#------------------------------------------------------------------------------ #$Date: 2025-08-19 11:01:59 +0100 (Tue, 19 Aug 2025) $ #$Revision: 301802 $ #$URL: svn://www.crystallography.net/cod/cif/2/10/50/2105013.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_2105013 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_paper_doi 10.1107/S0108768111045897 _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 11 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yb' _symmetry_space_group_name_H-M 'P 1 21/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 100.800(10) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 12.3190(10) _cell_length_b 12.5400(10) _cell_length_c 8.0620(10) _cell_measurement_reflns_used 2937 _cell_measurement_temperature 263(2) _cell_measurement_theta_max 27.48 _cell_measurement_theta_min 1.00 _cell_volume 1223.4(2) _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 263(2) _diffrn_detector_area_resol_mean 18 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _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 0.0429 _diffrn_reflns_av_sigmaI/netI 0.0564 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 5059 _diffrn_reflns_theta_full 26.50 _diffrn_reflns_theta_max 26.50 _diffrn_reflns_theta_min 1.68 _diffrn_standards_decay_% <2 _exptl_absorpt_coefficient_mu 0.877 _exptl_absorpt_correction_T_max 0.9174 _exptl_absorpt_correction_T_min 0.7789 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Scalepack (Otwinowski & Minor, 2006)' _exptl_crystal_colour 'pale green' _exptl_crystal_density_diffrn 1.485 _exptl_crystal_density_method 'not measured' _exptl_crystal_description 'elongated parallelepiped' _exptl_crystal_F_000 580 _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _refine_diff_density_max 0.630 _refine_diff_density_min -0.321 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 194 _refine_ls_number_reflns 2651 _refine_ls_number_restraints 35 _refine_ls_restrained_S_all 1.091 _refine_ls_R_factor_all 0.1025 _refine_ls_R_factor_gt 0.0561 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0900P)^2^+0.0030P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1446 _refine_ls_wR_factor_ref 0.1676 _reflns_number_gt 1676 _reflns_number_total 2651 _reflns_threshold_expression >2sigma(I) _cod_data_source_file hw5018.cif _cod_data_source_block 263K_II _cod_original_sg_symbol_H-M 'P 21/m' _cod_database_code 2105013 _cod_database_fobs_code 2105013 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' 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 0.0732(3) 0.2500 0.7372(5) 0.0759(12) Uani d SU 1 2 . . C C1 0.0358(4) 0.3436(4) 0.6494(6) 0.0940(16) Uani d U 1 1 . . H H1A -0.0416 0.3552 0.6531 0.113 Uiso calc R 1 1 . . H H1B 0.0432 0.3374 0.5322 0.113 Uiso calc R 1 1 . . C C2 0.1034(5) 0.4350(4) 0.7306(6) 0.0970(16) Uani d U 1 1 . . H H2A 0.0759 0.5016 0.6775 0.116 Uiso calc R 1 1 . . H H2B 0.1001 0.4388 0.8497 0.116 Uiso calc R 1 1 . . O O2 0.2141(3) 0.4170(3) 0.7092(4) 0.0908(10) Uani d U 1 1 . . C C3 0.2890(5) 0.4899(4) 0.7963(6) 0.1136(17) Uani d U 1 1 . . H H3A 0.2765 0.4984 0.9109 0.136 Uiso calc R 1 1 . . H H3B 0.2798 0.5588 0.7408 0.136 Uiso calc R 1 1 . . C C4 0.4022(5) 0.4489(4) 0.7985(6) 0.1098(18) Uani d DU 1 1 . . H H4A 0.4070 0.4239 0.6862 0.132 Uiso calc R 1 1 A 1 H H4B 0.4543 0.5072 0.8260 0.132 Uiso calc R 1 1 A 1 O O3 0.434(3) 0.364(3) 0.916(5) 0.108(5) Uani d PDU 0.50 1 . 1 C C5 0.5228(7) 0.2885(8) 0.9435(13) 0.106(4) Uani d PDU 0.50 1 . 1 H H5A 0.5679 0.3077 0.8616 0.127 Uiso calc PR 0.50 1 . 1 H H5B 0.5660 0.3077 1.0527 0.127 Uiso calc PR 0.50 1 . 1 O O3' 0.415(3) 0.357(3) 0.904(5) 0.108(5) Uani d PDU 0.50 1 . 2 C C6 0.4977(8) 0.3082(9) 0.8274(12) 0.103(4) Uani d PDU 0.50 1 . 2 H H6A 0.5694 0.3326 0.8859 0.124 Uiso calc PR 0.50 1 . 2 H H6B 0.4884 0.3326 0.7115 0.124 Uiso calc PR 0.50 1 . 2 Ni Ni 0.25452(4) 0.2500 0.26993(7) 0.0445(3) Uani d S 1 2 . . O O6 0.2787(3) 0.2500 0.5268(4) 0.0458(8) Uani d SD 1 2 . . H H6 0.253(3) 0.203(2) 0.581(4) 0.069 Uiso d D 1 1 . . O O7 0.2385(3) 0.2500 0.0157(4) 0.125(2) Uani d SD 1 2 . . H H7 0.184(4) 0.2500 -0.056(8) 0.187 Uiso d SD 1 2 . . H H7' 0.291(4) 0.2500 -0.034(9) 0.187 Uiso d SD 1 2 . . O O8 0.1369(2) 0.3651(2) 0.2598(4) 0.0617(7) Uani d D 1 1 . . H H8C 0.078(2) 0.355(3) 0.194(5) 0.093 Uiso d D 1 1 . . H H8D 0.154(3) 0.4283(18) 0.255(6) 0.093 Uiso d D 1 1 . . O O9 0.3733(2) 0.1360(3) 0.2817(4) 0.0839(10) Uani d D 1 1 . . H H9C 0.435(2) 0.156(4) 0.322(7) 0.126 Uiso d D 1 1 . . H H9D 0.363(4) 0.076(2) 0.307(7) 0.126 Uiso d D 1 1 . . N N1 0.6341(5) 0.2500 0.4731(7) 0.0863(19) Uani d S 1 2 . . O O12 0.5848(3) 0.3359(3) 0.4549(5) 0.1090(13) Uani d . 1 1 . . O O13 0.7343(4) 0.2500 0.5209(8) 0.135(2) Uani d S 1 2 . . N N2 -0.1111(4) 0.2500 0.0229(7) 0.0814(16) Uani d S 1 2 . . O O15 -0.0646(3) 0.3361(3) 0.0597(5) 0.1003(12) Uani d . 1 1 . . O O16 -0.2043(4) 0.2500 -0.0670(8) 0.124(2) Uani d S 1 2 . . O O18 0.2358(3) 0.5578(3) 0.2543(6) 0.1077(13) Uani d D 1 1 . . H H18C 0.249(5) 0.585(4) 0.344(3) 0.162 Uiso d D 1 1 . . H H18D 0.204(5) 0.598(4) 0.182(5) 0.162 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 0.072(3) 0.109(3) 0.049(2) 0.000 0.016(2) 0.000 C1 0.090(3) 0.131(5) 0.063(3) 0.061(3) 0.017(2) 0.026(3) C2 0.129(4) 0.093(4) 0.082(3) 0.054(3) 0.053(3) 0.020(3) O2 0.133(3) 0.069(2) 0.085(2) -0.0052(19) 0.056(2) -0.0161(16) C3 0.195(5) 0.065(4) 0.097(4) -0.039(3) 0.071(4) -0.023(3) C4 0.146(4) 0.099(4) 0.100(4) -0.085(3) 0.062(4) -0.041(3) O3 0.084(11) 0.089(4) 0.169(5) -0.044(7) 0.068(7) -0.041(4) C5 0.049(5) 0.163(11) 0.112(7) -0.042(4) 0.032(5) -0.062(7) O3' 0.084(11) 0.089(4) 0.169(5) -0.044(7) 0.068(7) -0.041(4) C6 0.073(7) 0.188(11) 0.058(5) -0.013(6) 0.034(5) 0.011(7) Ni 0.0389(4) 0.0612(5) 0.0335(4) 0.000 0.0069(3) 0.000 O6 0.0495(19) 0.058(2) 0.0310(16) 0.000 0.0105(14) 0.000 O7 0.048(2) 0.299(7) 0.0268(19) 0.000 0.0072(18) 0.000 O8 0.0528(16) 0.0510(16) 0.0740(18) 0.0006(13) -0.0068(13) 0.0094(15) O9 0.0516(16) 0.106(3) 0.087(2) 0.0219(17) -0.0044(16) -0.041(2) N1 0.053(4) 0.149(7) 0.055(3) 0.000 0.005(3) 0.000 O12 0.070(2) 0.112(3) 0.135(3) -0.004(2) -0.007(2) 0.041(3) O13 0.052(3) 0.175(6) 0.162(6) 0.000 -0.022(3) 0.000 N2 0.060(3) 0.090(5) 0.087(4) 0.000 -0.005(3) 0.000 O15 0.076(2) 0.082(3) 0.129(3) 0.0089(19) -0.016(2) -0.029(2) O16 0.063(3) 0.115(4) 0.166(6) 0.000 -0.050(3) 0.000 O18 0.108(3) 0.049(2) 0.169(4) 0.0017(17) 0.033(3) 0.009(2) 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 C1 O1 C1 4_565 . 113.6(5) no O1 C1 C2 . . 108.5(4) no O1 C1 H1A . . 110.0 no C2 C1 H1A . . 110.0 no O1 C1 H1B . . 110.0 no C2 C1 H1B . . 110.0 no H1A C1 H1B . . 108.4 no O2 C2 C1 . . 107.0(4) no O2 C2 H2A . . 110.3 no C1 C2 H2A . . 110.3 no O2 C2 H2B . . 110.3 no C1 C2 H2B . . 110.3 no H2A C2 H2B . . 108.6 no C3 O2 C2 . . 113.2(4) no O2 C3 C4 . . 108.1(4) no O2 C3 H3A . . 110.1 no C4 C3 H3A . . 110.1 no O2 C3 H3B . . 110.1 no C4 C3 H3B . . 110.1 no H3A C3 H3B . . 108.4 no O3' C4 O3 . . 10(4) no O3' C4 C3 . . 106.5(11) no O3 C4 C3 . . 113.8(10) no O3' C4 H4A . . 106.1 no O3 C4 H4A . . 108.8 no C3 C4 H4A . . 108.8 no O3' C4 H4B . . 118.7 no O3 C4 H4B . . 108.8 no C3 C4 H4B . . 108.8 no H4A C4 H4B . . 107.7 no C4 O3 C5 . . 134.4(12) no C5 C5 O3 4_565 . 131(2) no C5 C5 H5A 4_565 . 104.4 no O3 C5 H5A . . 104.4 no C5 C5 H5B 4_565 . 104.4 no O3 C5 H5B . . 104.4 no H5A C5 H5B . . 105.6 no C4 O3' C6 . . 95.6(9) no O3' C6 C6 . 4_565 115.5(15) no O3' C6 H6A . . 108.4 no C6 C6 H6A 4_565 . 108.4 no O3' C6 H6B . . 108.4 no C6 C6 H6B 4_565 . 108.4 no H6A C6 H6B . . 107.5 no O7 Ni O6 . . 177.23(14) no O7 Ni O8 . 4_565 91.48(12) no O6 Ni O8 . 4_565 90.48(10) no O7 Ni O8 . . 91.48(12) no O6 Ni O8 . . 90.48(10) no O8 Ni O8 4_565 . 90.25(15) no O7 Ni O9 . 4_565 88.85(13) no O6 Ni O9 . 4_565 89.18(12) no O8 Ni O9 4_565 4_565 179.40(11) no O8 Ni O9 . 4_565 90.24(14) no O7 Ni O9 . . 88.85(13) no O6 Ni O9 . . 89.18(12) no O8 Ni O9 4_565 . 90.24(14) no O8 Ni O9 . . 179.40(11) no O9 Ni O9 4_565 . 89.3(2) no Ni O6 H6 . . 123(2) no Ni O7 H7 . . 130(6) no Ni O7 H7' . . 124(6) no H7 O7 H7' . . 106(4) no Ni O8 H8C . . 116(3) no Ni O8 H8D . . 120(3) no H8C O8 H8D . . 108(3) no Ni O9 H9C . . 114(4) no Ni O9 H9D . . 122(4) no H9C O9 H9D . . 112(4) no O13 N1 O12 . 4_565 118.9(3) no O13 N1 O12 . . 118.9(3) no O12 N1 O12 4_565 . 122.0(6) no O15 N2 O15 . 4_565 122.3(6) no O15 N2 O16 . . 118.7(3) no O15 N2 O16 4_565 . 118.7(3) no H18C O18 H18D . . 112(4) 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 4_565 1.403(5) no O1 C1 . 1.403(5) no C1 C2 . 1.494(7) no C1 H1A . 0.9700 no C1 H1B . 0.9700 no C2 O2 . 1.424(5) no C2 H2A . 0.9700 no C2 H2B . 0.9700 no O2 C3 . 1.393(6) no C3 C4 . 1.483(7) no C3 H3A . 0.9700 no C3 H3B . 0.9700 no C4 O3' . 1.421(10) no C4 O3 . 1.426(9) no C4 H4A . 0.9700 no C4 H4B . 0.9700 no O3 C5 . 1.437(9) no C5 C5 4_565 0.96(2) no C5 H5A . 0.9700 no C5 H5B . 0.9700 no O3' C6 . 1.427(10) no C6 C6 4_565 1.46(2) no C6 H6A . 0.9700 no C6 H6B . 0.9700 no Ni O7 . 2.022(3) no Ni O6 . 2.036(3) no Ni O8 4_565 2.036(3) no Ni O8 . 2.036(3) no Ni O9 4_565 2.035(3) no Ni O9 . 2.035(3) no O6 H6 . 0.838(17) no O7 H7 . 0.80(2) no O7 H7' . 0.83(2) no O8 H8C . 0.823(18) no O8 H8D . 0.822(18) no O9 H9C . 0.810(18) no O9 H9D . 0.798(19) no N1 O13 . 1.222(7) no N1 O12 4_565 1.231(4) no N1 O12 . 1.231(4) no N2 O15 . 1.232(4) no N2 O15 4_565 1.232(4) no N2 O16 . 1.237(6) no O18 H18C . 0.793(19) no O18 H18D . 0.813(19) 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 4_565 0.838(17) 1.929(19) 2.760(4) 171(3) O7 H7 O1 1_554 0.80(2) 1.94(3) 2.734(5) 168(8) O7 H7' O3 1_554 0.83(2) 2.36(5) 3.04(4) 140(3) O8 H8C O15 . 0.823(18) 1.899(19) 2.719(4) 174(5) O8 H8D O18 . 0.822(18) 1.92(2) 2.712(5) 163(4) O9 H9C O12 4_565 0.810(18) 1.96(3) 2.739(4) 162(5) O9 H9D O18 4_565 0.798(19) 2.28(3) 2.947(5) 141(5) O18 H18C O12 3_666 0.793(19) 2.56(5) 3.196(5) 139(6) O18 H18C O13 3_666 0.793(19) 2.33(4) 2.996(6) 143(5) O18 H18D O15 3_565 0.813(19) 2.49(3) 3.260(5) 159(6) O18 H18D O16 3_565 0.813(19) 2.12(4) 2.832(5) 146(6) 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_site_symmetry_1 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag C1 O1 C1 C2 4_565 . -164.9(3) no O1 C1 C2 O2 . . 64.1(5) no C1 C2 O2 C3 . . -172.9(4) no C2 O2 C3 C4 . . 166.8(4) no O2 C3 C4 O3' . . -69(2) no O2 C3 C4 O3 . . -76(3) no O3' C4 O3 C5 . . 122(19) no C3 C4 O3 C5 . . 167(5) no C4 O3 C5 C5 . 4_565 -122(5) no O3 C4 O3' C6 . . -68(11) no C3 C4 O3' C6 . . 155(2) no C4 O3' C6 C6 . 4_565 -148.7(18) no loop_ _cod_related_entry_id _cod_related_entry_database _cod_related_entry_code 1 PubChem 168308384