#------------------------------------------------------------------------------ #$Date: 2016-03-23 23:02:51 +0200 (Wed, 23 Mar 2016) $ #$Revision: 179500 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/33/97/4339750.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_4339750 loop_ _publ_author_name 'Supe\/l, Joanna' 'Abram, Ulrich' 'Hagenbach, Adelheid' 'Seppelt, Konrad' _publ_section_title ; Technetium fluoride trioxide, TcO3F, preparation and properties. ; _journal_issue 14 _journal_name_full 'Inorganic chemistry' _journal_page_first 5591 _journal_page_last 5595 _journal_paper_doi 10.1021/ic070333y _journal_volume 46 _journal_year 2007 _chemical_formula_moiety CrO2F2 _chemical_formula_sum 'Cr F2 O2' _chemical_formula_weight 122.00 _chemical_name_common Chrom-difluoride-dioxide _chemical_name_systematic ; Chrom-difluoride-dioxide ; _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' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 92.95(5) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 5.655(3) _cell_length_b 4.8531(17) _cell_length_c 9.116(3) _cell_measurement_temperature 153(2) _cell_volume 249.85(18) _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 20 _diffrn_measured_fraction_theta_full 0.984 _diffrn_measured_fraction_theta_max 0.984 _diffrn_measurement_device_type `Bruker-SMART-CCD-Diffractometer` _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0196 _diffrn_reflns_av_sigmaI/netI 0.0183 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 7932 _diffrn_reflns_theta_full 40.92 _diffrn_reflns_theta_max 40.92 _diffrn_reflns_theta_min 3.61 _exptl_absorpt_coefficient_mu 4.399 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.5900 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour brown _exptl_crystal_density_diffrn 3.243 _exptl_crystal_density_method 'not measured' _exptl_crystal_description orthorhombic _exptl_crystal_F_000 232 _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.1 _refine_diff_density_max 1.064 _refine_diff_density_min -0.697 _refine_diff_density_rms 0.145 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.105 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 46 _refine_ls_number_reflns 1612 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.105 _refine_ls_R_factor_all 0.0282 _refine_ls_R_factor_gt 0.0230 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0352P)^2^+0.0677P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0586 _refine_ls_wR_factor_ref 0.0604 _reflns_number_gt 1427 _reflns_number_total 1612 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ic070333ysi20070221_053952.cif _cod_data_source_block cro2f2 _cod_original_cell_volume 249.85(17) _cod_original_sg_symbol_H-M P2(1)/c _cod_database_code 4339750 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag Cr Cr 0.67698(3) 0.05549(3) 0.373091(16) 0.00619(5) Uani 1 1 d F1 F 0.54945(11) 0.20281(13) 0.20373(7) 0.00870(10) Uani 1 1 d F2 F 0.65620(11) -0.14157(13) 0.54781(7) 0.00783(10) Uani 1 1 d O1 O 0.88934(14) -0.11291(17) 0.31251(9) 0.01045(12) Uani 1 1 d O2 O 0.79789(15) 0.32238(16) 0.44034(9) 0.01104(13) Uani 1 1 d loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cr 0.00742(7) 0.00658(7) 0.00458(7) 0.00049(4) 0.00049(4) 0.00015(4) F1 0.0117(2) 0.0088(2) 0.0056(2) 0.00186(18) -0.00012(18) 0.00129(19) F2 0.0097(2) 0.0086(2) 0.0051(2) 0.00102(18) 0.00013(18) 0.00133(18) O1 0.0106(3) 0.0117(3) 0.0091(3) 0.0002(2) 0.0021(2) 0.0019(2) O2 0.0141(3) 0.0094(3) 0.0095(3) -0.0006(2) -0.0006(2) -0.0019(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 O2 Cr O1 103.87(5) . . O2 Cr F1 98.78(5) . . O1 Cr F1 100.52(5) . . O2 Cr F2 97.72(5) . . O1 Cr F2 96.66(5) . . F1 Cr F2 152.51(3) . . O2 Cr F2 94.72(4) . 3_656 O1 Cr F2 159.99(4) . 3_656 F1 Cr F2 83.64(5) . 3_656 F2 Cr F2 73.21(5) . 3_656 O2 Cr F1 170.16(3) . 2_645 O1 Cr F1 85.84(5) . 2_645 F1 Cr F1 80.72(4) . 2_645 F2 Cr F1 79.30(4) . 2_645 F2 Cr F1 75.45(3) 3_656 2_645 Cr F1 Cr 139.98(4) . 2_655 Cr F2 Cr 106.79(5) . 3_656 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Cr O2 1.5742(9) . Cr O1 1.5758(10) . Cr F1 1.8167(9) . Cr F2 1.8667(8) . Cr F2 2.0938(12) 3_656 Cr F1 2.2287(9) 2_645 F1 Cr 2.2287(9) 2_655 F2 Cr 2.0938(12) 3_656