#------------------------------------------------------------------------------ #$Date: 2018-01-16 03:47:30 +0200 (Tue, 16 Jan 2018) $ #$Revision: 205232 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/12/11/7121140.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_7121140 loop_ _publ_author_name 'Sergeenko, Ania' 'Ovens, Jeffrey' 'Leznoff, Daniel B.' _publ_section_title ; Designing Anisotropic Cyanometallate Coordination Polymers with Unidirectional Thermal Expansion (TE): 2D Zero TE and 1D Colossal Positive TE ; _journal_name_full 'Chemical Communications' _journal_paper_doi 10.1039/C7CC09033A _journal_year 2018 _chemical_formula_moiety 'C4 H4 Br2 Cu N4 O2 Pt' _chemical_formula_sum 'C4 H4 Br2 Cu N4 O2 Pt' _chemical_formula_weight 558.53 _chemical_name_systematic 'bis(aqua)tetrakis(\m-2cyano)copper(II) dibromoplatinate(IV)' _chemical_properties_physical Heat-sensitive _space_group_crystal_system monoclinic _space_group_IT_number 11 _space_group_name_Hall '-P 2yb' _space_group_name_H-M_alt 'P 1 21/m 1' _symmetry_space_group_name_Hall '-P 2yb' _symmetry_space_group_name_H-M 'P 1 21/m 1' _atom_sites_solution_hydrogens difmap _audit_update_record ; 2017-10-15 deposited with the CCDC. 2018-01-15 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 110.207(2) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 6.3039(6) _cell_length_b 14.2946(13) _cell_length_c 6.5640(6) _cell_measurement_reflns_used 9996 _cell_measurement_temperature 135(2) _cell_measurement_theta_max 33.24 _cell_measurement_theta_min 2.85 _cell_volume 555.09(9) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2014 (Sheldrick 2014)' _computing_structure_solution 'SHELXS-97 (Sheldrick 2008)' _diffrn_ambient_temperature 135(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 2208 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 33.240 _diffrn_reflns_theta_min 2.850 _exptl_absorpt_coefficient_mu 21.680 _exptl_absorpt_correction_T_max 0.348 _exptl_absorpt_correction_T_min 0.253 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Sheldrick , 1996)' _exptl_crystal_colour green _exptl_crystal_density_diffrn 3.336 _exptl_crystal_description octahedral _exptl_crystal_F_000 496 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water' _exptl_crystal_size_max 0.145 _exptl_crystal_size_mid 0.103 _exptl_crystal_size_min 0.048 _refine_diff_density_max 1.160 _refine_diff_density_min -0.985 _refine_ls_extinction_coef 0.00104(13) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 79 _refine_ls_number_reflns 2208 _refine_ls_number_restraints 2 _refine_ls_restrained_S_all 1.074 _refine_ls_R_factor_all 0.0265 _refine_ls_R_factor_gt 0.0141 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0165P)^2^+0.0234P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0309 _refine_ls_wR_factor_ref 0.0338 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1665 _reflns_number_total 2208 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c7cc09033a2.cif _cod_data_source_block CuBr2_LT _cod_depositor_comments ; The following automatic conversions were performed: '_exptl_absorpt_correction_type' value 'Multi-scan' changed to 'multi-scan' according to /home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26. Automatic conversion script Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas ; _cod_database_code 7121140 _shelx_estimated_absorpt_t_min 0.145 _shelx_estimated_absorpt_t_max 0.423 _shelx_res_file ; TITL mo_AT_115_LT_070317_0m_4_a.res in P2(1)/m REM Old TITL mo_AT_115_LT_070317_0m_4 in P2(1)/m REM SHELXT solution in P2(1)/m REM R1 0.068, Rweak 0.001, Alpha 0.048, Orientation as input REM Formula found by SHELXT: Br2 Cu O10 Pt CELL 0.71073 6.3039 14.2946 6.5640 90.000 110.207 90.000 ZERR 2.000 0.0006 0.0013 0.0006 0.000 0.002 0.000 LATT 1 SYMM -X,Y+1/2,-Z SFAC C H BR CU N O PT UNIT 8 6 4 2 8 4 2 TEMP -138.160 SIZE 0.048 0.103 0.145 L.S. 10 BOND $H LIST 6 FMAP 2 acta bind Cu1 O1 bind Cu1 O2 PLAN 40 HTAB O2$14 O1 dfix 0.9 0.02 O2 H2 dfix 0.9 0.02 O1 H1 eqiv $1 -x, 1-y, 1-z eqiv $2 -x, 0.5+y, 1-z eqiv $3 -1+x, y, z bind Br1 Br1_$1 bind Br1 O1_$2 bind Br1 O2_$3 bind O1 O2_$3 WGHT 0.016500 0.023400 EXTI 0.001040 BASF 0.48414 FVAR 0.30830 PT1 7 0.000000 0.500000 0.000000 10.50000 0.00622 0.00332 = 0.00641 -0.00012 -0.00187 0.00019 O1 6 0.219013 0.250000 0.675596 10.50000 0.02578 0.02805 = 0.03153 0.00000 0.01653 0.00000 BR1 3 -0.233414 0.507042 0.235669 11.00000 0.01235 0.02174 = 0.01180 -0.00029 0.00345 0.00076 CU1 4 0.504675 0.250000 0.496530 10.50000 0.00722 0.00337 = 0.00756 0.00000 -0.00296 0.00000 N1 5 0.682228 0.347431 0.700578 11.00000 0.01151 0.00789 = 0.01264 0.00068 -0.00253 0.00079 H1 2 0.281563 0.289280 0.791505 11.00000 0.07649 C1 1 0.796208 0.402116 0.812115 11.00000 0.01059 0.00642 = 0.01094 0.00223 -0.00065 0.00288 N2 5 0.314231 0.347153 0.301973 11.00000 0.01147 0.00877 = 0.01260 0.00114 -0.00028 0.00104 H2 2 0.909939 0.250000 0.412829 10.50000 0.04967 O2 6 0.768176 0.250000 0.324347 10.50000 0.02028 0.05487 = 0.02538 0.00000 0.01055 0.00000 C2 1 0.197737 0.401829 0.191321 11.00000 0.00906 0.00822 = 0.00983 0.00106 -0.00024 0.00096 HKLF 5 REM mo_AT_115_LT_070317_0m_4_a.res in P2(1)/m REM R1 = 0.0141 for 1665 Fo > 4sig(Fo) and 0.0265 for all 2208 data REM 79 parameters refined using 2 restraints END WGHT 0.0157 0.0359 REM Highest difference peak 1.160, deepest hole -0.985, 1-sigma level 0.164 Q1 1 0.0862 0.4983 0.1026 11.00000 0.05 1.16 Q2 1 0.6091 0.2500 0.5432 10.50000 0.05 0.82 Q3 1 0.4750 0.2976 0.5299 11.00000 0.05 0.71 Q4 1 0.9157 0.4488 0.8214 11.00000 0.05 0.71 Q5 1 0.1251 0.4411 0.1267 11.00000 0.05 0.71 Q6 1 -0.1179 0.5074 0.2536 11.00000 0.05 0.70 Q7 1 0.8635 0.4396 0.9186 11.00000 0.05 0.69 Q8 1 0.6110 0.3074 0.5920 11.00000 0.05 0.67 Q9 1 0.7123 0.2500 0.4594 10.50000 0.05 0.65 Q10 1 -0.3616 0.4615 0.2116 11.00000 0.05 0.62 Q11 1 0.1190 0.2500 0.4915 10.50000 0.05 0.61 Q12 1 -0.3336 0.5186 0.1661 11.00000 0.05 0.55 Q13 1 -0.1718 0.4838 0.3744 11.00000 0.05 0.55 Q14 1 0.9120 0.2500 0.0355 10.50000 0.05 0.52 Q15 1 0.2725 0.2500 0.6127 10.50000 0.05 0.50 Q16 1 0.4387 0.3103 0.3657 11.00000 0.05 0.50 Q17 1 0.1344 0.3557 0.5330 11.00000 0.05 0.50 Q18 1 0.7208 0.3962 0.6710 11.00000 0.05 0.50 Q19 1 0.5842 0.3418 0.6835 11.00000 0.05 0.50 Q20 1 0.5069 0.3564 0.9402 11.00000 0.05 0.49 Q21 1 -0.1042 0.4302 0.3816 11.00000 0.05 0.48 Q22 1 0.8895 0.3261 0.4669 11.00000 0.05 0.47 Q23 1 0.2744 0.3746 0.7499 11.00000 0.05 0.46 Q24 1 0.7293 0.3678 0.7820 11.00000 0.05 0.46 Q25 1 -0.3051 0.5190 0.2821 11.00000 0.05 0.46 Q26 1 0.2282 0.3566 0.2064 11.00000 0.05 0.46 Q27 1 0.7291 0.3994 1.0659 11.00000 0.05 0.45 Q28 1 0.1148 0.4332 0.3384 11.00000 0.05 0.44 Q29 1 0.0100 0.4572 -0.0201 11.00000 0.05 0.44 Q30 1 -0.2757 0.5964 0.1366 11.00000 0.05 0.44 Q31 1 -0.4431 0.4199 0.1377 11.00000 0.05 0.43 Q32 1 0.7543 0.4901 0.8201 11.00000 0.05 0.43 Q33 1 0.6889 0.2500 0.7549 10.50000 0.05 0.43 Q34 1 0.5877 0.4740 0.8659 11.00000 0.05 0.43 Q35 1 0.0261 0.2500 1.0051 10.50000 0.05 0.43 Q36 1 0.4287 0.3784 0.8152 11.00000 0.05 0.42 Q37 1 0.2269 0.3758 0.2977 11.00000 0.05 0.41 Q38 1 0.2095 0.5188 0.0198 11.00000 0.05 0.41 Q39 1 -0.0880 0.6015 0.3981 11.00000 0.05 0.41 Q40 1 0.6606 0.3463 0.2806 11.00000 0.05 0.41 ; _shelx_res_checksum 226 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy Pt1 Pt 0.0000 0.5000 0.0000 0.00638(4) Uani 1 2 d S . P O1 O 0.2190(6) 0.2500 0.6756(6) 0.0267(8) Uani 1 2 d DS T P Br1 Br -0.23341(5) 0.50704(2) 0.23567(5) 0.01549(5) Uani 1 1 d . . . Cu1 Cu 0.50467(12) 0.2500 0.49653(11) 0.00749(6) Uani 1 2 d S T P N1 N 0.6822(5) 0.34743(16) 0.7006(5) 0.0124(6) Uani 1 1 d . . . H1 H 0.282(9) 0.289(2) 0.792(5) 0.076(19) Uiso 1 1 d D . . C1 C 0.7962(6) 0.40212(18) 0.8121(5) 0.0105(6) Uani 1 1 d . . . N2 N 0.3142(5) 0.34715(16) 0.3020(5) 0.0121(6) Uani 1 1 d . . . H2 H 0.910(5) 0.2500 0.413(8) 0.050(19) Uiso 1 2 d DS . P O2 O 0.7682(6) 0.2500 0.3243(6) 0.0328(9) Uani 1 2 d DS T P C2 C 0.1977(5) 0.40183(18) 0.1913(5) 0.0099(6) Uani 1 1 d . . . 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 Pt1 0.00622(5) 0.00332(5) 0.00641(5) -0.00012(6) -0.00187(4) 0.00019(6) O1 0.026(2) 0.0280(17) 0.032(2) 0.000 0.017(2) 0.000 Br1 0.01235(10) 0.02174(10) 0.01180(10) -0.00029(13) 0.00345(8) 0.00076(13) Cu1 0.00722(15) 0.00337(12) 0.00756(15) 0.000 -0.00296(11) 0.000 N1 0.0115(15) 0.0079(12) 0.0126(14) 0.0007(9) -0.0025(15) 0.0008(9) C1 0.0106(17) 0.0064(12) 0.0109(15) 0.0022(10) -0.0007(16) 0.0029(10) N2 0.0115(15) 0.0088(12) 0.0126(15) 0.0011(9) -0.0003(15) 0.0010(9) O2 0.020(2) 0.055(2) 0.025(2) 0.000 0.011(2) 0.000 C2 0.0091(16) 0.0082(12) 0.0098(15) 0.0011(10) -0.0002(16) 0.0010(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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 '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' Pt Pt -1.7033 8.3905 '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 C2 Pt1 C2 180.0 . 3_565 C2 Pt1 C1 88.60(7) . 3_666 C2 Pt1 C1 91.40(7) 3_565 3_666 C2 Pt1 C1 91.40(7) . 1_454 C2 Pt1 C1 88.60(7) 3_565 1_454 C1 Pt1 C1 180.0 3_666 1_454 C2 Pt1 Br1 90.70(7) . . C2 Pt1 Br1 89.30(7) 3_565 . C1 Pt1 Br1 88.86(7) 3_666 . C1 Pt1 Br1 91.14(7) 1_454 . C2 Pt1 Br1 89.30(7) . 3_565 C2 Pt1 Br1 90.70(7) 3_565 3_565 C1 Pt1 Br1 91.14(7) 3_666 3_565 C1 Pt1 Br1 88.86(7) 1_454 3_565 Br1 Pt1 Br1 180.0 . 3_565 Cu1 O1 O2 106.84(13) . 1_455 Cu1 O1 H1 103(4) . . O2 O1 H1 132(3) 1_455 . Pt1 Br1 O1 99.01(5) . 2_556 Pt1 Br1 Br1 97.577(14) . 3_566 O1 Br1 Br1 86.09(6) 2_556 3_566 Pt1 Br1 Br1 92.264(13) . 3_465 O1 Br1 Br1 98.98(6) 2_556 3_465 Br1 Br1 Br1 168.119(13) 3_566 3_465 Pt1 Br1 O2 95.02(5) . 1_455 O1 Br1 O2 161.97(7) 2_556 1_455 Br1 Br1 O2 80.86(6) 3_566 1_455 Br1 Br1 O2 91.70(6) 3_465 1_455 N2 Cu1 N2 88.77(16) 4_565 . N2 Cu1 N1 91.03(7) 4_565 4_565 N2 Cu1 N1 176.59(9) . 4_565 N2 Cu1 N1 176.59(9) 4_565 . N2 Cu1 N1 91.03(7) . . N1 Cu1 N1 88.96(16) 4_565 . N2 Cu1 O2 93.59(9) 4_565 . N2 Cu1 O2 93.59(9) . . N1 Cu1 O2 89.83(9) 4_565 . N1 Cu1 O2 89.83(9) . . N2 Cu1 O1 85.86(9) 4_565 . N2 Cu1 O1 85.86(9) . . N1 Cu1 O1 90.73(8) 4_565 . N1 Cu1 O1 90.73(8) . . O2 Cu1 O1 179.22(13) . . C1 N1 Cu1 175.1(2) . . N1 C1 Pt1 178.0(2) . 1_656 C2 N2 Cu1 177.5(2) . . Cu1 O2 H2 114(4) . . N2 C2 Pt1 178.5(3) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Pt1 C2 2.005(3) . Pt1 C2 2.005(3) 3_565 Pt1 C1 2.009(3) 3_666 Pt1 C1 2.009(3) 1_454 Pt1 Br1 2.4780(3) . Pt1 Br1 2.4780(3) 3_565 O1 Cu1 2.467(3) . O1 O2 2.978(5) 1_455 O1 H1 0.918(19) . Br1 O1 3.5175(6) 2_556 Br1 Br1 3.6997(7) 3_566 Br1 Br1 3.7048(8) 3_465 Br1 O2 3.7196(6) 1_455 Cu1 N2 1.985(3) 4_565 Cu1 N2 1.985(3) . Cu1 N1 1.988(3) 4_565 Cu1 N1 1.988(3) . Cu1 O2 2.309(3) . N1 C1 1.140(4) . C1 Pt1 2.009(3) 1_656 N2 C2 1.144(4) . O2 H2 0.88(2) .