#------------------------------------------------------------------------------ #$Date: 2012-02-24 19:13:23 +0200 (Fri, 24 Feb 2012) $ #$Revision: 34330 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/31/68/4316843.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_4316843 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_moiety 'C6 F2 N2 O6 P2 Zr' _chemical_formula_sum 'C6 F2 N2 O6 P2 Zr' _chemical_formula_weight 387.24 _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _audit_creation_method 'from EXP file using GSAS2CIF' _cell_angle_alpha 90.0 _cell_angle_beta 105.1748(12) _cell_angle_gamma 90.0 _cell_formula_units_Z 2 _cell_length_a 8.71482(18) _cell_length_b 8.17309(14) _cell_length_c 9.01343(16) _cell_measurement_temperature 298 _cell_volume 619.61(2) _computing_structure_refinement GSAS _computing_structure_solution FOX _diffrn_ambient_temperature 298 _diffrn_detector_type 'Panalytical X'Celerator' _diffrn_measurement_device_type 'Bragg-Brentano Diffractometer' _diffrn_radiation_polarisn_ratio 0.50 _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 2 _pd_proc_info_datetime 2010-07-13T11:32:19 _pd_proc_ls_background_function ; GSAS Background function number 1 with 18 terms. Shifted Chebyshev function of 1st kind 1: 505.232 2: -231.829 3: 122.168 4: 49.3194 5: -38.5786 6: 21.0472 7: -22.7744 8: 16.7219 9: -2.17111 10: -24.6409 11: 34.5788 12: -20.8852 13: 5.60928 14: 11.0862 15: -17.0268 16: 14.9077 17: 1.07036 18: 0.638268 ; _pd_proc_ls_peak_cutoff 0.00100 _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 0.0050 times the peak Aniso. broadening axis 0.0 0.0 1.0 ; _pd_proc_ls_prof_R_factor 0.0650 _pd_proc_ls_prof_wR_expected 0.0294 _pd_proc_ls_prof_wR_factor 0.0851 _refine_ls_goodness_of_fit_all 2.91 _refine_ls_matrix_type full _refine_ls_number_parameters 58 _refine_ls_number_restraints 0 _refine_ls_R_Fsqd_factor 0.06595 _refine_ls_shift/su_max 0.10 _refine_ls_shift/su_mean 0.04 _[local]_cod_data_source_file ic1014048_si_001_1.cif _[local]_cod_data_source_block Compound_2 _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 (29 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 (25 times). Automatic conversion script Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana ; _cod_original_cell_volume 619.615(21) _cod_database_code 4316843 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +x,+y,+z 2 -x,+y+1/2,-z+1/2 -1 -x,-y,-z -2 +x,-y+1/2,+z+1/2 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 1.0 0.0 0.0 1.0 Uiso 0.0120(4) 2 P P1 0.8388(4) 0.1515(4) 0.2821(4) 1.0 Uiso 0.0290(12) 4 O O1 0.9290(8) 0.2697(8) 0.4082(8) 1.0 Uiso 0.0291(11) 4 F F1 0.7737(6) -0.0792(6) -0.0710(7) 1.0 Uiso 0.0291(11) 4 O O2 0.7040(7) 0.2444(8) 0.1637(11) 1.0 Uiso 0.0291(11) 4 N N1 0.6470(9) 0.0207(12) 0.4606(9) 1.0 Uiso 0.0291(11) 4 O O3 0.9616(7) 0.0724(8) 0.2102(7) 1.0 Uiso 0.0291(11) 4 C C1 0.7577(11) -0.0265(13) 0.3754(10) 1.0 Uiso 0.0291(11) 4 C C2 0.4884(13) 0.0734(13) 0.3440(12) 1.0 Uiso 0.0291(11) 4 C C3 0.6205(13) -0.1219(14) 0.5620(15) 1.0 Uiso 0.0291(11) 4 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 2.0 -0.314 2.245 17.8765 1.27618 10.9480 11.9160 5.41732 0.11762 3.65721 87.6627 2.06929 International_Tables_Vol_C P 4.0 0.283 0.434 6.43450 1.90670 4.17910 27.1570 1.78000 0.52600 1.49080 68.1645 1.11490 International_Tables_Vol_C O 12.0 0.047 0.032 3.04850 13.2771 2.28680 5.70110 1.54630 0.32390 0.86700 32.9089 0.25080 International_Tables_Vol_C N 4.0 0.029 0.018 12.2126 0.00570 3.13220 9.89330 2.01250 28.9975 1.16630 0.58260 -11.529 International_Tables_Vol_C C 12.0 0.017 0.009 2.31000 20.8439 1.02000 10.2075 1.58860 0.56870 0.86500 51.6512 0.21560 International_Tables_Vol_C F 4.0 0.069 0.053 3.53920 10.2825 2.64120 4.29440 1.51700 0.26150 1.02430 26.1476 0.27760 International_Tables_Vol_C loop_ _diffrn_radiation_wavelength _diffrn_radiation_wavelength_wt _diffrn_radiation_type _diffrn_radiation_wavelength_id 1.540500 1.000 K\a~1~ 1 1.544300 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 O1 Zr1 O1 179.972 2_745 . -2_565 n O1 Zr1 F1 90.01(21) 2_745 . 1_555 n O1 Zr1 F1 89.99(21) 2_745 . -1_755 n O1 Zr1 O3 89.83(23) 2_745 . 1_555 n O1 Zr1 O3 90.17(23) 2_745 . -1_755 n O1 Zr1 F1 89.99(21) -2_565 . 1_555 n O1 Zr1 F1 90.01(21) -2_565 . -1_755 n O1 Zr1 O3 90.17(23) -2_565 . 1_555 n O1 Zr1 O3 89.83(23) -2_565 . -1_755 n F1 Zr1 F1 179.9406 1_555 . -1_755 n F1 Zr1 O3 90.19(23) 1_555 . 1_555 n F1 Zr1 O3 89.81(23) 1_555 . -1_755 n F1 Zr1 O3 89.81(23) -1_755 . 1_555 n F1 Zr1 O3 90.19(23) -1_755 . -1_755 n O3 Zr1 O3 180.0 1_555 . -1_755 n O1 P1 O2 110.3(5) 1_555 . 1_555 n O1 P1 O3 107.4(4) 1_555 . 1_555 n O1 P1 C1 109.3(4) 1_555 . 1_555 n O2 P1 O3 113.6(5) 1_555 . 1_555 n O2 P1 C1 111.9(4) 1_555 . 1_555 n O3 P1 C1 104.2(4) 1_555 . 1_555 n Zr1 O1 P1 154.2(5) 2_755 . 1_555 n C1 N1 C2 108.3(8) 1_555 . 1_555 n C1 N1 C3 110.0(9) 1_555 . 1_555 n C2 N1 C3 111.4(9) 1_555 . 1_555 n Zr1 O3 P1 142.8(4) 1_555 . 1_555 n P1 C1 N1 114.2(8) 1_555 . 1_555 n N1 C2 C3 106.0(8) 1_555 . -1_656 n N1 C3 C2 110.8(9) 1_555 . -1_656 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 O1 2.084(7) . 2_745 n Zr1 O1 2.084(7) . -2_554 n Zr1 F1 2.014(5) . 1_555 n Zr1 F1 2.014(5) . -1_755 n Zr1 O3 2.093(7) . 1_555 n Zr1 O3 2.093(7) . -1_755 n P1 O1 1.542(7) . 1_555 n P1 O2 1.562(8) . 1_555 n P1 O3 1.532(7) . 1_555 n P1 C1 1.906(10) . 1_555 n O1 Zr1 2.084(7) . 2_755 n O1 P1 1.542(7) . 1_555 n F1 Zr1 2.014(5) . 1_555 n O2 P1 1.562(8) . 1_555 n N1 C1 1.434(10) . 1_555 n N1 C2 1.562(10) . 1_555 n N1 C3 1.535(13) . 1_555 n O3 Zr1 2.093(7) . 1_555 n O3 P1 1.532(7) . 1_555 n C1 P1 1.906(10) . 1_555 n C1 N1 1.434(10) . 1_555 n C2 N1 1.562(10) . 1_555 n C2 C3 1.482(12) . -1_656 n C3 N1 1.535(13) . 1_555 n C3 C2 1.482(12) . -1_656 n