# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Parsons, Simon' _publ_contact_author_name 'Parsons, Simon' _publ_contact_author_email S.PARSONS@ED.AC.UK _publ_section_title ; The Effect of Pressure on the Crystal Structure of [Gd(PhCOO)3(DMF)] n to 3.7 GPa and the transition to a second phase at 5.0 GPa ; # Attachment '- Gd_polymer_cifs.cif' data_GDRT01_Phase1_0GPa _database_code_depnum_ccdc_archive 'CCDC 768036' #TrackingRef '- Gd_polymer_cifs.cif' #Ambient pressure and temperature data set. _audit_creation_date 08-06-05 _audit_creation_method CRYSTALS_ver_12.85 _oxford_structure_analysis_title 'gdrt01 in P4(2)/n' _chemical_name_systematic ; catena-((\m~2~-Benzoato-O,O')-bis(\m~2~-benzoato-O,O',O')-(dimethylformamide-O )-gadolinium) ; _chemical_melting_point ? _publ_section_exptl_refinement ; 232_ALERT_2_C Hirshfeld Test Diff (M-X) Gd1 -- O7 .. 5.91 su 232_ALERT_2_C Hirshfeld Test Diff (M-X) Gd1 -- O1_a .. 6.41 su No action. Ton Spek says this often happens with bonds between heavy & light atoms with good data sets. The reason is probably inadequate modelling of bonding density. 220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.20 Ratio 241_ALERT_2_C Check High Ueq as Compared to Neighbors for C4 242_ALERT_2_C Check Low Ueq as Compared to Neighbors for N1 These are caused by slightly larger than expected thermal elicpsoids on one of the methyl C-atoms on the DMF ligand. This type of thermal motion is not unexpeted for methyl groups on the perifery of the molecule especially at RT. 911_ALERT_3_C # Missing FCF Refl Between THmin & STh/L= 0.600 1 913_ALERT_3_C # Missing Very Strong Reflections in FCF ....... 1 912_ALERT_4_C # Missing FCF Reflections Above STh/L= 0.600 68 #============================================================================== Resolution & Completeness Statistics (Cumulative and Friedel Pairs Averaged) #============================================================================== Theta sin(th)/Lambda Complete Expected Measured Missing #------------------------------------------------------------------------------ 20.82 0.500 1.000 2422 2421 1 23.01 0.550 1.000 3233 3232 1 25.24 0.600 1.000 4180 4179 1 #----------------------------------------------------------- ACTA Min. Res. --- 27.51 0.650 1.000 5337 5336 1 29.84 0.700 0.997 6660 6640 20 30.54 0.715 0.990 7085 7016 69 128_ALERT_4_C Non-standard setting of Space-group P42/n .... P42/n:1 The origin was shifted from the -1 to the -4 for comparison with the high-pressure phase (see text). 199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K 200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K This is correct. ; #end of refcif _cell_length_a 22.4915(6) _cell_length_b 22.4915(6) _cell_length_c 9.1640(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 4635.8(2) _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'P 42/n:1' _symmetry_space_group_name_Hall 'P 4n -1n' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,z -y+1/2,x+1/2,z+1/2 y+1/2,-x+1/2,z+1/2 -x+1/2,-y+1/2,-z+1/2 x+1/2,y+1/2,-z+1/2 y,-x,-z -y,x,-z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Gd -0.1653 3.9035 25.0709 2.2534 19.0798 0.1820 13.8518 12.9331 3.5454 101.3980 2.4196 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 8 _chemical_formula_sum 'C24 H22 Gd1 N1 O7' _chemical_formula_moiety ; (C24 H22 Gd1 N1 O7)n ; _chemical_compound_source ? _chemical_formula_weight 593.69 _cell_measurement_reflns_used 9820 _cell_measurement_theta_min 3 _cell_measurement_theta_max 30 _cell_measurement_temperature 293 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_min 0.12 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_max 0.23 _exptl_crystal_density_diffrn 1.701 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 2344 _exptl_absorpt_coefficient_mu 2.906 # Sheldrick geometric approximatio 0.63 0.71 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.56 _exptl_absorpt_correction_T_max 0.71 _diffrn_measurement_device 'Bruker Kappa Apex2' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method '\f & \w scans' # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'Apex2 (Bruker AXS, 2006)' _computing_cell_refinement 'Apex2 (Bruker AXS, 2006)' _computing_data_reduction 'Apex2 (Bruker AXS, 2006)' _computing_structure_solution 'USER DEFINED STRUCTURE SOLUTION' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 293 _diffrn_reflns_number 77931 _reflns_number_total 7016 _diffrn_reflns_av_R_equivalents 0.067 # Number of reflections with Friedels Law is 7016 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 3550 _diffrn_reflns_theta_min 1.280 _diffrn_reflns_theta_max 30.545 _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 29.628 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 9 _reflns_limit_h_min -22 _reflns_limit_h_max 22 _reflns_limit_k_min 0 _reflns_limit_k_max 32 _reflns_limit_l_min 0 _reflns_limit_l_max 12 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.18 _refine_diff_density_max 1.48 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-10.0\s(I) _refine_ls_number_reflns 7016 _refine_ls_number_restraints 0 _refine_ls_number_parameters 298 _oxford_refine_ls_R_factor_ref 0.0510 _refine_ls_wR_factor_ref 0.0675 _refine_ls_goodness_of_fit_ref 1.0509 _refine_ls_shift/su_max 0.003251 # The values computed from all data _oxford_reflns_number_all 7016 _refine_ls_R_factor_all 0.0510 _refine_ls_wR_factor_all 0.0675 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 4714 _refine_ls_R_factor_gt 0.0243 _refine_ls_wR_factor_gt 0.0519 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.02P)^2^ + 3.46P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Insert your own references if required - in alphabetical order _publ_section_references ; User-defined structure solution reference Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Siemens Industrial Automation, Inc (1996). SADABS: Area-Detector Absorption Correction;: Madison, WI. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. Bruker Analytical X-ray Systems, Inc., 2006. Apex2, Version 2 User Manual, M86-E01078, Madison, WI. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Gd1 Gd 0.740916(5) 0.749268(5) -0.038648(14) 0.0252 1.0000 Uani . . . . . . . O1 O 0.79114(9) 0.70018(8) -0.2238(2) 0.0316 1.0000 Uani . . . . . . . O2 O 0.84603(9) 0.68502(10) -0.4166(2) 0.0383 1.0000 Uani . . . . . . . O3 O 0.67176(9) 0.68431(9) -0.1550(2) 0.0383 1.0000 Uani . . . . . . . O4 O 0.69284(10) 0.67454(10) -0.3913(2) 0.0415 1.0000 Uani . . . . . . . O5 O 0.72120(10) 0.67265(9) 0.1266(2) 0.0382 1.0000 Uani . . . . . . . O6 O 0.76432(10) 0.68933(8) 0.3398(2) 0.0375 1.0000 Uani . . . . . . . O7 O 0.83508(10) 0.72439(10) 0.0689(2) 0.0423 1.0000 Uani . . . . . . . N1 N 0.90662(13) 0.72902(15) 0.2397(3) 0.0501 1.0000 Uani . . . . . . . C1 C 0.83242(12) 0.67292(12) -0.2881(3) 0.0291 1.0000 Uani . . . . . . . C2 C 0.86288(13) 0.62354(13) -0.2092(4) 0.0336 1.0000 Uani . . . . . . . C3 C 0.91878(17) 0.60585(18) -0.2529(4) 0.0560 1.0000 Uani . . . . . . . C4 C 0.94819(18) 0.5623(2) -0.1769(6) 0.0744 1.0000 Uani . . . . . . . C5 C 0.92128(19) 0.53470(17) -0.0617(5) 0.0609 1.0000 Uani . . . . . . . C6 C 0.86613(18) 0.55138(15) -0.0192(4) 0.0513 1.0000 Uani . . . . . . . C7 C 0.83686(15) 0.59625(13) -0.0919(4) 0.0400 1.0000 Uani . . . . . . . C8 C 0.67017(13) 0.65707(13) -0.2744(3) 0.0327 1.0000 Uani . . . . . . . C9 C 0.63883(13) 0.59838(13) -0.2772(4) 0.0350 1.0000 Uani . . . . . . . C10 C 0.61250(14) 0.57617(14) -0.1524(4) 0.0456 1.0000 Uani . . . . . . . C11 C 0.58469(18) 0.52170(17) -0.1547(6) 0.0653 1.0000 Uani . . . . . . . C12 C 0.58220(18) 0.48928(18) -0.2800(6) 0.0688 1.0000 Uani . . . . . . . C13 C 0.60758(18) 0.51064(17) -0.4057(5) 0.0641 1.0000 Uani . . . . . . . C14 C 0.63629(16) 0.56489(15) -0.4034(4) 0.0497 1.0000 Uani . . . . . . . C15 C 0.74342(13) 0.65585(12) 0.2450(3) 0.0300 1.0000 Uani . . . . . . . C16 C 0.74466(14) 0.58993(12) 0.2741(3) 0.0339 1.0000 Uani . . . . . . . C17 C 0.77781(17) 0.56765(14) 0.3865(4) 0.0492 1.0000 Uani . . . . . . . C18 C 0.7781(2) 0.50698(16) 0.4140(5) 0.0672 1.0000 Uani . . . . . . . C19 C 0.7443(2) 0.46949(16) 0.3321(5) 0.0693 1.0000 Uani . . . . . . . C20 C 0.7108(2) 0.49107(17) 0.2198(5) 0.0663 1.0000 Uani . . . . . . . C21 C 0.71144(17) 0.55171(14) 0.1894(4) 0.0499 1.0000 Uani . . . . . . . C22 C 0.86738(14) 0.75281(16) 0.1499(4) 0.0431 1.0000 Uani . . . . . . . C23 C 0.9414(2) 0.7659(2) 0.3376(6) 0.0931 1.0000 Uani . . . . . . . C24 C 0.91294(18) 0.66584(19) 0.2506(5) 0.0630 1.0000 Uani . . . . . . . H31 H 0.9366 0.6234 -0.3337 0.0679 1.0000 Uiso R . . . . . . H41 H 0.9865 0.5518 -0.2043 0.0898 1.0000 Uiso R . . . . . . H51 H 0.9409 0.5043 -0.0121 0.0741 1.0000 Uiso R . . . . . . H61 H 0.8480 0.5325 0.0593 0.0619 1.0000 Uiso R . . . . . . H71 H 0.7993 0.6081 -0.0615 0.0487 1.0000 Uiso R . . . . . . H101 H 0.6137 0.5980 -0.0663 0.0552 1.0000 Uiso R . . . . . . H111 H 0.5675 0.5070 -0.0699 0.0780 1.0000 Uiso R . . . . . . H121 H 0.5632 0.4525 -0.2799 0.0823 1.0000 Uiso R . . . . . . H131 H 0.6053 0.4888 -0.4919 0.0766 1.0000 Uiso R . . . . . . H141 H 0.6543 0.5790 -0.4881 0.0594 1.0000 Uiso R . . . . . . H171 H 0.8002 0.5931 0.4448 0.0595 1.0000 Uiso R . . . . . . H181 H 0.8014 0.4920 0.4893 0.0814 1.0000 Uiso R . . . . . . H191 H 0.7438 0.4288 0.3530 0.0837 1.0000 Uiso R . . . . . . H201 H 0.6875 0.4653 0.1641 0.0803 1.0000 Uiso R . . . . . . H211 H 0.6897 0.5665 0.1104 0.0597 1.0000 Uiso R . . . . . . H221 H 0.8639 0.7940 0.1482 0.0523 1.0000 Uiso R . . . . . . H231 H 0.9358 0.7526 0.4356 0.1101 1.0000 Uiso R . . . . . . H232 H 0.9829 0.7622 0.3108 0.1101 1.0000 Uiso R . . . . . . H233 H 0.9292 0.8067 0.3279 0.1101 1.0000 Uiso R . . . . . . H241 H 0.9050 0.6534 0.3484 0.0753 1.0000 Uiso R . . . . . . H242 H 0.9528 0.6547 0.2245 0.0753 1.0000 Uiso R . . . . . . H243 H 0.8855 0.6467 0.1860 0.0753 1.0000 Uiso 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 Gd1 0.03306(7) 0.02709(6) 0.01535(7) 0.00158(6) 0.00001(5) 0.00252(6) O1 0.0378(10) 0.0348(10) 0.0223(11) -0.0006(8) 0.0005(8) 0.0121(9) O2 0.0456(11) 0.0485(12) 0.0209(11) 0.0032(9) 0.0049(9) 0.0144(10) O3 0.0437(11) 0.0455(11) 0.0256(12) -0.0008(10) -0.0003(9) -0.0086(10) O4 0.0534(12) 0.0459(11) 0.0252(12) 0.0039(10) -0.0019(10) -0.0166(10) O5 0.0580(13) 0.0343(10) 0.0222(12) 0.0075(9) -0.0067(10) -0.0051(9) O6 0.0614(13) 0.0321(9) 0.0191(11) -0.0007(8) -0.0011(10) 0.0001(10) O7 0.0428(11) 0.0553(13) 0.0288(13) 0.0004(10) -0.0044(10) 0.0057(11) N1 0.0461(15) 0.0652(19) 0.0388(19) 0.0036(14) -0.0106(13) -0.0069(15) C1 0.0314(12) 0.0316(12) 0.0243(15) 0.0002(12) -0.0025(12) 0.0030(11) C2 0.0369(14) 0.0362(14) 0.0277(16) -0.0005(12) -0.0002(13) 0.0070(12) C3 0.052(2) 0.064(2) 0.052(3) 0.0225(18) 0.0159(17) 0.0204(18) C4 0.055(2) 0.081(3) 0.087(4) 0.024(3) 0.013(2) 0.035(2) C5 0.072(2) 0.0521(19) 0.059(3) 0.0181(19) 0.000(2) 0.0259(19) C6 0.071(2) 0.0404(16) 0.042(2) 0.0130(15) 0.0070(18) 0.0117(17) C7 0.0492(17) 0.0372(14) 0.0336(19) 0.0059(13) 0.0069(14) 0.0095(13) C8 0.0334(13) 0.0370(14) 0.0276(17) 0.0026(13) -0.0027(12) -0.0044(12) C9 0.0329(13) 0.0339(13) 0.0382(19) 0.0050(13) 0.0000(13) -0.0023(12) C10 0.0475(17) 0.0432(16) 0.046(2) 0.0010(15) 0.0122(16) -0.0038(14) C11 0.062(2) 0.051(2) 0.084(4) 0.013(2) 0.025(2) -0.0075(18) C12 0.057(2) 0.0450(19) 0.104(4) 0.001(2) 0.010(2) -0.0190(18) C13 0.070(2) 0.052(2) 0.070(3) -0.012(2) 0.000(2) -0.020(2) C14 0.058(2) 0.0468(18) 0.044(2) -0.0017(16) -0.0015(17) -0.0123(16) C15 0.0406(14) 0.0296(12) 0.0198(15) 0.0033(11) 0.0050(12) 0.0030(12) C16 0.0490(16) 0.0290(12) 0.0237(16) 0.0040(11) 0.0046(13) 0.0013(12) C17 0.070(2) 0.0369(15) 0.041(2) 0.0076(15) -0.0034(18) 0.0052(16) C18 0.099(3) 0.0413(18) 0.061(3) 0.0213(18) -0.008(2) 0.011(2) C19 0.104(3) 0.0301(16) 0.074(3) 0.0126(19) 0.011(3) 0.003(2) C20 0.095(3) 0.0416(18) 0.062(3) -0.0099(19) 0.006(3) -0.017(2) C21 0.074(2) 0.0389(16) 0.037(2) 0.0004(15) -0.0034(18) -0.0119(17) C22 0.0430(16) 0.0551(18) 0.0311(19) 0.0014(15) 0.0020(14) 0.0014(15) C23 0.088(3) 0.113(4) 0.078(4) -0.009(3) -0.041(3) -0.021(3) C24 0.057(2) 0.073(3) 0.059(3) 0.011(2) -0.0128(19) 0.010(2) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.044790(4) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Gd1 . O1 5_664 2.559(2) yes Gd1 . O2 5_664 2.485(2) yes Gd1 . C1 5_664 2.882(3) yes Gd1 . O4 5_664 2.360(2) yes Gd1 . O6 5_665 2.290(2) yes Gd1 . O1 . 2.3184(19) yes Gd1 . O3 . 2.385(2) yes Gd1 . O5 . 2.3365(19) yes Gd1 . O7 . 2.402(2) yes O1 . C1 . 1.259(3) yes O2 . C1 . 1.247(4) yes O3 . C8 . 1.255(4) yes O4 . C8 . 1.250(4) yes O5 . C15 . 1.253(3) yes O6 . C15 . 1.242(3) yes O7 . C22 . 1.219(4) yes N1 . C22 . 1.320(4) yes N1 . C23 . 1.450(5) yes N1 . C24 . 1.432(5) yes C1 . C2 . 1.491(4) yes C2 . C3 . 1.378(4) yes C2 . C7 . 1.370(4) yes C3 . C4 . 1.372(5) yes C3 . H31 . 0.930 no C4 . C5 . 1.366(6) yes C4 . H41 . 0.928 no C5 . C6 . 1.353(5) yes C5 . H51 . 0.932 no C6 . C7 . 1.377(4) yes C6 . H61 . 0.929 no C7 . H71 . 0.928 no C8 . C9 . 1.497(4) yes C9 . C10 . 1.382(5) yes C9 . C14 . 1.381(5) yes C10 . C11 . 1.376(5) yes C10 . H101 . 0.930 no C11 . C12 . 1.362(6) yes C11 . H111 . 0.928 no C12 . C13 . 1.372(6) yes C12 . H121 . 0.932 no C13 . C14 . 1.381(5) yes C13 . H131 . 0.932 no C14 . H141 . 0.932 no C15 . C16 . 1.507(4) yes C16 . C17 . 1.366(5) yes C16 . C21 . 1.378(5) yes C17 . C18 . 1.388(4) yes C17 . H171 . 0.932 no C18 . C19 . 1.360(6) yes C18 . H181 . 0.930 no C19 . C20 . 1.365(6) yes C19 . H191 . 0.934 no C20 . C21 . 1.392(5) yes C20 . H201 . 0.933 no C21 . H211 . 0.935 no C22 . H221 . 0.930 no C23 . H231 . 0.954 no C23 . H232 . 0.969 no C23 . H233 . 0.961 no C24 . H241 . 0.956 no C24 . H242 . 0.961 no C24 . H243 . 0.957 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1 5_664 Gd1 . O2 5_664 51.23(6) yes O1 5_664 Gd1 . C1 5_664 25.89(7) yes O2 5_664 Gd1 . C1 5_664 25.53(7) yes O1 5_664 Gd1 . O4 5_664 67.92(7) yes O2 5_664 Gd1 . O4 5_664 91.15(7) yes C1 5_664 Gd1 . O4 5_664 76.74(8) yes O1 5_664 Gd1 . O6 5_665 113.24(7) yes O2 5_664 Gd1 . O6 5_665 74.47(7) yes C1 5_664 Gd1 . O6 5_665 92.46(8) yes O4 5_664 Gd1 . O6 5_665 79.10(8) yes O1 5_664 Gd1 . O1 . 74.12(7) yes O2 5_664 Gd1 . O1 . 123.08(7) yes C1 5_664 Gd1 . O1 . 99.48(8) yes O4 5_664 Gd1 . O1 . 80.74(8) yes O6 5_665 Gd1 . O1 . 153.50(8) yes O1 5_664 Gd1 . O3 . 73.04(7) yes O2 5_664 Gd1 . O3 . 77.14(7) yes C1 5_664 Gd1 . O3 . 75.67(7) yes O4 5_664 Gd1 . O3 . 137.31(8) yes O6 5_665 Gd1 . O3 . 133.75(8) yes O1 5_664 Gd1 . O5 . 145.62(7) yes O2 5_664 Gd1 . O5 . 113.34(7) yes C1 5_664 Gd1 . O5 . 134.14(8) yes O4 5_664 Gd1 . O5 . 146.27(8) yes O6 5_665 Gd1 . O5 . 85.37(7) yes O1 5_664 Gd1 . O7 . 134.50(7) yes O2 5_664 Gd1 . O7 . 154.15(8) yes C1 5_664 Gd1 . O7 . 150.71(8) yes O4 5_664 Gd1 . O7 . 73.98(8) yes O6 5_665 Gd1 . O7 . 81.90(8) yes O1 . Gd1 . O3 . 72.48(7) yes O1 . Gd1 . O5 . 102.45(7) yes O3 . Gd1 . O5 . 73.38(7) yes O1 . Gd1 . O7 . 76.10(7) yes O3 . Gd1 . O7 . 128.00(8) yes O5 . Gd1 . O7 . 74.31(8) yes Gd1 5_664 O1 . Gd1 . 105.88(7) yes Gd1 5_664 O1 . C1 . 91.52(17) yes Gd1 . O1 . C1 . 159.02(19) yes Gd1 5_664 O2 . C1 . 95.31(16) yes Gd1 . O3 . C8 . 135.02(19) yes Gd1 5_664 O4 . C8 . 136.0(2) yes Gd1 . O5 . C15 . 135.06(19) yes Gd1 5_665 O6 . C15 . 154.5(2) yes Gd1 . O7 . C22 . 130.8(2) yes C22 . N1 . C23 . 120.9(4) yes C22 . N1 . C24 . 120.8(3) yes C23 . N1 . C24 . 118.1(3) yes Gd1 5_664 C1 . O1 . 62.60(14) yes Gd1 5_664 C1 . O2 . 59.16(14) yes O1 . C1 . O2 . 121.1(3) yes Gd1 5_664 C1 . C2 . 169.1(2) yes O1 . C1 . C2 . 118.4(3) yes O2 . C1 . C2 . 120.5(3) yes C1 . C2 . C3 . 119.6(3) yes C1 . C2 . C7 . 121.2(3) yes C3 . C2 . C7 . 119.2(3) yes C2 . C3 . C4 . 119.9(4) yes C2 . C3 . H31 . 120.1 no C4 . C3 . H31 . 120.0 no C3 . C4 . C5 . 120.2(4) yes C3 . C4 . H41 . 119.5 no C5 . C4 . H41 . 120.3 no C4 . C5 . C6 . 120.2(3) yes C4 . C5 . H51 . 120.0 no C6 . C5 . H51 . 119.8 no C5 . C6 . C7 . 120.1(3) yes C5 . C6 . H61 . 119.9 no C7 . C6 . H61 . 120.0 no C6 . C7 . C2 . 120.3(3) yes C6 . C7 . H71 . 120.0 no C2 . C7 . H71 . 119.7 no O3 . C8 . O4 . 125.6(3) yes O3 . C8 . C9 . 117.4(3) yes O4 . C8 . C9 . 117.0(3) yes C8 . C9 . C10 . 120.4(3) yes C8 . C9 . C14 . 121.0(3) yes C10 . C9 . C14 . 118.5(3) yes C9 . C10 . C11 . 120.3(4) yes C9 . C10 . H101 . 120.0 no C11 . C10 . H101 . 119.7 no C10 . C11 . C12 . 120.6(4) yes C10 . C11 . H111 . 119.5 no C12 . C11 . H111 . 119.9 no C11 . C12 . C13 . 120.2(4) yes C11 . C12 . H121 . 119.6 no C13 . C12 . H121 . 120.2 no C12 . C13 . C14 . 119.4(4) yes C12 . C13 . H131 . 120.3 no C14 . C13 . H131 . 120.3 no C9 . C14 . C13 . 121.0(4) yes C9 . C14 . H141 . 119.5 no C13 . C14 . H141 . 119.5 no O5 . C15 . O6 . 125.0(3) yes O5 . C15 . C16 . 117.2(3) yes O6 . C15 . C16 . 117.8(3) yes C15 . C16 . C17 . 120.3(3) yes C15 . C16 . C21 . 120.3(3) yes C17 . C16 . C21 . 119.4(3) yes C16 . C17 . C18 . 120.0(4) yes C16 . C17 . H171 . 120.1 no C18 . C17 . H171 . 119.9 no C17 . C18 . C19 . 120.4(4) yes C17 . C18 . H181 . 119.6 no C19 . C18 . H181 . 120.0 no C18 . C19 . C20 . 120.3(3) yes C18 . C19 . H191 . 120.0 no C20 . C19 . H191 . 119.7 no C19 . C20 . C21 . 119.6(4) yes C19 . C20 . H201 . 120.2 no C21 . C20 . H201 . 120.2 no C20 . C21 . C16 . 120.2(4) yes C20 . C21 . H211 . 119.9 no C16 . C21 . H211 . 119.8 no N1 . C22 . O7 . 124.4(3) yes N1 . C22 . H221 . 118.1 no O7 . C22 . H221 . 117.5 no N1 . C23 . H231 . 109.5 no N1 . C23 . H232 . 108.3 no H231 . C23 . H232 . 109.7 no N1 . C23 . H233 . 109.6 no H231 . C23 . H233 . 110.4 no H232 . C23 . H233 . 109.4 no N1 . C24 . H241 . 109.7 no N1 . C24 . H242 . 109.5 no H241 . C24 . H242 . 109.4 no N1 . C24 . H243 . 109.8 no H241 . C24 . H243 . 109.1 no H242 . C24 . H243 . 109.3 no data_gdpol2_Phase1_0_1GPa _database_code_depnum_ccdc_archive 'CCDC 768037' #TrackingRef '- Gd_polymer_cifs.cif' #0.1 GPa data set _audit_creation_date 08-06-30 _audit_creation_method CRYSTALS_ver_12.85 _oxford_structure_analysis_title 'gdpol2 in P4(2)/n' _chemical_name_systematic ; catena-((\m~2~-Benzoato-O,O')-bis(\m~2~-benzoato-O,O',O')-(dimethylformamide-O )-gadolinium) ; _chemical_melting_point ? _publ_section_exptl_prep ; ? ; _publ_section_exptl_refinement ; Pressure = 0.10 GPa. H atoms placed geometrically after each cycle. Because completeness is less than 100% the ligands were restrained to have the same bond distances and angles as at ambient pressure. Checkcif output: 027_ALERT_3_A _diffrn_reflns_theta_full (too) Low ............ 15.25 Deg. 029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.69 911_ALERT_3_B # Missing FCF Refl Between THmin & STh/L= 0.600 1444 910_ALERT_3_C # Missing FCF Reflections Below Th(Min) ........ 1 913_ALERT_3_C # Missing Very Strong Reflections in FCF ....... 81 912_ALERT_4_C # Missing FCF Reflections Above STh/L= 0.600 1565 Data are incomplete becasue of shading of reciprocal space by the body of the pressure cell. 919_ALERT_3_B # Reflections Likely Affected by the Beamstop .. 3 ...or maybe by the gasket. 220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.07 Ratio Noted, but no action taken. Not unexpected for organic ligands at RT. 342_ALERT_3_C Low Bond Precision on C-C Bonds (x 1000) Ang ... 10 This will be due to relatively low completeness and the presence of a very heavy atom. 860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 86 See above. 042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? The one given is more chemically meaningful. 128_ALERT_4_C Non-standard setting of Space-group P42/n .... P42/n:1 See text. This makes comparison with the high pressure phase simpler. 034_ALERT_1_C No Flack Parameter Given. Z .GT. Si, NonCentro . ? This is a bug in Checkcif. The space group operation '-x+1/2,-y+1/2,-z+1/2' is an inversion centre at [1/4 1/4 1/4]. This test shouldn't be applied, but presumably is triggered when the -1 is not on the origin. 199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K 200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K Correct. ; #end of refcif _cell_length_a 22.4953(9) _cell_length_b 22.4953(9) _cell_length_c 9.1830(6) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 4647.0(4) _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'P 42/n:1' _symmetry_space_group_name_Hall 'P 4n -1n' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,z -y+1/2,x+1/2,z+1/2 y+1/2,-x+1/2,z+1/2 -x+1/2,-y+1/2,-z+1/2 x+1/2,y+1/2,-z+1/2 y,-x,-z -y,x,-z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0010 0.0010 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0020 0.0010 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0040 0.0030 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Gd -0.5090 2.0340 25.0709 2.2534 19.0798 0.1820 13.8518 12.9331 3.5454 101.3980 2.4196 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 8 _chemical_formula_sum 'C24 H22 Gd1 N1 O7' _chemical_formula_moiety ; (C24 H22 Gd1 N1 O7)n ; _chemical_compound_source ? _chemical_formula_weight 593.69 _cell_measurement_reflns_used 5201 _cell_measurement_theta_min 2 _cell_measurement_theta_max 20 _cell_measurement_temperature 293 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_max 0.20 _exptl_crystal_density_diffrn 1.697 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 2344 _exptl_absorpt_coefficient_mu 0.924 # Sheldrick geometric approximatio 0.56 0.75 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.01 _exptl_absorpt_correction_T_max 0.75 _diffrn_measurement_device 'Bruker SMART' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator Silicon _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.48650 _diffrn_source synchrotron _diffrn_measurement_method \w _computing_data_collection 'SMART (Siemens, 1993)' _computing_cell_refinement 'SAINT (Siemens ,1995)' _computing_data_reduction 'SAINT (Siemens ,1995)' _computing_structure_solution 'USER DEFINED STRUCTURE SOLUTION' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'DIAMOND Crystal Impact (2004)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 293 _diffrn_reflns_number 25106 _reflns_number_total 4095 _diffrn_reflns_av_R_equivalents 0.097 _diffrn_reflns_theta_min 1.239 _diffrn_reflns_theta_max 20.339 _diffrn_measured_fraction_theta_max 0.577 _diffrn_reflns_theta_full 15.254 _diffrn_measured_fraction_theta_full 0.692 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _reflns_limit_h_min -13 _reflns_limit_h_max 16 _reflns_limit_k_min 0 _reflns_limit_k_max 30 _reflns_limit_l_min 0 _reflns_limit_l_max 13 _oxford_diffrn_Wilson_B_factor 1.23 _oxford_diffrn_Wilson_scale 13.46 _atom_sites_solution_primary direct _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.04 _refine_diff_density_max 1.50 # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>2.0\s(I) _refine_ls_number_reflns 2769 _refine_ls_number_restraints 86 _refine_ls_number_parameters 298 _oxford_refine_ls_R_factor_ref 0.0543 _refine_ls_wR_factor_ref 0.0637 _refine_ls_goodness_of_fit_ref 0.9297 _refine_ls_shift/su_max 0.001209 # The values computed from all data _oxford_reflns_number_all 3966 _refine_ls_R_factor_all 0.0793 _refine_ls_wR_factor_all 0.0845 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 2769 _refine_ls_R_factor_gt 0.0543 _refine_ls_wR_factor_gt 0.0637 _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment noref # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 1.63 0.768 0.708 ; _publ_section_references ; User-defined structure solution reference Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Siemens Industrial Automation, Inc (1993). SMART: Area-Detector Software Package; Madison, WI. Siemens Industrial Automation, Inc (1995). SAINT: Area-Detector Integration Software.; Madison, WI. Siemens Industrial Automation, Inc (1996). SADABS: Area-Detector Absorption Correction;: Madison, WI. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Gd1 Gd 0.740795(17) 0.749307(15) -0.03865(3) 0.0216 1.0000 Uani . . . . . . . O1 O 0.7911(2) 0.7005(2) -0.2241(5) 0.0276 1.0000 Uani D . . . . . . O2 O 0.8469(3) 0.6849(3) -0.4159(5) 0.0364 1.0000 Uani D . . . . . . O3 O 0.6716(3) 0.6848(2) -0.1562(5) 0.0336 1.0000 Uani D . . . . . . O4 O 0.6929(3) 0.6747(3) -0.3918(5) 0.0377 1.0000 Uani D . . . . . . O5 O 0.7206(3) 0.6727(2) 0.1273(4) 0.0358 1.0000 Uani D . . . . . . O6 O 0.7642(3) 0.6893(2) 0.3392(5) 0.0348 1.0000 Uani D . . . . . . O7 O 0.8350(3) 0.7239(3) 0.0681(5) 0.0356 1.0000 Uani D . . . . . . N1 N 0.9073(3) 0.7292(3) 0.2403(7) 0.0450 1.0000 Uani D . . . . . . C1 C 0.8331(3) 0.6728(3) -0.2878(5) 0.0289 1.0000 Uani D . . . . . . C2 C 0.8630(3) 0.6233(3) -0.2088(6) 0.0301 1.0000 Uani D . . . . . . C3 C 0.9191(3) 0.6062(3) -0.2496(7) 0.0550 1.0000 Uani D . . . . . . C4 C 0.9494(4) 0.5621(4) -0.1741(9) 0.0682 1.0000 Uani D . . . . . . C5 C 0.9223(4) 0.5351(3) -0.0588(8) 0.0553 1.0000 Uani D . . . . . . C6 C 0.8661(4) 0.5515(3) -0.0172(7) 0.0481 1.0000 Uani D . . . . . . C7 C 0.8368(3) 0.5957(3) -0.0910(6) 0.0382 1.0000 Uani D . . . . . . C8 C 0.6696(4) 0.6562(3) -0.2732(5) 0.0311 1.0000 Uani D . . . . . . C9 C 0.6390(3) 0.5974(3) -0.2774(6) 0.0296 1.0000 Uani D . . . . . . C10 C 0.6126(3) 0.5756(3) -0.1527(7) 0.0446 1.0000 Uani D . . . . . . C11 C 0.5846(3) 0.5203(4) -0.1538(9) 0.0584 1.0000 Uani D . . . . . . C12 C 0.5825(4) 0.4882(3) -0.2799(10) 0.0680 1.0000 Uani D . . . . . . C13 C 0.6081(4) 0.5096(4) -0.4047(9) 0.0588 1.0000 Uani D . . . . . . C14 C 0.6363(3) 0.5639(3) -0.4045(7) 0.0458 1.0000 Uani D . . . . . . C15 C 0.7444(3) 0.6547(2) 0.2452(5) 0.0276 1.0000 Uani D . . . . . . C16 C 0.7444(3) 0.5895(2) 0.2733(6) 0.0319 1.0000 Uani D . . . . . . C17 C 0.7778(3) 0.5670(3) 0.3858(7) 0.0432 1.0000 Uani D . . . . . . C18 C 0.7781(4) 0.5062(4) 0.4161(8) 0.0622 1.0000 Uani D . . . . . . C19 C 0.7443(4) 0.4692(3) 0.3326(9) 0.0630 1.0000 Uani D . . . . . . C20 C 0.7107(4) 0.4910(3) 0.2201(8) 0.0555 1.0000 Uani D . . . . . . C21 C 0.7107(3) 0.5513(3) 0.1896(7) 0.0466 1.0000 Uani D . . . . . . C22 C 0.8683(4) 0.7532(3) 0.1515(8) 0.0433 1.0000 Uani D . . . . . . C23 C 0.9427(6) 0.7652(5) 0.3378(13) 0.0851 1.0000 Uani D . . . . . . C24 C 0.9124(5) 0.6659(4) 0.2528(9) 0.0527 1.0000 Uani D . . . . . . H231 H 0.9250 0.8039 0.3474 0.1022 1.0000 Uiso . . . . . . . H232 H 0.9822 0.7696 0.2982 0.1022 1.0000 Uiso . . . . . . . H233 H 0.9451 0.7466 0.4312 0.1022 1.0000 Uiso . . . . . . . H241 H 0.8874 0.6472 0.1815 0.0634 1.0000 Uiso . . . . . . . H242 H 0.9530 0.6541 0.2365 0.0634 1.0000 Uiso . . . . . . . H243 H 0.9002 0.6535 0.3484 0.0634 1.0000 Uiso . . . . . . . H31 H 0.9372 0.6245 -0.3289 0.0660 1.0000 Uiso . . . . . . . H41 H 0.9876 0.5511 -0.2018 0.0818 1.0000 Uiso . . . . . . . H51 H 0.9422 0.5054 -0.0079 0.0664 1.0000 Uiso . . . . . . . H61 H 0.8479 0.5326 0.0610 0.0577 1.0000 Uiso . . . . . . . H71 H 0.7989 0.6071 -0.0614 0.0459 1.0000 Uiso . . . . . . . H101 H 0.6135 0.5979 -0.0675 0.0535 1.0000 Uiso . . . . . . . H111 H 0.5674 0.5053 -0.0692 0.0701 1.0000 Uiso . . . . . . . H121 H 0.5636 0.4514 -0.2811 0.0816 1.0000 Uiso . . . . . . . H131 H 0.6063 0.4874 -0.4899 0.0706 1.0000 Uiso . . . . . . . H141 H 0.6535 0.5782 -0.4896 0.0549 1.0000 Uiso . . . . . . . H171 H 0.8006 0.5926 0.4425 0.0518 1.0000 Uiso . . . . . . . H181 H 0.8009 0.4912 0.4921 0.0747 1.0000 Uiso . . . . . . . H191 H 0.7441 0.4287 0.3522 0.0756 1.0000 Uiso . . . . . . . H201 H 0.6878 0.4652 0.1642 0.0667 1.0000 Uiso . . . . . . . H211 H 0.6880 0.5660 0.1130 0.0559 1.0000 Uiso . . . . . . . H221 H 0.8652 0.7944 0.1501 0.0519 1.0000 Uiso . . . . . . . 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 Gd1 0.0281(2) 0.0225(2) 0.01436(16) 0.00131(10) 0.00027(10) 0.0023(2) O1 0.031(3) 0.028(3) 0.0237(19) -0.0011(18) -0.0002(19) 0.007(4) O2 0.038(3) 0.046(3) 0.026(2) 0.002(2) 0.002(2) 0.009(4) O3 0.038(3) 0.037(3) 0.026(2) -0.005(2) -0.002(2) -0.001(4) O4 0.046(3) 0.042(3) 0.025(2) 0.002(2) 0.003(2) -0.012(4) O5 0.049(3) 0.036(3) 0.023(2) 0.006(2) -0.004(2) -0.004(4) O6 0.053(4) 0.028(3) 0.023(2) -0.0027(19) 0.003(2) 0.000(4) O7 0.030(3) 0.047(4) 0.030(2) -0.001(2) -0.004(2) 0.004(4) N1 0.036(4) 0.059(5) 0.039(4) 0.005(3) -0.008(3) -0.005(6) C1 0.030(4) 0.032(4) 0.024(3) 0.001(3) 0.001(3) 0.017(5) C2 0.032(4) 0.032(4) 0.027(3) -0.001(3) 0.001(3) 0.010(5) C3 0.052(6) 0.056(7) 0.056(5) 0.022(5) 0.016(4) 0.030(8) C4 0.054(7) 0.062(7) 0.088(7) 0.023(6) 0.012(6) 0.039(9) C5 0.064(7) 0.045(6) 0.058(5) 0.014(4) -0.006(5) 0.012(8) C6 0.061(6) 0.042(5) 0.041(4) 0.011(4) 0.009(4) 0.013(8) C7 0.045(5) 0.038(4) 0.032(3) 0.008(3) 0.010(3) 0.019(6) C8 0.037(4) 0.030(4) 0.026(3) 0.002(3) -0.003(3) -0.002(5) C9 0.025(4) 0.026(4) 0.038(3) 0.001(3) -0.002(3) -0.011(5) C10 0.048(5) 0.041(5) 0.045(4) 0.003(3) 0.013(4) -0.010(7) C11 0.057(7) 0.042(5) 0.076(6) 0.004(5) 0.025(6) -0.014(8) C12 0.058(7) 0.046(6) 0.100(8) 0.002(6) 0.009(7) -0.020(9) C13 0.054(7) 0.055(6) 0.068(6) -0.010(5) -0.002(5) -0.014(9) C14 0.051(6) 0.047(5) 0.040(4) -0.005(4) -0.007(4) -0.016(7) C15 0.040(4) 0.022(3) 0.021(3) 0.001(2) -0.001(2) 0.015(5) C16 0.046(5) 0.026(4) 0.025(3) 0.001(3) 0.005(3) 0.003(5) C17 0.062(6) 0.030(4) 0.038(4) 0.008(3) -0.009(4) 0.012(6) C18 0.089(9) 0.048(6) 0.049(5) 0.020(4) -0.004(5) 0.015(9) C19 0.102(11) 0.029(4) 0.058(5) 0.007(4) 0.002(6) 0.004(8) C20 0.077(8) 0.032(5) 0.057(5) -0.006(4) 0.008(6) -0.015(8) C21 0.060(6) 0.043(5) 0.036(4) -0.002(3) 0.000(4) -0.013(7) C22 0.041(5) 0.053(6) 0.036(4) 0.002(4) 0.002(3) 0.006(7) C23 0.087(9) 0.095(10) 0.073(7) 0.001(7) -0.045(7) -0.033(12) C24 0.050(6) 0.057(6) 0.051(5) 0.005(4) -0.007(4) 0.028(8) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.2832(8) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Gd1 . O1 5_664 2.557(5) yes Gd1 . O2 5_664 2.501(6) yes Gd1 . O4 5_664 2.356(5) yes Gd1 . O6 5_665 2.297(4) yes Gd1 . O1 . 2.321(4) yes Gd1 . O3 . 2.386(5) yes Gd1 . O5 . 2.344(5) yes Gd1 . O7 . 2.404(5) yes O1 . C1 . 1.273(6) yes O2 . C1 . 1.246(6) yes O3 . C8 . 1.252(6) yes O4 . C8 . 1.279(6) yes O5 . C15 . 1.275(6) yes O6 . C15 . 1.246(6) yes O7 . C22 . 1.259(7) yes N1 . C22 . 1.313(7) yes N1 . C23 . 1.446(8) yes N1 . C24 . 1.434(8) yes C1 . C2 . 1.490(6) yes C2 . C3 . 1.372(7) yes C2 . C7 . 1.380(7) yes C3 . C4 . 1.389(8) yes C3 . H31 . 0.930 no C4 . C5 . 1.363(8) yes C4 . H41 . 0.930 no C5 . C6 . 1.371(8) yes C5 . H51 . 0.930 no C6 . C7 . 1.373(7) yes C6 . H61 . 0.930 no C7 . H71 . 0.930 no C8 . C9 . 1.491(6) yes C9 . C10 . 1.380(7) yes C9 . C14 . 1.392(7) yes C10 . C11 . 1.396(8) yes C10 . H101 . 0.930 no C11 . C12 . 1.365(8) yes C11 . H111 . 0.930 no C12 . C13 . 1.369(8) yes C12 . H121 . 0.930 no C13 . C14 . 1.375(8) yes C13 . H131 . 0.930 no C14 . H141 . 0.930 no C15 . C16 . 1.488(6) yes C16 . C17 . 1.375(7) yes C16 . C21 . 1.379(7) yes C17 . C18 . 1.394(7) yes C17 . H171 . 0.930 no C18 . C19 . 1.363(8) yes C18 . H181 . 0.930 no C19 . C20 . 1.371(8) yes C19 . H191 . 0.930 no C20 . C21 . 1.386(7) yes C20 . H201 . 0.930 no C21 . H211 . 0.930 no C22 . H221 . 0.930 no C23 . H231 . 0.960 no C23 . H232 . 0.964 no C23 . H233 . 0.956 no C24 . H241 . 0.961 no C24 . H242 . 0.963 no C24 . H243 . 0.960 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1 5_664 Gd1 . O2 5_664 51.31(14) yes O1 5_664 Gd1 . O4 5_664 68.08(17) yes O2 5_664 Gd1 . O4 5_664 91.4(2) yes O1 5_664 Gd1 . O6 5_665 113.59(17) yes O2 5_664 Gd1 . O6 5_665 74.83(19) yes O4 5_664 Gd1 . O6 5_665 79.14(18) yes O1 5_664 Gd1 . O1 . 73.81(19) yes O2 5_664 Gd1 . O1 . 122.85(15) yes O4 5_664 Gd1 . O1 . 80.52(19) yes O6 5_665 Gd1 . O1 . 153.3(2) yes O1 5_664 Gd1 . O3 . 72.55(17) yes O2 5_664 Gd1 . O3 . 76.73(19) yes O4 5_664 Gd1 . O3 . 137.01(15) yes O6 5_665 Gd1 . O3 . 134.0(2) yes O1 . Gd1 . O3 . 72.45(18) yes O1 5_664 Gd1 . O5 . 145.50(18) yes O2 5_664 Gd1 . O5 . 113.00(19) yes O4 5_664 Gd1 . O5 . 146.25(19) yes O6 5_665 Gd1 . O5 . 85.05(17) yes O1 . Gd1 . O5 . 102.91(18) yes O1 5_664 Gd1 . O7 . 134.44(17) yes O2 5_664 Gd1 . O7 . 154.71(19) yes O4 5_664 Gd1 . O7 . 74.0(2) yes O6 5_665 Gd1 . O7 . 82.0(2) yes O1 . Gd1 . O7 . 75.89(17) yes O3 . Gd1 . O5 . 73.78(17) yes O3 . Gd1 . O7 . 127.9(2) yes O5 . Gd1 . O7 . 74.4(2) yes Gd1 5_664 O1 . Gd1 . 106.19(19) yes Gd1 5_664 O1 . C1 . 91.8(3) yes Gd1 . O1 . C1 . 158.5(4) yes Gd1 5_664 O2 . C1 . 95.2(4) yes Gd1 . O3 . C8 . 136.4(5) yes Gd1 5_664 O4 . C8 . 136.6(4) yes Gd1 . O5 . C15 . 134.9(5) yes Gd1 5_665 O6 . C15 . 155.7(6) yes Gd1 . O7 . C22 . 130.4(5) yes C22 . N1 . C23 . 121.5(6) yes C22 . N1 . C24 . 120.7(5) yes C23 . N1 . C24 . 117.5(6) yes O1 . C1 . O2 . 120.8(5) yes O1 . C1 . C2 . 118.4(4) yes O2 . C1 . C2 . 120.7(4) yes C1 . C2 . C3 . 119.5(5) yes C1 . C2 . C7 . 121.7(4) yes C3 . C2 . C7 . 118.8(5) yes C2 . C3 . C4 . 121.0(5) yes C2 . C3 . H31 . 119.5 no C4 . C3 . H31 . 119.5 no C3 . C4 . C5 . 119.2(6) yes C3 . C4 . H41 . 120.4 no C5 . C4 . H41 . 120.4 no C4 . C5 . C6 . 120.5(6) yes C4 . C5 . H51 . 119.7 no C6 . C5 . H51 . 119.7 no C5 . C6 . C7 . 120.1(5) yes C5 . C6 . H61 . 120.0 no C7 . C6 . H61 . 120.0 no C2 . C7 . C6 . 120.5(5) yes C2 . C7 . H71 . 119.8 no C6 . C7 . H71 . 119.8 no O4 . C8 . O3 . 123.3(5) yes O4 . C8 . C9 . 117.1(4) yes O3 . C8 . C9 . 119.6(4) yes C8 . C9 . C10 . 119.5(4) yes C8 . C9 . C14 . 121.6(4) yes C10 . C9 . C14 . 119.0(5) yes C9 . C10 . C11 . 120.4(5) yes C9 . C10 . H101 . 119.8 no C11 . C10 . H101 . 119.8 no C10 . C11 . C12 . 119.5(6) yes C10 . C11 . H111 . 120.3 no C12 . C11 . H111 . 120.3 no C11 . C12 . C13 . 120.7(6) yes C11 . C12 . H121 . 119.6 no C13 . C12 . H121 . 119.7 no C12 . C13 . C14 . 120.3(6) yes C12 . C13 . H131 . 119.8 no C14 . C13 . H131 . 119.9 no C9 . C14 . C13 . 120.2(5) yes C9 . C14 . H141 . 119.9 no C13 . C14 . H141 . 119.9 no O5 . C15 . O6 . 122.6(5) yes O5 . C15 . C16 . 117.5(4) yes O6 . C15 . C16 . 119.8(4) yes C15 . C16 . C17 . 119.5(4) yes C15 . C16 . C21 . 121.2(4) yes C17 . C16 . C21 . 119.3(5) yes C16 . C17 . C18 . 120.8(5) yes C16 . C17 . H171 . 119.6 no C18 . C17 . H171 . 119.6 no C17 . C18 . C19 . 119.0(5) yes C17 . C18 . H181 . 120.5 no C19 . C18 . H181 . 120.5 no C18 . C19 . C20 . 120.9(5) yes C18 . C19 . H191 . 119.6 no C20 . C19 . H191 . 119.5 no C19 . C20 . C21 . 120.1(6) yes C19 . C20 . H201 . 120.0 no C21 . C20 . H201 . 120.0 no C20 . C21 . C16 . 119.8(5) yes C20 . C21 . H211 . 120.1 no C16 . C21 . H211 . 120.1 no N1 . C22 . O7 . 124.1(6) yes N1 . C22 . H221 . 117.9 no O7 . C22 . H221 . 117.9 no N1 . C23 . H231 . 109.5 no N1 . C23 . H232 . 109.3 no H231 . C23 . H232 . 109.1 no N1 . C23 . H233 . 109.9 no H231 . C23 . H233 . 109.7 no H232 . C23 . H233 . 109.4 no N1 . C24 . H241 . 109.5 no N1 . C24 . H242 . 109.7 no H241 . C24 . H242 . 109.2 no N1 . C24 . H243 . 109.8 no H241 . C24 . H243 . 109.2 no H242 . C24 . H243 . 109.5 no data_gdpol3_Phase1_0_55GPa _database_code_depnum_ccdc_archive 'CCDC 768038' #TrackingRef '- Gd_polymer_cifs.cif' #0.55 GPa data set. _audit_creation_date 08-06-27 _audit_creation_method CRYSTALS_ver_12.85 _oxford_structure_analysis_title 'gdpol3 in P4(2)/n' _chemical_name_systematic ; catena-((\m~2~-Benzoato-O,O')-bis(\m~2~-benzoato-O,O',O')-(dimethylformamide-O )-gadolinium) ; _chemical_melting_point ? _publ_section_exptl_prep ; ? ; #end of refcif _publ_section_exptl_refinement ; Pressure = 0.55 GPa. H atoms placed geometrically after each cycle. Because completeness is less than 100% the ligands were restrained to have the same bond distances and angles as at ambient pressure. Checkcif alerts: 027_ALERT_3_A _diffrn_reflns_theta_full (too) Low ............ 15.34 Deg. 029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.70 911_ALERT_3_B # Missing FCF Refl Between THmin & STh/L= 0.600 1315 913_ALERT_3_B # Missing Very Strong Reflections in FCF ....... 167 910_ALERT_3_C # Missing FCF Reflections Below Th(Min) ........ 2 912_ALERT_4_C # Missing FCF Reflections Above STh/L= 0.600 1608 Data are incomplete becasue of shading of reciprocal space by the body of the pressure cell. 232_ALERT_2_C Hirshfeld Test Diff (M-X) Gd1 -- O1_a .. 5.01 su 232_ALERT_2_C Hirshfeld Test Diff (M-X) Gd1 -- O2_a .. 6.11 su No action taken. There is no question about the identities of the atoms, though adps will be distorted if completeness is low in one direction of reciprocal space, as is the case here. 213_ALERT_2_C Atom C4 has ADP max/min Ratio ............. 3.30 oblat 220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.70 Ratio 342_ALERT_3_C Low Bond Precision on C-C Bonds (x 1000) Ang ... 9 None of this is surprising given the completeness, temperature and presence of the heavy atom. 860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 86 See above 042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? The one given is more chemically meanigful. 128_ALERT_4_C Non-standard setting of Space-group P42/n .... P42/n:1 See text. This makes comparison with the high pressure phase simpler. 034_ALERT_1_C No Flack Parameter Given. Z .GT. Si, NonCentro . ? This is a bug in Checkcif. The space group operation '-x+1/2,-y+1/2,-z+1/2' is an inversion centre at [1/4 1/4 1/4]. This test shouldn't be applied, but presumably is triggered when the -1 is not on the origin. 199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K 200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K Correct. ; _cell_length_a 22.0678(4) _cell_length_b 22.0678(4) _cell_length_c 9.1203(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 4441.48(19) _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'P 42/n:1' _symmetry_space_group_name_Hall 'P 4n -1n' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,z -y+1/2,x+1/2,z+1/2 y+1/2,-x+1/2,z+1/2 -x+1/2,-y+1/2,-z+1/2 x+1/2,y+1/2,-z+1/2 y,-x,-z -y,x,-z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0010 0.0010 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0020 0.0010 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0040 0.0030 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Gd -0.5090 2.0340 25.0709 2.2534 19.0798 0.1820 13.8518 12.9331 3.5454 101.3980 2.4196 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 8 _chemical_formula_sum 'C24 H22 Gd1 N1 O7' _chemical_formula_moiety ; (C24 H22 Gd1 N1 O7)n ; _chemical_compound_source ? _chemical_formula_weight 593.69 _cell_measurement_reflns_used 4685 _cell_measurement_theta_min 3 _cell_measurement_theta_max 20 _cell_measurement_temperature 293 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_max 0.20 _exptl_crystal_density_diffrn 1.776 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 2344 _exptl_absorpt_coefficient_mu 0.967 # Sheldrick geometric approximatio 0.55 0.74 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.07 _exptl_absorpt_correction_T_max 0.74 _diffrn_measurement_device 'Bruker SMART' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator Silicon _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.48650 _diffrn_source synchrotron _diffrn_measurement_method \w _computing_data_collection 'SMART (Siemens, 1993)' _computing_cell_refinement 'SAINT (Siemens ,1995)' _computing_data_reduction 'SAINT (Siemens ,1995)' _computing_structure_solution 'USER DEFINED STRUCTURE SOLUTION' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'DIAMOND Crystal Impact (2004)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 293 _diffrn_reflns_number 24076 _reflns_number_total 3876 _diffrn_reflns_av_R_equivalents 0.097 _diffrn_reflns_theta_min 1.263 _diffrn_reflns_theta_max 20.458 _diffrn_measured_fraction_theta_max 0.562 _diffrn_reflns_theta_full 15.343 _diffrn_measured_fraction_theta_full 0.700 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _reflns_limit_h_min -12 _reflns_limit_h_max 14 _reflns_limit_k_min 0 _reflns_limit_k_max 29 _reflns_limit_l_min 0 _reflns_limit_l_max 13 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom _atom_sites_solution_hydrogens geom _refine_diff_density_min -4.43 _refine_diff_density_max 2.61 _oxford_reflns_threshold_expression_ref I>2.0\s(I) _refine_ls_number_reflns 2805 _refine_ls_number_restraints 86 _refine_ls_number_parameters 298 _oxford_refine_ls_R_factor_ref 0.0729 _refine_ls_wR_factor_ref 0.0759 _refine_ls_goodness_of_fit_ref 1.0284 _refine_ls_shift/su_max 0.001877 # The values computed from all data _oxford_reflns_number_all 3873 _refine_ls_R_factor_all 0.0965 _refine_ls_wR_factor_all 0.0965 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 2805 _refine_ls_R_factor_gt 0.0729 _refine_ls_wR_factor_gt 0.0759 _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment noref # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 2.27 2.10 1.44 ; _publ_section_references ; User-defined structure solution reference Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Siemens Industrial Automation, Inc (1993). SMART: Area-Detector Software Package; Madison, WI. Siemens Industrial Automation, Inc (1995). SAINT: Area-Detector Integration Software.; Madison, WI. Siemens Industrial Automation, Inc (1996). SADABS: Area-Detector Absorption Correction;: Madison, WI. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Gd1 Gd 0.739780(19) 0.749318(15) -0.03805(3) 0.0185 1.0000 Uani . . . . . . . O1 O 0.7910(2) 0.6997(2) -0.2245(4) 0.0234 1.0000 Uani D . . . . . . O2 O 0.8496(2) 0.6833(3) -0.4148(4) 0.0327 1.0000 Uani D . . . . . . O3 O 0.6698(2) 0.6826(2) -0.1579(4) 0.0271 1.0000 Uani D . . . . . . O4 O 0.6924(3) 0.6723(2) -0.3957(4) 0.0324 1.0000 Uani D . . . . . . O5 O 0.7186(3) 0.6708(2) 0.1272(4) 0.0330 1.0000 Uani D . . . . . . O6 O 0.7657(3) 0.6891(2) 0.3372(4) 0.0288 1.0000 Uani D . . . . . . O7 O 0.8358(2) 0.7231(3) 0.0693(4) 0.0324 1.0000 Uani D . . . . . . N1 N 0.9075(3) 0.7275(3) 0.2463(6) 0.0381 1.0000 Uani D . . . . . . C1 C 0.8339(3) 0.6711(3) -0.2865(5) 0.0238 1.0000 Uani D . . . . . . C2 C 0.8632(2) 0.6214(3) -0.2030(5) 0.0256 1.0000 Uani D . . . . . . C3 C 0.9222(3) 0.6057(3) -0.2351(7) 0.0412 1.0000 Uani D . . . . . . C4 C 0.9524(3) 0.5620(3) -0.1521(8) 0.0564 1.0000 Uani D . . . . . . C5 C 0.9228(4) 0.5340(3) -0.0377(7) 0.0482 1.0000 Uani D . . . . . . C6 C 0.8638(3) 0.5497(3) -0.0061(6) 0.0426 1.0000 Uani D . . . . . . C7 C 0.8344(3) 0.5933(3) -0.0871(5) 0.0318 1.0000 Uani D . . . . . . C8 C 0.6681(3) 0.6536(3) -0.2765(5) 0.0244 1.0000 Uani D . . . . . . C9 C 0.6389(2) 0.5928(2) -0.2791(5) 0.0232 1.0000 Uani D . . . . . . C10 C 0.6129(3) 0.5705(3) -0.1524(6) 0.0419 1.0000 Uani D . . . . . . C11 C 0.5849(3) 0.5141(3) -0.1531(7) 0.0443 1.0000 Uani D . . . . . . C12 C 0.5823(3) 0.4813(3) -0.2802(9) 0.0554 1.0000 Uani D . . . . . . C13 C 0.6078(3) 0.5032(3) -0.4060(7) 0.0500 1.0000 Uani D . . . . . . C14 C 0.6359(3) 0.5586(3) -0.4062(6) 0.0377 1.0000 Uani D . . . . . . C15 C 0.7433(3) 0.6534(2) 0.2460(5) 0.0289 1.0000 Uani D . . . . . . C16 C 0.7433(3) 0.5868(2) 0.2760(5) 0.0236 1.0000 Uani D . . . . . . C17 C 0.7777(3) 0.5648(3) 0.3911(6) 0.0363 1.0000 Uani D . . . . . . C18 C 0.7772(3) 0.5027(3) 0.4209(7) 0.0470 1.0000 Uani D . . . . . . C19 C 0.7425(3) 0.4648(3) 0.3380(7) 0.0468 1.0000 Uani D . . . . . . C20 C 0.7084(3) 0.4864(3) 0.2240(7) 0.0417 1.0000 Uani D . . . . . . C21 C 0.7094(3) 0.5477(3) 0.1921(6) 0.0353 1.0000 Uani D . . . . . . C22 C 0.8688(3) 0.7522(3) 0.1540(6) 0.0313 1.0000 Uani D . . . . . . C23 C 0.9433(5) 0.7641(4) 0.3459(10) 0.0627 1.0000 Uani D . . . . . . C24 C 0.9144(4) 0.6626(4) 0.2554(7) 0.0430 1.0000 Uani D . . . . . . H231 H 0.9322 0.8060 0.3355 0.0685 1.0000 Uiso . . . . . . . H232 H 0.9856 0.7596 0.3224 0.0685 1.0000 Uiso . . . . . . . H233 H 0.9365 0.7513 0.4449 0.0685 1.0000 Uiso . . . . . . . H241 H 0.8888 0.6437 0.1838 0.0464 1.0000 Uiso . . . . . . . H242 H 0.9560 0.6519 0.2371 0.0464 1.0000 Uiso . . . . . . . H243 H 0.9029 0.6489 0.3515 0.0464 1.0000 Uiso . . . . . . . H31 H 0.9421 0.6245 -0.3128 0.0495 1.0000 Uiso . . . . . . . H41 H 0.9923 0.5518 -0.1738 0.0677 1.0000 Uiso . . . . . . . H51 H 0.9424 0.5046 0.0177 0.0579 1.0000 Uiso . . . . . . . H61 H 0.8436 0.5306 0.0707 0.0511 1.0000 Uiso . . . . . . . H71 H 0.7948 0.6040 -0.0635 0.0383 1.0000 Uiso . . . . . . . H101 H 0.6142 0.5932 -0.0666 0.0502 1.0000 Uiso . . . . . . . H111 H 0.5680 0.4987 -0.0675 0.0531 1.0000 Uiso . . . . . . . H121 H 0.5631 0.4438 -0.2810 0.0664 1.0000 Uiso . . . . . . . H131 H 0.6062 0.4805 -0.4918 0.0600 1.0000 Uiso . . . . . . . H141 H 0.6530 0.5733 -0.4923 0.0453 1.0000 Uiso . . . . . . . H171 H 0.8010 0.5910 0.4478 0.0436 1.0000 Uiso . . . . . . . H181 H 0.8005 0.4872 0.4972 0.0565 1.0000 Uiso . . . . . . . H191 H 0.7420 0.4235 0.3591 0.0561 1.0000 Uiso . . . . . . . H201 H 0.6847 0.4601 0.1686 0.0501 1.0000 Uiso . . . . . . . H211 H 0.6871 0.5625 0.1134 0.0423 1.0000 Uiso . . . . . . . H221 H 0.8661 0.7943 0.1523 0.0376 1.0000 Uiso . . . . . . . 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 Gd1 0.0233(2) 0.0192(2) 0.0129(2) 0.00136(9) 0.00026(9) 0.00115(17) O1 0.025(3) 0.022(2) 0.0238(16) -0.0058(17) -0.0018(16) 0.010(3) O2 0.035(3) 0.041(3) 0.0227(19) 0.0021(19) 0.0028(19) 0.001(4) O3 0.027(3) 0.032(3) 0.0220(18) -0.0027(17) -0.0011(16) -0.006(3) O4 0.040(3) 0.034(3) 0.0233(19) 0.0055(18) -0.004(2) -0.013(4) O5 0.044(3) 0.034(3) 0.0209(17) 0.0113(19) -0.0060(19) -0.006(4) O6 0.043(3) 0.027(3) 0.0162(16) -0.0060(16) 0.0008(17) 0.002(3) O7 0.031(3) 0.039(3) 0.026(2) -0.002(2) -0.0029(19) 0.014(4) N1 0.028(4) 0.051(5) 0.035(3) 0.003(3) -0.010(2) -0.005(5) C1 0.027(3) 0.023(3) 0.022(2) -0.003(2) 0.004(2) 0.009(4) C2 0.029(4) 0.030(4) 0.018(2) 0.000(2) 0.002(2) 0.009(5) C3 0.033(4) 0.039(5) 0.051(4) 0.015(4) 0.015(3) 0.012(6) C4 0.047(6) 0.046(6) 0.076(6) 0.016(5) 0.008(4) 0.037(7) C5 0.062(7) 0.031(5) 0.052(4) 0.016(3) -0.003(4) 0.027(7) C6 0.065(6) 0.029(5) 0.034(3) 0.008(3) 0.011(4) 0.024(6) C7 0.043(4) 0.030(4) 0.023(2) 0.000(2) 0.007(3) 0.013(5) C8 0.022(3) 0.027(4) 0.025(2) 0.005(2) -0.004(2) -0.004(4) C9 0.014(3) 0.030(4) 0.026(2) 0.006(2) 0.003(2) -0.010(4) C10 0.038(5) 0.049(5) 0.039(3) 0.004(3) 0.013(3) -0.015(6) C11 0.048(6) 0.030(4) 0.055(4) 0.010(3) 0.027(4) 0.004(6) C12 0.039(5) 0.029(5) 0.098(7) -0.001(4) 0.009(5) -0.013(6) C13 0.052(6) 0.043(5) 0.055(5) -0.011(4) 0.007(4) -0.004(7) C14 0.038(5) 0.043(5) 0.032(3) -0.001(3) -0.002(3) -0.018(6) C15 0.049(5) 0.018(3) 0.019(3) 0.000(2) 0.006(3) 0.010(5) C16 0.032(4) 0.019(3) 0.020(2) -0.001(2) 0.003(2) -0.012(4) C17 0.045(5) 0.034(4) 0.030(3) 0.008(3) -0.010(3) -0.004(5) C18 0.057(6) 0.038(5) 0.046(4) 0.015(3) -0.010(4) -0.011(7) C19 0.067(7) 0.023(4) 0.050(4) 0.010(3) 0.008(4) 0.006(6) C20 0.054(6) 0.025(4) 0.046(3) -0.005(3) 0.005(4) -0.015(6) C21 0.048(5) 0.028(4) 0.031(3) -0.002(3) 0.002(3) -0.006(6) C22 0.021(3) 0.046(5) 0.027(3) 0.006(3) 0.002(2) -0.008(5) C23 0.057(7) 0.062(7) 0.069(6) 0.004(5) -0.034(5) -0.016(8) C24 0.038(5) 0.055(6) 0.037(4) 0.006(4) -0.011(3) 0.004(6) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.2548(9) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Gd1 . O2 5_664 2.506(5) yes Gd1 . C1 5_664 2.880(5) yes Gd1 . O4 5_664 2.366(5) yes Gd1 . O6 5_665 2.284(4) yes Gd1 . O3 . 2.398(5) yes Gd1 . O5 . 2.344(4) yes Gd1 . O7 . 2.405(5) yes O1 . C1 . 1.271(6) yes O2 . C1 . 1.250(5) yes O3 . C8 . 1.257(5) yes O4 . C8 . 1.280(5) yes O5 . C15 . 1.272(5) yes O6 . C15 . 1.248(6) yes O7 . C22 . 1.241(6) yes N1 . C22 . 1.317(6) yes N1 . C23 . 1.451(7) yes N1 . C24 . 1.442(8) yes C1 . C2 . 1.482(6) yes C2 . C3 . 1.379(7) yes C2 . C7 . 1.381(6) yes C3 . C4 . 1.397(7) yes C3 . H31 . 0.930 no C4 . C5 . 1.377(7) yes C4 . H41 . 0.930 no C5 . C6 . 1.378(8) yes C5 . H51 . 0.930 no C6 . C7 . 1.376(7) yes C6 . H61 . 0.930 no C7 . H71 . 0.930 no C8 . C9 . 1.490(6) yes C9 . C10 . 1.381(6) yes C9 . C14 . 1.385(6) yes C10 . C11 . 1.390(7) yes C10 . H101 . 0.930 no C11 . C12 . 1.368(7) yes C11 . H111 . 0.930 no C12 . C13 . 1.367(7) yes C12 . H121 . 0.930 no C13 . C14 . 1.370(7) yes C13 . H131 . 0.930 no C14 . H141 . 0.930 no C15 . C16 . 1.495(6) yes C16 . C17 . 1.384(6) yes C16 . C21 . 1.374(7) yes C17 . C18 . 1.398(7) yes C17 . H171 . 0.930 no C18 . C19 . 1.363(7) yes C18 . H181 . 0.930 no C19 . C20 . 1.369(7) yes C19 . H191 . 0.930 no C20 . C21 . 1.384(7) yes C20 . H201 . 0.930 no C21 . H211 . 0.930 no C22 . H221 . 0.930 no C23 . H231 . 0.961 no C23 . H232 . 0.963 no C23 . H233 . 0.958 no C24 . H241 . 0.959 no C24 . H242 . 0.961 no C24 . H243 . 0.962 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O2 5_664 Gd1 . C1 5_664 25.65(12) yes O2 5_664 Gd1 . O4 5_664 91.18(17) yes C1 5_664 Gd1 . O4 5_664 76.69(19) yes O2 5_664 Gd1 . O6 5_665 75.09(17) yes C1 5_664 Gd1 . O6 5_665 93.00(16) yes O4 5_664 Gd1 . O6 5_665 78.63(17) yes O2 5_664 Gd1 . O3 . 77.23(17) yes C1 5_664 Gd1 . O3 . 75.95(18) yes O4 5_664 Gd1 . O3 . 137.75(13) yes O6 5_665 Gd1 . O3 . 134.19(17) yes O2 5_664 Gd1 . O5 . 113.06(18) yes C1 5_664 Gd1 . O5 . 134.08(19) yes O4 5_664 Gd1 . O5 . 146.19(17) yes O6 5_665 Gd1 . O5 . 85.07(16) yes O3 . Gd1 . O5 . 73.19(16) yes O2 5_664 Gd1 . O7 . 154.89(17) yes C1 5_664 Gd1 . O7 . 150.5(2) yes O4 5_664 Gd1 . O7 . 73.84(19) yes O6 5_665 Gd1 . O7 . 82.15(18) yes O3 . Gd1 . O7 . 127.30(19) yes O5 . Gd1 . O7 . 74.73(19) yes Gd1 5_664 O2 . C1 . 94.1(3) yes Gd1 . O3 . C8 . 136.3(4) yes Gd1 5_664 O4 . C8 . 135.8(3) yes Gd1 . O5 . C15 . 133.3(4) yes Gd1 5_665 O6 . C15 . 152.8(5) yes Gd1 . O7 . C22 . 130.3(4) yes C22 . N1 . C23 . 121.5(5) yes C22 . N1 . C24 . 121.2(5) yes C23 . N1 . C24 . 117.3(5) yes Gd1 5_664 C1 . O1 . 61.5(3) yes Gd1 5_664 C1 . O2 . 60.2(3) yes O1 . C1 . O2 . 121.0(5) yes Gd1 5_664 C1 . C2 . 169.2(5) yes O1 . C1 . C2 . 117.6(4) yes O2 . C1 . C2 . 121.4(4) yes C1 . C2 . C3 . 119.2(4) yes C1 . C2 . C7 . 121.6(4) yes C3 . C2 . C7 . 119.0(4) yes C2 . C3 . C4 . 120.6(5) yes C2 . C3 . H31 . 119.7 no C4 . C3 . H31 . 119.7 no C3 . C4 . C5 . 119.6(5) yes C3 . C4 . H41 . 120.2 no C5 . C4 . H41 . 120.2 no C4 . C5 . C6 . 119.7(5) yes C4 . C5 . H51 . 120.1 no C6 . C5 . H51 . 120.2 no C5 . C6 . C7 . 120.6(5) yes C5 . C6 . H61 . 119.7 no C7 . C6 . H61 . 119.7 no C2 . C7 . C6 . 120.5(5) yes C2 . C7 . H71 . 119.7 no C6 . C7 . H71 . 119.7 no O4 . C8 . O3 . 123.7(5) yes O4 . C8 . C9 . 117.2(4) yes O3 . C8 . C9 . 119.0(4) yes C8 . C9 . C10 . 119.2(4) yes C8 . C9 . C14 . 121.7(4) yes C10 . C9 . C14 . 119.1(4) yes C9 . C10 . C11 . 120.0(5) yes C9 . C10 . H101 . 120.0 no C11 . C10 . H101 . 120.0 no C10 . C11 . C12 . 119.8(5) yes C10 . C11 . H111 . 120.1 no C12 . C11 . H111 . 120.1 no C11 . C12 . C13 . 120.4(5) yes C11 . C12 . H121 . 119.8 no C13 . C12 . H121 . 119.8 no C12 . C13 . C14 . 120.2(5) yes C12 . C13 . H131 . 119.9 no C14 . C13 . H131 . 119.9 no C9 . C14 . C13 . 120.4(5) yes C9 . C14 . H141 . 119.8 no C13 . C14 . H141 . 119.8 no O5 . C15 . O6 . 123.2(5) yes O5 . C15 . C16 . 116.9(4) yes O6 . C15 . C16 . 119.9(4) yes C15 . C16 . C17 . 118.9(4) yes C15 . C16 . C21 . 121.0(4) yes C17 . C16 . C21 . 120.1(4) yes C16 . C17 . C18 . 119.1(5) yes C16 . C17 . H171 . 120.5 no C18 . C17 . H171 . 120.4 no C17 . C18 . C19 . 119.9(5) yes C17 . C18 . H181 . 120.1 no C19 . C18 . H181 . 120.0 no C18 . C19 . C20 . 121.1(5) yes C18 . C19 . H191 . 119.5 no C20 . C19 . H191 . 119.4 no C19 . C20 . C21 . 119.4(5) yes C19 . C20 . H201 . 120.3 no C21 . C20 . H201 . 120.3 no C20 . C21 . C16 . 120.4(5) yes C20 . C21 . H211 . 119.8 no C16 . C21 . H211 . 119.8 no N1 . C22 . O7 . 124.3(5) yes N1 . C22 . H221 . 117.8 no O7 . C22 . H221 . 117.9 no N1 . C23 . H231 . 109.5 no N1 . C23 . H232 . 109.4 no H231 . C23 . H232 . 109.0 no N1 . C23 . H233 . 109.9 no H231 . C23 . H233 . 109.6 no H232 . C23 . H233 . 109.4 no N1 . C24 . H241 . 109.3 no N1 . C24 . H242 . 109.7 no H241 . C24 . H242 . 109.7 no N1 . C24 . H243 . 109.6 no H241 . C24 . H243 . 109.1 no H242 . C24 . H243 . 109.5 no data_gdpol4_Phase1_1_18GPa _database_code_depnum_ccdc_archive 'CCDC 768039' #TrackingRef '- Gd_polymer_cifs.cif' #1.18 GPa data set _audit_creation_date 08-06-30 _audit_creation_method CRYSTALS_ver_12.85 _oxford_structure_analysis_title 'gdpol4 in P4(2)/n' _chemical_name_systematic ; catena-((\m~2~-Benzoato-O,O')-bis(\m~2~-benzoato-O,O',O')-(dimethylformamide-O )-gadolinium) ; _chemical_melting_point ? _publ_section_exptl_prep ; ? ; #end of refcif _publ_section_exptl_refinement ; Pressure = 1.18 GPa. H atoms placed geometrically after each cycle. Because completeness is less than 100% the ligands were restrained to have the same bond distances and angles as at ambient pressure. Checkcif alerts: 027_ALERT_3_A _diffrn_reflns_theta_full (too) Low ............ 15.29 Deg. 029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.71 911_ALERT_3_B # Missing FCF Refl Between THmin & STh/L= 0.600 1218 913_ALERT_3_B # Missing Very Strong Reflections in FCF ....... 127 912_ALERT_4_C # Missing FCF Reflections Above STh/L= 0.600 1466 910_ALERT_3_C # Missing FCF Reflections Below Th(Min) ........ 2 Data are incomplete becasue of shading of reciprocal space by the body of the pressure cell. 919_ALERT_3_B # Reflections Likely Affected by the Beamstop .. 1 ...or the gasket 220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.81 Ratio Some distortion of the adps is expected given the completeness, temperature and presence of the heavy atom. 860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 86 See above. 042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? The one given is more chemically meaningful. 128_ALERT_4_C Non-standard setting of Space-group P42/n .... P42/n:1 See text. This makes comparison with the high pressure phase simpler. 034_ALERT_1_C No Flack Parameter Given. Z .GT. Si, NonCentro . ? This is a bug in Checkcif. The space group operation '-x+1/2,-y+1/2,-z+1/2' is an inversion centre at [1/4 1/4 1/4]. This test shouldn't be applied, but presumably is triggered when the -1 is not on the origin. 141_ALERT_4_C su on a - Axis Small or Missing (x 100000) ..... 20 Ang. No action 199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K 200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K Correct. 792_ALERT_1_G Check the Absolute Configuration of C1 = ... S The sum of the angles around C1 is 359.9(6) deg, so it is planar within error. Perhaps the algorithm is being 'put off' by a long Gd1-C1 'bond' in the connetivity list. No action. ; _cell_length_a 21.5853(2) _cell_length_b 21.5853(2) _cell_length_c 9.04340(10) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 4213.55(7) _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'P 42/n:1' _symmetry_space_group_name_Hall 'P 4n -1n' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,z -y+1/2,x+1/2,z+1/2 y+1/2,-x+1/2,z+1/2 -x+1/2,-y+1/2,-z+1/2 x+1/2,y+1/2,-z+1/2 y,-x,-z -y,x,-z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0010 0.0010 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0020 0.0010 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0040 0.0030 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Gd -0.5090 2.0340 25.0709 2.2534 19.0798 0.1820 13.8518 12.9331 3.5454 101.3980 2.4196 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 8 _chemical_formula_sum 'C24 H22 Gd1 N1 O7' _chemical_formula_moiety ; (C24 H22 Gd1 N1 O7)n ; _chemical_compound_source ? _chemical_formula_weight 593.69 _cell_measurement_reflns_used 7446 _cell_measurement_theta_min 3 _cell_measurement_theta_max 20 _cell_measurement_temperature 293 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_max 0.20 _exptl_crystal_density_diffrn 1.872 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 2344 _exptl_absorpt_coefficient_mu 1.019 # Sheldrick geometric approximatio 0.53 0.73 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.04 _exptl_absorpt_correction_T_max 0.73 _diffrn_measurement_device 'Bruker SMART' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator Silicon _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.48650 _diffrn_source synchrotron _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'SMART (Siemens, 1993)' _computing_cell_refinement 'SAINT (Siemens ,1995)' _computing_data_reduction 'SAINT (Siemens ,1995)' _computing_structure_solution 'USER DEFINED STRUCTURE SOLUTION' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' __computing_molecular_graphics 'DIAMOND Crystal Impact (2004)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 293 _diffrn_reflns_number 22343 _reflns_number_total 3763 _diffrn_reflns_av_R_equivalents 0.072 _diffrn_reflns_theta_min 1.291 _diffrn_reflns_theta_max 20.382 _diffrn_measured_fraction_theta_max 0.581 _diffrn_reflns_theta_full 15.287 _diffrn_measured_fraction_theta_full 0.710 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _reflns_limit_h_min -14 _reflns_limit_h_max 15 _reflns_limit_k_min 0 _reflns_limit_k_max 29 _reflns_limit_l_min 0 _reflns_limit_l_max 12 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom _atom_sites_solution_hydrogens geom _refine_diff_density_min -3.17 _refine_diff_density_max 2.44 # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>2.0\s(I) _refine_ls_number_reflns 2954 _refine_ls_number_restraints 86 _refine_ls_number_parameters 298 _oxford_refine_ls_R_factor_ref 0.0575 _refine_ls_wR_factor_ref 0.0614 _refine_ls_goodness_of_fit_ref 1.0248 _refine_ls_shift/su_max 0.002296 # The values computed from all data _oxford_reflns_number_all 3749 _refine_ls_R_factor_all 0.0760 _refine_ls_wR_factor_all 0.0744 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 2954 _refine_ls_R_factor_gt 0.0575 _refine_ls_wR_factor_gt 0.0614 _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment noref # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 1.76 1.23 1.08 ; # Insert your own references if required - in alphabetical order _publ_section_references ; User-defined structure solution reference Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Siemens Industrial Automation, Inc (1993). SMART: Area-Detector Software Package; Madison, WI. Siemens Industrial Automation, Inc (1995). SAINT: Area-Detector Integration Software.; Madison, WI. Siemens Industrial Automation, Inc (1996). SADABS: Area-Detector Absorption Correction;: Madison, WI. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Gd1 Gd 0.738612(15) 0.749186(12) -0.03743(2) 0.0143 1.0000 Uani . . . . . . . O1 O 0.79179(18) 0.69977(18) -0.2266(3) 0.0218 1.0000 Uani D . . . . . . O2 O 0.85248(19) 0.6808(2) -0.4143(3) 0.0281 1.0000 Uani D . . . . . . O3 O 0.66939(19) 0.6801(2) -0.1590(3) 0.0248 1.0000 Uani D . . . . . . O4 O 0.6924(2) 0.66948(19) -0.3990(3) 0.0279 1.0000 Uani D . . . . . . O5 O 0.7158(2) 0.66962(18) 0.1282(3) 0.0270 1.0000 Uani D . . . . . . O6 O 0.7674(2) 0.68793(18) 0.3352(3) 0.0251 1.0000 Uani D . . . . . . O7 O 0.83670(19) 0.7223(2) 0.0689(3) 0.0273 1.0000 Uani D . . . . . . N1 N 0.9084(2) 0.7260(2) 0.2507(4) 0.0285 1.0000 Uani D . . . . . . C1 C 0.8360(2) 0.6697(2) -0.2855(4) 0.0171 1.0000 Uani D . . . . . . C2 C 0.8640(2) 0.6190(2) -0.1974(4) 0.0200 1.0000 Uani D . . . . . . C3 C 0.9257(3) 0.6044(3) -0.2221(5) 0.0352 1.0000 Uani D . . . . . . C4 C 0.9555(3) 0.5615(3) -0.1320(6) 0.0477 1.0000 Uani D . . . . . . C5 C 0.9233(3) 0.5337(3) -0.0197(5) 0.0358 1.0000 Uani D . . . . . . C6 C 0.8616(3) 0.5469(3) 0.0029(5) 0.0304 1.0000 Uani D . . . . . . C7 C 0.8319(2) 0.5904(2) -0.0847(4) 0.0251 1.0000 Uani D . . . . . . C8 C 0.6687(2) 0.6500(2) -0.2784(4) 0.0181 1.0000 Uani D . . . . . . C9 C 0.6393(2) 0.5875(2) -0.2811(4) 0.0223 1.0000 Uani D . . . . . . C10 C 0.6115(2) 0.5649(2) -0.1533(5) 0.0271 1.0000 Uani D . . . . . . C11 C 0.5826(3) 0.5073(3) -0.1552(5) 0.0379 1.0000 Uani D . . . . . . C12 C 0.5816(3) 0.4726(3) -0.2828(6) 0.0400 1.0000 Uani D . . . . . . C13 C 0.6094(3) 0.4948(3) -0.4100(5) 0.0389 1.0000 Uani D . . . . . . C14 C 0.6377(3) 0.5522(2) -0.4090(5) 0.0298 1.0000 Uani D . . . . . . C15 C 0.7430(2) 0.6517(2) 0.2452(4) 0.0220 1.0000 Uani D . . . . . . C16 C 0.7424(2) 0.5844(2) 0.2779(4) 0.0205 1.0000 Uani D . . . . . . C17 C 0.7781(2) 0.5614(2) 0.3935(5) 0.0262 1.0000 Uani D . . . . . . C18 C 0.7774(3) 0.4981(3) 0.4241(5) 0.0380 1.0000 Uani D . . . . . . C19 C 0.7413(3) 0.4592(2) 0.3410(5) 0.0389 1.0000 Uani D . . . . . . C20 C 0.7063(3) 0.4815(2) 0.2251(5) 0.0324 1.0000 Uani D . . . . . . C21 C 0.7072(3) 0.5439(2) 0.1933(5) 0.0269 1.0000 Uani D . . . . . . C22 C 0.8691(2) 0.7517(3) 0.1579(5) 0.0279 1.0000 Uani D . . . . . . C23 C 0.9437(4) 0.7634(3) 0.3537(7) 0.0450 1.0000 Uani D . . . . . . C24 C 0.9152(3) 0.6594(3) 0.2594(5) 0.0368 1.0000 Uani D . . . . . . H231 H 0.9261 0.8043 0.3572 0.0521 1.0000 Uiso . . . . . . . H232 H 0.9860 0.7658 0.3211 0.0521 1.0000 Uiso . . . . . . . H233 H 0.9421 0.7449 0.4504 0.0521 1.0000 Uiso . . . . . . . H241 H 0.8902 0.6401 0.1849 0.0388 1.0000 Uiso . . . . . . . H242 H 0.9580 0.6485 0.2431 0.0388 1.0000 Uiso . . . . . . . H243 H 0.9027 0.6449 0.3552 0.0388 1.0000 Uiso . . . . . . . H31 H 0.9472 0.6233 -0.2990 0.0422 1.0000 Uiso . . . . . . . H41 H 0.9970 0.5519 -0.1479 0.0571 1.0000 Uiso . . . . . . . H51 H 0.9433 0.5055 0.0419 0.0429 1.0000 Uiso . . . . . . . H61 H 0.8398 0.5266 0.0772 0.0364 1.0000 Uiso . . . . . . . H71 H 0.7906 0.6002 -0.0677 0.0301 1.0000 Uiso . . . . . . . H101 H 0.6123 0.5883 -0.0669 0.0325 1.0000 Uiso . . . . . . . H111 H 0.5639 0.4923 -0.0699 0.0456 1.0000 Uiso . . . . . . . H121 H 0.5621 0.4342 -0.2835 0.0480 1.0000 Uiso . . . . . . . H131 H 0.6090 0.4712 -0.4959 0.0467 1.0000 Uiso . . . . . . . H141 H 0.6558 0.5673 -0.4951 0.0358 1.0000 Uiso . . . . . . . H171 H 0.8022 0.5881 0.4501 0.0314 1.0000 Uiso . . . . . . . H181 H 0.8015 0.4824 0.5007 0.0456 1.0000 Uiso . . . . . . . H191 H 0.7403 0.4171 0.3632 0.0466 1.0000 Uiso . . . . . . . H201 H 0.6822 0.4547 0.1687 0.0388 1.0000 Uiso . . . . . . . H211 H 0.6841 0.5590 0.1145 0.0323 1.0000 Uiso . . . . . . . H221 H 0.8654 0.7947 0.1591 0.0335 1.0000 Uiso . . . . . . . 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 Gd1 0.01780(19) 0.01517(19) 0.00995(15) 0.00128(6) -0.00001(6) 0.00080(12) O1 0.027(2) 0.021(2) 0.0172(12) -0.0018(12) 0.0002(12) 0.012(2) O2 0.031(2) 0.037(3) 0.0161(13) 0.0034(14) 0.0026(13) 0.015(3) O3 0.023(2) 0.033(2) 0.0191(13) -0.0012(13) -0.0016(12) -0.004(2) O4 0.036(2) 0.030(2) 0.0179(13) 0.0030(13) 0.0012(14) -0.006(3) O5 0.040(3) 0.024(2) 0.0176(13) 0.0077(13) -0.0054(14) 0.000(3) O6 0.036(2) 0.023(2) 0.0166(12) -0.0016(12) 0.0031(13) -0.005(2) O7 0.022(2) 0.037(3) 0.0236(14) -0.0001(15) -0.0033(13) 0.008(3) N1 0.028(3) 0.037(3) 0.0205(18) 0.0000(17) -0.0061(16) -0.001(3) C1 0.016(3) 0.017(3) 0.0182(17) 0.0006(15) 0.0000(15) 0.000(3) C2 0.020(3) 0.021(3) 0.0195(17) 0.0025(16) 0.0024(16) 0.004(3) C3 0.027(3) 0.038(4) 0.041(3) 0.021(3) 0.012(2) 0.018(4) C4 0.025(4) 0.055(5) 0.063(4) 0.018(4) 0.006(3) 0.017(5) C5 0.045(4) 0.030(4) 0.032(2) 0.008(2) 0.001(2) 0.017(5) C6 0.038(4) 0.026(3) 0.027(2) 0.009(2) 0.006(2) 0.006(4) C7 0.027(3) 0.026(3) 0.0225(18) 0.0009(19) 0.0023(18) 0.013(3) C8 0.019(3) 0.017(3) 0.0184(15) 0.0019(16) -0.0013(16) 0.000(3) C9 0.022(3) 0.022(3) 0.0227(18) 0.0004(17) 0.0041(17) -0.002(3) C10 0.027(3) 0.026(3) 0.028(2) 0.0067(19) 0.0041(19) -0.001(4) C11 0.044(4) 0.025(3) 0.044(3) 0.009(2) 0.015(3) 0.011(4) C12 0.038(4) 0.019(3) 0.064(4) 0.001(3) 0.009(3) 0.004(4) C13 0.047(5) 0.033(4) 0.037(3) -0.005(2) 0.004(3) -0.006(5) C14 0.037(4) 0.025(3) 0.028(2) -0.0010(19) 0.005(2) 0.000(4) C15 0.031(3) 0.020(3) 0.0145(18) 0.0010(15) 0.0078(17) -0.001(3) C16 0.027(3) 0.020(3) 0.0151(15) 0.0023(15) -0.0014(17) -0.005(3) C17 0.030(3) 0.025(3) 0.0233(19) 0.0026(18) -0.0024(19) 0.003(4) C18 0.051(5) 0.030(4) 0.033(2) 0.012(2) -0.009(3) 0.000(5) C19 0.061(5) 0.017(3) 0.039(3) 0.002(2) 0.009(3) -0.001(4) C20 0.037(4) 0.023(3) 0.037(2) -0.004(2) 0.001(2) -0.005(4) C21 0.028(3) 0.026(3) 0.026(2) 0.0004(19) 0.000(2) -0.008(4) C22 0.016(3) 0.045(4) 0.023(2) 0.005(2) 0.0027(17) -0.012(3) C23 0.037(4) 0.051(5) 0.047(3) -0.002(3) -0.017(3) -0.020(5) C24 0.039(4) 0.044(4) 0.028(2) 0.000(2) -0.008(2) 0.007(4) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.3197(9) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Gd1 . O2 5_664 2.518(4) yes Gd1 . O1 5_664 2.489(3) yes Gd1 . O4 5_664 2.372(4) yes Gd1 . O6 5_665 2.281(3) yes Gd1 . O1 . 2.320(3) yes Gd1 . O3 . 2.379(4) yes Gd1 . O5 . 2.331(3) yes Gd1 . O7 . 2.397(4) yes O1 . C1 . 1.270(5) yes O2 . C1 . 1.241(4) yes O3 . C8 . 1.261(5) yes O4 . C8 . 1.276(4) yes O5 . C15 . 1.271(5) yes O6 . C15 . 1.246(5) yes O7 . C22 . 1.242(5) yes N1 . C22 . 1.315(5) yes N1 . C23 . 1.449(6) yes N1 . C24 . 1.448(7) yes C1 . C2 . 1.484(5) yes C2 . C3 . 1.387(6) yes C2 . C7 . 1.378(5) yes C3 . C4 . 1.391(6) yes C3 . H31 . 0.930 no C4 . C5 . 1.370(6) yes C4 . H41 . 0.930 no C5 . C6 . 1.378(7) yes C5 . H51 . 0.930 no C6 . C7 . 1.385(6) yes C6 . H61 . 0.930 no C7 . H71 . 0.930 no C8 . C9 . 1.491(5) yes C9 . C10 . 1.390(5) yes C9 . C14 . 1.386(5) yes C10 . C11 . 1.391(6) yes C10 . H101 . 0.930 no C11 . C12 . 1.376(6) yes C11 . H111 . 0.930 no C12 . C13 . 1.383(6) yes C12 . H121 . 0.930 no C13 . C14 . 1.381(6) yes C13 . H131 . 0.930 no C14 . H141 . 0.930 no C15 . C16 . 1.482(5) yes C16 . C17 . 1.389(5) yes C16 . C21 . 1.389(6) yes C17 . C18 . 1.394(6) yes C17 . H171 . 0.930 no C18 . C19 . 1.371(6) yes C18 . H181 . 0.930 no C19 . C20 . 1.380(6) yes C19 . H191 . 0.930 no C20 . C21 . 1.375(6) yes C20 . H201 . 0.930 no C21 . H211 . 0.930 no C22 . H221 . 0.930 no C23 . H231 . 0.961 no C23 . H232 . 0.960 no C23 . H233 . 0.962 no C24 . H241 . 0.958 no C24 . H242 . 0.965 no C24 . H243 . 0.960 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O2 5_664 Gd1 . O1 5_664 51.68(10) yes O2 5_664 Gd1 . O4 5_664 90.23(14) yes O1 5_664 Gd1 . O4 5_664 68.31(13) yes O2 5_664 Gd1 . O6 5_665 74.77(13) yes O1 5_664 Gd1 . O6 5_665 114.12(12) yes O4 5_664 Gd1 . O6 5_665 77.85(13) yes O2 5_664 Gd1 . O1 . 122.31(11) yes O1 5_664 Gd1 . O1 . 72.66(14) yes O4 5_664 Gd1 . O1 . 81.44(14) yes O6 5_665 Gd1 . O1 . 153.25(15) yes O2 5_664 Gd1 . O3 . 78.77(15) yes O1 5_664 Gd1 . O3 . 73.49(13) yes O4 5_664 Gd1 . O3 . 138.22(10) yes O6 5_665 Gd1 . O3 . 135.00(14) yes O1 . Gd1 . O3 . 71.47(14) yes O2 5_664 Gd1 . O5 . 112.85(14) yes O1 5_664 Gd1 . O5 . 145.18(14) yes O4 5_664 Gd1 . O5 . 146.44(13) yes O6 5_665 Gd1 . O5 . 84.91(12) yes O1 . Gd1 . O5 . 103.86(13) yes O2 5_664 Gd1 . O7 . 154.79(14) yes O1 5_664 Gd1 . O7 . 133.15(13) yes O4 5_664 Gd1 . O7 . 73.86(15) yes O6 5_665 Gd1 . O7 . 82.70(14) yes O1 . Gd1 . O7 . 75.37(12) yes O3 . Gd1 . O5 . 72.70(12) yes O3 . Gd1 . O7 . 126.04(15) yes O5 . Gd1 . O7 . 75.55(15) yes Gd1 5_664 O1 . Gd1 . 107.34(14) yes Gd1 5_664 O1 . C1 . 93.7(2) yes Gd1 . O1 . C1 . 156.2(3) yes Gd1 5_664 O2 . C1 . 93.1(3) yes Gd1 . O3 . C8 . 136.5(3) yes Gd1 5_664 O4 . C8 . 134.6(3) yes Gd1 . O5 . C15 . 131.4(3) yes Gd1 5_665 O6 . C15 . 150.8(4) yes Gd1 . O7 . C22 . 129.3(4) yes C22 . N1 . C23 . 120.9(4) yes C22 . N1 . C24 . 121.3(4) yes C23 . N1 . C24 . 117.7(4) yes O1 . C1 . O2 . 120.7(4) yes O1 . C1 . C2 . 117.3(3) yes O2 . C1 . C2 . 121.9(4) yes C1 . C2 . C3 . 118.2(4) yes C1 . C2 . C7 . 121.5(4) yes C3 . C2 . C7 . 120.0(4) yes C2 . C3 . C4 . 120.1(4) yes C2 . C3 . H31 . 120.0 no C4 . C3 . H31 . 120.0 no C3 . C4 . C5 . 119.5(5) yes C3 . C4 . H41 . 120.3 no C5 . C4 . H41 . 120.3 no C4 . C5 . C6 . 120.6(5) yes C4 . C5 . H51 . 119.7 no C6 . C5 . H51 . 119.7 no C5 . C6 . C7 . 120.2(4) yes C5 . C6 . H61 . 119.9 no C7 . C6 . H61 . 119.9 no C6 . C7 . C2 . 119.6(4) yes C6 . C7 . H71 . 120.2 no C2 . C7 . H71 . 120.2 no O4 . C8 . O3 . 123.9(4) yes O4 . C8 . C9 . 117.0(3) yes O3 . C8 . C9 . 119.0(3) yes C8 . C9 . C10 . 119.2(3) yes C8 . C9 . C14 . 121.5(3) yes C10 . C9 . C14 . 119.3(4) yes C9 . C10 . C11 . 119.8(4) yes C9 . C10 . H101 . 120.1 no C11 . C10 . H101 . 120.1 no C10 . C11 . C12 . 120.3(4) yes C10 . C11 . H111 . 119.8 no C12 . C11 . H111 . 119.9 no C11 . C12 . C13 . 120.1(4) yes C11 . C12 . H121 . 119.9 no C13 . C12 . H121 . 120.0 no C12 . C13 . C14 . 119.9(4) yes C12 . C13 . H131 . 120.1 no C14 . C13 . H131 . 120.1 no C9 . C14 . C13 . 120.6(4) yes C9 . C14 . H141 . 119.7 no C13 . C14 . H141 . 119.7 no O5 . C15 . O6 . 123.2(4) yes O5 . C15 . C16 . 117.5(4) yes O6 . C15 . C16 . 119.2(3) yes C15 . C16 . C17 . 119.7(4) yes C15 . C16 . C21 . 120.7(4) yes C17 . C16 . C21 . 119.5(4) yes C16 . C17 . C18 . 119.6(4) yes C16 . C17 . H171 . 120.2 no C18 . C17 . H171 . 120.2 no C17 . C18 . C19 . 119.9(4) yes C17 . C18 . H181 . 120.1 no C19 . C18 . H181 . 120.0 no C18 . C19 . C20 . 120.8(4) yes C18 . C19 . H191 . 119.6 no C20 . C19 . H191 . 119.5 no C19 . C20 . C21 . 119.5(4) yes C19 . C20 . H201 . 120.2 no C21 . C20 . H201 . 120.2 no C16 . C21 . C20 . 120.6(4) yes C16 . C21 . H211 . 119.7 no C20 . C21 . H211 . 119.7 no N1 . C22 . O7 . 124.1(5) yes N1 . C22 . H221 . 117.9 no O7 . C22 . H221 . 118.0 no N1 . C23 . H231 . 108.9 no N1 . C23 . H232 . 109.5 no H231 . C23 . H232 . 109.6 no N1 . C23 . H233 . 109.6 no H231 . C23 . H233 . 109.6 no H232 . C23 . H233 . 109.7 no N1 . C24 . H241 . 109.6 no N1 . C24 . H242 . 109.4 no H241 . C24 . H242 . 109.0 no N1 . C24 . H243 . 110.1 no H241 . C24 . H243 . 109.6 no H242 . C24 . H243 . 109.2 no data_gdpol5_Phase1_1_67GPa _database_code_depnum_ccdc_archive 'CCDC 768040' #TrackingRef '- Gd_polymer_cifs.cif' #1.67 GPa data set _audit_creation_date 08-06-30 _audit_creation_method CRYSTALS_ver_12.85 _oxford_structure_analysis_title 'gdpol5 in P4(2)/n' _chemical_name_systematic ; catena-((\m~2~-Benzoato-O,O')-bis(\m~2~-benzoato-O,O',O')-(dimethylformamide-O )-gadolinium) ; _chemical_melting_point ? _publ_section_exptl_prep ; ? ; #end of refcif _publ_section_exptl_refinement ; Pressure = 1.67 GPa. H atoms placed geometrically after each cycle. Because completeness is less than 100% the ligands were restrained to have the same bond distances and angles as at ambient pressure. Checkcif alerts: 027_ALERT_3_A _diffrn_reflns_theta_full (too) Low ............ 15.22 Deg. 029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.70 911_ALERT_3_B # Missing FCF Refl Between THmin & STh/L= 0.600 1242 910_ALERT_3_C # Missing FCF Reflections Below Th(Min) ........ 1 913_ALERT_3_C # Missing Very Strong Reflections in FCF ....... 85 912_ALERT_4_C # Missing FCF Reflections Above STh/L= 0.600 1348 Data are incomplete becasue of shading of reciprocal space by the body of the pressure cell. 919_ALERT_3_B # Reflections Likely Affected by the Beamstop .. 1 ...or the gasket. 213_ALERT_2_C Atom C18 has ADP max/min Ratio ............. 3.20 oblat 220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.69 Ratio Some distortion of the adps is expected given the completeness, temperature and presence of the heavy atom. 860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 86 See above. 042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? The one given is more chemically meaningful. 128_ALERT_4_C Non-standard setting of Space-group P42/n .... P42/n:1 See text. This makes comparison with the high pressure phase simpler. 034_ALERT_1_C No Flack Parameter Given. Z .GT. Si, NonCentro . ? This is a bug in Checkcif. The space group operation '-x+1/2,-y+1/2,-z+1/2' is an inversion centre at [1/4 1/4 1/4]. This test shouldn't be applied, but presumably is triggered when the -1 is not on the origin. 141_ALERT_4_C su on a - Axis Small or Missing (x 100000) ..... 20 Ang. No action 199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K 200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K Correct. 792_ALERT_1_G Check the Absolute Configuration of C1 = ... S The sum of the angles around C1 is 360.1 deg, so it is planar within error. Perhaps the algorithm is being 'put off' by a long Gd1-C1 'bond' in the connetivity list. No action. ; _cell_length_a 21.3751(2) _cell_length_b 21.3751(2) _cell_length_c 9.00870(10) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 4116.03(7) _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'P 42/n:1' _symmetry_space_group_name_Hall 'P 4n -1n' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,z -y+1/2,x+1/2,z+1/2 y+1/2,-x+1/2,z+1/2 -x+1/2,-y+1/2,-z+1/2 x+1/2,y+1/2,-z+1/2 y,-x,-z -y,x,-z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0010 0.0010 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0020 0.0010 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0040 0.0030 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Gd -0.5090 2.0340 25.0709 2.2534 19.0798 0.1820 13.8518 12.9331 3.5454 101.3980 2.4196 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 8 _chemical_formula_sum 'C24 H22 Gd1 N1 O7' _chemical_formula_moiety ; (C24 H22 Gd1 N1 O7)n ; _chemical_compound_source ? _chemical_formula_weight 593.69 _cell_measurement_reflns_used 6866 _cell_measurement_theta_min 2 _cell_measurement_theta_max 20 _cell_measurement_temperature 293 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_max 0.20 _exptl_crystal_density_diffrn 1.916 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 2344 _exptl_absorpt_coefficient_mu 1.043 # Sheldrick geometric approximatio 0.52 0.72 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.07 _exptl_absorpt_correction_T_max 0.72 _diffrn_measurement_device 'Bruker SMART' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator Silicon _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.48650 _diffrn_source synchrotron _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'SMART (Siemens, 1993)' _computing_cell_refinement 'SAINT (Siemens ,1995)' _computing_data_reduction 'SAINT (Siemens ,1995)' _computing_structure_solution 'USER DEFINED STRUCTURE SOLUTION' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'DIAMOND Crystal Impact (2004)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 293 _diffrn_reflns_number 22005 _reflns_number_total 3629 _diffrn_reflns_av_R_equivalents 0.075 _diffrn_reflns_theta_min 1.304 _diffrn_reflns_theta_max 20.292 _diffrn_measured_fraction_theta_max 0.581 _diffrn_reflns_theta_full 15.219 _diffrn_measured_fraction_theta_full 0.705 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _reflns_limit_h_min -13 _reflns_limit_h_max 14 _reflns_limit_k_min 0 _reflns_limit_k_max 28 _reflns_limit_l_min 0 _reflns_limit_l_max 12 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.26 _refine_diff_density_max 1.66 # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>2.0\s(I) _refine_ls_number_reflns 2827 _refine_ls_number_restraints 86 _refine_ls_number_parameters 298 _oxford_refine_ls_R_factor_ref 0.0461 _refine_ls_wR_factor_ref 0.0579 _refine_ls_goodness_of_fit_ref 0.9251 _refine_ls_shift/su_max 0.000391 # The values computed from all data _oxford_reflns_number_all 3459 _refine_ls_R_factor_all 0.0566 _refine_ls_wR_factor_all 0.0693 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 2827 _refine_ls_R_factor_gt 0.0461 _refine_ls_wR_factor_gt 0.0579 _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment noref # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 1.88 1.04 1.12 ; _publ_section_references ; User-defined structure solution reference Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Siemens Industrial Automation, Inc (1993). SMART: Area-Detector Software Package; Madison, WI. Siemens Industrial Automation, Inc (1995). SAINT: Area-Detector Integration Software.; Madison, WI. Siemens Industrial Automation, Inc (1996). SADABS: Area-Detector Absorption Correction;: Madison, WI. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Gd1 Gd 0.738056(15) 0.749110(13) -0.03713(2) 0.0133 1.0000 Uani . . . . . . . O1 O 0.79229(19) 0.70026(19) -0.2260(3) 0.0185 1.0000 Uani D . . . . . . O2 O 0.8538(2) 0.6800(2) -0.4151(3) 0.0262 1.0000 Uani D . . . . . . O3 O 0.6691(2) 0.6786(2) -0.1597(3) 0.0223 1.0000 Uani D . . . . . . O4 O 0.6929(2) 0.6681(2) -0.4003(3) 0.0245 1.0000 Uani D . . . . . . O5 O 0.7142(2) 0.6691(2) 0.1289(3) 0.0246 1.0000 Uani D . . . . . . O6 O 0.7684(2) 0.68782(19) 0.3348(3) 0.0231 1.0000 Uani D . . . . . . O7 O 0.8368(2) 0.7213(2) 0.0686(4) 0.0258 1.0000 Uani D . . . . . . N1 N 0.9090(3) 0.7256(2) 0.2531(4) 0.0268 1.0000 Uani D . . . . . . C1 C 0.8363(2) 0.6689(2) -0.2854(4) 0.0179 1.0000 Uani D . . . . . . C2 C 0.8641(2) 0.6179(2) -0.1958(4) 0.0191 1.0000 Uani D . . . . . . C3 C 0.9261(3) 0.6036(3) -0.2169(6) 0.0349 1.0000 Uani D . . . . . . C4 C 0.9564(3) 0.5622(3) -0.1229(7) 0.0446 1.0000 Uani D . . . . . . C5 C 0.9230(3) 0.5331(3) -0.0114(6) 0.0320 1.0000 Uani D . . . . . . C6 C 0.8605(3) 0.5467(3) 0.0086(5) 0.0265 1.0000 Uani D . . . . . . C7 C 0.8309(2) 0.5889(2) -0.0830(5) 0.0218 1.0000 Uani D . . . . . . C8 C 0.6692(3) 0.6483(2) -0.2792(4) 0.0170 1.0000 Uani D . . . . . . C9 C 0.6391(2) 0.5854(2) -0.2819(4) 0.0172 1.0000 Uani D . . . . . . C10 C 0.6115(3) 0.5621(3) -0.1538(5) 0.0266 1.0000 Uani D . . . . . . C11 C 0.5827(3) 0.5038(3) -0.1549(6) 0.0348 1.0000 Uani D . . . . . . C12 C 0.5817(3) 0.4695(3) -0.2832(7) 0.0382 1.0000 Uani D . . . . . . C13 C 0.6097(3) 0.4916(3) -0.4104(6) 0.0358 1.0000 Uani D . . . . . . C14 C 0.6383(3) 0.5492(3) -0.4094(5) 0.0260 1.0000 Uani D . . . . . . C15 C 0.7428(3) 0.6511(2) 0.2454(4) 0.0175 1.0000 Uani D . . . . . . C16 C 0.7420(2) 0.5832(2) 0.2777(4) 0.0167 1.0000 Uani D . . . . . . C17 C 0.7780(3) 0.5602(2) 0.3942(5) 0.0233 1.0000 Uani D . . . . . . C18 C 0.7771(3) 0.4965(3) 0.4258(6) 0.0349 1.0000 Uani D . . . . . . C19 C 0.7410(3) 0.4569(3) 0.3420(6) 0.0343 1.0000 Uani D . . . . . . C20 C 0.7054(3) 0.4799(3) 0.2264(5) 0.0272 1.0000 Uani D . . . . . . C21 C 0.7065(3) 0.5428(2) 0.1931(5) 0.0228 1.0000 Uani D . . . . . . C22 C 0.8697(3) 0.7518(3) 0.1583(5) 0.0257 1.0000 Uani D . . . . . . C23 C 0.9441(4) 0.7631(4) 0.3575(7) 0.0420 1.0000 Uani D . . . . . . C24 C 0.9162(3) 0.6587(3) 0.2606(6) 0.0316 1.0000 Uani D . . . . . . H231 H 0.9295 0.8055 0.3532 0.0504 1.0000 Uiso . . . . . . . H232 H 0.9877 0.7619 0.3322 0.0504 1.0000 Uiso . . . . . . . H233 H 0.9381 0.7469 0.4559 0.0504 1.0000 Uiso . . . . . . . H241 H 0.8924 0.6398 0.1824 0.0380 1.0000 Uiso . . . . . . . H242 H 0.9596 0.6479 0.2498 0.0380 1.0000 Uiso . . . . . . . H243 H 0.9010 0.6440 0.3547 0.0380 1.0000 Uiso . . . . . . . H31 H 0.9480 0.6218 -0.2950 0.0419 1.0000 Uiso . . . . . . . H41 H 0.9989 0.5540 -0.1348 0.0535 1.0000 Uiso . . . . . . . H51 H 0.9427 0.5044 0.0503 0.0384 1.0000 Uiso . . . . . . . H61 H 0.8383 0.5273 0.0844 0.0318 1.0000 Uiso . . . . . . . H71 H 0.7887 0.5979 -0.0693 0.0262 1.0000 Uiso . . . . . . . H101 H 0.6124 0.5855 -0.0669 0.0319 1.0000 Uiso . . . . . . . H111 H 0.5641 0.4883 -0.0691 0.0417 1.0000 Uiso . . . . . . . H121 H 0.5619 0.4307 -0.2845 0.0459 1.0000 Uiso . . . . . . . H131 H 0.6093 0.4677 -0.4966 0.0430 1.0000 Uiso . . . . . . . H141 H 0.6573 0.5641 -0.4953 0.0312 1.0000 Uiso . . . . . . . H171 H 0.8025 0.5872 0.4506 0.0279 1.0000 Uiso . . . . . . . H181 H 0.8009 0.4808 0.5037 0.0418 1.0000 Uiso . . . . . . . H191 H 0.7406 0.4143 0.3631 0.0412 1.0000 Uiso . . . . . . . H201 H 0.6806 0.4529 0.1710 0.0327 1.0000 Uiso . . . . . . . H211 H 0.6834 0.5580 0.1135 0.0273 1.0000 Uiso . . . . . . . H221 H 0.8662 0.7952 0.1583 0.0308 1.0000 Uiso . . . . . . . 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 Gd1 0.01647(19) 0.01377(18) 0.00970(14) 0.00112(7) -0.00006(7) 0.00039(14) O1 0.020(2) 0.020(2) 0.0156(13) 0.0011(13) 0.0004(13) 0.007(2) O2 0.032(3) 0.030(3) 0.0166(14) 0.0050(15) 0.0054(15) 0.008(3) O3 0.023(2) 0.025(2) 0.0189(15) -0.0024(14) -0.0002(14) -0.005(2) O4 0.031(2) 0.025(2) 0.0175(14) 0.0008(14) 0.0015(15) -0.009(3) O5 0.036(3) 0.020(2) 0.0180(14) 0.0077(14) -0.0048(15) 0.003(3) O6 0.036(3) 0.016(2) 0.0172(14) -0.0022(13) 0.0023(15) -0.002(3) O7 0.022(2) 0.034(3) 0.0211(15) 0.0014(16) -0.0020(15) 0.006(3) N1 0.024(3) 0.032(3) 0.025(2) -0.0027(19) -0.0046(18) 0.000(3) C1 0.018(3) 0.019(3) 0.0170(19) 0.0020(17) 0.0013(17) -0.003(3) C2 0.020(3) 0.017(3) 0.020(2) 0.0025(18) 0.0039(18) -0.002(4) C3 0.027(4) 0.040(4) 0.038(3) 0.019(3) 0.012(2) 0.004(5) C4 0.041(5) 0.035(4) 0.058(4) 0.011(4) 0.002(3) 0.018(5) C5 0.037(4) 0.024(4) 0.035(3) 0.007(3) 0.002(3) 0.019(5) C6 0.036(4) 0.019(3) 0.025(2) 0.008(2) 0.006(2) 0.013(4) C7 0.021(3) 0.023(3) 0.022(2) -0.0013(19) 0.0015(19) 0.002(4) C8 0.012(3) 0.021(3) 0.0185(18) 0.0024(17) -0.0010(16) -0.003(3) C9 0.018(3) 0.015(3) 0.0190(18) 0.0000(17) -0.0002(17) 0.004(3) C10 0.027(4) 0.030(4) 0.023(2) 0.005(2) 0.005(2) -0.003(4) C11 0.033(4) 0.027(4) 0.044(3) 0.007(3) 0.017(3) 0.008(5) C12 0.036(4) 0.025(4) 0.054(4) 0.001(3) 0.008(3) -0.011(5) C13 0.035(4) 0.035(4) 0.037(3) -0.008(3) 0.002(3) -0.006(5) C14 0.032(4) 0.022(3) 0.023(2) -0.004(2) 0.003(2) -0.007(4) C15 0.020(3) 0.018(3) 0.0152(19) 0.0033(17) 0.0051(17) -0.002(3) C16 0.022(3) 0.016(3) 0.0120(16) 0.0021(16) 0.0005(17) -0.001(3) C17 0.029(3) 0.020(3) 0.021(2) 0.0000(19) -0.006(2) 0.004(4) C18 0.054(5) 0.020(3) 0.031(3) 0.009(2) -0.008(3) 0.019(5) C19 0.048(5) 0.016(3) 0.039(3) 0.004(2) 0.004(3) 0.004(5) C20 0.034(4) 0.016(3) 0.032(2) -0.004(2) 0.006(2) -0.004(4) C21 0.029(3) 0.021(3) 0.0177(19) 0.0019(18) -0.001(2) -0.004(4) C22 0.026(3) 0.031(4) 0.020(2) 0.005(2) -0.0007(19) 0.000(4) C23 0.037(4) 0.049(5) 0.040(3) -0.003(3) -0.009(3) -0.008(5) C24 0.033(4) 0.034(4) 0.028(2) -0.001(2) -0.003(2) 0.000(4) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.2904(8) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Gd1 . O2 5_664 2.518(4) yes Gd1 . O1 5_664 2.479(3) yes Gd1 . C1 5_664 2.855(4) yes Gd1 . O4 5_664 2.373(4) yes Gd1 . O6 5_665 2.272(3) yes Gd1 . O1 . 2.309(3) yes Gd1 . O3 . 2.380(4) yes Gd1 . O5 . 2.328(4) yes Gd1 . O7 . 2.391(4) yes O1 . C1 . 1.272(5) yes O2 . C1 . 1.250(5) yes O3 . C8 . 1.256(5) yes O4 . C8 . 1.274(5) yes O5 . C15 . 1.274(5) yes O6 . C15 . 1.250(5) yes O7 . C22 . 1.253(6) yes N1 . C22 . 1.323(6) yes N1 . C23 . 1.445(6) yes N1 . C24 . 1.441(7) yes C1 . C2 . 1.482(6) yes C2 . C3 . 1.374(6) yes C2 . C7 . 1.386(6) yes C3 . C4 . 1.386(7) yes C3 . H31 . 0.930 no C4 . C5 . 1.380(7) yes C4 . H41 . 0.930 no C5 . C6 . 1.379(7) yes C5 . H51 . 0.930 no C6 . C7 . 1.376(6) yes C6 . H61 . 0.930 no C7 . H71 . 0.930 no C8 . C9 . 1.491(6) yes C9 . C10 . 1.389(5) yes C9 . C14 . 1.384(5) yes C10 . C11 . 1.389(7) yes C10 . H101 . 0.930 no C11 . C12 . 1.370(7) yes C11 . H111 . 0.930 no C12 . C13 . 1.377(7) yes C12 . H121 . 0.930 no C13 . C14 . 1.374(7) yes C13 . H131 . 0.930 no C14 . H141 . 0.930 no C15 . C16 . 1.480(5) yes C16 . C17 . 1.392(5) yes C16 . C21 . 1.379(6) yes C17 . C18 . 1.391(6) yes C17 . H171 . 0.930 no C18 . C19 . 1.371(7) yes C18 . H181 . 0.930 no C19 . C20 . 1.380(7) yes C19 . H191 . 0.930 no C20 . C21 . 1.378(6) yes C20 . H201 . 0.930 no C21 . H211 . 0.930 no C22 . H221 . 0.930 no C23 . H231 . 0.959 no C23 . H232 . 0.960 no C23 . H233 . 0.960 no C24 . H241 . 0.959 no C24 . H242 . 0.960 no C24 . H243 . 0.961 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O2 5_664 Gd1 . O1 5_664 52.12(11) yes O2 5_664 Gd1 . C1 5_664 25.94(10) yes O1 5_664 Gd1 . C1 5_664 26.41(11) yes O2 5_664 Gd1 . O4 5_664 89.77(15) yes O1 5_664 Gd1 . O4 5_664 68.46(14) yes C1 5_664 Gd1 . O4 5_664 75.86(16) yes O2 5_664 Gd1 . O6 5_665 74.50(14) yes O1 5_664 Gd1 . O6 5_665 114.57(13) yes C1 5_664 Gd1 . O6 5_665 92.96(14) yes O4 5_664 Gd1 . O6 5_665 77.62(14) yes O2 5_664 Gd1 . O1 . 122.54(12) yes O1 5_664 Gd1 . O1 . 72.21(15) yes C1 5_664 Gd1 . O1 . 98.29(12) yes O4 5_664 Gd1 . O1 . 81.36(14) yes O6 5_665 Gd1 . O1 . 152.92(17) yes O2 5_664 Gd1 . O3 . 79.58(15) yes O1 5_664 Gd1 . O3 . 73.46(13) yes C1 5_664 Gd1 . O3 . 77.55(16) yes O4 5_664 Gd1 . O3 . 138.39(11) yes O6 5_665 Gd1 . O3 . 135.31(15) yes O2 5_664 Gd1 . O5 . 112.37(15) yes O1 5_664 Gd1 . O5 . 144.70(15) yes C1 5_664 Gd1 . O5 . 133.49(15) yes O4 5_664 Gd1 . O5 . 146.80(14) yes O6 5_665 Gd1 . O5 . 84.65(14) yes O2 5_664 Gd1 . O7 . 155.01(15) yes O1 5_664 Gd1 . O7 . 133.02(13) yes C1 5_664 Gd1 . O7 . 150.10(16) yes O4 5_664 Gd1 . O7 . 74.34(16) yes O6 5_665 Gd1 . O7 . 83.17(16) yes O1 . Gd1 . O3 . 71.47(14) yes O1 . Gd1 . O5 . 104.58(14) yes O3 . Gd1 . O5 . 72.36(13) yes O1 . Gd1 . O7 . 74.80(13) yes O3 . Gd1 . O7 . 125.04(16) yes O5 . Gd1 . O7 . 75.86(15) yes Gd1 5_664 O1 . Gd1 . 107.79(15) yes Gd1 5_664 O1 . C1 . 93.5(2) yes Gd1 . O1 . C1 . 156.8(3) yes Gd1 5_664 O2 . C1 . 92.2(3) yes Gd1 . O3 . C8 . 136.3(3) yes Gd1 5_664 O4 . C8 . 134.2(3) yes Gd1 . O5 . C15 . 130.2(3) yes Gd1 5_665 O6 . C15 . 149.6(4) yes Gd1 . O7 . C22 . 128.5(4) yes C22 . N1 . C23 . 121.0(5) yes C22 . N1 . C24 . 121.2(4) yes C23 . N1 . C24 . 117.7(4) yes Gd1 5_664 C1 . O1 . 60.1(2) yes Gd1 5_664 C1 . O2 . 61.8(3) yes O1 . C1 . O2 . 121.1(4) yes Gd1 5_664 C1 . C2 . 168.6(4) yes O1 . C1 . C2 . 117.1(3) yes O2 . C1 . C2 . 121.9(4) yes C1 . C2 . C3 . 118.4(4) yes C1 . C2 . C7 . 121.6(4) yes C3 . C2 . C7 . 119.7(4) yes C2 . C3 . C4 . 120.6(4) yes C2 . C3 . H31 . 119.7 no C4 . C3 . H31 . 119.7 no C3 . C4 . C5 . 119.3(5) yes C3 . C4 . H41 . 120.3 no C5 . C4 . H41 . 120.3 no C4 . C5 . C6 . 120.1(5) yes C4 . C5 . H51 . 119.9 no C6 . C5 . H51 . 119.9 no C5 . C6 . C7 . 120.3(4) yes C5 . C6 . H61 . 119.8 no C7 . C6 . H61 . 119.8 no C2 . C7 . C6 . 119.8(4) yes C2 . C7 . H71 . 120.1 no C6 . C7 . H71 . 120.1 no O4 . C8 . O3 . 124.3(4) yes O4 . C8 . C9 . 117.1(4) yes O3 . C8 . C9 . 118.5(4) yes C8 . C9 . C10 . 119.6(4) yes C8 . C9 . C14 . 121.5(4) yes C10 . C9 . C14 . 118.9(4) yes C9 . C10 . C11 . 120.3(4) yes C9 . C10 . H101 . 119.9 no C11 . C10 . H101 . 119.9 no C10 . C11 . C12 . 119.6(4) yes C10 . C11 . H111 . 120.2 no C12 . C11 . H111 . 120.2 no C11 . C12 . C13 . 120.7(5) yes C11 . C12 . H121 . 119.6 no C13 . C12 . H121 . 119.6 no C12 . C13 . C14 . 119.7(4) yes C12 . C13 . H131 . 120.1 no C14 . C13 . H131 . 120.1 no C9 . C14 . C13 . 120.8(4) yes C9 . C14 . H141 . 119.6 no C13 . C14 . H141 . 119.6 no O5 . C15 . O6 . 123.4(4) yes O5 . C15 . C16 . 116.9(4) yes O6 . C15 . C16 . 119.6(3) yes C15 . C16 . C17 . 119.3(4) yes C15 . C16 . C21 . 120.8(4) yes C17 . C16 . C21 . 119.9(4) yes C16 . C17 . C18 . 119.5(4) yes C16 . C17 . H171 . 120.2 no C18 . C17 . H171 . 120.2 no C17 . C18 . C19 . 120.0(4) yes C17 . C18 . H181 . 120.0 no C19 . C18 . H181 . 120.0 no C18 . C19 . C20 . 120.4(4) yes C18 . C19 . H191 . 119.8 no C20 . C19 . H191 . 119.8 no C19 . C20 . C21 . 120.2(5) yes C19 . C20 . H201 . 119.9 no C21 . C20 . H201 . 119.9 no C16 . C21 . C20 . 120.0(4) yes C16 . C21 . H211 . 120.0 no C20 . C21 . H211 . 120.0 no N1 . C22 . O7 . 123.6(5) yes N1 . C22 . H221 . 118.2 no O7 . C22 . H221 . 118.2 no N1 . C23 . H231 . 109.2 no N1 . C23 . H232 . 109.5 no H231 . C23 . H232 . 109.4 no N1 . C23 . H233 . 109.4 no H231 . C23 . H233 . 109.5 no H232 . C23 . H233 . 109.8 no N1 . C24 . H241 . 109.1 no N1 . C24 . H242 . 109.7 no H241 . C24 . H242 . 109.8 no N1 . C24 . H243 . 109.3 no H241 . C24 . H243 . 109.2 no H242 . C24 . H243 . 109.8 no data_gdpol6_Phase1_2_65GPa _database_code_depnum_ccdc_archive 'CCDC 768041' #TrackingRef '- Gd_polymer_cifs.cif' #2.65 GPa data set _audit_creation_date 08-06-30 _audit_creation_method CRYSTALS_ver_12.85 _oxford_structure_analysis_title 'gdpol6 in P4(2)/n' _chemical_name_systematic ; catena-((\m~2~-Benzoato-O,O')-bis(\m~2~-benzoato-O,O',O')-(dimethylformamide-O )-gadolinium) ; _chemical_melting_point ? _publ_section_exptl_prep ; ? ; #end of refcif _publ_section_exptl_refinement ; Pressure = 2.65 GPa. H atoms placed geometrically after each cycle. Because completeness is less than 100% the ligands were restrained to have the same bond distances and angles as at ambient pressure. Checkcif alerts: 027_ALERT_3_A _diffrn_reflns_theta_full (too) Low ............ 15.33 Deg. 029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.71 911_ALERT_3_B # Missing FCF Refl Between THmin & STh/L= 0.600 1163 913_ALERT_3_B # Missing Very Strong Reflections in FCF ....... 105 910_ALERT_3_C # Missing FCF Reflections Below Th(Min) ........ 1 912_ALERT_4_C # Missing FCF Reflections Above STh/L= 0.600 1403 Data are incomplete becasue of shading of reciprocal space by the body of the pressure cell. 919_ALERT_3_B # Reflections Likely Affected by the Beamstop .. 1 ...or the gasket 220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.57 Ratio 232_ALERT_2_C Hirshfeld Test Diff (M-X) Gd1 -- O2_a .. 5.14 su Some distortion of the adps is expected given the completeness, temperature and presence of the heavy atom. 411_ALERT_2_C Short Inter H...H Contact H31 .. H61 .. 2.10 Ang. See text. This is a high-pressure structure. 860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 86 See above. 128_ALERT_4_C Non-standard setting of Space-group P42/n .... P42/n:1 See text. This makes comparison with the high pressure phase simpler. 034_ALERT_1_C No Flack Parameter Given. Z .GT. Si, NonCentro . ? This is a bug in Checkcif. The space group operation '-x+1/2,-y+1/2,-z+1/2' is an inversion centre at [1/4 1/4 1/4]. This test shouldn't be applied, but presumably is triggered when the -1 is not on the origin. 042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? The one given is more chemically meaningful. 141_ALERT_4_C su on a - Axis Small or Missing (x 100000) ..... 20 Ang. No action 199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K 200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K Correct. 792_ALERT_1_G Check the Absolute Configuration of C1 = ... S The sum of the angles around C1 is 357.1(6) deg, so it is essentailly planar. Perhaps the algorithm is being 'put off' by a long Gd1-C1 'bond' in the connetivity list. No action. ; _cell_length_a 21.0414(2) _cell_length_b 21.0414(2) _cell_length_c 8.95130(10) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3963.10(7) _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'P 42/n:1' _symmetry_space_group_name_Hall 'P 4n -1n' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,z -y+1/2,x+1/2,z+1/2 y+1/2,-x+1/2,z+1/2 -x+1/2,-y+1/2,-z+1/2 x+1/2,y+1/2,-z+1/2 y,-x,-z -y,x,-z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0010 0.0010 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0020 0.0010 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0040 0.0030 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Gd -0.5090 2.0340 25.0709 2.2534 19.0798 0.1820 13.8518 12.9331 3.5454 101.3980 2.4196 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 8 _chemical_formula_sum 'C24 H22 Gd1 N1 O7' _chemical_formula_moiety ; (C24 H22 Gd1 N1 O7)n ; _chemical_compound_source ? _chemical_formula_weight 593.69 _cell_measurement_reflns_used 7018 _cell_measurement_theta_min 3 _cell_measurement_theta_max 20 _cell_measurement_temperature 293 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_max 0.20 _exptl_crystal_density_diffrn 1.990 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 2344 _exptl_absorpt_coefficient_mu 1.084 # Sheldrick geometric approximatio 0.51 0.71 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.06 _exptl_absorpt_correction_T_max 0.71 _diffrn_measurement_device 'Bruker SMART' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator Silicon _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.48650 _diffrn_source synchrotron _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'SMART (Siemens, 1993)' _computing_cell_refinement 'SAINT (Siemens ,1995)' _computing_data_reduction 'SAINT (Siemens ,1995)' _computing_structure_solution 'USER DEFINED STRUCTURE SOLUTION' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'DIAMOND Crystal Impact (2004)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 293 _diffrn_reflns_number 21658 _reflns_number_total 3582 _diffrn_reflns_av_R_equivalents 0.069 _diffrn_reflns_theta_min 1.325 _diffrn_reflns_theta_max 20.442 _diffrn_measured_fraction_theta_max 0.583 _diffrn_reflns_theta_full 15.331 _diffrn_measured_fraction_theta_full 0.711 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _reflns_limit_h_min -13 _reflns_limit_h_max 14 _reflns_limit_k_min 0 _reflns_limit_k_max 28 _reflns_limit_l_min 0 _reflns_limit_l_max 12 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.99 _refine_diff_density_max 1.03 # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>2.0\s(I) _refine_ls_number_reflns 2767 _refine_ls_number_restraints 86 _refine_ls_number_parameters 298 _oxford_refine_ls_R_factor_ref 0.0360 _refine_ls_wR_factor_ref 0.0423 _refine_ls_goodness_of_fit_ref 0.9259 _refine_ls_shift/su_max 0.000894 # The values computed from all data _oxford_reflns_number_all 3481 _refine_ls_R_factor_all 0.0480 _refine_ls_wR_factor_all 0.0541 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 2767 _refine_ls_R_factor_gt 0.0360 _refine_ls_wR_factor_gt 0.0423 _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment noref # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 1.20 0.446 0.452 ; _publ_section_references ; User-defined structure solution reference Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Siemens Industrial Automation, Inc (1993). SMART: Area-Detector Software Package; Madison, WI. Siemens Industrial Automation, Inc (1995). SAINT: Area-Detector Integration Software.; Madison, WI. Siemens Industrial Automation, Inc (1996). SADABS: Area-Detector Absorption Correction;: Madison, WI. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Gd1 Gd 0.737232(12) 0.748846(11) -0.03658(2) 0.0120 1.0000 Uani . . . . . . . O1 O 0.79286(17) 0.70040(18) -0.2265(3) 0.0176 1.0000 Uani D . . . . . . O2 O 0.85593(19) 0.6793(2) -0.4148(3) 0.0241 1.0000 Uani D . . . . . . O3 O 0.66944(18) 0.67603(19) -0.1609(3) 0.0206 1.0000 Uani D . . . . . . O4 O 0.6937(2) 0.66562(18) -0.4032(3) 0.0221 1.0000 Uani D . . . . . . O5 O 0.7118(2) 0.66840(17) 0.1300(3) 0.0223 1.0000 Uani D . . . . . . O6 O 0.7692(2) 0.68715(17) 0.3330(3) 0.0203 1.0000 Uani D . . . . . . O7 O 0.83743(19) 0.7203(2) 0.0686(3) 0.0240 1.0000 Uani D . . . . . . N1 N 0.9093(2) 0.7251(2) 0.2566(4) 0.0201 1.0000 Uani D . . . . . . C1 C 0.8374(2) 0.6678(2) -0.2853(4) 0.0151 1.0000 Uani D . . . . . . C2 C 0.8647(2) 0.6158(2) -0.1941(4) 0.0198 1.0000 Uani D . . . . . . C3 C 0.9281(3) 0.6028(3) -0.2104(5) 0.0323 1.0000 Uani D . . . . . . C4 C 0.9582(3) 0.5623(3) -0.1110(6) 0.0395 1.0000 Uani D . . . . . . C5 C 0.9239(3) 0.5338(3) -0.0001(5) 0.0287 1.0000 Uani D . . . . . . C6 C 0.8597(3) 0.5452(3) 0.0138(5) 0.0249 1.0000 Uani D . . . . . . C7 C 0.8300(2) 0.5872(2) -0.0814(4) 0.0203 1.0000 Uani D . . . . . . C8 C 0.6701(2) 0.6454(2) -0.2811(4) 0.0170 1.0000 Uani D . . . . . . C9 C 0.6395(2) 0.5814(2) -0.2834(4) 0.0171 1.0000 Uani D . . . . . . C10 C 0.6104(2) 0.5583(2) -0.1560(5) 0.0232 1.0000 Uani D . . . . . . C11 C 0.5810(3) 0.4990(3) -0.1576(5) 0.0318 1.0000 Uani D . . . . . . C12 C 0.5803(3) 0.4639(3) -0.2862(6) 0.0357 1.0000 Uani D . . . . . . C13 C 0.6095(3) 0.4864(3) -0.4132(5) 0.0314 1.0000 Uani D . . . . . . C14 C 0.6390(2) 0.5447(2) -0.4117(4) 0.0223 1.0000 Uani D . . . . . . C15 C 0.7421(2) 0.6503(2) 0.2456(4) 0.0178 1.0000 Uani D . . . . . . C16 C 0.7420(2) 0.5816(2) 0.2786(4) 0.0160 1.0000 Uani D . . . . . . C17 C 0.7781(2) 0.5582(2) 0.3950(4) 0.0210 1.0000 Uani D . . . . . . C18 C 0.7772(3) 0.4936(3) 0.4266(5) 0.0305 1.0000 Uani D . . . . . . C19 C 0.7404(3) 0.4534(2) 0.3430(5) 0.0310 1.0000 Uani D . . . . . . C20 C 0.7044(3) 0.4762(2) 0.2262(5) 0.0238 1.0000 Uani D . . . . . . C21 C 0.7057(2) 0.5405(2) 0.1931(4) 0.0223 1.0000 Uani D . . . . . . C22 C 0.8700(2) 0.7509(2) 0.1591(4) 0.0211 1.0000 Uani D . . . . . . C23 C 0.9454(3) 0.7637(3) 0.3599(6) 0.0364 1.0000 Uani D . . . . . . C24 C 0.9178(3) 0.6569(3) 0.2630(5) 0.0269 1.0000 Uani D . . . . . . H231 H 0.9291 0.8064 0.3590 0.0437 1.0000 Uiso . . . . . . . H232 H 0.9892 0.7641 0.3301 0.0437 1.0000 Uiso . . . . . . . H233 H 0.9417 0.7463 0.4585 0.0437 1.0000 Uiso . . . . . . . H241 H 0.8897 0.6371 0.1927 0.0323 1.0000 Uiso . . . . . . . H242 H 0.9610 0.6464 0.2384 0.0323 1.0000 Uiso . . . . . . . H243 H 0.9082 0.6419 0.3619 0.0323 1.0000 Uiso . . . . . . . H31 H 0.9510 0.6212 -0.2881 0.0387 1.0000 Uiso . . . . . . . H41 H 1.0016 0.5545 -0.1198 0.0474 1.0000 Uiso . . . . . . . H51 H 0.9440 0.5065 0.0665 0.0344 1.0000 Uiso . . . . . . . H61 H 0.8364 0.5245 0.0875 0.0299 1.0000 Uiso . . . . . . . H71 H 0.7870 0.5962 -0.0700 0.0244 1.0000 Uiso . . . . . . . H101 H 0.6104 0.5825 -0.0689 0.0278 1.0000 Uiso . . . . . . . H111 H 0.5619 0.4833 -0.0714 0.0382 1.0000 Uiso . . . . . . . H121 H 0.5600 0.4246 -0.2878 0.0429 1.0000 Uiso . . . . . . . H131 H 0.6093 0.4621 -0.5001 0.0377 1.0000 Uiso . . . . . . . H141 H 0.6588 0.5596 -0.4978 0.0268 1.0000 Uiso . . . . . . . H171 H 0.8030 0.5855 0.4519 0.0252 1.0000 Uiso . . . . . . . H181 H 0.8015 0.4776 0.5048 0.0366 1.0000 Uiso . . . . . . . H191 H 0.7398 0.4102 0.3654 0.0372 1.0000 Uiso . . . . . . . H201 H 0.6795 0.4486 0.1699 0.0286 1.0000 Uiso . . . . . . . H211 H 0.6822 0.5561 0.1132 0.0267 1.0000 Uiso . . . . . . . H221 H 0.8665 0.7950 0.1582 0.0253 1.0000 Uiso . . . . . . . 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 Gd1 0.01458(15) 0.01252(14) 0.00898(11) 0.00111(7) -0.00011(7) 0.00010(13) O1 0.0172(18) 0.0185(19) 0.0171(12) 0.0016(12) -0.0006(12) 0.004(2) O2 0.026(2) 0.030(2) 0.0160(13) 0.0035(14) 0.0031(13) 0.005(3) O3 0.0185(19) 0.026(2) 0.0174(13) -0.0022(13) -0.0009(12) -0.006(2) O4 0.025(2) 0.022(2) 0.0191(13) 0.0003(13) 0.0003(13) -0.007(2) O5 0.033(2) 0.0161(18) 0.0183(13) 0.0054(12) -0.0032(14) -0.002(2) O6 0.031(2) 0.0153(18) 0.0150(13) -0.0018(12) 0.0029(13) -0.002(2) O7 0.019(2) 0.034(2) 0.0192(14) -0.0016(14) -0.0014(12) 0.003(3) N1 0.014(2) 0.027(2) 0.0195(16) 0.0001(16) -0.0059(14) 0.001(3) C1 0.015(2) 0.014(2) 0.0169(17) 0.0011(15) 0.0011(15) 0.002(3) C2 0.023(3) 0.018(3) 0.0177(18) 0.0019(17) 0.0039(17) 0.005(3) C3 0.030(3) 0.030(3) 0.038(3) 0.011(2) 0.012(2) 0.010(4) C4 0.024(3) 0.038(4) 0.056(3) 0.011(3) 0.009(3) 0.012(4) C5 0.031(3) 0.026(3) 0.029(2) 0.010(2) 0.000(2) 0.010(4) C6 0.033(3) 0.021(3) 0.0207(19) 0.0028(18) 0.0086(19) 0.004(4) C7 0.020(3) 0.020(3) 0.0203(18) -0.0004(17) 0.0030(17) 0.004(3) C8 0.016(2) 0.019(3) 0.0155(16) 0.0011(16) -0.0050(15) 0.002(3) C9 0.019(3) 0.015(3) 0.0171(17) 0.0034(16) -0.0016(16) 0.000(3) C10 0.025(3) 0.022(3) 0.023(2) 0.0048(18) 0.0030(18) 0.006(4) C11 0.037(4) 0.025(3) 0.034(3) 0.007(2) 0.014(2) -0.001(4) C12 0.034(4) 0.025(3) 0.048(3) -0.002(2) 0.011(3) -0.016(4) C13 0.040(4) 0.022(3) 0.032(2) -0.005(2) 0.006(2) 0.001(4) C14 0.021(3) 0.024(3) 0.0218(19) -0.0018(18) 0.0032(18) -0.011(3) C15 0.027(3) 0.017(2) 0.0097(16) 0.0012(15) 0.0039(16) 0.006(3) C16 0.019(3) 0.013(2) 0.0162(16) 0.0007(15) -0.0016(16) 0.000(3) C17 0.024(3) 0.020(3) 0.0191(18) 0.0033(17) 0.0014(18) -0.001(3) C18 0.040(4) 0.025(3) 0.027(2) 0.012(2) -0.004(2) 0.001(4) C19 0.042(4) 0.017(3) 0.033(2) 0.008(2) 0.002(2) -0.004(4) C20 0.033(3) 0.014(3) 0.0250(19) -0.0052(17) 0.003(2) 0.000(4) C21 0.028(3) 0.024(3) 0.0157(18) -0.0032(17) -0.0021(18) -0.003(3) C22 0.018(3) 0.026(3) 0.0183(19) 0.0012(17) -0.0010(17) 0.002(3) C23 0.038(4) 0.039(4) 0.032(2) 0.000(2) -0.013(2) -0.014(4) C24 0.027(3) 0.029(3) 0.025(2) -0.003(2) -0.006(2) 0.006(4) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.2906(6) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Gd1 . O2 5_664 2.514(4) yes Gd1 . O1 5_664 2.458(3) yes Gd1 . C1 5_664 2.843(4) yes Gd1 . O4 5_664 2.376(4) yes Gd1 . O6 5_665 2.270(3) yes Gd1 . O1 . 2.302(3) yes Gd1 . O3 . 2.371(4) yes Gd1 . O5 . 2.318(3) yes Gd1 . O7 . 2.386(4) yes O1 . C1 . 1.276(5) yes O2 . C1 . 1.246(4) yes O3 . C8 . 1.254(5) yes O4 . C8 . 1.274(5) yes O5 . C15 . 1.273(5) yes O6 . C15 . 1.241(5) yes O7 . C22 . 1.242(5) yes N1 . C22 . 1.318(5) yes N1 . C23 . 1.447(6) yes N1 . C24 . 1.447(6) yes C1 . C2 . 1.482(5) yes C2 . C3 . 1.370(6) yes C2 . C7 . 1.384(5) yes C3 . C4 . 1.386(6) yes C3 . H31 . 0.930 no C4 . C5 . 1.367(6) yes C4 . H41 . 0.930 no C5 . C6 . 1.377(6) yes C5 . H51 . 0.930 no C6 . C7 . 1.378(6) yes C6 . H61 . 0.930 no C7 . H71 . 0.930 no C8 . C9 . 1.492(5) yes C9 . C10 . 1.383(5) yes C9 . C14 . 1.384(5) yes C10 . C11 . 1.393(6) yes C10 . H101 . 0.930 no C11 . C12 . 1.369(6) yes C11 . H111 . 0.930 no C12 . C13 . 1.377(6) yes C12 . H121 . 0.930 no C13 . C14 . 1.376(6) yes C13 . H131 . 0.930 no C14 . H141 . 0.930 no C15 . C16 . 1.476(5) yes C16 . C17 . 1.382(5) yes C16 . C21 . 1.384(5) yes C17 . C18 . 1.388(6) yes C17 . H171 . 0.930 no C18 . C19 . 1.369(6) yes C18 . H181 . 0.930 no C19 . C20 . 1.378(6) yes C19 . H191 . 0.930 no C20 . C21 . 1.386(6) yes C20 . H201 . 0.930 no C21 . H211 . 0.930 no C22 . H221 . 0.930 no C23 . H231 . 0.961 no C23 . H232 . 0.959 no C23 . H233 . 0.958 no C24 . H241 . 0.958 no C24 . H242 . 0.961 no C24 . H243 . 0.961 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O2 5_664 Gd1 . O1 5_664 52.29(10) yes O2 5_664 Gd1 . C1 5_664 25.98(10) yes O1 5_664 Gd1 . C1 5_664 26.60(10) yes O2 5_664 Gd1 . O4 5_664 88.98(13) yes O1 5_664 Gd1 . O4 5_664 68.45(12) yes C1 5_664 Gd1 . O4 5_664 75.16(14) yes O2 5_664 Gd1 . O6 5_665 74.64(13) yes O1 5_664 Gd1 . O6 5_665 114.80(12) yes C1 5_664 Gd1 . O6 5_665 92.93(13) yes O4 5_664 Gd1 . O6 5_665 76.67(12) yes O2 5_664 Gd1 . O1 . 122.36(11) yes O1 5_664 Gd1 . O1 . 71.71(14) yes C1 5_664 Gd1 . O1 . 98.05(11) yes O4 5_664 Gd1 . O1 . 81.76(13) yes O6 5_665 Gd1 . O1 . 152.38(14) yes O2 5_664 Gd1 . O3 . 80.70(14) yes O1 5_664 Gd1 . O3 . 73.78(12) yes C1 5_664 Gd1 . O3 . 78.63(14) yes O4 5_664 Gd1 . O3 . 138.71(11) yes O6 5_665 Gd1 . O3 . 136.39(13) yes O2 5_664 Gd1 . O5 . 111.75(13) yes O1 5_664 Gd1 . O5 . 144.38(13) yes C1 5_664 Gd1 . O5 . 133.10(14) yes O4 5_664 Gd1 . O5 . 147.17(12) yes O6 5_665 Gd1 . O5 . 84.44(12) yes O2 5_664 Gd1 . O7 . 155.36(14) yes O1 5_664 Gd1 . O7 . 132.67(12) yes C1 5_664 Gd1 . O7 . 149.88(14) yes O4 5_664 Gd1 . O7 . 74.91(14) yes O6 5_665 Gd1 . O7 . 83.44(14) yes O1 . Gd1 . O3 . 70.93(13) yes O1 . Gd1 . O5 . 105.60(13) yes O3 . Gd1 . O5 . 72.01(12) yes O1 . Gd1 . O7 . 74.37(12) yes O3 . Gd1 . O7 . 123.64(14) yes O5 . Gd1 . O7 . 76.47(14) yes Gd1 5_664 O1 . Gd1 . 108.29(14) yes Gd1 5_664 O1 . C1 . 93.8(2) yes Gd1 . O1 . C1 . 156.5(3) yes Gd1 5_664 O2 . C1 . 91.9(3) yes Gd1 . O3 . C8 . 136.7(3) yes Gd1 5_664 O4 . C8 . 133.3(3) yes Gd1 . O5 . C15 . 128.7(3) yes Gd1 5_665 O6 . C15 . 148.2(4) yes Gd1 . O7 . C22 . 127.9(3) yes C22 . N1 . C23 . 121.4(4) yes C22 . N1 . C24 . 120.8(4) yes C23 . N1 . C24 . 117.8(4) yes Gd1 5_664 C1 . O1 . 59.6(2) yes Gd1 5_664 C1 . O2 . 62.1(2) yes O1 . C1 . O2 . 120.7(4) yes Gd1 5_664 C1 . C2 . 168.2(3) yes O1 . C1 . C2 . 117.0(3) yes O2 . C1 . C2 . 122.3(4) yes C1 . C2 . C3 . 117.8(4) yes C1 . C2 . C7 . 121.2(4) yes C3 . C2 . C7 . 120.4(4) yes C2 . C3 . C4 . 120.0(4) yes C2 . C3 . H31 . 120.0 no C4 . C3 . H31 . 120.0 no C3 . C4 . C5 . 119.6(4) yes C3 . C4 . H41 . 120.2 no C5 . C4 . H41 . 120.2 no C4 . C5 . C6 . 120.6(4) yes C4 . C5 . H51 . 119.7 no C6 . C5 . H51 . 119.7 no C5 . C6 . C7 . 120.0(4) yes C5 . C6 . H61 . 120.0 no C7 . C6 . H61 . 120.0 no C2 . C7 . C6 . 119.3(4) yes C2 . C7 . H71 . 120.3 no C6 . C7 . H71 . 120.3 no O4 . C8 . O3 . 124.7(4) yes O4 . C8 . C9 . 117.2(3) yes O3 . C8 . C9 . 118.1(3) yes C8 . C9 . C10 . 119.7(3) yes C8 . C9 . C14 . 121.3(3) yes C10 . C9 . C14 . 119.0(4) yes C9 . C10 . C11 . 120.2(4) yes C9 . C10 . H101 . 119.9 no C11 . C10 . H101 . 119.9 no C10 . C11 . C12 . 119.9(4) yes C10 . C11 . H111 . 120.1 no C12 . C11 . H111 . 120.1 no C11 . C12 . C13 . 120.3(4) yes C11 . C12 . H121 . 119.9 no C13 . C12 . H121 . 119.9 no C12 . C13 . C14 . 120.0(4) yes C12 . C13 . H131 . 120.0 no C14 . C13 . H131 . 120.0 no C9 . C14 . C13 . 120.7(4) yes C9 . C14 . H141 . 119.7 no C13 . C14 . H141 . 119.7 no O5 . C15 . O6 . 123.8(4) yes O5 . C15 . C16 . 117.0(3) yes O6 . C15 . C16 . 119.1(3) yes C15 . C16 . C17 . 120.0(3) yes C15 . C16 . C21 . 120.2(3) yes C17 . C16 . C21 . 119.9(4) yes C16 . C17 . C18 . 119.6(4) yes C16 . C17 . H171 . 120.2 no C18 . C17 . H171 . 120.2 no C17 . C18 . C19 . 120.2(4) yes C17 . C18 . H181 . 119.9 no C19 . C18 . H181 . 119.9 no C18 . C19 . C20 . 120.7(4) yes C18 . C19 . H191 . 119.7 no C20 . C19 . H191 . 119.7 no C19 . C20 . C21 . 119.4(4) yes C19 . C20 . H201 . 120.3 no C21 . C20 . H201 . 120.3 no C20 . C21 . C16 . 120.2(4) yes C20 . C21 . H211 . 119.9 no C16 . C21 . H211 . 119.9 no N1 . C22 . O7 . 124.3(4) yes N1 . C22 . H221 . 117.9 no O7 . C22 . H221 . 117.9 no N1 . C23 . H231 . 109.4 no N1 . C23 . H232 . 109.4 no H231 . C23 . H232 . 109.3 no N1 . C23 . H233 . 109.4 no H231 . C23 . H233 . 109.5 no H232 . C23 . H233 . 109.8 no N1 . C24 . H241 . 109.2 no N1 . C24 . H242 . 109.6 no H241 . C24 . H242 . 109.5 no N1 . C24 . H243 . 109.6 no H241 . C24 . H243 . 109.5 no H242 . C24 . H243 . 109.5 no data_gdpol7_Phase1_3_20GPa _database_code_depnum_ccdc_archive 'CCDC 768042' #TrackingRef '- Gd_polymer_cifs.cif' #3.20 GPa data set _audit_creation_date 08-06-30 _audit_creation_method CRYSTALS_ver_12.85 _oxford_structure_analysis_title 'gdpol7 in P4(2)/n' _chemical_name_systematic ; catena-((\m~2~-Benzoato-O,O')-bis(\m~2~-benzoato-O,O',O')-(dimethylformamide-O )-gadolinium) ; _chemical_melting_point ? _publ_section_exptl_prep ; ? ; #end of refcif _publ_section_exptl_refinement ; Pressure = 3.20 GPa. H atoms placed geometrically after each cycle. Because completeness is less than 100% the ligands were restrained to have the same bond distances and angles as at ambient pressure. Checkcif alerts: 027_ALERT_3_A _diffrn_reflns_theta_full (too) Low ............ 15.25 Deg. 029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.75 911_ALERT_3_B # Missing FCF Refl Between THmin & STh/L= 0.600 992 910_ALERT_3_C # Missing FCF Reflections Below Th(Min) ........ 1 913_ALERT_3_C # Missing Very Strong Reflections in FCF ....... 81 912_ALERT_4_C # Missing FCF Reflections Above STh/L= 0.600 1217 Data are incomplete becasue of shading of reciprocal space by the body of the pressure cell. 919_ALERT_3_B # Reflections Likely Affected by the Beamstop .. 2 ...or the gasket 411_ALERT_2_B Short Inter H...H Contact H31 .. H61 .. 2.06 Ang. See text. This is a high-pressure structure. 860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 86 See above 128_ALERT_4_C Non-standard setting of Space-group P42/n .... P42/n:1 See text. This makes comparison with the high pressure phase simpler. 034_ALERT_1_C No Flack Parameter Given. Z .GT. Si, NonCentro . ? This is a bug in Checkcif. The space group operation '-x+1/2,-y+1/2,-z+1/2' is an inversion centre at [1/4 1/4 1/4]. This test shouldn't be applied, but presumably is triggered when the -1 is not on the origin. 042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? The one given is more chemically meaningful. 141_ALERT_4_C su on a - Axis Small or Missing (x 100000) ..... 20 Ang. No action 199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K 200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K Correct 792_ALERT_1_G Check the Absolute Configuration of C1 = ... S The sum of the angles around C1 is 356.4(6) deg, so it is essentailly planar. Perhaps the algorithm is being 'put off' by a long Gd1-C1 'bond' in the connetivity list. No action. ; _cell_length_a 20.8918(2) _cell_length_b 20.8918(2) _cell_length_c 8.9248(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3895.38(10) _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'P 42/n:1' _symmetry_space_group_name_Hall 'P 4n -1n' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,z -y+1/2,x+1/2,z+1/2 y+1/2,-x+1/2,z+1/2 -x+1/2,-y+1/2,-z+1/2 x+1/2,y+1/2,-z+1/2 y,-x,-z -y,x,-z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0010 0.0010 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0020 0.0010 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0040 0.0030 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Gd -0.5090 2.0340 25.0709 2.2534 19.0798 0.1820 13.8518 12.9331 3.5454 101.3980 2.4196 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 8 _chemical_formula_sum 'C24 H22 Gd1 N1 O7' _chemical_formula_moiety ; (C24 H22 Gd1 N1 O7)n ; _chemical_compound_source ? _chemical_formula_weight 593.69 _cell_measurement_reflns_used 8066 _cell_measurement_theta_min 3 _cell_measurement_theta_max 20 _cell_measurement_temperature 293 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_max 0.20 _exptl_crystal_density_diffrn 2.025 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 2344 _exptl_absorpt_coefficient_mu 1.102 # Sheldrick geometric approximatio 0.50 0.71 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.12 _exptl_absorpt_correction_T_max 0.71 _diffrn_measurement_device 'Bruker SMART' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator Silicon _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.48650 _diffrn_source synchrotron _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'SMART (Siemens, 1993)' _computing_cell_refinement 'SAINT (Siemens ,1995)' _computing_data_reduction 'SAINT (Siemens ,1995)' _computing_structure_solution 'USER DEFINED STRUCTURE SOLUTION' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'DIAMOND Crystal Impact (2004)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 293 _diffrn_reflns_number 25354 _reflns_number_total 3773 _diffrn_reflns_av_R_equivalents 0.073 _diffrn_reflns_theta_min 1.334 _diffrn_reflns_theta_max 20.337 _diffrn_measured_fraction_theta_max 0.633 _diffrn_reflns_theta_full 15.253 _diffrn_measured_fraction_theta_full 0.747 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _reflns_limit_h_min -13 _reflns_limit_h_max 15 _reflns_limit_k_min 0 _reflns_limit_k_max 28 _reflns_limit_l_min 0 _reflns_limit_l_max 12 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.93 _refine_diff_density_max 1.81 # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>2.0\s(I) _refine_ls_number_reflns 3017 _refine_ls_number_restraints 86 _refine_ls_number_parameters 298 _oxford_refine_ls_R_factor_ref 0.0388 _refine_ls_wR_factor_ref 0.0474 _refine_ls_goodness_of_fit_ref 0.9057 _refine_ls_shift/su_max 0.002716 # The values computed from all data _oxford_reflns_number_all 3705 _refine_ls_R_factor_all 0.0489 _refine_ls_wR_factor_all 0.0571 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 3017 _refine_ls_R_factor_gt 0.0388 _refine_ls_wR_factor_gt 0.0474 _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment noref # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 1.36 0.596 0.645 ; # Insert your own references if required - in alphabetical order _publ_section_references ; User-defined structure solution reference Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Siemens Industrial Automation, Inc (1993). SMART: Area-Detector Software Package; Madison, WI. Siemens Industrial Automation, Inc (1995). SAINT: Area-Detector Integration Software.; Madison, WI. Siemens Industrial Automation, Inc (1996). SADABS: Area-Detector Absorption Correction;: Madison, WI. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Gd1 Gd 0.736927(12) 0.748723(11) -0.03632(2) 0.0117 1.0000 Uani . . . . . . . O1 O 0.79378(18) 0.70065(17) -0.2266(3) 0.0179 1.0000 Uani D . . . . . . O2 O 0.85640(19) 0.6785(2) -0.4154(3) 0.0240 1.0000 Uani D . . . . . . O3 O 0.66993(19) 0.67478(18) -0.1611(3) 0.0203 1.0000 Uani D . . . . . . O4 O 0.6942(2) 0.66437(18) -0.4043(3) 0.0216 1.0000 Uani D . . . . . . O5 O 0.7106(2) 0.66832(18) 0.1308(3) 0.0224 1.0000 Uani D . . . . . . O6 O 0.7699(2) 0.68765(17) 0.3324(3) 0.0202 1.0000 Uani D . . . . . . O7 O 0.83771(18) 0.7202(2) 0.0676(3) 0.0228 1.0000 Uani D . . . . . . N1 N 0.9096(2) 0.7249(2) 0.2572(4) 0.0223 1.0000 Uani D . . . . . . C1 C 0.8375(2) 0.6674(2) -0.2857(4) 0.0167 1.0000 Uani D . . . . . . C2 C 0.8646(2) 0.6152(2) -0.1932(4) 0.0181 1.0000 Uani D . . . . . . C3 C 0.9289(3) 0.6025(3) -0.2085(5) 0.0304 1.0000 Uani D . . . . . . C4 C 0.9594(3) 0.5622(3) -0.1072(6) 0.0377 1.0000 Uani D . . . . . . C5 C 0.9242(3) 0.5340(3) 0.0047(5) 0.0298 1.0000 Uani D . . . . . . C6 C 0.8593(3) 0.5441(2) 0.0156(5) 0.0236 1.0000 Uani D . . . . . . C7 C 0.8297(2) 0.5863(2) -0.0806(4) 0.0183 1.0000 Uani D . . . . . . C8 C 0.6699(2) 0.6443(2) -0.2821(4) 0.0158 1.0000 Uani D . . . . . . C9 C 0.6393(2) 0.5796(2) -0.2845(4) 0.0176 1.0000 Uani D . . . . . . C10 C 0.6098(2) 0.5565(2) -0.1566(4) 0.0211 1.0000 Uani D . . . . . . C11 C 0.5799(3) 0.4974(2) -0.1589(5) 0.0275 1.0000 Uani D . . . . . . C12 C 0.5799(3) 0.4617(3) -0.2871(6) 0.0327 1.0000 Uani D . . . . . . C13 C 0.6102(3) 0.4837(3) -0.4146(5) 0.0324 1.0000 Uani D . . . . . . C14 C 0.6398(2) 0.5426(2) -0.4134(4) 0.0233 1.0000 Uani D . . . . . . C15 C 0.7419(2) 0.6501(2) 0.2453(4) 0.0171 1.0000 Uani D . . . . . . C16 C 0.7421(2) 0.5805(2) 0.2781(4) 0.0157 1.0000 Uani D . . . . . . C17 C 0.7789(2) 0.5575(2) 0.3953(4) 0.0197 1.0000 Uani D . . . . . . C18 C 0.7774(3) 0.4922(2) 0.4276(5) 0.0278 1.0000 Uani D . . . . . . C19 C 0.7398(3) 0.4519(2) 0.3435(5) 0.0291 1.0000 Uani D . . . . . . C20 C 0.7036(3) 0.4752(2) 0.2265(5) 0.0236 1.0000 Uani D . . . . . . C21 C 0.7051(2) 0.5398(2) 0.1932(4) 0.0192 1.0000 Uani D . . . . . . C22 C 0.8703(2) 0.7508(2) 0.1599(4) 0.0213 1.0000 Uani D . . . . . . C23 C 0.9451(3) 0.7635(3) 0.3625(6) 0.0369 1.0000 Uani D . . . . . . C24 C 0.9177(3) 0.6562(3) 0.2641(5) 0.0268 1.0000 Uani D . . . . . . H231 H 0.9283 0.8063 0.3621 0.0443 1.0000 Uiso . . . . . . . H232 H 0.9894 0.7646 0.3335 0.0443 1.0000 Uiso . . . . . . . H233 H 0.9413 0.7456 0.4611 0.0443 1.0000 Uiso . . . . . . . H241 H 0.8904 0.6359 0.1920 0.0322 1.0000 Uiso . . . . . . . H242 H 0.9615 0.6453 0.2425 0.0322 1.0000 Uiso . . . . . . . H243 H 0.9070 0.6410 0.3626 0.0322 1.0000 Uiso . . . . . . . H31 H 0.9520 0.6209 -0.2866 0.0365 1.0000 Uiso . . . . . . . H41 H 1.0031 0.5544 -0.1151 0.0452 1.0000 Uiso . . . . . . . H51 H 0.9445 0.5077 0.0740 0.0357 1.0000 Uiso . . . . . . . H61 H 0.8355 0.5225 0.0877 0.0283 1.0000 Uiso . . . . . . . H71 H 0.7864 0.5953 -0.0696 0.0220 1.0000 Uiso . . . . . . . H101 H 0.6100 0.5806 -0.0691 0.0253 1.0000 Uiso . . . . . . . H111 H 0.5598 0.4820 -0.0732 0.0330 1.0000 Uiso . . . . . . . H121 H 0.5593 0.4222 -0.2886 0.0392 1.0000 Uiso . . . . . . . H131 H 0.6107 0.4588 -0.5010 0.0389 1.0000 Uiso . . . . . . . H141 H 0.6601 0.5576 -0.4992 0.0280 1.0000 Uiso . . . . . . . H171 H 0.8042 0.5851 0.4515 0.0237 1.0000 Uiso . . . . . . . H181 H 0.8018 0.4759 0.5060 0.0334 1.0000 Uiso . . . . . . . H191 H 0.7388 0.4084 0.3658 0.0349 1.0000 Uiso . . . . . . . H201 H 0.6783 0.4476 0.1702 0.0283 1.0000 Uiso . . . . . . . H211 H 0.6813 0.5557 0.1136 0.0231 1.0000 Uiso . . . . . . . H221 H 0.8666 0.7952 0.1598 0.0256 1.0000 Uiso . . . . . . . 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 Gd1 0.01423(14) 0.01195(14) 0.00904(11) 0.00101(6) -0.00026(6) 0.00007(12) O1 0.0205(18) 0.0175(17) 0.0156(12) 0.0014(11) -0.0001(12) 0.008(2) O2 0.028(2) 0.027(2) 0.0165(13) 0.0054(13) 0.0029(13) 0.009(2) O3 0.0188(18) 0.0244(19) 0.0176(13) -0.0033(12) 0.0010(12) -0.008(2) O4 0.029(2) 0.0202(18) 0.0154(12) 0.0006(12) 0.0018(13) -0.008(2) O5 0.031(2) 0.0169(18) 0.0197(13) 0.0071(12) -0.0030(13) 0.005(2) O6 0.031(2) 0.0157(17) 0.0142(12) -0.0003(11) 0.0004(13) -0.001(2) O7 0.0195(19) 0.032(2) 0.0166(13) -0.0012(13) -0.0023(12) 0.006(2) N1 0.021(2) 0.027(2) 0.0194(17) -0.0018(15) -0.0031(15) 0.001(3) C1 0.014(2) 0.019(2) 0.0167(17) -0.0013(16) -0.0010(15) 0.000(3) C2 0.017(2) 0.017(2) 0.0200(18) 0.0023(16) 0.0033(16) 0.001(3) C3 0.023(3) 0.030(3) 0.039(3) 0.018(2) 0.014(2) 0.010(4) C4 0.023(3) 0.035(4) 0.055(3) 0.018(3) 0.007(3) 0.014(4) C5 0.031(3) 0.030(3) 0.028(2) 0.011(2) -0.004(2) 0.007(4) C6 0.030(3) 0.021(3) 0.0205(19) 0.0052(17) 0.0041(18) 0.009(3) C7 0.016(2) 0.016(2) 0.0235(19) 0.0023(17) 0.0044(16) 0.007(3) C8 0.012(2) 0.020(2) 0.0154(16) 0.0034(15) -0.0033(14) 0.002(3) C9 0.017(2) 0.019(3) 0.0172(17) 0.0021(16) 0.0036(15) 0.001(3) C10 0.023(3) 0.021(3) 0.0190(19) 0.0044(16) 0.0028(16) 0.001(3) C11 0.031(3) 0.019(3) 0.033(2) 0.0041(19) 0.012(2) 0.002(4) C12 0.033(3) 0.022(3) 0.043(3) 0.000(2) 0.006(2) -0.011(4) C13 0.039(4) 0.024(3) 0.034(2) -0.007(2) 0.006(2) -0.002(4) C14 0.027(3) 0.025(3) 0.0179(18) 0.0007(17) 0.0035(17) -0.009(3) C15 0.019(2) 0.019(2) 0.0125(17) 0.0023(15) 0.0049(15) 0.000(3) C16 0.017(2) 0.017(2) 0.0128(15) 0.0019(14) 0.0014(14) -0.002(3) C17 0.026(3) 0.014(2) 0.0188(18) 0.0023(16) -0.0017(17) 0.005(3) C18 0.039(4) 0.019(3) 0.025(2) 0.0063(18) -0.003(2) 0.004(4) C19 0.041(4) 0.015(3) 0.032(2) 0.0046(18) 0.003(2) 0.000(4) C20 0.028(3) 0.019(3) 0.0244(19) -0.0021(17) 0.0028(19) -0.004(3) C21 0.022(3) 0.019(2) 0.0171(17) 0.0003(16) 0.0044(16) -0.001(3) C22 0.018(2) 0.030(3) 0.0162(18) 0.0034(17) 0.0018(15) -0.001(3) C23 0.036(3) 0.043(4) 0.032(2) -0.001(2) -0.017(2) -0.014(4) C24 0.026(3) 0.032(3) 0.0227(19) -0.002(2) -0.0018(19) -0.001(3) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.2769(6) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Gd1 . O2 5_664 2.509(4) yes Gd1 . C1 5_664 2.830(4) yes Gd1 . O1 5_664 2.451(3) yes Gd1 . O4 5_664 2.377(4) yes Gd1 . O6 5_665 2.259(3) yes Gd1 . O1 . 2.303(3) yes Gd1 . O3 . 2.364(4) yes Gd1 . O5 . 2.313(3) yes Gd1 . O7 . 2.377(4) yes O1 . C1 . 1.262(5) yes O2 . C1 . 1.245(4) yes O3 . C8 . 1.254(4) yes O4 . C8 . 1.273(4) yes O5 . C15 . 1.272(5) yes O6 . C15 . 1.250(5) yes O7 . C22 . 1.245(5) yes N1 . C22 . 1.312(5) yes N1 . C23 . 1.445(6) yes N1 . C24 . 1.446(6) yes C1 . C2 . 1.480(5) yes C2 . C3 . 1.378(6) yes C2 . C7 . 1.380(5) yes C3 . C4 . 1.390(6) yes C3 . H31 . 0.930 no C4 . C5 . 1.373(6) yes C4 . H41 . 0.930 no C5 . C6 . 1.376(6) yes C5 . H51 . 0.930 no C6 . C7 . 1.377(6) yes C6 . H61 . 0.930 no C7 . H71 . 0.930 no C8 . C9 . 1.495(5) yes C9 . C10 . 1.385(5) yes C9 . C14 . 1.386(5) yes C10 . C11 . 1.383(6) yes C10 . H101 . 0.930 no C11 . C12 . 1.366(6) yes C11 . H111 . 0.930 no C12 . C13 . 1.381(6) yes C12 . H121 . 0.930 no C13 . C14 . 1.379(6) yes C13 . H131 . 0.930 no C14 . H141 . 0.930 no C15 . C16 . 1.484(5) yes C16 . C17 . 1.385(5) yes C16 . C21 . 1.375(5) yes C17 . C18 . 1.394(6) yes C17 . H171 . 0.930 no C18 . C19 . 1.374(6) yes C18 . H181 . 0.930 no C19 . C20 . 1.378(6) yes C19 . H191 . 0.930 no C20 . C21 . 1.382(6) yes C20 . H201 . 0.930 no C21 . H211 . 0.930 no C22 . H221 . 0.930 no C23 . H231 . 0.961 no C23 . H232 . 0.961 no C23 . H233 . 0.959 no C24 . H241 . 0.958 no C24 . H242 . 0.962 no C24 . H243 . 0.962 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O2 5_664 Gd1 . C1 5_664 26.09(10) yes O2 5_664 Gd1 . O1 5_664 52.19(10) yes C1 5_664 Gd1 . O1 5_664 26.43(10) yes O2 5_664 Gd1 . O4 5_664 88.27(13) yes C1 5_664 Gd1 . O4 5_664 74.63(14) yes O1 5_664 Gd1 . O4 5_664 68.68(12) yes O2 5_664 Gd1 . O6 5_665 74.50(13) yes C1 5_664 Gd1 . O6 5_665 93.06(12) yes O1 5_664 Gd1 . O6 5_665 115.16(12) yes O4 5_664 Gd1 . O6 5_665 76.63(12) yes O2 5_664 Gd1 . O1 . 122.57(11) yes C1 5_664 Gd1 . O1 . 98.01(11) yes O1 5_664 Gd1 . O1 . 71.74(14) yes O4 5_664 Gd1 . O1 . 81.74(12) yes O6 5_665 Gd1 . O1 . 152.10(14) yes O2 5_664 Gd1 . O3 . 81.65(14) yes C1 5_664 Gd1 . O3 . 79.31(13) yes O1 5_664 Gd1 . O3 . 73.76(12) yes O4 5_664 Gd1 . O3 . 138.84(10) yes O6 5_665 Gd1 . O3 . 136.62(13) yes O2 5_664 Gd1 . O5 . 111.44(13) yes C1 5_664 Gd1 . O5 . 132.89(14) yes O1 5_664 Gd1 . O5 . 143.88(13) yes O4 5_664 Gd1 . O5 . 147.43(12) yes O6 5_665 Gd1 . O5 . 83.84(12) yes O2 5_664 Gd1 . O7 . 155.13(13) yes C1 5_664 Gd1 . O7 . 149.43(14) yes O1 5_664 Gd1 . O7 . 132.61(12) yes O4 5_664 Gd1 . O7 . 75.05(14) yes O6 5_665 Gd1 . O7 . 83.65(13) yes O1 . Gd1 . O3 . 70.91(13) yes O1 . Gd1 . O5 . 106.35(13) yes O3 . Gd1 . O5 . 71.82(12) yes O1 . Gd1 . O7 . 73.82(12) yes O3 . Gd1 . O7 . 123.00(14) yes O5 . Gd1 . O7 . 77.13(14) yes Gd1 5_664 O1 . Gd1 . 108.26(14) yes Gd1 5_664 O1 . C1 . 93.8(2) yes Gd1 . O1 . C1 . 157.1(3) yes Gd1 5_664 O2 . C1 . 91.5(3) yes Gd1 . O3 . C8 . 137.5(3) yes Gd1 5_664 O4 . C8 . 133.1(3) yes Gd1 . O5 . C15 . 127.8(3) yes Gd1 5_665 O6 . C15 . 147.2(3) yes Gd1 . O7 . C22 . 127.8(3) yes C22 . N1 . C23 . 121.4(4) yes C22 . N1 . C24 . 120.8(4) yes C23 . N1 . C24 . 117.8(4) yes Gd1 5_664 C1 . O1 . 59.8(2) yes Gd1 5_664 C1 . O2 . 62.4(2) yes O1 . C1 . O2 . 121.0(4) yes Gd1 5_664 C1 . C2 . 168.2(3) yes O1 . C1 . C2 . 116.7(3) yes O2 . C1 . C2 . 122.3(4) yes C1 . C2 . C3 . 117.4(4) yes C1 . C2 . C7 . 121.8(4) yes C3 . C2 . C7 . 120.2(4) yes C2 . C3 . C4 . 120.0(4) yes C2 . C3 . H31 . 120.0 no C4 . C3 . H31 . 120.0 no C3 . C4 . C5 . 119.2(4) yes C3 . C4 . H41 . 120.4 no C5 . C4 . H41 . 120.4 no C4 . C5 . C6 . 120.9(4) yes C4 . C5 . H51 . 119.6 no C6 . C5 . H51 . 119.6 no C5 . C6 . C7 . 119.8(4) yes C5 . C6 . H61 . 120.1 no C7 . C6 . H61 . 120.1 no C2 . C7 . C6 . 119.8(4) yes C2 . C7 . H71 . 120.1 no C6 . C7 . H71 . 120.1 no O4 . C8 . O3 . 124.8(4) yes O4 . C8 . C9 . 117.1(3) yes O3 . C8 . C9 . 118.1(3) yes C8 . C9 . C10 . 119.7(3) yes C8 . C9 . C14 . 120.8(3) yes C10 . C9 . C14 . 119.5(4) yes C9 . C10 . C11 . 120.1(4) yes C9 . C10 . H101 . 120.0 no C11 . C10 . H101 . 120.0 no C10 . C11 . C12 . 120.0(4) yes C10 . C11 . H111 . 120.0 no C12 . C11 . H111 . 120.0 no C11 . C12 . C13 . 120.5(4) yes C11 . C12 . H121 . 119.7 no C13 . C12 . H121 . 119.7 no C12 . C13 . C14 . 119.8(4) yes C12 . C13 . H131 . 120.1 no C14 . C13 . H131 . 120.1 no C9 . C14 . C13 . 120.1(4) yes C9 . C14 . H141 . 120.0 no C13 . C14 . H141 . 120.0 no O5 . C15 . O6 . 123.5(4) yes O5 . C15 . C16 . 117.0(3) yes O6 . C15 . C16 . 119.4(3) yes C15 . C16 . C17 . 119.4(3) yes C15 . C16 . C21 . 119.7(3) yes C17 . C16 . C21 . 120.9(4) yes C16 . C17 . C18 . 118.9(4) yes C16 . C17 . H171 . 120.6 no C18 . C17 . H171 . 120.6 no C17 . C18 . C19 . 120.0(4) yes C17 . C18 . H181 . 120.0 no C19 . C18 . H181 . 120.0 no C18 . C19 . C20 . 120.8(4) yes C18 . C19 . H191 . 119.6 no C20 . C19 . H191 . 119.6 no C19 . C20 . C21 . 119.6(4) yes C19 . C20 . H201 . 120.2 no C21 . C20 . H201 . 120.2 no C20 . C21 . C16 . 119.9(4) yes C20 . C21 . H211 . 120.1 no C16 . C21 . H211 . 120.1 no N1 . C22 . O7 . 124.6(4) yes N1 . C22 . H221 . 117.7 no O7 . C22 . H221 . 117.7 no N1 . C23 . H231 . 109.2 no N1 . C23 . H232 . 109.5 no H231 . C23 . H232 . 109.2 no N1 . C23 . H233 . 109.6 no H231 . C23 . H233 . 109.7 no H232 . C23 . H233 . 109.6 no N1 . C24 . H241 . 109.8 no N1 . C24 . H242 . 109.8 no H241 . C24 . H242 . 109.0 no N1 . C24 . H243 . 109.8 no H241 . C24 . H243 . 109.2 no H242 . C24 . H243 . 109.1 no data_gdpol8_Phase1_3_73GPa _database_code_depnum_ccdc_archive 'CCDC 768043' #TrackingRef '- Gd_polymer_cifs.cif' #3.73 GPa data set _audit_creation_date 08-06-30 _audit_creation_method CRYSTALS_ver_12.85 _oxford_structure_analysis_title 'gdpol8 in P4(2)/n' _chemical_name_systematic ; catena-((\m~2~-Benzoato-O,O')-bis(\m~2~-benzoato-O,O',O')-(dimethylformamide-O )-gadolinium) ; _chemical_melting_point ? _publ_section_exptl_prep ; ? ; #end of refcif _publ_section_exptl_refinement ; Pressure = 3.73 GPa. H atoms placed geometrically after each cycle. Because completeness is less than 100% the ligands were restrained to have the same bond distances and angles as at ambient pressure. Checkcif alerts: 027_ALERT_3_A _diffrn_reflns_theta_full (too) Low ............ 15.25 Deg. 029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.71 911_ALERT_3_B # Missing FCF Refl Between THmin & STh/L= 0.600 1157 913_ALERT_3_B # Missing Very Strong Reflections in FCF ....... 248 910_ALERT_3_C # Missing FCF Reflections Below Th(Min) ........ 2 912_ALERT_4_C # Missing FCF Reflections Above STh/L= 0.600 1326 Data are incomplete becasue of shading of reciprocal space by the body of the pressure cell. 411_ALERT_2_B Short Inter H...H Contact H31 .. H61 .. 2.05 Ang. 411_ALERT_2_C Short Inter H...H Contact H31 .. H51 .. 2.12 Ang. See text. This is a high-pressure structure. 220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.70 Ratio 232_ALERT_2_C Hirshfeld Test Diff (M-X) Gd1 -- O2_a .. 5.06 su Some distortion of the adps is expected given the completeness, temperature and presence of the heavy atom. 860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 86 See above 128_ALERT_4_C Non-standard setting of Space-group P42/n .... P42/n:1 See text. This makes comparison with the high pressure phase simpler. 034_ALERT_1_C No Flack Parameter Given. Z .GT. Si, NonCentro . ? This is a bug in Checkcif. The space group operation '-x+1/2,-y+1/2,-z+1/2' is an inversion centre at [1/4 1/4 1/4]. This test shouldn't be applied, but presumably is triggered when the -1 is not on the origin. 042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? The one given is more chemically meaningful. 199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K 200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K Correct 792_ALERT_1_G Check the Absolute Configuration of C1 = ... S The sum of the angles around C1 is 360.0(6) deg, so it is essentailly planar. Perhaps the algorithm is being 'put off' by a long Gd1-C1 'bond' in the connetivity list. No action. ; _cell_length_a 20.7490(3) _cell_length_b 20.7490(3) _cell_length_c 8.8988(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3831.12(12) _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'P 42/n:1' _symmetry_space_group_name_Hall 'P 4n -1n' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,z -y+1/2,x+1/2,z+1/2 y+1/2,-x+1/2,z+1/2 -x+1/2,-y+1/2,-z+1/2 x+1/2,y+1/2,-z+1/2 y,-x,-z -y,x,-z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0010 0.0010 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0020 0.0010 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0040 0.0030 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Gd -0.5090 2.0340 25.0709 2.2534 19.0798 0.1820 13.8518 12.9331 3.5454 101.3980 2.4196 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 8 _chemical_formula_sum 'C24 H22 Gd1 N1 O7' _chemical_formula_moiety ; (C24 H22 Gd1 N1 O7)n ; _chemical_compound_source ? _chemical_formula_weight 593.69 _cell_measurement_reflns_used 6458 _cell_measurement_theta_min 3 _cell_measurement_theta_max 20 _cell_measurement_temperature 293 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_max 0.20 _exptl_crystal_density_diffrn 2.058 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 2344 _exptl_absorpt_coefficient_mu 1.121 # Sheldrick geometric approximatio 0.50 0.70 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.27 _exptl_absorpt_correction_T_max 0.70 _diffrn_measurement_device 'Bruker SMART' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator Silicon _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.48650 _diffrn_source synchrotron _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'SMART (Siemens, 1993)' _computing_cell_refinement 'SAINT (Siemens ,1995)' _computing_data_reduction 'SAINT (Siemens ,1995)' _computing_structure_solution 'USER DEFINED STRUCTURE SOLUTION' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'DIAMOND Crystal Impact (2004)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 293 _diffrn_reflns_number 21264 _reflns_number_total 3398 _diffrn_reflns_av_R_equivalents 0.069 _diffrn_reflns_theta_min 1.344 _diffrn_reflns_theta_max 20.332 _diffrn_measured_fraction_theta_max 0.582 _diffrn_reflns_theta_full 15.249 _diffrn_measured_fraction_theta_full 0.709 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _reflns_limit_h_min -12 _reflns_limit_h_max 14 _reflns_limit_k_min 0 _reflns_limit_k_max 28 _reflns_limit_l_min 0 _reflns_limit_l_max 12 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.75 _refine_diff_density_max 0.80 # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>2.0\s(I) _refine_ls_number_reflns 2646 _refine_ls_number_restraints 86 _refine_ls_number_parameters 298 _oxford_refine_ls_R_factor_ref 0.0322 _refine_ls_wR_factor_ref 0.0369 _refine_ls_goodness_of_fit_ref 1.1218 _refine_ls_shift/su_max 0.002593 # The values computed from all data _oxford_reflns_number_all 3298 _refine_ls_R_factor_all 0.0433 _refine_ls_wR_factor_all 0.0477 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 2646 _refine_ls_R_factor_gt 0.0322 _refine_ls_wR_factor_gt 0.0369 _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment noref # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.763 0.373 0.224 ; _publ_section_references ; User-defined structure solution reference Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Siemens Industrial Automation, Inc (1993). SMART: Area-Detector Software Package; Madison, WI. Siemens Industrial Automation, Inc (1995). SAINT: Area-Detector Integration Software.; Madison, WI. Siemens Industrial Automation, Inc (1996). SADABS: Area-Detector Absorption Correction;: Madison, WI. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Gd1 Gd 0.736651(11) 0.748524(10) -0.036034(18) 0.0119 1.0000 Uani . . . . . . . O1 O 0.79380(16) 0.70090(16) -0.2274(3) 0.0170 1.0000 Uani D . . . . . . O2 O 0.85734(18) 0.67819(18) -0.4161(3) 0.0223 1.0000 Uani D . . . . . . O3 O 0.66984(17) 0.67337(17) -0.1616(3) 0.0201 1.0000 Uani D . . . . . . O4 O 0.69461(18) 0.66368(17) -0.4052(3) 0.0222 1.0000 Uani D . . . . . . O5 O 0.70955(19) 0.66802(17) 0.1313(3) 0.0236 1.0000 Uani D . . . . . . O6 O 0.77002(18) 0.68729(16) 0.3316(3) 0.0205 1.0000 Uani D . . . . . . O7 O 0.83779(17) 0.7193(2) 0.0676(3) 0.0234 1.0000 Uani D . . . . . . N1 N 0.9100(2) 0.7240(2) 0.2586(4) 0.0228 1.0000 Uani D . . . . . . C1 C 0.8381(2) 0.6672(2) -0.2860(4) 0.0162 1.0000 Uani D . . . . . . C2 C 0.8650(2) 0.6144(2) -0.1928(4) 0.0175 1.0000 Uani D . . . . . . C3 C 0.9297(2) 0.6017(3) -0.2062(5) 0.0322 1.0000 Uani D . . . . . . C4 C 0.9598(2) 0.5627(3) -0.1027(6) 0.0405 1.0000 Uani D . . . . . . C5 C 0.9241(2) 0.5339(2) 0.0082(5) 0.0254 1.0000 Uani D . . . . . . C6 C 0.8590(2) 0.5440(2) 0.0182(4) 0.0250 1.0000 Uani D . . . . . . C7 C 0.8290(2) 0.5856(2) -0.0800(4) 0.0198 1.0000 Uani D . . . . . . C8 C 0.6704(2) 0.6424(2) -0.2826(4) 0.0166 1.0000 Uani D . . . . . . C9 C 0.6400(2) 0.5779(2) -0.2847(4) 0.0148 1.0000 Uani D . . . . . . C10 C 0.6097(2) 0.5553(2) -0.1568(4) 0.0229 1.0000 Uani D . . . . . . C11 C 0.5796(2) 0.4957(2) -0.1588(4) 0.0266 1.0000 Uani D . . . . . . C12 C 0.5796(3) 0.4595(2) -0.2885(5) 0.0336 1.0000 Uani D . . . . . . C13 C 0.6105(3) 0.4812(2) -0.4162(5) 0.0298 1.0000 Uani D . . . . . . C14 C 0.6406(2) 0.5405(2) -0.4140(4) 0.0189 1.0000 Uani D . . . . . . C15 C 0.7416(2) 0.64983(19) 0.2457(3) 0.0161 1.0000 Uani D . . . . . . C16 C 0.7419(2) 0.58016(19) 0.2781(4) 0.0156 1.0000 Uani D . . . . . . C17 C 0.7794(2) 0.5563(2) 0.3952(4) 0.0231 1.0000 Uani D . . . . . . C18 C 0.7773(3) 0.4910(2) 0.4276(4) 0.0268 1.0000 Uani D . . . . . . C19 C 0.7399(3) 0.4510(2) 0.3424(5) 0.0289 1.0000 Uani D . . . . . . C20 C 0.7034(2) 0.4740(2) 0.2254(4) 0.0213 1.0000 Uani D . . . . . . C21 C 0.7048(2) 0.5388(2) 0.1926(4) 0.0183 1.0000 Uani D . . . . . . C22 C 0.8709(2) 0.7506(2) 0.1596(4) 0.0226 1.0000 Uani D . . . . . . C23 C 0.9460(3) 0.7633(3) 0.3637(5) 0.0348 1.0000 Uani D . . . . . . C24 C 0.9183(3) 0.6553(3) 0.2656(5) 0.0262 1.0000 Uani D . . . . . . H231 H 0.9268 0.8054 0.3685 0.0417 1.0000 Uiso . . . . . . . H232 H 0.9898 0.7669 0.3311 0.0417 1.0000 Uiso . . . . . . . H233 H 0.9444 0.7438 0.4619 0.0417 1.0000 Uiso . . . . . . . H241 H 0.8904 0.6353 0.1941 0.0315 1.0000 Uiso . . . . . . . H242 H 0.9624 0.6447 0.2432 0.0315 1.0000 Uiso . . . . . . . H243 H 0.9079 0.6406 0.3649 0.0315 1.0000 Uiso . . . . . . . H31 H 0.9531 0.6194 -0.2851 0.0386 1.0000 Uiso . . . . . . . H41 H 1.0040 0.5560 -0.1079 0.0486 1.0000 Uiso . . . . . . . H51 H 0.9444 0.5071 0.0775 0.0305 1.0000 Uiso . . . . . . . H61 H 0.8350 0.5228 0.0913 0.0300 1.0000 Uiso . . . . . . . H71 H 0.7852 0.5942 -0.0708 0.0238 1.0000 Uiso . . . . . . . H101 H 0.6096 0.5800 -0.0696 0.0275 1.0000 Uiso . . . . . . . H111 H 0.5593 0.4802 -0.0728 0.0319 1.0000 Uiso . . . . . . . H121 H 0.5586 0.4200 -0.2900 0.0403 1.0000 Uiso . . . . . . . H131 H 0.6111 0.4561 -0.5028 0.0358 1.0000 Uiso . . . . . . . H141 H 0.6615 0.5554 -0.4997 0.0226 1.0000 Uiso . . . . . . . H171 H 0.8056 0.5838 0.4510 0.0278 1.0000 Uiso . . . . . . . H181 H 0.8013 0.4745 0.5070 0.0321 1.0000 Uiso . . . . . . . H191 H 0.7392 0.4072 0.3641 0.0347 1.0000 Uiso . . . . . . . H201 H 0.6780 0.4461 0.1689 0.0256 1.0000 Uiso . . . . . . . H211 H 0.6807 0.5548 0.1128 0.0220 1.0000 Uiso . . . . . . . H221 H 0.8677 0.7953 0.1581 0.0271 1.0000 Uiso . . . . . . . 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 Gd1 0.01465(13) 0.01226(13) 0.00873(10) 0.00096(6) -0.00027(6) -0.00034(12) O1 0.0191(17) 0.0178(16) 0.0143(11) 0.0019(11) -0.0015(11) 0.011(2) O2 0.0259(19) 0.0268(19) 0.0142(12) 0.0041(12) 0.0037(12) 0.004(2) O3 0.0144(16) 0.0290(19) 0.0169(12) -0.0055(12) 0.0008(11) -0.014(2) O4 0.030(2) 0.0217(18) 0.0153(11) 0.0006(11) 0.0036(12) -0.007(2) O5 0.034(2) 0.0195(17) 0.0173(12) 0.0047(11) -0.0039(13) -0.002(2) O6 0.0301(19) 0.0164(16) 0.0149(11) -0.0024(11) 0.0047(12) -0.006(2) O7 0.0191(18) 0.035(2) 0.0164(12) 0.0013(13) -0.0023(11) 0.007(2) N1 0.021(2) 0.029(2) 0.0177(15) -0.0023(15) -0.0029(14) -0.003(3) C1 0.018(2) 0.013(2) 0.0172(16) 0.0029(15) 0.0021(15) 0.003(3) C2 0.020(2) 0.014(2) 0.0183(16) 0.0052(15) 0.0066(15) 0.004(3) C3 0.031(3) 0.025(3) 0.041(3) 0.011(2) 0.019(2) 0.013(4) C4 0.016(3) 0.045(4) 0.060(3) 0.020(3) 0.006(2) 0.009(4) C5 0.025(3) 0.022(3) 0.029(2) 0.0092(19) -0.0039(18) 0.009(3) C6 0.028(3) 0.027(3) 0.0205(18) 0.0062(17) 0.0059(17) 0.007(3) C7 0.018(2) 0.019(2) 0.0225(18) 0.0007(16) 0.0057(16) 0.002(3) C8 0.012(2) 0.020(2) 0.0171(15) 0.0029(15) -0.0013(14) -0.001(3) C9 0.012(2) 0.016(2) 0.0166(15) 0.0001(14) 0.0000(14) 0.002(3) C10 0.026(3) 0.026(3) 0.0173(17) 0.0038(16) 0.0061(16) 0.005(3) C11 0.025(3) 0.025(3) 0.029(2) 0.0042(19) 0.0125(19) -0.006(4) C12 0.041(4) 0.017(3) 0.043(3) 0.001(2) 0.008(2) -0.010(4) C13 0.039(3) 0.023(3) 0.028(2) -0.0076(18) 0.006(2) 0.000(4) C14 0.022(2) 0.016(2) 0.0188(17) 0.0013(15) 0.0028(16) -0.005(3) C15 0.019(2) 0.018(2) 0.0109(14) 0.0018(14) 0.0067(14) -0.003(3) C16 0.021(2) 0.014(2) 0.0121(14) 0.0003(13) 0.0051(14) -0.001(3) C17 0.035(3) 0.018(2) 0.0163(16) -0.0006(15) -0.0004(18) 0.006(3) C18 0.035(3) 0.023(3) 0.0221(18) 0.0105(17) -0.0040(19) 0.000(3) C19 0.043(4) 0.015(2) 0.029(2) 0.0024(17) 0.007(2) 0.003(4) C20 0.026(3) 0.013(2) 0.0241(17) -0.0036(15) 0.0030(17) -0.001(3) C21 0.021(2) 0.017(2) 0.0172(16) 0.0008(15) 0.0015(15) 0.000(3) C22 0.018(2) 0.033(3) 0.0163(16) 0.0038(17) 0.0022(15) 0.002(3) C23 0.035(3) 0.037(3) 0.032(2) -0.004(2) -0.009(2) -0.015(4) C24 0.024(3) 0.032(3) 0.0228(18) -0.0011(18) -0.0025(17) -0.003(3) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.2749(5) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Gd1 . O2 5_664 2.509(4) yes Gd1 . O1 5_664 2.436(3) yes Gd1 . O4 5_664 2.372(3) yes Gd1 . O6 5_665 2.259(3) yes Gd1 . O1 . 2.298(3) yes Gd1 . O3 . 2.367(3) yes Gd1 . O5 . 2.307(3) yes Gd1 . O7 . 2.371(3) yes O1 . C1 . 1.267(5) yes O2 . C1 . 1.245(4) yes O3 . C8 . 1.254(4) yes O4 . C8 . 1.280(4) yes O5 . C15 . 1.273(4) yes O6 . C15 . 1.240(4) yes O7 . C22 . 1.249(5) yes N1 . C22 . 1.319(5) yes N1 . C23 . 1.448(5) yes N1 . C24 . 1.436(6) yes C1 . C2 . 1.482(5) yes C2 . C3 . 1.374(6) yes C2 . C7 . 1.386(5) yes C3 . C4 . 1.375(6) yes C3 . H31 . 0.930 no C4 . C5 . 1.371(6) yes C4 . H41 . 0.930 no C5 . C6 . 1.371(6) yes C5 . H51 . 0.930 no C6 . C7 . 1.376(5) yes C6 . H61 . 0.930 no C7 . H71 . 0.930 no C8 . C9 . 1.481(5) yes C9 . C10 . 1.382(5) yes C9 . C14 . 1.388(5) yes C10 . C11 . 1.385(6) yes C10 . H101 . 0.930 no C11 . C12 . 1.377(6) yes C11 . H111 . 0.930 no C12 . C13 . 1.380(6) yes C12 . H121 . 0.930 no C13 . C14 . 1.379(6) yes C13 . H131 . 0.930 no C14 . H141 . 0.930 no C15 . C16 . 1.474(5) yes C16 . C17 . 1.392(5) yes C16 . C21 . 1.382(5) yes C17 . C18 . 1.385(6) yes C17 . H171 . 0.930 no C18 . C19 . 1.366(6) yes C18 . H181 . 0.930 no C19 . C20 . 1.373(6) yes C19 . H191 . 0.930 no C20 . C21 . 1.375(5) yes C20 . H201 . 0.930 no C21 . H211 . 0.930 no C22 . H221 . 0.930 no C23 . H231 . 0.961 no C23 . H232 . 0.957 no C23 . H233 . 0.963 no C24 . H241 . 0.956 no C24 . H242 . 0.962 no C24 . H243 . 0.960 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O2 5_664 Gd1 . O1 5_664 52.45(9) yes O2 5_664 Gd1 . O4 5_664 87.97(12) yes O1 5_664 Gd1 . O4 5_664 68.57(11) yes O2 5_664 Gd1 . O6 5_665 74.45(12) yes O1 5_664 Gd1 . O6 5_665 115.22(11) yes O4 5_664 Gd1 . O6 5_665 76.20(11) yes O2 5_664 Gd1 . O1 . 122.39(9) yes O1 5_664 Gd1 . O1 . 71.26(12) yes O4 5_664 Gd1 . O1 . 81.76(11) yes O6 5_665 Gd1 . O1 . 151.87(13) yes O2 5_664 Gd1 . O3 . 82.17(12) yes O1 5_664 Gd1 . O3 . 73.97(11) yes O4 5_664 Gd1 . O3 . 138.95(10) yes O6 5_665 Gd1 . O3 . 137.12(12) yes O1 . Gd1 . O3 . 70.68(11) yes O2 5_664 Gd1 . O5 . 111.03(12) yes O1 5_664 Gd1 . O5 . 143.76(11) yes O4 5_664 Gd1 . O5 . 147.65(11) yes O6 5_665 Gd1 . O5 . 83.81(11) yes O1 . Gd1 . O5 . 107.01(12) yes O2 5_664 Gd1 . O7 . 155.33(12) yes O1 5_664 Gd1 . O7 . 132.53(11) yes O4 5_664 Gd1 . O7 . 75.51(13) yes O6 5_665 Gd1 . O7 . 83.77(13) yes O1 . Gd1 . O7 . 73.85(11) yes O3 . Gd1 . O5 . 71.64(11) yes O3 . Gd1 . O7 . 122.26(13) yes O5 . Gd1 . O7 . 77.27(13) yes Gd1 5_664 O1 . Gd1 . 108.74(12) yes Gd1 5_664 O1 . C1 . 94.0(2) yes Gd1 . O1 . C1 . 156.4(2) yes Gd1 5_664 O2 . C1 . 91.1(3) yes Gd1 . O3 . C8 . 137.5(3) yes Gd1 5_664 O4 . C8 . 133.5(3) yes Gd1 . O5 . C15 . 127.1(3) yes Gd1 5_665 O6 . C15 . 146.8(3) yes Gd1 . O7 . C22 . 127.5(3) yes C22 . N1 . C23 . 120.9(4) yes C22 . N1 . C24 . 121.1(4) yes C23 . N1 . C24 . 118.0(4) yes O1 . C1 . O2 . 120.9(3) yes O1 . C1 . C2 . 116.8(3) yes O2 . C1 . C2 . 122.3(3) yes C1 . C2 . C3 . 117.5(3) yes C1 . C2 . C7 . 121.4(3) yes C3 . C2 . C7 . 120.4(4) yes C2 . C3 . C4 . 119.9(4) yes C2 . C3 . H31 . 120.0 no C4 . C3 . H31 . 120.0 no C3 . C4 . C5 . 119.6(4) yes C3 . C4 . H41 . 120.2 no C5 . C4 . H41 . 120.2 no C4 . C5 . C6 . 120.7(4) yes C4 . C5 . H51 . 119.6 no C6 . C5 . H51 . 119.6 no C5 . C6 . C7 . 120.0(4) yes C5 . C6 . H61 . 120.0 no C7 . C6 . H61 . 120.0 no C2 . C7 . C6 . 119.2(4) yes C2 . C7 . H71 . 120.4 no C6 . C7 . H71 . 120.4 no O4 . C8 . O3 . 124.0(4) yes O4 . C8 . C9 . 117.9(3) yes O3 . C8 . C9 . 118.1(3) yes C8 . C9 . C10 . 119.4(3) yes C8 . C9 . C14 . 120.8(3) yes C10 . C9 . C14 . 119.8(3) yes C9 . C10 . C11 . 119.8(3) yes C9 . C10 . H101 . 120.1 no C11 . C10 . H101 . 120.1 no C10 . C11 . C12 . 119.8(4) yes C10 . C11 . H111 . 120.1 no C12 . C11 . H111 . 120.1 no C11 . C12 . C13 . 120.9(4) yes C11 . C12 . H121 . 119.6 no C13 . C12 . H121 . 119.6 no C12 . C13 . C14 . 119.3(4) yes C12 . C13 . H131 . 120.3 no C14 . C13 . H131 . 120.4 no C9 . C14 . C13 . 120.4(3) yes C9 . C14 . H141 . 119.8 no C13 . C14 . H141 . 119.8 no O5 . C15 . O6 . 123.8(4) yes O5 . C15 . C16 . 116.7(3) yes O6 . C15 . C16 . 119.4(3) yes C15 . C16 . C17 . 119.9(3) yes C15 . C16 . C21 . 119.9(3) yes C17 . C16 . C21 . 120.2(3) yes C16 . C17 . C18 . 119.1(4) yes C16 . C17 . H171 . 120.5 no C18 . C17 . H171 . 120.5 no C17 . C18 . C19 . 119.8(4) yes C17 . C18 . H181 . 120.1 no C19 . C18 . H181 . 120.1 no C18 . C19 . C20 . 121.6(4) yes C18 . C19 . H191 . 119.2 no C20 . C19 . H191 . 119.2 no C19 . C20 . C21 . 119.2(4) yes C19 . C20 . H201 . 120.4 no C21 . C20 . H201 . 120.4 no C16 . C21 . C20 . 120.1(3) yes C16 . C21 . H211 . 119.9 no C20 . C21 . H211 . 119.9 no N1 . C22 . O7 . 124.0(4) yes N1 . C22 . H221 . 118.0 no O7 . C22 . H221 . 118.0 no N1 . C23 . H231 . 109.1 no N1 . C23 . H232 . 109.7 no H231 . C23 . H232 . 109.6 no N1 . C23 . H233 . 109.3 no H231 . C23 . H233 . 109.2 no H232 . C23 . H233 . 109.9 no N1 . C24 . H241 . 109.3 no N1 . C24 . H242 . 109.5 no H241 . C24 . H242 . 109.9 no N1 . C24 . H243 . 109.1 no H241 . C24 . H243 . 109.7 no H242 . C24 . H243 . 109.3 no data_gdpol9_Phase2_5_0GPa _database_code_depnum_ccdc_archive 'CCDC 768044' #TrackingRef '- Gd_polymer_cifs.cif' #5.01 GPa data set. Phase 2 _audit_creation_date 10-02-27 _audit_creation_method CRYSTALS_ver_12.87 _oxford_structure_analysis_title 'p-4 in P-4' _chemical_name_systematic ? _chemical_melting_point ? _publ_section_exptl_refinement ; #5.01 GPa data set H atoms placed geometrically after each cycle Because completeness is less than 100% the ligands were restrained to have the same bond distances and angles as at ambient pressure. The data quality deteriorated as a result of the phase transition, and only the Gd atoms were refined with adps. Checkcif output: 027_ALERT_3_A _diffrn_reflns_theta_full (too) Low ............ 15.23 Deg. 029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.71 911_ALERT_3_B Missing # FCF Refl Between THmin & STh/L= 0.600 1126 910_ALERT_3_C Missing # of FCF Reflections Below Th(Min) ..... 2 915_ALERT_3_C Low Friedel Pair Coverage ...................... 53.45 Perc 912_ALERT_4_C Missing # of FCF Reflections Above STh/L= 0.600 1293 950_ALERT_1_C Reported and Calculated Hmax Values Differ by .. 14 Data are incomplete becasue of shading of reciprocal space by the body of the pressure cell. 201_ALERT_2_A Isotropic non-H Atoms in Main Residue(s) ....... 64 See above. 919_ALERT_3_B Reflection(s) # Likely Affected by the Beamstop 3 ...or gasket 220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.62 Ratio 342_ALERT_3_C Low Bond Precision on C-C Bonds (x 1000) Ang ... 10 Some distortion of the adps is expected given the completeness, temperature and presence of the heavy atom. 411_ALERT_2_C Short Inter H...H Contact H1041 .. H71 .. 2.06 Ang. 411_ALERT_2_C Short Inter H...H Contact H101 .. H111 .. 2.08 Ang. See test: this is a high pressure structure. 860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 172 See above. 141_ALERT_4_C su on a - Axis Small or Missing (x 100000) ..... 20 Ang. No action 033_ALERT_4_G Flack x Parameter Value Deviates from Zero ..... 0.83 The structure is twinned by inversion becasue the low-pressure phase was centrosymmetric. The 'hand' was chosen to facilitate comparison with phase 1. 092_ALERT_4_G Check: Wavelength given is not Cu,Mo or Ag Ka .. 0.49 Ang. 720_ALERT_4_G Number of Unusual/Non-Standard Labels .......... 22 760_ALERT_1_G CIF Contains no Torsion Angles ................. ? 796_ALERT_4_G O-Atom in CIF Coordinate List out of Sequence .. O3 No action 929_ALERT_4_G No Interpretable (SHELX) Weight Parameters found ? A Shelx weighting scheme wasn't used! See below. ; _cell_length_a 20.0734(2) _cell_length_b 20.0734(2) _cell_length_c 9.13850(10) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3682.28(7) _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'P -4 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z y,-x,-z -x,-y,z -y,x,-z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0000 0.0010 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0010 0.0010 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0030 0.0030 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Gd -0.5390 1.9630 25.0709 2.2534 19.0798 0.1820 13.8518 12.9331 3.5454 101.3980 2.4196 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C19 H19 Gd4 N1 O4 # Dc = 1.72 Fooo = 2344.00 Mu = 71.24 M = 954.36 # Found Formula = C48 H44 Gd2 N2 O14 # Dc = 2.14 FOOO = 2344.00 Mu = 36.58 M = 1187.38 _chemical_formula_sum 'C48 H44 Gd2 N2 O14' _chemical_formula_moiety 'C48 H44 Gd2 N2 O14' _chemical_compound_source ? _chemical_formula_weight 1187.38 _cell_measurement_reflns_used 7883 _cell_measurement_theta_min 2 _cell_measurement_theta_max 20 _cell_measurement_temperature 293 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_max 0.20 _exptl_crystal_density_diffrn 2.142 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 2344 _exptl_absorpt_coefficient_mu 1.166 # Sheldrick geometric approximatio 0.48 0.69 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.34 _exptl_absorpt_correction_T_max 0.69 _diffrn_measurement_device 'Bruker SMART' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator Silicon _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.48650 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'SMART (Siemens, 1993)' _computing_cell_refinement 'SAINT (Siemens ,1995)' _computing_data_reduction 'SAINT (Siemens ,1995)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 293 _diffrn_reflns_number 19799 _reflns_number_total 6303 _diffrn_reflns_av_R_equivalents 0.068 # Number of reflections with Friedels Law is 3482 # Number of reflections without Friedels Law is 6303 # Theoretical number of reflections is about 5602 _diffrn_reflns_theta_min 1.389 _diffrn_reflns_theta_max 20.310 _diffrn_measured_fraction_theta_max 0.586 _diffrn_reflns_theta_full 15.232 _diffrn_measured_fraction_theta_full 0.712 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _reflns_limit_h_min -27 _reflns_limit_h_max 27 _reflns_limit_k_min 0 _reflns_limit_k_max 26 _reflns_limit_l_min 0 _reflns_limit_l_max 13 _oxford_diffrn_Wilson_B_factor 0.74 _oxford_diffrn_Wilson_scale 119.42 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -2.62 _refine_diff_density_max 1.96 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>2.0\s(I) _refine_ls_number_reflns 5867 _refine_ls_number_restraints 172 _refine_ls_number_parameters 276 _oxford_refine_ls_R_factor_ref 0.0512 _refine_ls_wR_factor_ref 0.0543 _refine_ls_goodness_of_fit_ref 0.9479 _refine_ls_shift/su_max 0.001905 # The values computed from all data _oxford_reflns_number_all 6303 _refine_ls_R_factor_all 0.0573 _refine_ls_wR_factor_all 0.0831 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 5867 _refine_ls_R_factor_gt 0.0512 _refine_ls_wR_factor_gt 0.0543 _refine_ls_abs_structure_Flack 0.83(3) _refine_ls_abs_structure_details 'Flack (1983), 2821 Friedel-pairs' # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration ad _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment none # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 1.81 0.266 0.779 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Flack, H. D. (1983). Acta Cryst. A39, 876-881. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Siemens Industrial Automation, Inc (1993). SMART: Area-Detector Software Package; Madison, WI. Siemens Industrial Automation, Inc (1995). SAINT: Area-Detector Integration Software.; Madison, WI. Siemens Industrial Automation, Inc (1996). SADABS: Area-Detector Absorption Correction;: Madison, WI. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Gd1 Gd 0.23638(2) 0.27165(2) -0.44345(3) 0.0114 1.0000 Uani . . . . . . . Gd2 Gd 0.20954(2) 0.27744(2) -0.02790(3) 0.0127 1.0000 Uani . . . . . . . N1 N 0.3817(5) 0.2695(4) 0.2796(7) 0.0251(18) 1.0000 Uiso D . . . . . . N10 N 0.0641(4) 0.2724(3) -0.7492(7) 0.0195(15) 1.0000 Uiso D . . . . . . O1 O 0.2768(3) 0.2289(3) -0.2003(5) 0.0134(10) 1.0000 Uiso D . . . . . . O2 O 0.3314(3) 0.1973(3) -0.3951(5) 0.0155(12) 1.0000 Uiso D . . . . . . O4 O 0.1535(4) 0.1817(4) -0.1382(6) 0.0201(13) 1.0000 Uiso D . . . . . . O3 O 0.1821(4) 0.1766(3) -0.3750(6) 0.0186(13) 1.0000 Uiso D . . . . . . O6 O 0.2546(3) 0.2148(3) -0.6537(5) 0.0164(12) 1.0000 Uiso D . . . . . . O5 O 0.1982(4) 0.1956(3) -0.8587(6) 0.0183(13) 1.0000 Uiso D . . . . . . O7 O 0.3162(4) 0.2614(3) 0.0786(6) 0.0204(13) 1.0000 Uiso D . . . . . . O10 O 0.1678(3) 0.3212(4) -0.2680(6) 0.0185(13) 1.0000 Uiso D . . . . . . O20 O 0.1175(3) 0.3590(3) -0.0718(6) 0.0171(12) 1.0000 Uiso D . . . . . . O30 O 0.3027(4) 0.3522(4) -0.3369(6) 0.0220(14) 1.0000 Uiso D . . . . . . O40 O 0.2732(3) 0.3690(3) -0.1037(6) 0.0171(12) 1.0000 Uiso D . . . . . . O60 O 0.2416(4) 0.3582(4) -0.6035(6) 0.0225(14) 1.0000 Uiso D . . . . . . O50 O 0.1949(3) 0.3390(3) -0.8189(6) 0.0160(12) 1.0000 Uiso D . . . . . . O70 O 0.1290(4) 0.2768(4) -0.5470(6) 0.0231(13) 1.0000 Uiso D . . . . . . C1 C 0.3173(4) 0.1902(4) -0.2644(6) 0.0126(15) 1.0000 Uiso D . . . . . . C2 C 0.3494(3) 0.1355(3) -0.1806(6) 0.0142(15) 1.0000 Uiso D . . . . . . C3 C 0.3194(3) 0.1075(3) -0.0591(7) 0.0149(15) 1.0000 Uiso D . . . . . . C4 C 0.3520(4) 0.0579(3) 0.0185(7) 0.0149(15) 1.0000 Uiso D . . . . . . C5 C 0.4145(4) 0.0379(4) -0.0250(7) 0.0203(17) 1.0000 Uiso D . . . . . . C6 C 0.4451(4) 0.0658(4) -0.1440(7) 0.0176(16) 1.0000 Uiso D . . . . . . C7 C 0.4121(4) 0.1139(4) -0.2225(7) 0.0193(17) 1.0000 Uiso D . . . . . . C8 C 0.1598(4) 0.1503(3) -0.2605(6) 0.0156(16) 1.0000 Uiso D . . . . . . C9 C 0.1341(3) 0.0810(3) -0.2725(6) 0.0185(17) 1.0000 Uiso D . . . . . . C10 C 0.0993(4) 0.0522(4) -0.1602(7) 0.0207(18) 1.0000 Uiso D . . . . . . C11 C 0.0721(4) -0.0111(4) -0.1774(7) 0.0236(19) 1.0000 Uiso D . . . . . . C12 C 0.0800(4) -0.0434(4) -0.3075(8) 0.029(2) 1.0000 Uiso D . . . . . . C13 C 0.1150(4) -0.0152(4) -0.4204(8) 0.028(2) 1.0000 Uiso D . . . . . . C14 C 0.1422(4) 0.0470(4) -0.4017(7) 0.0214(18) 1.0000 Uiso D . . . . . . C15 C 0.2316(4) 0.1762(3) -0.7464(7) 0.0140(15) 1.0000 Uiso D . . . . . . C16 C 0.2372(4) 0.1030(3) -0.7271(6) 0.0135(15) 1.0000 Uiso D . . . . . . C17 C 0.2805(4) 0.0775(4) -0.6245(7) 0.0200(17) 1.0000 Uiso D . . . . . . C18 C 0.2862(4) 0.0090(4) -0.6073(7) 0.0207(18) 1.0000 Uiso D . . . . . . C19 C 0.2475(4) -0.0320(4) -0.6911(8) 0.025(2) 1.0000 Uiso D . . . . . . C20 C 0.2041(4) -0.0066(4) -0.7938(8) 0.024(2) 1.0000 Uiso D . . . . . . C21 C 0.1992(4) 0.0611(4) -0.8114(7) 0.0206(18) 1.0000 Uiso D . . . . . . C22 C 0.3420(5) 0.2945(4) 0.1786(8) 0.025(2) 1.0000 Uiso D . . . . . . C23 C 0.4016(6) 0.3073(6) 0.4077(10) 0.033(2) 1.0000 Uiso D . . . . . . C24 C 0.4002(7) 0.2004(5) 0.2790(11) 0.032(2) 1.0000 Uiso D . . . . . . C80 C 0.3058(4) 0.3843(4) -0.2196(6) 0.0161(16) 1.0000 Uiso D . . . . . . C90 C 0.3493(3) 0.4436(3) -0.2130(6) 0.0157(15) 1.0000 Uiso D . . . . . . C100 C 0.3853(4) 0.4618(4) -0.3350(7) 0.0172(16) 1.0000 Uiso D . . . . . . C101 C 0.1325(5) 0.3656(4) -0.2032(6) 0.0190(17) 1.0000 Uiso D . . . . . . C102 C 0.1121(3) 0.4255(3) -0.2890(6) 0.0170(16) 1.0000 Uiso D . . . . . . C103 C 0.1163(4) 0.4239(4) -0.4391(7) 0.0195(17) 1.0000 Uiso D . . . . . . C104 C 0.0957(4) 0.4779(4) -0.5227(7) 0.0243(19) 1.0000 Uiso D . . . . . . C105 C 0.0716(4) 0.5332(4) -0.4542(8) 0.0250(19) 1.0000 Uiso D . . . . . . C106 C 0.0674(4) 0.5358(4) -0.3036(7) 0.0216(18) 1.0000 Uiso D . . . . . . C107 C 0.0881(4) 0.4824(4) -0.2213(7) 0.0224(18) 1.0000 Uiso D . . . . . . C110 C 0.4283(4) 0.5162(4) -0.3272(7) 0.0224(18) 1.0000 Uiso D . . . . . . C120 C 0.4337(4) 0.5509(4) -0.1985(8) 0.027(2) 1.0000 Uiso D . . . . . . C130 C 0.3975(4) 0.5327(4) -0.0775(8) 0.026(2) 1.0000 Uiso D . . . . . . C140 C 0.3551(4) 0.4792(4) -0.0847(7) 0.0204(18) 1.0000 Uiso D . . . . . . C150 C 0.2236(5) 0.3771(3) -0.7269(6) 0.0133(15) 1.0000 Uiso D . . . . . . C160 C 0.2390(3) 0.4468(3) -0.7697(6) 0.0188(17) 1.0000 Uiso D . . . . . . C170 C 0.2115(4) 0.4742(4) -0.8937(7) 0.0191(17) 1.0000 Uiso D . . . . . . C180 C 0.2302(4) 0.5380(4) -0.9372(7) 0.0205(17) 1.0000 Uiso D . . . . . . C190 C 0.2759(4) 0.5723(4) -0.8561(8) 0.027(2) 1.0000 Uiso D . . . . . . C200 C 0.3035(4) 0.5450(4) -0.7319(7) 0.0234(19) 1.0000 Uiso D . . . . . . C210 C 0.2843(4) 0.4826(4) -0.6879(7) 0.0210(18) 1.0000 Uiso D . . . . . . C220 C 0.1044(5) 0.2454(4) -0.6520(7) 0.0179(17) 1.0000 Uiso D . . . . . . C230 C 0.0457(6) 0.3414(4) -0.7415(10) 0.026(2) 1.0000 Uiso D . . . . . . C240 C 0.0432(6) 0.2365(5) -0.8771(9) 0.0248(19) 1.0000 Uiso D . . . . . . H231 H 0.3895 0.3534 0.3944 0.0382 1.0000 Uiso . . . . . . . H232 H 0.4486 0.3038 0.4215 0.0382 1.0000 Uiso . . . . . . . H233 H 0.3788 0.2902 0.4924 0.0382 1.0000 Uiso . . . . . . . H241 H 0.3785 0.1781 0.1995 0.0355 1.0000 Uiso . . . . . . . H242 H 0.4477 0.1969 0.2678 0.0355 1.0000 Uiso . . . . . . . H243 H 0.3872 0.1804 0.3700 0.0355 1.0000 Uiso . . . . . . . H2401 H 0.0649 0.1941 -0.8804 0.0297 1.0000 Uiso . . . . . . . H2402 H 0.0544 0.2616 -0.9632 0.0297 1.0000 Uiso . . . . . . . H2403 H -0.0042 0.2300 -0.8738 0.0297 1.0000 Uiso . . . . . . . H2301 H 0.0660 0.3612 -0.6564 0.0292 1.0000 Uiso . . . . . . . H2302 H 0.0614 0.3641 -0.8272 0.0292 1.0000 Uiso . . . . . . . H2303 H -0.0016 0.3451 -0.7343 0.0292 1.0000 Uiso . . . . . . . H31 H 0.2776 0.1221 -0.0294 0.0171 1.0000 Uiso . . . . . . . H41 H 0.3318 0.0383 0.0993 0.0171 1.0000 Uiso . . . . . . . H51 H 0.4361 0.0044 0.0269 0.0237 1.0000 Uiso . . . . . . . H61 H 0.4876 0.0521 -0.1715 0.0202 1.0000 Uiso . . . . . . . H71 H 0.4323 0.1324 -0.3048 0.0226 1.0000 Uiso . . . . . . . H101 H 0.0931 0.0752 -0.0729 0.0243 1.0000 Uiso . . . . . . . H111 H 0.0493 -0.0314 -0.1010 0.0276 1.0000 Uiso . . . . . . . H121 H 0.0626 -0.0861 -0.3188 0.0341 1.0000 Uiso . . . . . . . H131 H 0.1208 -0.0380 -0.5080 0.0330 1.0000 Uiso . . . . . . . H141 H 0.1656 0.0667 -0.4780 0.0252 1.0000 Uiso . . . . . . . H171 H 0.3059 0.1061 -0.5670 0.0235 1.0000 Uiso . . . . . . . H181 H 0.3161 -0.0086 -0.5398 0.0243 1.0000 Uiso . . . . . . . H191 H 0.2506 -0.0779 -0.6786 0.0296 1.0000 Uiso . . . . . . . H201 H 0.1783 -0.0351 -0.8503 0.0285 1.0000 Uiso . . . . . . . H211 H 0.1701 0.0785 -0.8806 0.0242 1.0000 Uiso . . . . . . . H221 H 0.3326 0.3399 0.1825 0.0291 1.0000 Uiso . . . . . . . H1001 H 0.3813 0.4377 -0.4216 0.0202 1.0000 Uiso . . . . . . . H1101 H 0.4531 0.5290 -0.4085 0.0260 1.0000 Uiso . . . . . . . H1201 H 0.4618 0.5876 -0.1934 0.0322 1.0000 Uiso . . . . . . . H1301 H 0.4014 0.5567 0.0089 0.0303 1.0000 Uiso . . . . . . . H1401 H 0.3307 0.4665 -0.0029 0.0239 1.0000 Uiso . . . . . . . H1031 H 0.1328 0.3861 -0.4853 0.0226 1.0000 Uiso . . . . . . . H1041 H 0.0984 0.4764 -0.6243 0.0290 1.0000 Uiso . . . . . . . H1051 H 0.0584 0.5698 -0.5094 0.0295 1.0000 Uiso . . . . . . . H1061 H 0.0509 0.5737 -0.2577 0.0252 1.0000 Uiso . . . . . . . H1071 H 0.0855 0.4842 -0.1198 0.0261 1.0000 Uiso . . . . . . . H1701 H 0.1812 0.4498 -0.9488 0.0227 1.0000 Uiso . . . . . . . H1801 H 0.2114 0.5571 -1.0202 0.0237 1.0000 Uiso . . . . . . . H1901 H 0.2875 0.6154 -0.8839 0.0322 1.0000 Uiso . . . . . . . H2001 H 0.3343 0.5690 -0.6776 0.0275 1.0000 Uiso . . . . . . . H2101 H 0.3027 0.4639 -0.6039 0.0250 1.0000 Uiso . . . . . . . H2201 H 0.1152 0.2005 -0.6622 0.0208 1.0000 Uiso . . . . . . . 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 Gd1 0.0143(2) 0.0112(2) 0.00860(13) 0.00057(12) -0.00044(12) 0.0003(2) Gd2 0.0151(2) 0.0137(2) 0.00928(13) 0.00050(13) -0.00019(12) 0.0020(2) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.3096(5) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Gd1 . O1 . 2.516(5) yes Gd1 . O2 . 2.462(7) yes Gd1 . O3 . 2.284(7) yes Gd1 . O6 . 2.265(6) yes Gd1 . O10 . 2.336(6) yes Gd1 . O30 . 2.309(7) yes Gd1 . O60 . 2.273(6) yes Gd1 . O70 . 2.357(7) yes Gd2 . O50 1_556 2.294(6) yes Gd2 . O5 1_556 2.268(6) yes Gd2 . O1 . 2.292(5) yes Gd2 . O4 . 2.445(7) yes Gd2 . O7 . 2.375(7) yes Gd2 . O10 . 2.508(6) yes Gd2 . O20 . 2.501(7) yes Gd2 . O40 . 2.343(7) yes N1 . C22 . 1.319(8) yes N1 . C23 . 1.452(8) yes N1 . C24 . 1.437(8) yes N10 . C220 . 1.318(7) yes N10 . C230 . 1.434(8) yes N10 . C240 . 1.436(8) yes O1 . C1 . 1.267(7) yes O2 . C1 . 1.236(6) yes O4 . C8 . 1.289(7) yes O3 . C8 . 1.255(7) yes O6 . C15 . 1.237(7) yes O5 . C15 . 1.286(7) yes O7 . C22 . 1.243(7) yes O10 . C101 . 1.283(7) yes O20 . C101 . 1.246(6) yes O30 . C80 . 1.253(7) yes O40 . C80 . 1.282(7) yes O60 . C150 . 1.244(7) yes O50 . C150 . 1.274(6) yes O70 . C220 . 1.249(7) yes C1 . C2 . 1.487(7) yes C2 . C3 . 1.383(7) yes C2 . C7 . 1.385(8) yes C3 . C4 . 1.388(7) yes C3 . H31 . 0.928 no C4 . C5 . 1.375(8) yes C4 . H41 . 0.931 no C5 . C6 . 1.370(7) yes C5 . H51 . 0.930 no C6 . C7 . 1.374(8) yes C6 . H61 . 0.930 no C7 . H71 . 0.932 no C8 . C9 . 1.488(7) yes C9 . C10 . 1.370(7) yes C9 . C14 . 1.373(7) yes C10 . C11 . 1.392(8) yes C10 . H101 . 0.930 no C11 . C12 . 1.364(8) yes C11 . H111 . 0.929 no C12 . C13 . 1.371(8) yes C12 . H121 . 0.930 no C13 . C14 . 1.373(8) yes C13 . H131 . 0.930 no C14 . H141 . 0.929 no C15 . C16 . 1.485(7) yes C16 . C17 . 1.377(7) yes C16 . C21 . 1.372(7) yes C17 . C18 . 1.388(8) yes C17 . H171 . 0.930 no C18 . C19 . 1.367(8) yes C18 . H181 . 0.930 no C19 . C20 . 1.379(8) yes C19 . H191 . 0.930 no C20 . C21 . 1.370(8) yes C20 . H201 . 0.929 no C21 . H211 . 0.929 no C22 . H221 . 0.931 no C23 . H231 . 0.963 no C23 . H232 . 0.954 no C23 . H233 . 0.962 no C24 . H241 . 0.957 no C24 . H242 . 0.961 no C24 . H243 . 0.960 no C80 . C90 . 1.478(7) yes C90 . C100 . 1.379(7) yes C90 . C140 . 1.377(7) yes C100 . C110 . 1.395(8) yes C100 . H1001 . 0.930 no C101 . C102 . 1.492(7) yes C102 . C103 . 1.375(7) yes C102 . C107 . 1.385(8) yes C103 . C104 . 1.390(8) yes C103 . H1031 . 0.930 no C104 . C105 . 1.363(8) yes C104 . H1041 . 0.930 no C105 . C106 . 1.379(7) yes C105 . H1051 . 0.930 no C106 . C107 . 1.374(8) yes C106 . H1061 . 0.930 no C107 . H1071 . 0.930 no C110 . C120 . 1.370(8) yes C110 . H1101 . 0.930 no C120 . C130 . 1.372(8) yes C120 . H1201 . 0.929 no C130 . C140 . 1.371(8) yes C130 . H1301 . 0.929 no C140 . H1401 . 0.929 no C150 . C160 . 1.485(7) yes C160 . C170 . 1.375(7) yes C160 . C210 . 1.378(7) yes C170 . C180 . 1.393(8) yes C170 . H1701 . 0.928 no C180 . C190 . 1.365(8) yes C180 . H1801 . 0.930 no C190 . C200 . 1.377(8) yes C190 . H1901 . 0.930 no C200 . C210 . 1.371(8) yes C200 . H2001 . 0.928 no C210 . H2101 . 0.931 no C220 . H2201 . 0.932 no C230 . H2301 . 0.964 no C230 . H2302 . 0.959 no C230 . H2303 . 0.956 no C240 . H2401 . 0.957 no C240 . H2402 . 0.962 no C240 . H2403 . 0.962 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1 . Gd1 . O2 . 52.04(17) yes O1 . Gd1 . O3 . 68.1(2) yes O2 . Gd1 . O3 . 79.3(2) yes O1 . Gd1 . O6 . 121.7(2) yes O2 . Gd1 . O6 . 73.8(2) yes O3 . Gd1 . O6 . 83.6(2) yes O1 . Gd1 . O10 . 74.29(19) yes O2 . Gd1 . O10 . 126.27(18) yes O3 . Gd1 . O10 . 83.5(2) yes O6 . Gd1 . O10 . 153.2(2) yes O1 . Gd1 . O30 . 71.4(2) yes O2 . Gd1 . O30 . 84.4(2) yes O3 . Gd1 . O30 . 138.1(2) yes O6 . Gd1 . O30 . 128.1(2) yes O10 . Gd1 . O30 . 75.7(3) yes O1 . Gd1 . O60 . 144.5(2) yes O2 . Gd1 . O60 . 122.9(2) yes O3 . Gd1 . O60 . 146.7(2) yes O6 . Gd1 . O60 . 80.3(2) yes O10 . Gd1 . O60 . 98.2(3) yes O1 . Gd1 . O70 . 131.6(2) yes O2 . Gd1 . O70 . 143.9(2) yes O3 . Gd1 . O70 . 73.1(3) yes O6 . Gd1 . O70 . 80.2(2) yes O10 . Gd1 . O70 . 73.6(2) yes O30 . Gd1 . O60 . 73.1(2) yes O30 . Gd1 . O70 . 131.7(3) yes O60 . Gd1 . O70 . 75.5(3) yes O50 1_556 Gd2 . O5 1_556 79.0(2) yes O50 1_556 Gd2 . O1 . 151.3(2) yes O5 1_556 Gd2 . O1 . 102.7(2) yes O50 1_556 Gd2 . O4 . 135.1(2) yes O5 1_556 Gd2 . O4 . 70.4(2) yes O1 . Gd2 . O4 . 69.7(2) yes O50 1_556 Gd2 . O7 . 81.3(2) yes O5 1_556 Gd2 . O7 . 73.3(2) yes O1 . Gd2 . O7 . 72.1(2) yes O4 . Gd2 . O7 . 118.5(2) yes O50 1_556 Gd2 . O10 . 119.8(2) yes O5 1_556 Gd2 . O10 . 144.8(2) yes O1 . Gd2 . O10 . 75.20(19) yes O4 . Gd2 . O10 . 76.2(2) yes O7 . Gd2 . O10 . 135.0(2) yes O50 1_556 Gd2 . O20 . 71.7(2) yes O5 1_556 Gd2 . O20 . 120.6(2) yes O1 . Gd2 . O20 . 127.10(17) yes O4 . Gd2 . O20 . 96.2(2) yes O7 . Gd2 . O20 . 145.2(2) yes O50 1_556 Gd2 . O40 . 83.9(2) yes O5 1_556 Gd2 . O40 . 145.6(2) yes O1 . Gd2 . O40 . 79.0(2) yes O4 . Gd2 . O40 . 138.24(19) yes O7 . Gd2 . O40 . 74.7(2) yes O10 . Gd2 . O20 . 51.93(18) yes O10 . Gd2 . O40 . 69.4(2) yes O20 . Gd2 . O40 . 80.9(2) yes C22 . N1 . C23 . 122.2(6) yes C22 . N1 . C24 . 121.5(6) yes C23 . N1 . C24 . 115.9(6) yes C220 . N10 . C230 . 121.4(5) yes C220 . N10 . C240 . 121.5(5) yes C230 . N10 . C240 . 116.7(6) yes Gd1 . O1 . Gd2 . 105.8(2) yes Gd1 . O1 . C1 . 90.4(3) yes Gd2 . O1 . C1 . 162.9(4) yes Gd1 . O2 . C1 . 93.7(4) yes Gd2 . O4 . C8 . 134.1(5) yes Gd1 . O3 . C8 . 138.6(5) yes Gd1 . O6 . C15 . 146.7(6) yes Gd2 1_554 O5 . C15 . 135.3(5) yes Gd2 . O7 . C22 . 127.1(6) yes Gd2 . O10 . Gd1 . 104.7(2) yes Gd2 . O10 . C101 . 91.4(4) yes Gd1 . O10 . C101 . 159.7(5) yes Gd2 . O20 . C101 . 92.6(4) yes Gd1 . O30 . C80 . 138.6(5) yes Gd2 . O40 . C80 . 135.2(5) yes Gd1 . O60 . C150 . 143.5(5) yes Gd2 1_554 O50 . C150 . 144.6(6) yes Gd1 . O70 . C220 . 130.4(6) yes O1 . C1 . O2 . 121.6(5) yes O1 . C1 . C2 . 119.5(4) yes O2 . C1 . C2 . 118.9(5) yes C1 . C2 . C3 . 121.6(5) yes C1 . C2 . C7 . 118.9(5) yes C3 . C2 . C7 . 119.4(5) yes C2 . C3 . C4 . 119.7(5) yes C2 . C3 . H31 . 120.1 no C4 . C3 . H31 . 120.2 no C3 . C4 . C5 . 119.5(5) yes C3 . C4 . H41 . 120.2 no C5 . C4 . H41 . 120.3 no C4 . C5 . C6 . 121.3(6) yes C4 . C5 . H51 . 119.3 no C6 . C5 . H51 . 119.4 no C5 . C6 . C7 . 119.0(6) yes C5 . C6 . H61 . 120.4 no C7 . C6 . H61 . 120.6 no C2 . C7 . C6 . 121.0(5) yes C2 . C7 . H71 . 119.6 no C6 . C7 . H71 . 119.4 no O4 . C8 . O3 . 123.5(6) yes O4 . C8 . C9 . 119.1(5) yes O3 . C8 . C9 . 117.1(5) yes C8 . C9 . C10 . 121.1(5) yes C8 . C9 . C14 . 119.2(5) yes C10 . C9 . C14 . 119.7(5) yes C9 . C10 . C11 . 120.0(5) yes C9 . C10 . H101 . 120.0 no C11 . C10 . H101 . 119.9 no C10 . C11 . C12 . 119.1(6) yes C10 . C11 . H111 . 120.5 no C12 . C11 . H111 . 120.4 no C11 . C12 . C13 . 121.3(6) yes C11 . C12 . H121 . 119.4 no C13 . C12 . H121 . 119.3 no C12 . C13 . C14 . 119.1(6) yes C12 . C13 . H131 . 120.5 no C14 . C13 . H131 . 120.4 no C9 . C14 . C13 . 120.8(5) yes C9 . C14 . H141 . 119.5 no C13 . C14 . H141 . 119.7 no O5 . C15 . O6 . 123.5(5) yes O5 . C15 . C16 . 115.7(5) yes O6 . C15 . C16 . 120.7(5) yes C15 . C16 . C17 . 119.8(5) yes C15 . C16 . C21 . 119.9(5) yes C17 . C16 . C21 . 120.3(5) yes C16 . C17 . C18 . 119.8(5) yes C16 . C17 . H171 . 120.1 no C18 . C17 . H171 . 120.1 no C17 . C18 . C19 . 119.1(6) yes C17 . C18 . H181 . 120.4 no C19 . C18 . H181 . 120.6 no C18 . C19 . C20 . 121.2(6) yes C18 . C19 . H191 . 119.3 no C20 . C19 . H191 . 119.5 no C19 . C20 . C21 . 119.5(6) yes C19 . C20 . H201 . 120.2 no C21 . C20 . H201 . 120.4 no C16 . C21 . C20 . 120.1(5) yes C16 . C21 . H211 . 120.0 no C20 . C21 . H211 . 119.9 no N1 . C22 . O7 . 124.1(6) yes N1 . C22 . H221 . 117.9 no O7 . C22 . H221 . 117.9 no N1 . C23 . H231 . 109.3 no N1 . C23 . H232 . 109.9 no H231 . C23 . H232 . 109.8 no N1 . C23 . H233 . 109.3 no H231 . C23 . H233 . 108.8 no H232 . C23 . H233 . 109.7 no N1 . C24 . H241 . 109.6 no N1 . C24 . H242 . 109.1 no H241 . C24 . H242 . 109.6 no N1 . C24 . H243 . 109.2 no H241 . C24 . H243 . 109.8 no H242 . C24 . H243 . 109.4 no O40 . C80 . O30 . 124.0(5) yes O40 . C80 . C90 . 117.4(5) yes O30 . C80 . C90 . 118.6(5) yes C80 . C90 . C100 . 119.4(5) yes C80 . C90 . C140 . 120.2(5) yes C100 . C90 . C140 . 120.4(5) yes C90 . C100 . C110 . 119.4(5) yes C90 . C100 . H1001 . 120.4 no C110 . C100 . H1001 . 120.2 no O10 . C101 . O20 . 120.2(5) yes O10 . C101 . C102 . 117.9(5) yes O20 . C101 . C102 . 121.8(5) yes C101 . C102 . C103 . 119.3(5) yes C101 . C102 . C107 . 121.6(4) yes C103 . C102 . C107 . 119.1(5) yes C102 . C103 . C104 . 120.8(5) yes C102 . C103 . H1031 . 119.6 no C104 . C103 . H1031 . 119.6 no C103 . C104 . C105 . 119.3(5) yes C103 . C104 . H1041 . 120.4 no C105 . C104 . H1041 . 120.4 no C104 . C105 . C106 . 120.7(6) yes C104 . C105 . H1051 . 119.7 no C106 . C105 . H1051 . 119.6 no C105 . C106 . C107 . 119.9(6) yes C105 . C106 . H1061 . 120.1 no C107 . C106 . H1061 . 120.0 no C102 . C107 . C106 . 120.3(5) yes C102 . C107 . H1071 . 119.8 no C106 . C107 . H1071 . 119.9 no C100 . C110 . C120 . 119.4(5) yes C100 . C110 . H1101 . 120.4 no C120 . C110 . H1101 . 120.3 no C110 . C120 . C130 . 121.0(6) yes C110 . C120 . H1201 . 119.6 no C130 . C120 . H1201 . 119.5 no C120 . C130 . C140 . 119.9(6) yes C120 . C130 . H1301 . 120.1 no C140 . C130 . H1301 . 120.0 no C90 . C140 . C130 . 120.0(5) yes C90 . C140 . H1401 . 119.9 no C130 . C140 . H1401 . 120.1 no O50 . C150 . O60 . 123.1(5) yes O50 . C150 . C160 . 119.1(4) yes O60 . C150 . C160 . 117.8(5) yes C150 . C160 . C170 . 120.6(5) yes C150 . C160 . C210 . 119.1(5) yes C170 . C160 . C210 . 120.2(5) yes C160 . C170 . C180 . 119.6(5) yes C160 . C170 . H1701 . 120.0 no C180 . C170 . H1701 . 120.4 no C170 . C180 . C190 . 119.4(5) yes C170 . C180 . H1801 . 120.1 no C190 . C180 . H1801 . 120.5 no C180 . C190 . C200 . 121.1(6) yes C180 . C190 . H1901 . 119.2 no C200 . C190 . H1901 . 119.6 no C190 . C200 . C210 . 119.5(6) yes C190 . C200 . H2001 . 120.1 no C210 . C200 . H2001 . 120.4 no C160 . C210 . C200 . 120.2(5) yes C160 . C210 . H2101 . 120.0 no C200 . C210 . H2101 . 119.8 no N10 . C220 . O70 . 123.6(6) yes N10 . C220 . H2201 . 118.2 no O70 . C220 . H2201 . 118.2 no N10 . C230 . H2301 . 109.3 no N10 . C230 . H2302 . 109.5 no H2301 . C230 . H2302 . 108.8 no N10 . C230 . H2303 . 109.6 no H2301 . C230 . H2303 . 109.4 no H2302 . C230 . H2303 . 110.1 no N10 . C240 . H2401 . 109.8 no N10 . C240 . H2402 . 109.5 no H2401 . C240 . H2402 . 109.5 no N10 . C240 . H2403 . 109.4 no H2401 . C240 . H2403 . 109.3 no H2402 . C240 . H2403 . 109.1 no