#------------------------------------------------------------------------------ #$Date: 2016-03-26 16:33:12 +0200 (Sat, 26 Mar 2016) $ #$Revision: 180342 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/20/11/7201193.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_7201193 loop_ _publ_author_name 'Kutasi, Anna M.' 'Turner, David R.' 'Jensen, Paul' 'Moubaraki, Boujemaa' 'Batten, Stuart R.' 'Murray, Keith S.' _publ_section_title ; Coordination polymers of nitrocyanamide, O2NNCN−: synthesis, structure and magnetism ; _journal_issue 10 _journal_name_full CrystEngComm _journal_page_first 2089 _journal_paper_doi 10.1039/b905970a _journal_volume 11 _journal_year 2009 _chemical_formula_moiety 'C12 H12 Mn N8 O6, (C10 H8 N2)' _chemical_formula_sum 'C22 H20 Mn N10 O6' _chemical_formula_weight 575.42 _chemical_name_common {[Mn(CAN)2(4,4'-bipy)(H2O)2].4,4'-bipy} _chemical_name_systematic ; {[Mn(CAN)2(4,4'-bipy)(H2O)2].4,4'-bipy} ; _space_group_IT_number 13 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yc' _symmetry_space_group_name_H-M 'P 1 2/c 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 101.865(1) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 7.3102(1) _cell_length_b 11.5900(2) _cell_length_c 15.2784(3) _cell_measurement_reflns_used 14237 _cell_measurement_temperature 123(1) _cell_measurement_theta_max 27.50 _cell_measurement_theta_min 3.77 _cell_volume 1266.81(4) _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_collection 'Collect (Hooft, 1999)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 123(1) _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'phi and omega 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 0.0668 _diffrn_reflns_av_sigmaI/netI 0.0510 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 14237 _diffrn_reflns_theta_full 27.50 _diffrn_reflns_theta_max 27.50 _diffrn_reflns_theta_min 3.77 _exptl_absorpt_coefficient_mu 0.580 _exptl_absorpt_correction_T_max 0.9442 _exptl_absorpt_correction_T_min 0.8451 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details SORTAV _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.509 _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 590 _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.10 _refine_diff_density_max 0.472 _refine_diff_density_min -0.520 _refine_diff_density_rms 0.105 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 187 _refine_ls_number_reflns 2899 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.071 _refine_ls_R_factor_all 0.0648 _refine_ls_R_factor_gt 0.0378 _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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0893 _refine_ls_wR_factor_ref 0.1013 _reflns_number_gt 2125 _reflns_number_total 2899 _reflns_threshold_expression >2sigma(I) _cod_data_source_file b905970a.txt _cod_data_source_block 3Mn _cod_depositor_comments ; The following automatic conversions were performed: '_exptl_absorpt_correction_type' value 'Empirical' changed to 'empirical' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_original_sg_symbol_H-M P2/c _cod_database_code 7201193 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' 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 Mn1 Mn 0.5000 0.34288(3) 0.2500 0.01332(14) Uani 1 2 d S . . N20 N 0.5000 0.53633(18) 0.2500 0.0154(5) Uani 1 2 d S . . C21 C 0.5915(2) 0.59692(16) 0.32069(12) 0.0161(4) Uani 1 1 d . . . H21 H 0.6571 0.5557 0.3712 0.019 Uiso 1 1 calc R . . N21 N 0.5000 1.14855(17) 0.2500 0.0152(5) Uani 1 2 d S . . C23 C 0.5000 0.7785(2) 0.2500 0.0133(5) Uani 1 2 d S . . C24 C 0.5000 0.9068(2) 0.2500 0.0149(5) Uani 1 2 d S . . C25 C 0.5385(3) 0.96904(16) 0.32917(12) 0.0204(4) Uani 1 1 d . . . H25 H 0.5650 0.9300 0.3850 0.025 Uiso 1 1 calc R . . C22 C 0.5948(2) 0.71575(15) 0.32355(12) 0.0153(4) Uani 1 1 d . . . H22 H 0.6610 0.7547 0.3751 0.018 Uiso 1 1 calc R . . C26 C 0.5382(3) 1.08817(16) 0.32633(12) 0.0211(4) Uani 1 1 d . . . H26 H 0.5666 1.1293 0.3812 0.025 Uiso 1 1 calc R . . O20 O 0.4553(2) 0.35111(11) 0.38644(9) 0.0169(3) Uani 1 1 d . . . H2B H 0.353(4) 0.3288(19) 0.4002(16) 0.038(7) Uiso 1 1 d . . . H2A H 0.550(3) 0.321(2) 0.4300(17) 0.045(7) Uiso 1 1 d . . . N10 N 0.8058(2) 0.33806(13) 0.30806(11) 0.0208(4) Uani 1 1 d . . . N11 N 1.1000(2) 0.27189(14) 0.40653(11) 0.0223(4) Uani 1 1 d . . . C11 C 0.9389(3) 0.30091(17) 0.35320(13) 0.0180(4) Uani 1 1 d . . . N12 N 1.1141(2) 0.15491(14) 0.41973(11) 0.0236(4) Uani 1 1 d . . . O11 O 1.2621(2) 0.12197(14) 0.46767(10) 0.0350(4) Uani 1 1 d . . . O10 O 0.9856(2) 0.09028(13) 0.38576(11) 0.0376(4) Uani 1 1 d . . . C34 C 0.1309(2) 0.60987(17) 0.33786(12) 0.0184(4) Uani 1 1 d . . . H34 H 0.1117 0.5385 0.3068 0.022 Uiso 1 1 calc R . . C35 C 0.2348(3) 0.61456(17) 0.42412(13) 0.0206(4) Uani 1 1 d . . . H35 H 0.2861 0.5446 0.4510 0.025 Uiso 1 1 calc R . . N30 N 0.2677(2) 0.71159(14) 0.47225(10) 0.0215(4) Uani 1 1 d . . . C32 C 0.0846(3) 0.81215(17) 0.34767(13) 0.0208(4) Uani 1 1 d . . . H32 H 0.0323 0.8831 0.3233 0.025 Uiso 1 1 calc R . . C33 C 0.0544(2) 0.71146(16) 0.29692(12) 0.0158(4) Uani 1 1 d . . . C31 C 0.1910(3) 0.80843(18) 0.43360(13) 0.0221(4) Uani 1 1 d . . . H31 H 0.2106 0.8782 0.4669 0.027 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 Mn1 0.0158(2) 0.0081(2) 0.0147(2) 0.000 -0.00004(16) 0.000 N20 0.0202(11) 0.0102(11) 0.0162(11) 0.000 0.0049(9) 0.000 C21 0.0196(9) 0.0129(10) 0.0151(10) -0.0001(7) 0.0017(8) -0.0007(7) N21 0.0180(11) 0.0098(11) 0.0167(11) 0.000 0.0009(9) 0.000 C23 0.0152(12) 0.0102(13) 0.0154(13) 0.000 0.0051(10) 0.000 C24 0.0137(12) 0.0131(13) 0.0174(14) 0.000 0.0022(10) 0.000 C25 0.0322(10) 0.0132(10) 0.0139(10) 0.0017(8) 0.0001(8) 0.0003(8) C22 0.0169(9) 0.0133(10) 0.0148(10) -0.0012(7) 0.0008(8) -0.0017(7) C26 0.0333(11) 0.0133(10) 0.0146(10) -0.0022(8) 0.0001(8) 0.0003(8) O20 0.0168(7) 0.0175(7) 0.0152(7) 0.0011(6) 0.0004(6) -0.0003(6) N10 0.0166(8) 0.0193(9) 0.0250(9) 0.0011(7) 0.0007(7) -0.0014(7) N11 0.0172(8) 0.0224(9) 0.0251(9) 0.0041(7) -0.0009(7) 0.0008(7) C11 0.0195(10) 0.0164(10) 0.0189(10) -0.0003(8) 0.0059(8) -0.0041(8) N12 0.0231(9) 0.0252(10) 0.0227(9) 0.0050(8) 0.0050(8) 0.0040(7) O11 0.0285(8) 0.0438(10) 0.0303(9) 0.0158(7) 0.0002(7) 0.0157(7) O10 0.0333(9) 0.0214(8) 0.0538(11) 0.0000(8) -0.0011(8) 0.0002(7) C34 0.0187(10) 0.0161(10) 0.0193(10) -0.0003(8) 0.0011(8) -0.0001(8) C35 0.0210(10) 0.0209(10) 0.0182(10) 0.0039(8) 0.0002(8) 0.0033(8) N30 0.0207(8) 0.0252(10) 0.0173(9) 0.0006(7) 0.0008(7) 0.0004(7) C32 0.0224(10) 0.0181(10) 0.0206(11) -0.0001(8) 0.0010(8) 0.0013(8) C33 0.0143(9) 0.0185(10) 0.0147(10) -0.0001(8) 0.0035(8) -0.0023(8) C31 0.0231(10) 0.0228(10) 0.0195(10) -0.0048(9) 0.0021(8) -0.0009(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' Mn Mn 0.3368 0.7283 '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 O20 Mn1 O20 174.98(7) 2_655 . ? O20 Mn1 N10 92.66(6) 2_655 . ? O20 Mn1 N10 87.47(6) . . ? O20 Mn1 N10 87.47(6) 2_655 2_655 ? O20 Mn1 N10 92.66(6) . 2_655 ? N10 Mn1 N10 177.13(8) . 2_655 ? O20 Mn1 N20 87.49(3) 2_655 . ? O20 Mn1 N20 87.49(3) . . ? N10 Mn1 N20 91.43(4) . . ? N10 Mn1 N20 91.43(4) 2_655 . ? O20 Mn1 N21 92.51(3) 2_655 1_545 ? O20 Mn1 N21 92.51(3) . 1_545 ? N10 Mn1 N21 88.57(4) . 1_545 ? N10 Mn1 N21 88.57(4) 2_655 1_545 ? N20 Mn1 N21 180.0 . 1_545 ? C21 N20 C21 117.1(2) . 2_655 ? C21 N20 Mn1 121.47(11) . . ? C21 N20 Mn1 121.47(11) 2_655 . ? N20 C21 C22 123.35(17) . . ? N20 C21 H21 118.3 . . ? C22 C21 H21 118.3 . . ? C26 N21 C26 117.0(2) 2_655 . ? C26 N21 Mn1 121.50(11) 2_655 1_565 ? C26 N21 Mn1 121.50(11) . 1_565 ? C22 C23 C22 117.3(2) 2_655 . ? C22 C23 C24 121.37(11) 2_655 . ? C22 C23 C24 121.37(11) . . ? C25 C24 C25 117.3(2) . 2_655 ? C25 C24 C23 121.35(12) . . ? C25 C24 C23 121.35(12) 2_655 . ? C26 C25 C24 119.60(18) . . ? C26 C25 H25 120.2 . . ? C24 C25 H25 120.2 . . ? C21 C22 C23 119.48(17) . . ? C21 C22 H22 120.3 . . ? C23 C22 H22 120.3 . . ? N21 C26 C25 123.24(18) . . ? N21 C26 H26 118.4 . . ? C25 C26 H26 118.4 . . ? Mn1 O20 H2B 122.1(16) . . ? Mn1 O20 H2A 115.9(15) . . ? H2B O20 H2A 106(2) . . ? C11 N10 Mn1 154.17(15) . . ? C11 N11 N12 111.74(16) . . ? N10 C11 N11 172.7(2) . . ? O10 N12 O11 124.16(18) . . ? O10 N12 N11 120.82(16) . . ? O11 N12 N11 115.02(16) . . ? C35 C34 C33 119.08(18) . . ? C35 C34 H34 120.5 . . ? C33 C34 H34 120.5 . . ? N30 C35 C34 124.00(18) . . ? N30 C35 H35 118.0 . . ? C34 C35 H35 118.0 . . ? C31 N30 C35 116.83(17) . . ? C31 C32 C33 119.76(18) . . ? C31 C32 H32 120.1 . . ? C33 C32 H32 120.1 . . ? C34 C33 C32 117.02(17) . . ? C34 C33 C33 121.13(11) . 2 ? C32 C33 C33 121.86(11) . 2 ? N30 C31 C32 123.28(19) . . ? N30 C31 H31 118.4 . . ? C32 C31 H31 118.4 . . ? 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 Mn1 O20 2.1775(13) 2_655 ? Mn1 O20 2.1775(13) . ? Mn1 N10 2.2298(15) . ? Mn1 N10 2.2298(15) 2_655 ? Mn1 N20 2.242(2) . ? Mn1 N21 2.252(2) 1_545 ? N20 C21 1.345(2) . ? N20 C21 1.345(2) 2_655 ? C21 C22 1.378(3) . ? C21 H21 0.9500 . ? N21 C26 1.339(2) 2_655 ? N21 C26 1.339(2) . ? N21 Mn1 2.252(2) 1_565 ? C23 C22 1.397(2) 2_655 ? C23 C22 1.397(2) . ? C23 C24 1.487(4) . ? C24 C25 1.387(2) . ? C24 C25 1.387(2) 2_655 ? C25 C26 1.381(3) . ? C25 H25 0.9500 . ? C22 H22 0.9500 . ? C26 H26 0.9500 . ? O20 H2B 0.86(3) . ? O20 H2A 0.92(2) . ? N10 C11 1.154(2) . ? N11 C11 1.330(2) . ? N11 N12 1.371(2) . ? N12 O10 1.230(2) . ? N12 O11 1.236(2) . ? C34 C35 1.380(3) . ? C34 C33 1.395(3) . ? C34 H34 0.9500 . ? C35 N30 1.338(3) . ? C35 H35 0.9500 . ? N30 C31 1.337(2) . ? C32 C31 1.382(3) . ? C32 C33 1.393(3) . ? C32 H32 0.9500 . ? C33 C33 1.490(4) 2 ? C31 H31 0.9500 . ? 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 O20 H2B N11 0.86(3) 1.98(3) 2.830(2) 169(2) 1_455 O20 H2A N30 0.92(2) 1.83(3) 2.737(2) 169(2) 3_666