C9a H7a . . 1.1042(16) yes C9a H8a . . 1.1105(16) yes C9a S3a . . 1.8137(16) yes Ni1a S1a . . 2.1468(16) yes Ni1a S2a . . 2.1428(16) yes Ni1a S3a . . 2.1496(16) yes Ni1a S4a . . 2.1487(16) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag F1a B1a F2a . . . 109.4(2) yes F1a B1a F3a . . . 109.5(2) yes F1a B1a F4a . . . 109.5(2) yes F2a B1a F3a . . . 109.5(2) yes F2a B1a F4a . . . 109.5(3) yes F3a B1a F4a . . . 109.5(2) yes F5a B2a F6a . . . 109.5(2) yes F5a B2a F7a . . . 109.5(2) yes F5a B2a F8a . . . 109.5(2) yes F6a B2a F7a . . . 109.5(2) yes F6a B2a F8a . . . 109.5(2) yes F7a B2a F8a . . . 109.4(2) yes C3a C1a H9a . . . 113.11(11) yes C3a C1a H10a . . . 111.02(11) yes C3a C1a S4a . . . 105.31(9) yes H9a C1a H10a . . . 109.56(13) yes H9a C1a S4a . . . 109.57(10) yes H10a C1a S4a . . . 108.06(10) yes C1a C3a H11a . . . 112.00(11) yes C1a C3a H12a . . . 112.60(11) yes C1a C3a S1a . . . 110.76(9) yes H11a C3a H12a . . . 108.59(13) yes H11a C3a S1a . . . 104.65(10) yes H12a C3a S1a . . . 107.85(10) yes C5a C4a H13a . . . 112.01(11) yes C5a C4a H14a . . . 111.59(11) yes C5a C4a S1a . . . 107.05(8) yes H13a C4a H14a . . . 109.30(13) yes H13a C4a S1a . . . 108.52(10) yes H14a C4a S1a . . . 108.23(10) yes C4a C5a H15a . . . 110.57(11) yes C4a C5a H16a . . . 113.29(11) yes C4a C5a S2a . . . 111.46(9) yes H15a C5a H16a . . . 108.20(13) yes H15a C5a S2a . . . 104.66(10) yes H16a C5a S2a . . . 108.25(10) yes C7a C6a H1a . . . 112.37(11) yes C7a C6a H2a . . . 112.42(11) yes C7a C6a S3a . . . 111.01(9) yes H1a C6a H2a . . . 108.33(13) yes H1a C6a S3a . . . 104.67(10) yes H2a C6a S3a . . . 107.64(10) yes C6a C7a H3a . . . 112.39(11) yes C6a C7a H4a . . . 111.89(11) yes C6a C7a S2a . . . 105.70(8) yes H3a C7a H4a . . . 109.21(12) yes H3a C7a S2a . . . 109.36(11) yes H4a C7a S2a . . . 108.13(11) yes C9a C8a H5a . . . 111.57(11) yes C9a C8a H6a . . . 112.30(11) yes C9a C8a S4a . . . 111.84(9) yes H5a C8a H6a . . . 108.36(13) yes H5a C8a S4a . . . 104.30(10) yes H6a C8a S4a . . . 108.09(10) yes C8a C9a H7a . . . 112.49(11) yes C8a C9a H8a . . . 112.01(11) yes C8a C9a S3a . . . 106.99(9) yes H7a C9a H8a . . . 108.44(13) yes H7a C9a S3a . . . 109.50(11) yes H8a C9a S3a . . . 107.25(10) yes S1a Ni1a S2a . . . 88.48(6) yes S1a Ni1a S3a . . . 168.14(7) yes S1a Ni1a S4a . . . 89.52(6) yes S2a Ni1a S3a . . . 89.57(6) yes S2a Ni1a S4a . . . 162.87(7) yes S3a Ni1a S4a . . . 88.90(6) yes C3a S1a C4a . . . 101.53(8) yes C3a S1a Ni1a . . . 103.44(7) yes C4a S1a Ni1a . . . 97.46(7) yes C5a S2a C7a . . . 103.39(8) yes C5a S2a Ni1a . . . 104.37(7) yes C7a S2a Ni1a . . . 97.15(7) yes C6a S3a C9a . . . 100.98(8) yes C6a S3a Ni1a . . . 103.37(7) yes C9a S3a Ni1a . . . 97.25(7) yes C1a S4a C8a . . . 103.67(8) yes C1a S4a Ni1a . . . 96.73(7) yes C8a S4a Ni1a . . . 103.77(7) yes #=======================================================================