#------------------------------------------------------------------------------ #$Date: 2016-02-18 15:37:37 +0000 (Thu, 18 Feb 2016) $ #$Revision: 176729 $ #$URL: svn://www.crystallography.net/cod/cif/1/50/00/1500038.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1500038 loop_ _publ_author_name 'Carmen R. Maldonado' 'Miguel Quir\'os' 'Juan M. Salas' _publ_contact_author_address ; Departamento de Qu\'imica Inorg\'anica Facultad de Ciencias Universidad de Granada 18071 Granada SPAIN ; _publ_contact_author_email mquiros@ugr.es _publ_contact_author_fax 34-58-248526 _publ_contact_author_name 'Miguel Quir\'os' _publ_contact_author_phone 34-58-240441 _journal_name_full Polyhedron _journal_page_first 372 _journal_page_last 378 _journal_paper_doi 10.1016/j.poly.2009.06.002 _journal_volume 29 _journal_year 2010 _chemical_formula_moiety 'C16 H28 N14 Ni O4, 3(H2 O)' _chemical_formula_sum 'C16 H34 N14 Ni O7' _chemical_formula_weight 593.28 _chemical_name_systematic ; ? ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 95.215(2) _cell_angle_beta 95.770(3) _cell_angle_gamma 117.933(2) _cell_formula_units_Z 1 _cell_length_a 8.1905(19) _cell_length_b 8.2396(13) _cell_length_c 10.8651(17) _cell_measurement_reflns_used 4966 _cell_measurement_temperature 295(2) _cell_measurement_theta_max 27.9 _cell_measurement_theta_min 2.8 _cell_volume 636.5(2) _computing_cell_refinement 'Bruker SMART' _computing_data_collection 'Bruker SMART (Bruker, 1999)' _computing_data_reduction 'Bruker SAINT (Bruker, 1999)' _computing_molecular_graphics 'Xtal_GX (Hall & du Boulay, 1997)' _computing_publication_material SHELXL-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _diffrn_ambient_temperature 295(2) _diffrn_detector_area_resol_mean 8.26 _diffrn_measured_fraction_theta_full 0.990 _diffrn_measured_fraction_theta_max 0.907 _diffrn_measurement_device_type 'Bruker SMART APEX CCD system' _diffrn_measurement_method '\f and \w scans' _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 0.0260 _diffrn_reflns_av_sigmaI/netI 0.0240 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 7343 _diffrn_reflns_theta_full 26.70 _diffrn_reflns_theta_max 28.24 _diffrn_reflns_theta_min 1.91 _diffrn_standards_decay_% 0.2 _diffrn_standards_number 179 _exptl_absorpt_coefficient_mu 0.829 _exptl_absorpt_correction_T_max 0.914 _exptl_absorpt_correction_T_min 0.698 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Bruker SADABS (Bruker, 1999)' _exptl_crystal_colour pink _exptl_crystal_density_diffrn 1.548 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prismatic _exptl_crystal_F_000 312 _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.11 _refine_diff_density_max 0.582 _refine_diff_density_min -0.456 _refine_diff_density_rms 0.073 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 187 _refine_ls_number_reflns 2851 _refine_ls_number_restraints 5 _refine_ls_restrained_S_all 1.068 _refine_ls_R_factor_all 0.0424 _refine_ls_R_factor_gt 0.0413 _refine_ls_shift/su_max 0.029 _refine_ls_shift/su_mean 0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0700P)^2^+0.3000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1139 _refine_ls_wR_factor_ref 0.1147 _reflns_number_gt 2729 _reflns_number_total 2851 _reflns_threshold_expression I>2\s(I) _cod_data_source_file niendmax.cif _cod_data_source_block nienax _cod_database_code 1500038 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' 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 Ni Ni 0.5000 0.5000 0.5000 0.02831(14) Uani 1 2 d S . . N1 N 0.2052(2) 0.3169(2) 0.27040(16) 0.0352(4) Uani 1 1 d . . . N2 N 0.3688(2) 0.4646(2) 0.31403(16) 0.0353(4) Uani 1 1 d . . . N3 N 0.4351(2) 0.5807(2) 0.22773(16) 0.0337(4) Uani 1 1 d . . . C3A C 0.3042(3) 0.4972(3) 0.12627(18) 0.0293(4) Uani 1 1 d . . . N4 N 0.3024(2) 0.5552(2) 0.01151(16) 0.0344(4) Uani 1 1 d . . . C4 C 0.4531(3) 0.7314(3) -0.0115(2) 0.0453(5) Uani 1 1 d . . . H41 H 0.5410 0.7086 -0.0520 0.054 Uiso 1 1 d R . . H42 H 0.5161 0.8130 0.0666 0.054 Uiso 1 1 d R . . H43 H 0.4010 0.7884 -0.0645 0.054 Uiso 1 1 d R . . C5 C 0.1556(3) 0.4463(3) -0.08334(19) 0.0334(4) Uani 1 1 d . . . O5 O 0.1478(3) 0.4921(2) -0.18642(15) 0.0469(4) Uani 1 1 d . . . N6 N 0.0124(2) 0.2800(2) -0.05720(16) 0.0339(4) Uani 1 1 d . . . C6 C -0.1372(3) 0.1626(3) -0.1627(2) 0.0434(5) Uani 1 1 d . . . H61 H -0.1992 0.0367 -0.1466 0.052 Uiso 1 1 d R . . H62 H -0.0845 0.1667 -0.2382 0.052 Uiso 1 1 d R . . H63 H -0.2262 0.2074 -0.1725 0.052 Uiso 1 1 d R . . C7 C 0.0016(3) 0.2137(3) 0.05770(19) 0.0331(4) Uani 1 1 d . . . O7 O -0.1334(2) 0.0686(2) 0.07098(16) 0.0469(4) Uani 1 1 d . . . C7A C 0.1610(3) 0.3342(3) 0.15082(18) 0.0308(4) Uani 1 1 d . . . N1E N 0.4280(4) 0.2184(3) 0.4678(2) 0.0637(7) Uani 1 1 d . . . H11E H 0.4352 0.1771 0.5410 0.076 Uiso 1 1 d R . . H12E H 0.3101 0.1503 0.4262 0.076 Uiso 1 1 d R . . C1E C 0.5608(8) 0.2028(6) 0.3936(3) 0.0865(13) Uani 1 1 d . . . H13E H 0.5261 0.2080 0.3066 0.104 Uiso 1 1 d R . . H14E H 0.5585 0.0847 0.3981 0.104 Uiso 1 1 d R . . C2E C 0.7543(7) 0.3613(7) 0.4448(3) 0.0924(15) Uani 1 1 d . . . H23E H 0.7926 0.3514 0.5300 0.111 Uiso 1 1 d R . . H24E H 0.8435 0.3570 0.3940 0.111 Uiso 1 1 d R . . N2E N 0.7494(3) 0.5359(4) 0.4420(2) 0.0548(6) Uani 1 1 d . . . H21E H 0.7531 0.5645 0.3640 0.066 Uiso 1 1 d R . . H22E H 0.8486 0.6290 0.4937 0.066 Uiso 1 1 d R . . O1W O 0.7897(3) 0.9175(3) 0.2983(2) 0.0696(6) Uani 1 1 d D . . H11W H 0.811(6) 0.976(5) 0.235(2) 0.084 Uiso 1 1 d D . . H12W H 0.685(3) 0.818(3) 0.276(3) 0.084 Uiso 1 1 d D . . O2W O 0.0643(6) 0.9081(6) 0.4655(4) 0.0585(9) Uiso 0.50 1 d PD . . H21W H 0.006(9) 0.954(9) 0.422(4) 0.070 Uiso 0.50 1 d PD . . H22W H 0.071(9) 0.953(9) 0.5420(18) 0.070 Uiso 0.50 1 d PD . . 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 Ni 0.02354(19) 0.02531(19) 0.0280(2) 0.00690(13) 0.00189(13) 0.00519(14) N1 0.0278(8) 0.0330(8) 0.0310(8) 0.0085(7) 0.0010(7) 0.0035(7) N2 0.0288(8) 0.0326(8) 0.0322(9) 0.0093(7) 0.0013(7) 0.0049(7) N3 0.0275(8) 0.0302(8) 0.0318(8) 0.0091(7) 0.0028(7) 0.0041(7) C3A 0.0256(9) 0.0270(9) 0.0297(9) 0.0062(7) 0.0042(7) 0.0078(7) N4 0.0315(9) 0.0310(8) 0.0313(8) 0.0111(7) 0.0051(7) 0.0065(7) C4 0.0393(12) 0.0369(11) 0.0467(12) 0.0175(10) 0.0111(10) 0.0052(10) C5 0.0350(10) 0.0346(10) 0.0298(9) 0.0066(8) 0.0065(8) 0.0157(9) O5 0.0534(10) 0.0499(10) 0.0307(8) 0.0129(7) 0.0045(7) 0.0188(8) N6 0.0302(8) 0.0324(8) 0.0292(8) 0.0026(7) 0.0005(7) 0.0083(7) C6 0.0393(11) 0.0440(12) 0.0331(11) -0.0019(9) -0.0047(9) 0.0123(10) C7 0.0279(9) 0.0308(9) 0.0324(10) 0.0051(8) 0.0029(8) 0.0079(8) O7 0.0337(8) 0.0378(8) 0.0434(9) 0.0096(7) 0.0002(7) -0.0032(7) C7A 0.0258(9) 0.0282(9) 0.0301(9) 0.0076(7) 0.0043(7) 0.0057(8) N1E 0.112(2) 0.0358(10) 0.0418(11) 0.0153(9) 0.0231(12) 0.0308(13) C1E 0.171(4) 0.090(3) 0.0499(17) 0.0195(17) 0.026(2) 0.102(3) C2E 0.133(4) 0.175(5) 0.0495(17) 0.036(2) 0.029(2) 0.133(4) N2E 0.0409(11) 0.0934(18) 0.0383(10) 0.0250(11) 0.0132(9) 0.0353(12) O1W 0.0528(11) 0.0628(13) 0.0483(11) 0.0198(9) -0.0015(9) -0.0088(10) 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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1E Ni N1E 180.0 2_666 . ? N1E Ni N2E 82.91(11) 2_666 2_666 ? N1E Ni N2E 97.09(11) . 2_666 ? N1E Ni N2E 97.09(11) 2_666 . ? N1E Ni N2E 82.91(11) . . ? N2E Ni N2E 180.0 2_666 . ? N1E Ni N2 92.29(9) 2_666 . ? N1E Ni N2 87.72(9) . . ? N2E Ni N2 87.47(8) 2_666 . ? N2E Ni N2 92.53(8) . . ? N1E Ni N2 87.71(9) 2_666 2_666 ? N1E Ni N2 92.28(9) . 2_666 ? N2E Ni N2 92.53(8) 2_666 2_666 ? N2E Ni N2 87.47(8) . 2_666 ? N2 Ni N2 180.00(11) . 2_666 ? N2 N1 C7A 105.63(16) . . ? N1 N2 N3 112.85(16) . . ? N1 N2 Ni 120.02(13) . . ? N3 N2 Ni 127.13(13) . . ? C3A N3 N2 104.16(16) . . ? N3 C3A N4 128.12(18) . . ? N3 C3A C7A 109.60(18) . . ? N4 C3A C7A 122.28(18) . . ? C5 N4 C3A 119.42(17) . . ? C5 N4 C4 119.14(18) . . ? C3A N4 C4 121.43(18) . . ? N4 C4 H41 109.6 . . ? N4 C4 H42 109.6 . . ? H41 C4 H42 109.4 . . ? N4 C4 H43 109.3 . . ? H41 C4 H43 109.5 . . ? H42 C4 H43 109.4 . . ? O5 C5 N4 121.7(2) . . ? O5 C5 N6 120.7(2) . . ? N4 C5 N6 117.53(17) . . ? C5 N6 C7 126.51(17) . . ? C5 N6 C6 115.95(18) . . ? C7 N6 C6 117.52(18) . . ? N6 C6 H61 109.5 . . ? N6 C6 H62 109.6 . . ? H61 C6 H62 109.4 . . ? N6 C6 H63 109.5 . . ? H61 C6 H63 109.4 . . ? H62 C6 H63 109.4 . . ? O7 C7 N6 120.93(19) . . ? O7 C7 C7A 126.75(19) . . ? N6 C7 C7A 112.32(17) . . ? N1 C7A C3A 107.76(17) . . ? N1 C7A C7 130.32(17) . . ? C3A C7A C7 121.92(18) . . ? C1E N1E Ni 107.1(2) . . ? C1E N1E H11E 110.1 . . ? Ni N1E H11E 110.3 . . ? C1E N1E H12E 110.5 . . ? Ni N1E H12E 110.2 . . ? H11E N1E H12E 108.5 . . ? N1E C1E C2E 108.7(3) . . ? N1E C1E H13E 109.8 . . ? C2E C1E H13E 110.0 . . ? N1E C1E H14E 109.9 . . ? C2E C1E H14E 110.1 . . ? H13E C1E H14E 108.4 . . ? N2E C2E C1E 108.3(3) . . ? N2E C2E H23E 110.1 . . ? C1E C2E H23E 110.1 . . ? N2E C2E H24E 110.0 . . ? C1E C2E H24E 109.9 . . ? H23E C2E H24E 108.4 . . ? C2E N2E Ni 107.5(2) . . ? C2E N2E H21E 110.2 . . ? Ni N2E H21E 110.2 . . ? C2E N2E H22E 110.2 . . ? Ni N2E H22E 110.2 . . ? H21E N2E H22E 108.5 . . ? H11W O1W H12W 107(4) . . ? H21W O2W H22W 103.1(16) . . ? 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 Ni N1E 2.093(2) 2_666 ? Ni N1E 2.093(2) . ? Ni N2E 2.093(2) 2_666 ? Ni N2E 2.093(2) . ? Ni N2 2.1179(17) . ? Ni N2 2.1179(17) 2_666 ? N1 N2 1.319(2) . ? N1 C7A 1.352(3) . ? N2 N3 1.367(2) . ? N3 C3A 1.331(3) . ? C3A N4 1.376(3) . ? C3A C7A 1.379(2) . ? N4 C5 1.373(3) . ? N4 C4 1.464(3) . ? C4 H41 0.9602 . ? C4 H42 0.9603 . ? C4 H43 0.9603 . ? C5 O5 1.219(3) . ? C5 N6 1.402(3) . ? N6 C7 1.402(3) . ? N6 C6 1.469(3) . ? C6 H61 0.9605 . ? C6 H62 0.9605 . ? C6 H63 0.9605 . ? C7 O7 1.224(3) . ? C7 C7A 1.433(3) . ? N1E C1E 1.463(5) . ? N1E H11E 0.9000 . ? N1E H12E 0.9000 . ? C1E C2E 1.509(7) . ? C1E H13E 0.9700 . ? C1E H14E 0.9700 . ? C2E N2E 1.461(5) . ? C2E H23E 0.9700 . ? C2E H24E 0.9700 . ? N2E H21E 0.9000 . ? N2E H22E 0.9000 . ? O1W H11W 0.858(10) . ? O1W H12W 0.854(10) . ? O2W H21W 0.863(10) . ? O2W H22W 0.866(10) . ? 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 H12W N3 0.854(10) 2.034(11) 2.888(3) 178(4) . O1W H11W O7 0.858(10) 2.016(13) 2.860(3) 168(4) 1_665 N1E H12E O2W 0.90 2.19 2.872(5) 132.5 1_545 N2E H22E O2W 0.90 2.22 2.905(5) 132.3 1_655 N2E H21E O5 0.90 2.26 3.002(3) 139.6 2_665 O2W H21W O1W 0.863(10) 2.00(3) 2.781(5) 150(6) 1_455 O2W H22W O1W 0.866(10) 1.89(3) 2.681(5) 151(6) 2_676