#------------------------------------------------------------------------------ #$Date: 2013-12-29 13:49:26 +0200 (Sun, 29 Dec 2013) $ #$Revision: 91935 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/31/68/4316844.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4316844 loop_ _publ_author_name 'Marco Taddei' 'Ferdinando Costantino' 'Riccardo Vivani' _publ_contact_author_address ; Dipartimento di Chimica, Perugia University, Via Elce di Sotto 8, 06123 Perugia, Italy. ; _publ_contact_author_email marcotaddei@hotmail.com _publ_contact_author_name 'Dr Marco Taddei' _publ_section_title ; Synthesis and Crystal Structure from X-ray Powder Diffraction Data of Two Zirconium Diphosphonates Containing Piperazine Groups ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 9664 _journal_page_last 9670 _journal_volume 49 _journal_year 2010 _chemical_formula_sum 'C18 N6 O27 P6 Zr2' _chemical_formula_weight 1100.5 _chemical_name_systematic ' ?' _space_group_IT_number 148 _symmetry_cell_setting trigonal _symmetry_space_group_name_Hall '-R 3' _symmetry_space_group_name_H-M 'R -3 :H' _audit_creation_method 'from EXP file using GSAS2CIF' _cell_angle_alpha 90.0 _cell_angle_beta 90.0 _cell_angle_gamma 120.0 _cell_formula_units_Z 3 _cell_length_a 19.9400(9) _cell_length_b 19.94 _cell_length_c 9.5728(6) _cell_measurement_temperature 298 _cell_volume 3296.2(3) _computing_structure_refinement GSAS _diffrn_ambient_temperature 298 _diffrn_detector_type 'Panalytical X'Celerator' _diffrn_measurement_device_type 'Bragg-Brentano Diffractometer' _diffrn_radiation_polarisn_ratio 0.5 _diffrn_radiation_probe x-ray _diffrn_source 'LFF tube' _diffrn_source_target Cu _pd_calc_method 'Rietveld Refinement' _pd_char_colour white _pd_phase_name 1 _pd_proc_info_datetime 2010-08-26T18:46:52 _pd_proc_ls_background_function ; GSAS Background function number 1 with 18 terms. Shifted Chebyshev function of 1st kind 1: 5675.30 2: -4517.38 3: 1664.20 4: -553.286 5: 545.183 6: -587.222 7: 565.836 8: -500.713 9: 262.741 10: 44.7604 11: -136.813 12: 34.2035 13: 118.311 14: -108.125 15: -38.2978 16: 153.730 17: -126.394 18: 64.5745 ; _pd_proc_ls_peak_cutoff 0.00100 _pd_proc_ls_pref_orient_corr ; March-Dollase AXIS 1 Ratio= 0.87595 h= 0.000 k= 0.000 l= 1.000 Prefered orientation correction range: Min= 0.81987, Max= 1.48769 ; _pd_proc_ls_profile_function ; CW Profile function number 3 with 19 terms Pseudovoigt profile coefficients as parameterized in P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. Asymmetry correction of L.W. Finger, D.E. Cox & A. P. Jephcoat (1994). J. Appl. Cryst.,27,892-900. Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 1.0 1.0 0.0 ; _pd_proc_ls_prof_R_factor 0.0327 _pd_proc_ls_prof_wR_expected 0.0119 _pd_proc_ls_prof_wR_factor 0.0435 _refine_ls_goodness_of_fit_all 4.04 _refine_ls_matrix_type full _refine_ls_number_parameters 63 _refine_ls_number_restraints 29 _refine_ls_R_Fsqd_factor 0.04626 _refine_ls_shift/su_max 0.10 _refine_ls_shift/su_mean 0.02 _[local]_cod_data_source_file ic1014048_si_001_2.cif _[local]_cod_data_source_block Compound_1 _[local]_cod_cif_authors_sg_H-M 'R -3' _cod_depositor_comments ; The following automatic conversions were performed: '_geom_angle_publ_flag' value 'N' changed to 'n' according to the built-in table from CIF Core dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (44 times). '_geom_bond_publ_flag' value 'N' changed to 'n' according to the built-in table from CIF Core dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (57 times). Automatic conversion script Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana ; _cod_original_cell_volume 3296.23(26) _cod_database_code 4316844 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +x,+y,+z 2 -y,x-y,+z 3 y-x,-x,+z -1 -x,-y,-z -2 +y,y-x,-z -3 x-y,+x,-z 101 +x+1/3,+y+2/3,+z+2/3 102 -y+1/3,x-y+2/3,+z+2/3 103 y-x+1/3,-x+2/3,+z+2/3 -101 -x+2/3,-y+1/3,-z+1/3 -102 +y+2/3,y-x+1/3,-z+1/3 -103 x-y+2/3,+x+1/3,-z+1/3 201 +x+2/3,+y+1/3,+z+1/3 202 -y+2/3,x-y+1/3,+z+1/3 203 y-x+2/3,-x+1/3,+z+1/3 -201 -x+1/3,-y+2/3,-z+2/3 -202 +y+1/3,y-x+2/3,-z+2/3 -203 x-y+1/3,+x+2/3,-z+2/3 loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_thermal_displace_type _atom_site_U_iso_or_equiv _atom_site_symmetry_multiplicity Zr ZR1 0.0 0.0 0.0 1.0 Uiso 0.010(1) 3 Zr ZR2 0.0 0.0 0.5 1.0 Uiso 0.010(1) 3 P P1 0.1351(4) 0.1131(4) 0.2478(9) 1.0 Uiso 0.042(4) 18 O O1 0.0807(4) 0.0712(4) 0.3746(5) 1.0 Uiso 0.055(4) 18 C C1 0.1191(11) 0.1926(6) 0.1944(16) 1.0 Uiso 0.055(4) 18 N N1 0.1526(12) 0.2663(6) 0.2655(15) 1.0 Uiso 0.055(4) 18 O O2 0.2248(6) 0.1457(9) 0.2742(14) 1.0 Uiso 0.055(4) 18 C C2 0.1791(14) 0.3325(10) 0.1633(11) 1.0 Uiso 0.055(4) 18 C C3 0.1573(14) 0.2717(9) 0.4158(15) 1.0 Uiso 0.055(4) 18 O O3 0.0897(4) 0.0530(4) 0.1235(5) 1.0 Uiso 0.055(4) 18 O Ow1 0.2888(9) 0.0698(8) 0.1289(18) 0.78(1) Uiso 0.055(4) 18 O Ow2 0.0097(10) 0.3433(9) -0.0155(24) 0.72(1) Uiso 0.055(4) 18 loop_ _atom_type_symbol _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source Zr 6.0 0.000 0.000 17.8765 1.27618 10.9480 11.9160 5.41732 0.11762 3.65721 87.6627 2.06929 International_Tables_Vol_C P 18.0 0.000 0.000 6.43450 1.90670 4.17910 27.1570 1.78000 0.52600 1.49080 68.1645 1.11490 International_Tables_Vol_C O 81.0 0.000 0.000 3.04850 13.2771 2.28680 5.70110 1.54630 0.32390 0.86700 32.9089 0.25080 International_Tables_Vol_C C 54.0 0.000 0.000 2.31000 20.8439 1.02000 10.2075 1.58860 0.56870 0.86500 51.6512 0.21560 International_Tables_Vol_C N 18.0 0.000 0.000 12.2126 0.00570 3.13220 9.89330 2.01250 28.9975 1.16630 0.58260 -11.529 International_Tables_Vol_C loop_ _diffrn_radiation_wavelength _diffrn_radiation_wavelength_wt _diffrn_radiation_type _diffrn_radiation_wavelength_id 1.540600 1.000 K\a~1~ 1 1.544400 0.500 K\a~2~ 2 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 ZR1 O3 87.22(25) 1_555 . 2_555 n O3 ZR1 O3 87.22(25) 1_555 . 3_555 n O3 ZR1 O3 180.0 1_555 . -1_555 n O3 ZR1 O3 92.78(25) 1_555 . -2_555 n O3 ZR1 O3 92.78(25) 1_555 . -3_555 n O3 ZR1 O3 87.22(25) 2_555 . 3_555 n O3 ZR1 O3 92.78(25) 2_555 . -1_555 n O3 ZR1 O3 180.0 2_555 . -2_555 n O3 ZR1 O3 92.78(25) 2_555 . -3_555 n O3 ZR1 O3 92.78(25) 3_555 . -1_555 n O3 ZR1 O3 92.78(25) 3_555 . -2_555 n O3 ZR1 O3 180.0 3_555 . -3_555 n O3 ZR1 O3 87.22(25) -1_555 . -2_555 n O3 ZR1 O3 87.22(25) -1_555 . -3_555 n O3 ZR1 O3 87.22(25) -2_555 . -3_555 n O1 ZR2 O1 85.71(25) 1_555 . 2_555 n O1 ZR2 O1 85.71(25) 1_555 . 3_555 n O1 ZR2 O1 179.972 1_555 . -1_556 n O1 ZR2 O1 94.29(25) 1_555 . -2_556 n O1 ZR2 O1 94.29(25) 1_555 . -3_556 n O1 ZR2 O1 85.71(25) 2_555 . 3_555 n O1 ZR2 O1 94.29(25) 2_555 . -1_556 n O1 ZR2 O1 179.9802 2_555 . -2_556 n O1 ZR2 O1 94.29(25) 2_555 . -3_556 n O1 ZR2 O1 94.29(25) 3_555 . -1_556 n O1 ZR2 O1 94.29(25) 3_555 . -2_556 n O1 ZR2 O1 179.9802 3_555 . -3_556 n O1 ZR2 O1 85.71(25) -1_556 . -2_556 n O1 ZR2 O1 85.71(25) -1_556 . -3_556 n O1 ZR2 O1 85.71(25) -2_556 . -3_556 n O1 P1 C1 107.8(8) 1_555 . 1_555 n O1 P1 O2 115.7(7) 1_555 . 1_555 n O1 P1 O3 101.2(5) 1_555 . 1_555 n C1 P1 O2 109.7(8) 1_555 . 1_555 n C1 P1 O3 99.2(6) 1_555 . 1_555 n O2 P1 O3 121.4(9) 1_555 . 1_555 n ZR2 O1 P1 166.5(5) 1_555 . 1_555 n P1 C1 N1 123.7(10) 1_555 . 1_555 n C1 N1 C2 111.4(12) 1_555 . 1_555 n C1 N1 C3 121.7(12) 1_555 . 1_555 n C2 N1 C3 126.8(10) 1_555 . 1_555 n N1 C2 C3 102.6(10) 1_555 . -101_555 n N1 C3 C2 125.5(13) 1_555 . -101_555 n ZR1 O3 P1 150.7(5) 1_555 . 1_555 n loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag ZR1 O3 1.955(6) . 1_555 n ZR1 O3 1.955(6) . 2_555 n ZR1 O3 1.955(6) . 3_555 n ZR1 O3 1.955(6) . -1_555 n ZR1 O3 1.955(6) . -2_555 n ZR1 O3 1.955(6) . -3_555 n ZR2 O1 1.939(6) . 1_555 n ZR2 O1 1.939(6) . 2_555 n ZR2 O1 1.939(6) . 3_555 n ZR2 O1 1.939(6) . -1_556 n ZR2 O1 1.939(6) . -2_556 n ZR2 O1 1.939(6) . -3_556 n P1 O1 1.562(8) . 1_555 n P1 C1 1.838(10) . 1_555 n P1 O2 1.590(9) . 1_555 n P1 O3 1.609(8) . 1_555 n O1 ZR2 1.939(6) . 1_555 n O1 P1 1.562(8) . 1_555 n O1 O1 2.638(12) . 2_555 n O1 O1 2.638(12) . 3_555 n O1 O1 2.843(9) . -2_556 n O1 O1 2.843(9) . -3_556 n O1 O2 2.669(11) . 1_555 n O1 O3 2.450(7) . 1_555 n C1 P1 1.838(10) . 1_555 n C1 N1 1.445(10) . 1_555 n C1 O3 2.629(10) . 1_555 n N1 C1 1.445(10) . 1_555 n N1 N1 2.766(15) . -101_444 n N1 C2 1.511(10) . 1_555 n N1 C3 1.443(10) . 1_555 n N1 C3 2.370(14) . -101_444 n O2 P1 1.590(9) . 1_555 n O2 O1 2.669(11) . 1_555 n O2 O3 2.789(12) . 1_555 n O2 Ow1 2.789(14) . 1_555 n O2 Ow1 2.847(14) . -201_444 n C2 N1 1.511(10) . 1_555 n C2 C3 1.527(11) . -101_444 n C3 N1 1.443(10) . 1_555 n C3 N1 2.370(14) . -101_444 n C3 C2 1.527(11) . -101_444 n O3 ZR1 1.955(6) . 1_555 n O3 P1 1.609(8) . 1_555 n O3 O1 2.450(7) . 1_555 n O3 C1 2.629(10) . 1_555 n O3 O2 2.789(12) . 1_555 n O3 O3 2.697(12) . 2_555 n O3 O3 2.697(12) . 3_555 n O3 O3 2.831(9) . -2_555 n O3 O3 2.831(9) . -3_555 n Ow1 O2 2.789(14) . 1_555 n Ow1 O2 2.847(14) . -201_444 n Ow1 Ow2 2.576(21) . 3_555 n Ow1 Ow2 2.582(21) . 202_555 n Ow2 Ow1 2.576(21) . 2_555 n Ow2 Ow1 2.582(21) . 103_554 n _journal_paper_doi 10.1021/ic1014048