# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Li-Min Zheng' _publ_contact_author_email LMZHENG@NETRA.NJU.EDU.CN _publ_section_title ; Tuning the field-induced magnetic transition in a layered cobalt phosphonate by reversible dehydration-hydration process ; loop_ _publ_author_name 'Li-Min Zheng' 'Robert E. Dinnebier' 'Yi Liao' 'Jing Ma' 'Yan-Hui Su' 'Ting-Hai Yang' # Attachment 'Co-1.cif' data_sad _database_code_depnum_ccdc_archive 'CCDC 707409' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H10 Co N O5 P' _chemical_formula_sum 'C6 H10 Co N O5 P' _chemical_formula_weight 266.05 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' 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_hall '-P 2ybc' 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 10.6973(19) _cell_length_b 7.3463(13) _cell_length_c 12.439(2) _cell_angle_alpha 90.00 _cell_angle_beta 110.358(3) _cell_angle_gamma 90.00 _cell_volume 916.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 1012 _cell_measurement_theta_min 3.2775 _cell_measurement_theta_max 28.037 _exptl_crystal_description block _exptl_crystal_colour purple-red _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.928 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 540 _exptl_absorpt_coefficient_mu 2.041 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.571 _exptl_absorpt_correction_T_max 0.695 _exptl_absorpt_process_details 'SADABS(Bruker, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4624 _diffrn_reflns_av_R_equivalents 0.0231 _diffrn_reflns_av_sigmaI/netI 0.0292 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 26.00 _reflns_number_total 1779 _reflns_number_gt 1676 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material 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. ; _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^)+(0.0497P)^2^+1.6738P] 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_number_reflns 1779 _refine_ls_number_parameters 127 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0396 _refine_ls_R_factor_gt 0.0366 _refine_ls_wR_factor_ref 0.0955 _refine_ls_wR_factor_gt 0.0931 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _refine_ls_shift/su_max 0.001 _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 Co1 Co 0.59838(4) 0.25934(5) -0.09300(3) 0.01646(16) Uani 1 1 d . . . P1 P 0.59416(7) 0.12129(10) 0.14963(6) 0.0165(2) Uani 1 1 d . . . O1 O 0.5541(2) 0.2672(3) 0.05505(18) 0.0205(5) Uani 1 1 d . . . O2 O 0.6530(2) 0.2091(3) 0.26684(18) 0.0231(5) Uani 1 1 d . . . O3 O 0.4766(2) -0.0018(3) 0.14195(18) 0.0220(5) Uani 1 1 d . . . O1W O 0.6665(2) 0.5516(3) -0.0568(2) 0.0352(6) Uani 1 1 d . . . H1WA H 0.6010 0.6173 -0.0457 0.053 Uiso 1 1 d R . . H1WB H 0.7016 0.4858 -0.0239 0.053 Uiso 1 1 d R . . O2W O 0.4043(2) 0.3869(3) -0.18209(19) 0.0249(5) Uani 1 1 d . . . H2WB H 0.4035 0.4294 -0.2433 0.037 Uiso 1 1 d R . . H2WA H 0.4021 0.4749 -0.1443 0.037 Uiso 1 1 d R . . N1 N 0.8004(2) 0.1809(4) 0.0079(2) 0.0212(6) Uani 1 1 d . . . C1 C 0.9001(3) 0.2590(4) -0.0174(3) 0.0270(7) Uani 1 1 d . . . H1 H 0.8787 0.3308 -0.0829 0.032 Uiso 1 1 calc R . . C2 C 1.0325(4) 0.2384(5) 0.0487(4) 0.0353(9) Uani 1 1 d . . . H2 H 1.0989 0.2927 0.0273 0.042 Uiso 1 1 calc R . . C3 C 1.0645(3) 0.1358(5) 0.1471(3) 0.0359(9) Uani 1 1 d . . . H3 H 1.1531 0.1203 0.1939 0.043 Uiso 1 1 calc R . . C4 C 0.9632(3) 0.0564(5) 0.1751(3) 0.0310(8) Uani 1 1 d . . . H4 H 0.9828 -0.0115 0.2421 0.037 Uiso 1 1 calc R . . C5 C 0.8319(3) 0.0782(4) 0.1032(3) 0.0208(6) Uani 1 1 d . . . C6 C 0.7201(3) -0.0197(4) 0.1247(3) 0.0205(6) Uani 1 1 d . . . H6A H 0.7580 -0.0982 0.1908 0.025 Uiso 1 1 calc R . . H6B H 0.6766 -0.0974 0.0593 0.025 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 Co1 0.0186(2) 0.0180(2) 0.0140(2) 0.00010(15) 0.00714(17) -0.00044(15) P1 0.0196(4) 0.0177(4) 0.0138(4) -0.0006(3) 0.0078(3) 0.0002(3) O1 0.0257(11) 0.0209(11) 0.0178(11) 0.0011(8) 0.0113(9) 0.0037(9) O2 0.0237(11) 0.0301(12) 0.0175(11) -0.0057(9) 0.0097(9) -0.0058(10) O3 0.0249(11) 0.0211(11) 0.0223(11) -0.0048(9) 0.0112(9) -0.0046(9) O1W 0.0299(13) 0.0245(12) 0.0525(16) -0.0019(11) 0.0162(12) 0.0052(10) O2W 0.0281(12) 0.0254(12) 0.0237(11) 0.0054(9) 0.0120(9) 0.0019(9) N1 0.0191(13) 0.0244(14) 0.0206(13) -0.0025(11) 0.0077(10) -0.0007(11) C1 0.0252(17) 0.0278(18) 0.0308(19) 0.0011(13) 0.0133(14) -0.0026(13) C2 0.0220(17) 0.036(2) 0.049(2) -0.0059(17) 0.0142(16) -0.0073(15) C3 0.0189(16) 0.040(2) 0.043(2) -0.0079(17) 0.0024(15) 0.0024(15) C4 0.0271(17) 0.0349(19) 0.0273(18) 0.0031(15) 0.0047(14) 0.0065(15) C5 0.0220(15) 0.0208(15) 0.0203(15) -0.0058(12) 0.0083(12) 0.0021(12) C6 0.0244(16) 0.0202(15) 0.0184(15) 0.0019(12) 0.0094(12) 0.0051(12) _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 Co1 O2 2.036(2) 4_565 ? Co1 O1 2.056(2) . ? Co1 O3 2.062(2) 3_655 ? Co1 N1 2.166(3) . ? Co1 O2W 2.194(2) . ? Co1 O1W 2.262(2) . ? Co1 H1WB 2.0162 . ? P1 O2 1.516(2) . ? P1 O3 1.525(2) . ? P1 O1 1.538(2) . ? P1 C6 1.810(3) . ? O2 Co1 2.036(2) 4_566 ? O3 Co1 2.062(2) 3_655 ? O1W H1WA 0.9002 . ? O1W H1WB 0.6597 . ? O2W H2WB 0.8200 . ? O2W H2WA 0.8040 . ? N1 C1 1.341(4) . ? N1 C5 1.345(4) . ? C1 C2 1.377(5) . ? C1 H1 0.9300 . ? C2 C3 1.375(6) . ? C2 H2 0.9300 . ? C3 C4 1.379(5) . ? C3 H3 0.9300 . ? C4 C5 1.387(4) . ? C4 H4 0.9300 . ? C5 C6 1.498(4) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? 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 Co1 O1 171.24(9) 4_565 . ? O2 Co1 O3 92.84(9) 4_565 3_655 ? O1 Co1 O3 95.92(8) . 3_655 ? O2 Co1 N1 90.03(9) 4_565 . ? O1 Co1 N1 89.02(9) . . ? O3 Co1 N1 97.71(9) 3_655 . ? O2 Co1 O2W 91.26(8) 4_565 . ? O1 Co1 O2W 88.18(8) . . ? O3 Co1 O2W 92.31(8) 3_655 . ? N1 Co1 O2W 169.83(9) . . ? O2 Co1 O1W 83.90(9) 4_565 . ? O1 Co1 O1W 87.35(9) . . ? O3 Co1 O1W 174.21(9) 3_655 . ? N1 Co1 O1W 87.11(10) . . ? O2W Co1 O1W 83.00(9) . . ? O2 Co1 H1WB 89.6 4_565 . ? O1 Co1 H1WB 81.8 . . ? O3 Co1 H1WB 169.0 3_655 . ? N1 Co1 H1WB 71.6 . . ? O2W Co1 H1WB 98.3 . . ? O1W Co1 H1WB 16.5 . . ? O2 P1 O3 111.72(12) . . ? O2 P1 O1 110.54(13) . . ? O3 P1 O1 111.18(12) . . ? O2 P1 C6 108.87(14) . . ? O3 P1 C6 107.26(14) . . ? O1 P1 C6 107.07(13) . . ? P1 O1 Co1 125.17(12) . . ? P1 O2 Co1 136.46(14) . 4_566 ? P1 O3 Co1 142.19(13) . 3_655 ? Co1 O1W H1WA 109.0 . . ? Co1 O1W H1WB 60.2 . . ? H1WA O1W H1WB 127.1 . . ? Co1 O2W H2WB 109.5 . . ? Co1 O2W H2WA 105.2 . . ? H2WB O2W H2WA 104.0 . . ? C1 N1 C5 118.1(3) . . ? C1 N1 Co1 117.7(2) . . ? C5 N1 Co1 123.6(2) . . ? N1 C1 C2 123.3(3) . . ? N1 C1 H1 118.3 . . ? C2 C1 H1 118.3 . . ? C3 C2 C1 118.6(3) . . ? C3 C2 H2 120.7 . . ? C1 C2 H2 120.7 . . ? C2 C3 C4 118.9(3) . . ? C2 C3 H3 120.6 . . ? C4 C3 H3 120.6 . . ? C3 C4 C5 119.8(3) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? N1 C5 C4 121.4(3) . . ? N1 C5 C6 117.1(3) . . ? C4 C5 C6 121.4(3) . . ? C5 C6 P1 116.4(2) . . ? C5 C6 H6A 108.2 . . ? P1 C6 H6A 108.2 . . ? C5 C6 H6B 108.2 . . ? P1 C6 H6B 108.2 . . ? H6A C6 H6B 107.3 . . ? 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 P1 O1 Co1 133.11(15) . . . . ? O3 P1 O1 Co1 -102.20(16) . . . . ? C6 P1 O1 Co1 14.7(2) . . . . ? O3 Co1 O1 P1 52.35(16) 3_655 . . . ? N1 Co1 O1 P1 -45.29(16) . . . . ? O2W Co1 O1 P1 144.48(16) . . . . ? O1W Co1 O1 P1 -132.45(16) . . . . ? O3 P1 O2 Co1 -13.0(3) . . . 4_566 ? O1 P1 O2 Co1 111.4(2) . . . 4_566 ? C6 P1 O2 Co1 -131.3(2) . . . 4_566 ? O2 P1 O3 Co1 -130.6(2) . . . 3_655 ? O1 P1 O3 Co1 105.4(2) . . . 3_655 ? C6 P1 O3 Co1 -11.3(3) . . . 3_655 ? O2 Co1 N1 C1 33.5(2) 4_565 . . . ? O1 Co1 N1 C1 -137.8(2) . . . . ? O3 Co1 N1 C1 126.4(2) 3_655 . . . ? O2W Co1 N1 C1 -63.8(6) . . . . ? O1W Co1 N1 C1 -50.4(2) . . . . ? O2 Co1 N1 C5 -155.8(2) 4_565 . . . ? O1 Co1 N1 C5 32.9(2) . . . . ? O3 Co1 N1 C5 -62.9(2) 3_655 . . . ? O2W Co1 N1 C5 106.9(5) . . . . ? O1W Co1 N1 C5 120.3(2) . . . . ? C5 N1 C1 C2 0.4(5) . . . . ? Co1 N1 C1 C2 171.7(3) . . . . ? N1 C1 C2 C3 -1.5(5) . . . . ? C1 C2 C3 C4 0.6(5) . . . . ? C2 C3 C4 C5 1.2(5) . . . . ? C1 N1 C5 C4 1.5(4) . . . . ? Co1 N1 C5 C4 -169.2(2) . . . . ? C1 N1 C5 C6 -175.2(3) . . . . ? Co1 N1 C5 C6 14.1(4) . . . . ? C3 C4 C5 N1 -2.3(5) . . . . ? C3 C4 C5 C6 174.3(3) . . . . ? N1 C5 C6 P1 -64.3(3) . . . . ? C4 C5 C6 P1 119.0(3) . . . . ? O2 P1 C6 C5 -71.7(3) . . . . ? O3 P1 C6 C5 167.3(2) . . . . ? O1 P1 C6 C5 47.9(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1WB N1 0.66 2.45 3.052(4) 153.0 . O2W H2WB O3 0.82 1.93 2.698(3) 157 4_565 O2W H2WA O1 0.80 2.16 2.943(3) 164 3_665 O1W H1WA O1 0.90 1.83 2.717(3) 167 3_665 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.512 _refine_diff_density_min -0.348 _refine_diff_density_rms 0.085 # Attachment 'Co-2.CIF' data_Co_2pmp2 _database_code_depnum_ccdc_archive 'CCDC 707410' _audit_creation_method TOPAS _chemical_name_systematic ; Rubidiumpentamethylcyclopentadienide ; _chemical_name_common Rubidiumpentamethylcyclopentadienide _chemical_formula_moiety 'C6 H8 N O4 P Co' _chemical_formula_sum 'C6 H6 N O3 P Co' _chemical_formula_weight 248.04 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz '-x, -y, -z' '-x+1/2, y+1/2, -z+1/2' 'x, y, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 8.85200(21) _cell_length_b 7.89607(13) _cell_length_c 12.79133(31) _cell_angle_alpha 90 _cell_angle_beta 112.2063(13) _cell_angle_gamma 90 _cell_volume 827.749(32) _cell_formula_units_Z 4 _cell_measurement_temperature 298 _exptl_crystal_description 'microcrystalline powder' _exptl_crystal_colour purple _exptl_crystal_density_diffrn 1.990 _exptl_absorpt_coefficient_mu 20.7 loop_ _atom_site_label _atom_site_type_symbol _atom_site_symmetry_multiplicity _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_B_iso_or_equiv O4 O 4 0.8860(13) 0.51920(94) 0.37263(64) 1 1.270(82) Co Co 4 0.79322(30) 0.76034(36) 0.40063(17) 1 2.729(76) C1 C 4 -0.29571(25) 0.89034(33) 0.59986(18) 1 1.270(82) N2 N 4 -0.35991(30) 0.79996(51) 0.49934(22) 1 1.270(82) C3 C 4 -0.51029(46) 0.70589(52) 0.47130(23) 1 1.270(82) C4 C 4 -0.59255(32) 0.70360(52) 0.54620(31) 1 1.270(82) C5 C 4 -0.52727(33) 0.79341(60) 0.64985(20) 1 1.270(82) C6 C 4 -0.37927(42) 0.88851(46) 0.67711(22) 1 1.270(82) C7 C 4 -0.13761(60) 0.99173(73) 0.62717(32) 1 1.270(82) P P 4 0.04380(63) 0.86819(46) 0.64668(40) 1 1.270(82) O1 O 4 0.1821(11) 0.0111(11) 0.67597(67) 1 1.270(82) O2 O 4 0.10044(98) 0.7826(12) 0.75437(63) 1 1.270(82) O3 O 4 0.00270(85) 0.7688(11) 0.54579(63) 1 1.270(82) # Powder diffraction data for histogram 1 #============================================================================== # 4. INSTRUMENT CHARACTERIZATION _exptl_special_details ; ? ; # if regions of the data are excluded, the reason(s) are supplied here: _pd_proc_info_excluded_regions ; ? ; # The following item is used to identify the equipment used to record # the powder pattern when the diffractogram was measured at a laboratory # other than the authors' home institution, e.g. when neutron or synchrotron # radiation is used. _pd_instr_location ; 'Beamline X16C, NSLS, BNL, USA' ; _pd_calibration_special_details # description of the method used # to calibrate the instrument ; 'Standard Reference Materials NIST SRM1976, Alumina Plate' ; _diffrn_ambient_temperature 298 _diffrn_source ? _diffrn_source_target ? _diffrn_source_type Synchrotron _diffrn_measurement_device_type ? _diffrn_detector ; 1-crystal analyzer with szintillation counters ; _diffrn_detector_type ? # make or model of detector _pd_meas_scan_method step _pd_meas_special_details ; ? ; # The following two items identify the program(s) used (if appropriate). _computing_data_collection ? _computing_data_reduction ? # Describe any processing performed on the data, prior to refinement. # For example: a manual Lp correction or a precomputed absorption correction _pd_proc_info_data_reduction binning # The following item is used for angular dispersive measurements only. _diffrn_radiation_monochromator 'silicon double monocromator' # The following items are used to define the size of the instrument. # Not all distances are appropriate for all instrument types. _pd_instr_dist_src/mono ? _pd_instr_dist_mono/spec ? _pd_instr_dist_src/spec ? _pd_instr_dist_spec/anal ? _pd_instr_dist_anal/detc ? _pd_instr_dist_spec/detc ? # 5. Specimen size and mounting information # The next three fields give the specimen dimensions in mm. The equatorial # plane contains the incident and diffracted beam. _pd_spec_size_axial ? # perpendicular to # equatorial plane _pd_spec_size_equat ? # parallel to # scattering vector # in transmission _pd_spec_size_thick ? # parallel to # scattering vector # in reflection _pd_spec_mounting # This field should be # used to give details of the # container. ; '0.5 mm glass capillary' ; _pd_spec_mount_mode transmission _pd_spec_shape cylinder _diffrn_radiation_probe X-ray _diffrn_radiation_polarisn_ratio '100% polarized' _diffrn_radiation_wavelength 0.69840(2) _diffrn_radiation_type synchrotron _refine_ls_number_parameters 67 _pd_proc_ls_prof_R_factor 0.0629 _pd_proc_ls_prof_wR_factor 0.0724 _pd_proc_ls_prof_wR_expected 0.0128 _refine_ls_R_Fsqd_factor 0.0299 _refine_ls_shift/su_max 'not given' _refine_ls_shift/su_mean 'not given' _pd_proc_ls_background_function ; 'Chebyshev polynomial' ; _exptl_absorpt_process_details ; ? ; _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _pd_proc_ls_profile_function ; Fundamental parameters ; _pd_proc_ls_peak_cutoff 0.00100 _pd_proc_info_datetime ? _pd_calc_method 'Rietveld Refinement' #---- raw/calc data loop ----- _pd_meas_2theta_range_min 3.0 _pd_meas_2theta_range_max 35.0 _pd_meas_2theta_range_inc 0.005 _pd_proc_2theta_range_min 3.0 _pd_proc_2theta_range_max 35.0 _pd_proc_2theta_range_inc 0.005 _reflns_number_total 554 _reflns_limit_h_min ? _reflns_limit_h_max ? _reflns_limit_k_min ? _reflns_limit_k_max ? _reflns_limit_l_min ? _reflns_limit_l_max ? _reflns_d_resolution_high ? _reflns_d_resolution_low ? #====================================================================== #End of Crystallographic Information File # Attachment 'Co-3.CIF' data_Co_2pmp _database_code_depnum_ccdc_archive 'CCDC 707411' _audit_creation_method TOPAS _chemical_name_systematic ; Rubidiumpentamethylcyclopentadienide ; _chemical_name_common Rubidiumpentamethylcyclopentadienide _chemical_formula_moiety 'C6 H6 N O3 P Co' _chemical_formula_sum 'C6 H6 N O3 P Co' _chemical_formula_weight 230.025 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz '-x, -y, -z' '-x+1/2, y+1/2, -z+1/2' 'x, y, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 9.84502(34) _cell_length_b 8.89545(40) _cell_length_c 9.67324(43) _cell_angle_alpha 90 _cell_angle_beta 112.3307(22) _cell_angle_gamma 90 _cell_volume 783.612(57) _cell_formula_units_Z 4 _cell_measurement_temperature 298 _exptl_crystal_description 'microcrystalline powder' _exptl_crystal_colour blue _exptl_crystal_density_diffrn 1.949 _exptl_absorpt_coefficient_mu 21.7 loop_ _atom_site_label _atom_site_type_symbol _atom_site_symmetry_multiplicity _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_B_iso_or_equiv Co Co 0 0.27899(31) 0.36621(33) 0.43265(31) 1 1.411(94) C1 C 0 0.32310(24) 0.48839(40) 0.74829(25) 1 0.000(95) N2 N 0 0.21694(32) 0.42451(50) 0.61958(31) 1 0.000(95) C3 C 0 0.08559(48) 0.38102(50) 0.61920(36) 1 0.000(95) C4 C 0 0.05395(33) 0.39837(54) 0.74472(41) 1 0.000(95) C5 C 0 0.15866(37) 0.45962(54) 0.87423(33) 1 0.000(95) C6 C 0 0.29319(43) 0.50517(44) 0.87525(40) 1 0.000(95) C7 C 0 0.46905(72) 0.54044(73) 0.74656(47) 1 0.000(95) P P 0 0.56856(58) 0.37502(65) 0.69218(53) 1 0.000(95) O1 O 0 0.7111(11) 0.4584(11) 0.68726(99) 1 0.000(95) O2 O 0 0.6254(10) 0.2716(12) 0.8277(12) 1 0.000(95) O3 O 0 0.4816(11) 0.31110(96) 0.5484(11) 1 0.000(95) # Powder diffraction data for histogram 1 #============================================================================== # 4. INSTRUMENT CHARACTERIZATION _exptl_special_details ; ? ; # if regions of the data are excluded, the reason(s) are supplied here: _pd_proc_info_excluded_regions ; ? ; # The following item is used to identify the equipment used to record # the powder pattern when the diffractogram was measured at a laboratory # other than the authors' home institution, e.g. when neutron or synchrotron # radiation is used. _pd_instr_location ; 'Beamline X16C, NSLS, BNL, USA' ; _pd_calibration_special_details # description of the method used # to calibrate the instrument ; 'Standard Reference Materials NIST SRM1976, Alumina Plate' ; _diffrn_ambient_temperature 298 _diffrn_source ? _diffrn_source_target ? _diffrn_source_type Synchrotron _diffrn_measurement_device_type ? _diffrn_detector ; 1-crystal analyzer with szintillation counters ; _diffrn_detector_type ? # make or model of detector _pd_meas_scan_method step _pd_meas_special_details ; ? ; # The following two items identify the program(s) used (if appropriate). _computing_data_collection ? _computing_data_reduction ? # Describe any processing performed on the data, prior to refinement. # For example: a manual Lp correction or a precomputed absorption correction _pd_proc_info_data_reduction binning # The following item is used for angular dispersive measurements only. _diffrn_radiation_monochromator 'silicon double monocromator' # The following items are used to define the size of the instrument. # Not all distances are appropriate for all instrument types. _pd_instr_dist_src/mono ? _pd_instr_dist_mono/spec ? _pd_instr_dist_src/spec ? _pd_instr_dist_spec/anal ? _pd_instr_dist_anal/detc ? _pd_instr_dist_spec/detc ? # 5. Specimen size and mounting information # The next three fields give the specimen dimensions in mm. The equatorial # plane contains the incident and diffracted beam. _pd_spec_size_axial ? # perpendicular to # equatorial plane _pd_spec_size_equat ? # parallel to # scattering vector # in transmission _pd_spec_size_thick ? # parallel to # scattering vector # in reflection _pd_spec_mounting # This field should be # used to give details of the # container. ; '0.5 mm glass capillary' ; _pd_spec_mount_mode transmission _pd_spec_shape cylinder _diffrn_radiation_probe X-ray _diffrn_radiation_polarisn_ratio '100% polarized' _diffrn_radiation_wavelength 0.69840(2) _diffrn_radiation_type synchrotron _refine_ls_number_parameters 74 _pd_proc_ls_prof_R_factor 0.0574 _pd_proc_ls_prof_wR_factor 0.0701 _pd_proc_ls_prof_wR_expected 0.0135 _refine_ls_R_Fsqd_factor 0.0168 _refine_ls_shift/su_max 'not given' _refine_ls_shift/su_mean 'not given' _pd_proc_ls_background_function ; 'Chebyshev polynomial' ; _exptl_absorpt_process_details ; ? ; _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _pd_proc_ls_profile_function ; Fundamental parameters ; _pd_proc_ls_peak_cutoff 0.00100 _pd_proc_info_datetime ? _pd_calc_method 'Rietveld Refinement' #---- raw/calc data loop ----- _pd_meas_2theta_range_min 3.0 _pd_meas_2theta_range_max 35.0 _pd_meas_2theta_range_inc 0.005 _pd_proc_2theta_range_min 3.0 _pd_proc_2theta_range_max 35.0 _pd_proc_2theta_range_inc 0.005 _reflns_number_total 523 _reflns_limit_h_min ? _reflns_limit_h_max ? _reflns_limit_k_min ? _reflns_limit_k_max ? _reflns_limit_l_min ? _reflns_limit_l_max ? _reflns_d_resolution_high ? _reflns_d_resolution_low ? #====================================================================== #End of Crystallographic Information File