#------------------------------------------------------------------------------ #$Date: 2016-03-23 20:41:30 +0200 (Wed, 23 Mar 2016) $ #$Revision: 179419 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/33/16/4331655.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_4331655 loop_ _publ_author_name 'Christopher C. Underwood' 'Colin D. McMillen' 'Hongyu Chen' 'Jeffery N. Anker' 'Joseph W. Kolis' _publ_contact_author_address ; Department of Chemistry Clemson University Clemson, SC, 29634 USA ; _publ_contact_author_email kjoseph@clemson.edu _publ_contact_author_fax 864-656-6613 _publ_contact_author_name 'Joseph W. Kolis' _publ_contact_author_phone 864-656-4739 _publ_section_title ; Hydrothermal Chemistry, Structures, and Luminescence Studies of Alkali Hafnium Fluorides ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 237 _journal_page_last 244 _journal_paper_doi 10.1021/ic301760a _journal_volume 52 _journal_year 2013 _chemical_formula_moiety 'F6 Hf, 2(Li)' _chemical_formula_sum 'F6 Hf Li2' _chemical_formula_weight 306.37 _chemical_name_systematic ; ? ; _space_group_IT_number 162 _symmetry_cell_setting trigonal _symmetry_space_group_name_Hall '-P 3 2' _symmetry_space_group_name_H-M 'P -3 1 m' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_formula_units_Z 1 _cell_length_a 4.9748(7) _cell_length_b 4.9748(7) _cell_length_c 4.6449(9) _cell_measurement_reflns_used 89 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 26.30 _cell_measurement_theta_min 4.39 _cell_volume 99.55(3) _computing_cell_refinement 'CrystalClear (Rigaku/MSC, 2006)' _computing_data_collection 'CrystalClear (Rigaku/MSC, 2006)' _computing_data_reduction 'CrystalClear (Rigaku/MSC, 2006)' _computing_molecular_graphics 'DIAMOND (Bradenburg, 1999)' _computing_publication_material 'SHELXTL 6.10 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXTL 6.10 (Sheldrick, 2008)' _computing_structure_solution 'SHELXTL 6.10 (Sheldrick, 2008)' _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean 14.6306 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Rigaku AFC8S' _diffrn_measurement_method dtprofit.ref _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 0.1080 _diffrn_reflns_av_sigmaI/netI 0.0383 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_l_max 5 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_number 935 _diffrn_reflns_theta_full 26.30 _diffrn_reflns_theta_max 26.30 _diffrn_reflns_theta_min 4.39 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 26.231 _exptl_absorpt_correction_T_max 0 _exptl_absorpt_correction_T_min 0 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'REQAB, CrystalClear' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 5.110 _exptl_crystal_description plate _exptl_crystal_F_000 132 _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _refine_diff_density_max 3.008 _refine_diff_density_min -2.662 _refine_diff_density_rms 0.492 _refine_ls_extinction_coef 0.23(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.215 _refine_ls_matrix_type full _refine_ls_number_parameters 12 _refine_ls_number_reflns 89 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.215 _refine_ls_R_factor_all 0.0319 _refine_ls_R_factor_gt 0.0319 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0484P)^2^+1.3570P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0770 _refine_ls_wR_factor_ref 0.0770 _reflns_number_gt 89 _reflns_number_total 89 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ic301760a_si_004_1.cif _cod_data_source_block cu67-1 _cod_database_code 4331655 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-y, -x, -z' '-x+y, y, -z' 'x, x-y, -z' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'y, x, z' 'x-y, -y, z' '-x, -x+y, z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags Hf1 Hf 0.0000 0.0000 0.0000 0.0027(11) Uani 1 12 d S Li1 Li 0.3333 0.6667 0.5000 0.009(8) Uani 1 6 d S F1 F 1.0000 0.3278(19) 0.2554(17) 0.0050(15) Uani 1 2 d S 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 Hf1 0.0035(11) 0.0035(11) 0.0011(12) 0.000 0.000 0.0017(6) Li1 0.010(13) 0.010(13) 0.007(19) 0.000 0.000 0.005(6) F1 0.007(4) 0.005(3) 0.004(4) -0.001(3) 0.000 0.003(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Li Li -0.0003 0.0001 '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' Hf Hf -0.5830 6.1852 '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 F1 Hf1 F1 180.0(4) 7_655 1_455 F1 Hf1 F1 88.9(3) 7_655 9_445 F1 Hf1 F1 91.1(3) 1_455 9_445 F1 Hf1 F1 91.1(3) 7_655 3_665 F1 Hf1 F1 88.9(3) 1_455 3_665 F1 Hf1 F1 180.0(4) 9_445 3_665 F1 Hf1 F1 91.1(3) 7_655 2_545 F1 Hf1 F1 88.9(3) 1_455 2_545 F1 Hf1 F1 91.1(3) 9_445 2_545 F1 Hf1 F1 88.9(3) 3_665 2_545 F1 Hf1 F1 88.9(3) 7_655 8_565 F1 Hf1 F1 91.1(3) 1_455 8_565 F1 Hf1 F1 88.9(3) 9_445 8_565 F1 Hf1 F1 91.1(3) 3_665 8_565 F1 Hf1 F1 180.0 2_545 8_565 F1 Li1 F1 178.7(5) 9_556 1_455 F1 Li1 F1 89.5(3) 9_556 3_675 F1 Li1 F1 91.5(3) 1_455 3_675 F1 Li1 F1 91.5(3) 9_556 7_666 F1 Li1 F1 89.5(3) 1_455 7_666 F1 Li1 F1 87.5(5) 3_675 7_666 F1 Li1 F1 87.5(5) 9_556 2_655 F1 Li1 F1 91.5(3) 1_455 2_655 F1 Li1 F1 91.5(3) 3_675 2_655 F1 Li1 F1 178.7(5) 7_666 2_655 F1 Li1 F1 91.5(3) 9_556 8_566 F1 Li1 F1 87.5(5) 1_455 8_566 F1 Li1 F1 178.7(5) 3_675 8_566 F1 Li1 F1 91.5(3) 7_666 8_566 F1 Li1 F1 89.5(3) 2_655 8_566 F1 Li1 Li1 136.2(3) 9_556 7_566 F1 Li1 Li1 44.73(17) 1_455 7_566 F1 Li1 Li1 89.3(2) 3_675 7_566 F1 Li1 Li1 44.73(17) 7_666 7_566 F1 Li1 Li1 136.2(3) 2_655 7_566 F1 Li1 Li1 89.3(2) 8_566 7_566 F1 Li1 Li1 44.73(17) 9_556 7_676 F1 Li1 Li1 136.2(3) 1_455 7_676 F1 Li1 Li1 44.73(17) 3_675 7_676 F1 Li1 Li1 89.3(2) 7_666 7_676 F1 Li1 Li1 89.3(2) 2_655 7_676 F1 Li1 Li1 136.2(3) 8_566 7_676 Li1 Li1 Li1 120.0 7_566 7_676 F1 Li1 Li1 89.3(2) 9_556 7_666 F1 Li1 Li1 89.3(2) 1_455 7_666 F1 Li1 Li1 136.2(3) 3_675 7_666 F1 Li1 Li1 136.2(3) 7_666 7_666 F1 Li1 Li1 44.73(17) 2_655 7_666 F1 Li1 Li1 44.73(17) 8_566 7_666 Li1 Li1 Li1 120.0 7_566 7_666 Li1 Li1 Li1 120.0 7_676 7_666 Hf1 F1 Li1 132.3(2) 1_655 1_655 Hf1 F1 Li1 132.3(2) 1_655 7_666 Li1 F1 Li1 90.5(3) 1_655 7_666 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Hf1 F1 2.017(9) 7_655 Hf1 F1 2.017(9) 1_455 Hf1 F1 2.017(9) 9_445 Hf1 F1 2.017(9) 3_665 Hf1 F1 2.017(9) 2_545 Hf1 F1 2.017(9) 8_565 Li1 F1 2.022(6) 9_556 Li1 F1 2.022(6) 1_455 Li1 F1 2.022(6) 3_675 Li1 F1 2.022(6) 7_666 Li1 F1 2.022(6) 2_655 Li1 F1 2.022(6) 8_566 F1 Hf1 2.017(9) 1_655 F1 Li1 2.022(6) 1_655 F1 Li1 2.022(6) 7_666