#------------------------------------------------------------------------------ #$Date: 2014-10-25 18:23:10 +0100 (Sat, 25 Oct 2014) $ #$Revision: 125873 $ #$URL: svn://www.crystallography.net/cod/cif/2/10/50/2105020.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2105020 loop_ _publ_author_name 'Siegler, Maxime A.' 'Hao, Xiang' 'Parkin, Sean' 'Brock, Carolyn Pratt' _publ_section_title ; [Ni(H~2~O)~6~](NO~3~)~2~·(15-crown-5)·2H~2~O: three phase transitions and an intermediate modulated phase stable over a range of ca 40K ; _journal_issue 6 _journal_name_full 'Acta Crystallographica Section B' _journal_page_first 486 _journal_page_last 498 _journal_volume 67 _journal_year 2011 _chemical_formula_moiety 'C10 H20 O5, H12 Ni O6 2+, 2(N O3 1-), 2(H2 O)' _chemical_formula_sum 'C10 H36 N2 Ni O19' _chemical_formula_weight 547.12 _chemical_name_systematic 'hexaquanickel(II) nitrate (15-crown-5) dihydrate' _space_group_IT_number 12 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-I 2y' _symmetry_space_group_name_H-M 'I 1 2/m 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 101.48(2) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 12.370(2) _cell_length_b 12.570(2) _cell_length_c 8.1140(10) _cell_measurement_reflns_used 1456 _cell_measurement_temperature 295(2) _cell_measurement_theta_max 27.48 _cell_measurement_theta_min 1.00 _cell_volume 1236.4(3) _computing_cell_refinement 'DENZO-SMN (Nonius, 1997)' _computing_data_collection 'COLLECT (Nonius, 1997)' _computing_data_reduction 'DENZO-SMN (Nonius, 1997)' _computing_molecular_graphics 'Mercury (Macrae et al., 2008)' _computing_publication_material 'SHELX-97 and local procedures' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _diffrn_ambient_temperature 295(2) _diffrn_detector_area_resol_mean 18 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'Nonius KappaCCD diffractometer' _diffrn_measurement_method '\w scans at fixed \c = 55\%' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0375 _diffrn_reflns_av_sigmaI/netI 0.0551 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 2698 _diffrn_reflns_theta_full 27.45 _diffrn_reflns_theta_max 27.45 _diffrn_reflns_theta_min 2.33 _exptl_absorpt_coefficient_mu 0.868 _exptl_absorpt_correction_T_max 0.9579 _exptl_absorpt_correction_T_min 0.7510 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Scalepack (Otwinowski & Minor, 2006)' _exptl_crystal_colour 'pale green' _exptl_crystal_density_diffrn 1.470 _exptl_crystal_density_method 'not measured' _exptl_crystal_description 'elongated parallelepiped' _exptl_crystal_F_000 580 _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.05 _refine_diff_density_max 0.501 _refine_diff_density_min -0.379 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 138 _refine_ls_number_reflns 1473 _refine_ls_number_restraints 28 _refine_ls_restrained_S_all 1.027 _refine_ls_R_factor_all 0.0888 _refine_ls_R_factor_gt 0.0575 _refine_ls_shift/su_max 0.012 _refine_ls_shift/su_mean 0.002 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1004P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1472 _refine_ls_wR_factor_ref 0.1633 _reflns_number_gt 1037 _reflns_number_total 1473 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file hw5018.cif _[local]_cod_data_source_block 295K_I _[local]_cod_cif_authors_sg_H-M 'I 2/m' _cod_database_code 2105020 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, -y+1/2, z+1/2' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_disorder_assembly _atom_site_disorder_group O O1 -0.1767(8) 0.0000 0.4765(16) 0.102(5) Uani d PDU 0.25 1 A -1 C C1 -0.2251(9) 0.0918(8) 0.3964(12) 0.095(3) Uani d PDU 0.50 1 A -1 H H1A -0.2978 0.1015 0.4221 0.114 Uiso calc PR 0.50 1 A -1 H H1B -0.2338 0.0837 0.2756 0.114 Uiso calc PR 0.50 1 A -1 C C2 -0.1567(8) 0.1863(13) 0.452(3) 0.117(5) Uani d PDU 0.50 1 A -1 H H2A -0.1833 0.2457 0.3785 0.141 Uiso calc PR 0.50 1 A -1 H H2B -0.1641 0.2052 0.5649 0.141 Uiso calc PR 0.50 1 A -1 O O2 -0.0452(6) 0.1686(5) 0.4495(9) 0.103(2) Uani d PDU 0.50 1 A -1 C C3 0.0317(9) 0.2418(7) 0.5347(17) 0.112(3) Uani d PDU 0.50 1 A -1 H H3A 0.0233 0.2502 0.6503 0.134 Uiso calc PR 0.50 1 A -1 H H3B 0.0229 0.3107 0.4797 0.134 Uiso calc PR 0.50 1 A -1 C C4 0.1409(12) 0.1944(12) 0.527(2) 0.113(4) Uani d PDU 0.50 1 A -1 H H4A 0.1402 0.1684 0.4141 0.135 Uiso calc PR 0.50 1 A -1 H H4B 0.1978 0.2484 0.5528 0.135 Uiso calc PR 0.50 1 A -1 O O3 0.1647(7) 0.1104(7) 0.6421(12) 0.127(3) Uani d PDU 0.50 1 A -1 C C5 0.2660(14) 0.0569(18) 0.680(3) 0.140(8) Uani d PDU 0.25 1 A -1 H H5A 0.2833 0.0339 0.7961 0.169 Uiso calc PR 0.25 1 A -1 H H5B 0.3257 0.1005 0.6557 0.169 Uiso calc PR 0.25 1 A -1 C C6 0.243(3) -0.034(2) 0.564(4) 0.130(12) Uani d PDU 0.25 1 A -1 H H6A 0.3004 -0.0603 0.5232 0.156 Uiso d P 0.25 1 B -1 H H6B 0.1907 0.0020 0.4491 0.156 Uiso d P 0.25 1 C -1 Ni Ni 0.0000 0.0000 0.0000 0.0509(4) Uani d S 1 4 . . O O6 -0.0200(3) 0.0000 -0.2565(5) 0.0934(14) Uani d SD 1 2 . . H H6 0.026(3) 0.044(3) -0.273(7) 0.140 Uiso d D 1 1 . . O O8 -0.1182(2) 0.1147(2) -0.0141(4) 0.0854(8) Uani d D 1 1 . . H H8C -0.177(3) 0.107(4) -0.085(5) 0.128 Uiso d D 1 1 . . H H8D -0.109(4) 0.1780(17) -0.006(7) 0.128 Uiso d D 1 1 . . N N1 0.3744(4) 0.0000 0.2201(8) 0.0989(17) Uani d S 1 2 . . O O12 0.3259(3) 0.0843(3) 0.1927(6) 0.1318(15) Uani d . 1 1 . . O O13 0.4710(4) 0.0000 0.2916(10) 0.166(3) Uani d S 1 2 . . O O18 0.0000 0.3096(5) 0.0000 0.139(2) Uani d SD 1 2 . . H H18 0.051(6) 0.319(6) 0.084(8) 0.209 Uiso d D 1 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 O1 0.074(7) 0.142(10) 0.093(8) 0.039(17) 0.023(7) 0.03(2) C1 0.056(5) 0.164(9) 0.064(6) 0.052(4) 0.010(5) 0.028(6) C2 0.125(5) 0.121(10) 0.094(10) 0.077(6) -0.006(8) -0.010(9) O2 0.126(4) 0.083(4) 0.109(6) -0.003(3) 0.046(4) -0.020(4) C3 0.174(6) 0.072(5) 0.097(11) -0.016(5) 0.044(7) -0.016(6) C4 0.142(5) 0.120(11) 0.098(10) -0.058(7) 0.076(8) -0.016(7) O3 0.091(5) 0.126(7) 0.177(8) -0.027(4) 0.058(5) 0.015(6) C5 0.085(12) 0.23(2) 0.106(16) -0.008(11) 0.011(13) -0.068(11) C6 0.16(3) 0.143(17) 0.12(2) -0.057(14) 0.11(2) -0.024(15) Ni 0.0457(5) 0.0603(6) 0.0470(5) 0.000 0.0098(3) 0.000 O6 0.072(2) 0.158(5) 0.0523(19) 0.000 0.0182(17) 0.000 O8 0.0637(16) 0.0719(17) 0.114(2) 0.0144(13) 0.0020(14) -0.0141(17) N1 0.071(3) 0.109(5) 0.107(4) 0.000 -0.007(3) 0.000 O12 0.090(2) 0.115(3) 0.173(4) -0.011(2) -0.015(2) 0.043(3) O13 0.075(3) 0.165(6) 0.226(7) 0.000 -0.047(4) 0.000 O18 0.163(6) 0.072(3) 0.189(7) 0.000 0.051(4) 0.000 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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_3 _geom_angle _geom_angle_publ_flag O1 C1 C2 . . 110.9(11) no O1 C1 H1A . . 109.5 no C2 C1 H1A . . 109.5 no O1 C1 H1B . . 109.5 no C2 C1 H1B . . 109.5 no H1A C1 H1B . . 108.0 no O2 C2 C1 . . 112.0(11) no O2 C2 H2A . . 109.2 no C1 C2 H2A . . 109.2 no O2 C2 H2B . . 109.2 no C1 C2 H2B . . 109.2 no H2A C2 H2B . . 107.9 no C2 O2 C3 . . 117.5(8) no O2 C3 C4 . . 104.4(10) no O2 C3 H3A . . 110.9 no C4 C3 H3A . . 110.9 no O2 C3 H3B . . 110.9 no C4 C3 H3B . . 110.9 no H3A C3 H3B . . 108.9 no O3 C4 C3 . . 110.1(9) no O3 C4 H4A . . 109.6 no C3 C4 H4A . . 109.6 no O3 C4 H4B . . 109.6 no C3 C4 H4B . . 109.6 no H4A C4 H4B . . 108.1 no C5 O3 C4 . . 124.5(14) no O3 C5 C6 . . 100(2) no O3 C5 H5A . . 111.7 no C6 C5 H5A . . 111.7 no O3 C5 H5B . . 111.7 no C6 C5 H5B . . 111.7 no H5A C5 H5B . . 109.5 no C5 C6 H6A . . 116.5 no C5 C6 H6B . . 103.1 no H6A C6 H6B . . 102.3 no O8 Ni O8 . 6 89.92(18) no O8 Ni O8 . 2 90.08(18) no O8 Ni O8 6 2 180.00(15) no O8 Ni O8 . 5 180.0 no O8 Ni O8 6 5 90.07(18) no O8 Ni O8 2 5 89.93(18) no O8 Ni O6 . 5 89.85(12) no O8 Ni O6 6 5 89.85(12) no O8 Ni O6 2 5 90.15(12) no O8 Ni O6 5 5 90.15(12) no O8 Ni O6 . . 90.15(12) no O8 Ni O6 6 . 90.15(12) no O8 Ni O6 2 . 89.85(12) no O8 Ni O6 5 . 89.85(12) no O6 Ni O6 5 . 180.0 no Ni O6 H6 . . 103(4) no Ni O8 H8C . . 118(4) no Ni O8 H8D . . 127(4) no H8C O8 H8D . . 105(3) no O12 N1 O12 6 . 121.2(6) no O12 N1 O13 6 . 119.2(3) no O12 N1 O13 . . 119.2(3) no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag O1 C1 . 1.399(8) no C1 C2 . 1.476(9) no C1 H1A . 0.9700 no C1 H1B . 0.9700 no C2 O2 . 1.402(9) no C2 H2A . 0.9700 no C2 H2B . 0.9700 no O2 C3 . 1.402(7) no C3 C4 . 1.490(9) no C3 H3A . 0.9700 no C3 H3B . 0.9700 no C4 O3 . 1.402(9) no C4 H4A . 0.9700 no C4 H4B . 0.9700 no O3 C5 . 1.401(10) no C5 C6 . 1.471(10) no C5 H5A . 0.9700 no C5 H5B . 0.9700 no C6 H6A . 0.9067 no C6 H6B . 1.1141 no Ni O8 . 2.040(3) no Ni O8 6 2.040(3) no Ni O8 2 2.040(3) no Ni O8 5 2.040(3) no Ni O6 5 2.046(4) no Ni O6 . 2.046(4) no O6 H6 . 0.825(19) no O8 H8C . 0.838(19) no O8 H8D . 0.805(19) no N1 O12 6 1.216(4) no N1 O12 . 1.216(4) no N1 O13 . 1.221(7) no O18 H18 . 0.84(2) no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA O6 H6 O2 2 0.825(19) 2.17(4) 2.845(7) 140(5) O6 H6 O3 1_554 0.825(19) 2.14(3) 2.928(8) 160(5) O8 H8C O12 2 0.838(19) 1.90(2) 2.714(4) 164(5) O8 H8D O18 . 0.805(19) 2.13(3) 2.844(7) 148(5) O18 H18 O12 7 0.84(2) 2.45(4) 3.240(5) 157(7) O18 H18 O13 7 0.84(2) 2.53(8) 2.911(7) 109(7) 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_publ_flag O1 C1 C2 O2 47.1(19) no C1 C2 O2 C3 -165.6(11) no C2 O2 C3 C4 173.3(15) no O2 C3 C4 O3 -76.0(15) no C3 C4 O3 C5 -172.5(14) no C4 O3 C5 C6 -95(2) no _cod_database_fobs_code 2105020 _journal_paper_doi 10.1107/S0108768111045897