#------------------------------------------------------------------------------ #$Date: 2015-04-02 12:22:18 +0100 (Thu, 02 Apr 2015) $ #$Revision: 134621 $ #$URL: svn://www.crystallography.net/cod/cif/4/11/63/4116345.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_4116345 loop_ _publ_author_name 'Larry R. Falvello' 'Michael A. Hitchman' 'Fernando Palacio' 'Isabel Pascual' 'Arthur J. Schultz' 'Horst Stratemeier' 'Milagros Tom\'as' 'Esteban P. Urriolabeitia' 'Dianna M. Young' _publ_section_title ; Tunable Molecular Distortion in a Nickel Complex Coupled to a Reversible Phase Transition in the Crystalline State ; _journal_name_full 'Journal of the American Chemical Society' _journal_page_first 2808 _journal_page_last 2819 _journal_paper_doi 10.1021/ja983247t _journal_volume 121 _journal_year 1999 _chemical_formula_sum 'C6 H16 N10 Ni O6' _chemical_formula_weight 383.00 _chemical_name_systematic ; ? ; _space_group_IT_number 63 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-C 2c 2' _symmetry_space_group_name_H-M 'C m c m' _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 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 12.015(2) _cell_length_b 7.226(2) _cell_length_c 15.766(3) _cell_measurement_reflns_used 25 _cell_measurement_temperature 139(1) _cell_measurement_theta_max 15.8 _cell_measurement_theta_min 12.1 _cell_volume 1368.8(5) _computing_cell_refinement CAD4/PC _computing_data_collection CAD4/PC _computing_data_reduction 'XCAD4B (Harms, 1996)' _computing_molecular_graphics 'SHELXTL Rel. 5.05/VMS (Siemens, 1996)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 139(1) _diffrn_measured_fraction_theta_full 0.000 _diffrn_measured_fraction_theta_max 0.465 _diffrn_measurement_device_type 'Nonius CAD-4' _diffrn_measurement_method 'omega-theta 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 0.0024 _diffrn_reflns_av_sigmaI/netI 0.0395 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 1069 _diffrn_reflns_theta_full 0.50 _diffrn_reflns_theta_max 29.95 _diffrn_reflns_theta_min 2.58 _exptl_absorpt_coefficient_mu 1.473 _exptl_absorpt_correction_type psi-scans _exptl_crystal_density_diffrn 1.859 _exptl_crystal_F_000 792 _refine_diff_density_max 0.421 _refine_diff_density_min -0.410 _refine_diff_density_rms 0.093 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.997 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 80 _refine_ls_number_reflns 1067 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.997 _refine_ls_R_factor_all 0.0510 _refine_ls_R_factor_gt 0.0334 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0469P)^2^+0.0991P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0822 _refine_ls_wR_factor_ref 0.0859 _reflns_number_gt 880 _reflns_number_total 1067 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file ja983247t_5.cif _[local]_cod_data_source_block 2b _cod_depositor_comments ; The following automatic conversions were performed: '_refine_ls_weighting_scheme' value 'calc w=1/[\s^2^(Fo^2^)+(0.0469P)^2^+0.0991P] where P=(Fo^2^+2Fc^2^)/3' was changed to 'calc'. New tag '_refine_ls_weighting_details' was created. The value of the new tag was set to 'w=1/[\s^2^(Fo^2^)+(0.0469P)^2^+0.0991P] where P=(Fo^2^+2Fc^2^)/3'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_database_code 4116345 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y, -z-1/2' 'x, -y, z-1/2' '-x, y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, y+1/2, -z-1/2' 'x+1/2, -y+1/2, z-1/2' '-x+1/2, y+1/2, 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_calc_flag _atom_site_refinement_flags Ni1 Ni 0.5000 0.17108(7) 0.7500 0.01058(14) Uani 1 d S N1 N 0.5000 0.1782(3) 0.60636(14) 0.0129(4) Uani 1 d S C2 C 0.40233(16) 0.2023(3) 0.56373(12) 0.0122(4) Uani 1 d . O2 O 0.30991(11) 0.1782(2) 0.59706(9) 0.0164(3) Uani 1 d . N3 N 0.40494(14) 0.2554(2) 0.47915(10) 0.0134(3) Uani 1 d . H3 H 0.342(2) 0.271(4) 0.4536(18) 0.027(7) Uiso 1 d . C4 C 0.5000 0.2863(4) 0.43422(17) 0.0124(5) Uani 1 d S O4 O 0.5000 0.3376(3) 0.36019(12) 0.0168(4) Uani 1 d S N4 N 0.6182(2) 0.3812(4) 0.7500 0.0148(5) Uani 1 d S H41 H 0.613(3) 0.457(5) 0.711(2) 0.058(11) Uiso 1 d . H42 H 0.691(5) 0.344(8) 0.7500 0.075(19) Uiso 1 d S N5 N 0.62116(19) -0.0318(4) 0.7500 0.0149(5) Uani 1 d S H51 H 0.666(2) -0.011(5) 0.7928(17) 0.032(7) Uiso 1 d . H52 H 0.599(5) -0.141(8) 0.7500 0.061(17) Uiso 1 d S 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 Ni1 0.0065(2) 0.0144(2) 0.0109(2) 0.000 0.000 0.000 N1 0.0078(9) 0.0187(10) 0.0121(10) 0.0014(9) 0.000 0.000 C2 0.0116(8) 0.0146(8) 0.0103(8) -0.0001(6) -0.0013(6) 0.0004(6) O2 0.0085(6) 0.0285(7) 0.0122(6) 0.0030(6) -0.0006(5) -0.0013(6) N3 0.0093(7) 0.0204(8) 0.0105(7) 0.0010(6) -0.0014(6) 0.0009(6) C4 0.0136(12) 0.0111(11) 0.0124(12) -0.0008(9) 0.000 0.000 O4 0.0167(9) 0.0223(10) 0.0113(9) 0.0065(8) 0.000 0.000 N4 0.0107(11) 0.0176(11) 0.0160(11) 0.000 0.000 -0.0027(9) N5 0.0100(10) 0.0184(12) 0.0162(11) 0.000 0.000 0.0001(9) 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 N5 Ni1 N5 89.60(15) . 3_656 N5 Ni1 N4 178.27(11) . 3_656 N5 Ni1 N4 92.12(10) . . N4 Ni1 N4 86.15(15) 3_656 . N5 Ni1 N1 90.93(4) . . N5 Ni1 N1 90.92(4) 3_656 . N4 Ni1 N1 89.05(5) . . N1 Ni1 N1 177.39(12) 10_557 . C2 N1 C2 118.8(2) . 12_655 C2 N1 Ni1 119.71(12) . . O2 C2 N1 122.93(17) . . O2 C2 N3 117.78(17) . . N1 C2 N3 119.29(18) . . C4 N3 C2 124.32(18) . . C4 N3 H3 117.9(18) . . C2 N3 H3 117.7(18) . . O4 C4 N3 123.04(12) . . N3 C4 N3 113.9(2) 12_655 . Ni1 N4 H41 116(2) . . Ni1 N4 H42 116(4) . . H41 N4 H42 105(3) . . Ni1 N5 H51 108(2) . . Ni1 N5 H52 116(4) . . H51 N5 H52 111(3) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Ni1 N5 2.066(2) Ni1 N4 2.079(2) Ni1 N1 2.265(2) N1 C2 1.364(2) C2 O2 1.241(2) C2 N3 1.388(2) N3 C4 1.362(2) N3 H3 0.86(3) C4 O4 1.224(3) N4 H41 0.82(4) N4 H42 0.91(6) N5 H51 0.87(3) N5 H52 0.83(6)