#------------------------------------------------------------------------------ #$Date: 2013-12-28 09:07:06 +0200 (Sat, 28 Dec 2013) $ #$Revision: 91932 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/50/85/1508533.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_1508533 loop_ _publ_author_name 'Rude, Line H.' 'Corno, Marta' 'Ugliengo, Piero' 'Baricco, Marcello' 'Lee, Young-Su' 'Cho, Young Whan' 'Besenbacher, Flemming' 'Overgaard, Jacob' 'Jensen, Torben R.' _publ_section_title ; Synthesis and Structural Investigation of Zr(BH4)4 ; _journal_issue 38 _journal_name_full 'The Journal of Physical Chemistry C' _journal_page_first 20239 _journal_volume 116 _journal_year 2012 _chemical_absolute_configuration ad _chemical_compound_source 'synthesis as described' _chemical_formula_moiety 'B4 H16 Zr1' _chemical_formula_sum 'B4 H16 Zr' _chemical_formula_weight 150.59 _chemical_name_systematic ; ? ; _space_group_IT_number 215 _symmetry_cell_setting cubic _symmetry_Int_Tables_number 215 _symmetry_space_group_name_Hall 'P -4 2 3' _symmetry_space_group_name_H-M 'P -4 3 m' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_date 2011-07-22T14:54:12-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 1 _cell_length_a 5.8387(4) _cell_length_b 5.8387(4) _cell_length_c 5.8387(4) _cell_measurement_reflns_used 2871 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 42.88 _cell_measurement_theta_min 3.49 _cell_measurement_wavelength 0.71073 _cell_volume 199.04(2) _computing_cell_refinement 'Saint+ v7.68A (Bruker-Nonius, 2011)' _computing_data_collection 'Apex2 (Bruker-Nonius, 2011)' _computing_data_reduction 'Saint+ v7.68A (Bruker-Nonius, 2011)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_solution 'SHELXS (Sheldrick, 2008)' _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 12.00 _diffrn_detector_type 'APEX2 charged-coupled device' _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.974 _diffrn_measurement_device_type 'Bruker X8 APEX-II diffractometer' _diffrn_measurement_method ; Narrow slices collected using \f- and \w-scans ; _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0512 _diffrn_reflns_av_unetI/netI 0.0211 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_number 2851 _diffrn_reflns_theta_full 35.00 _diffrn_reflns_theta_max 42.88 _diffrn_reflns_theta_min 3.49 _diffrn_source 'fine-focus sealed tube' _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 1.259 _exptl_absorpt_correction_type none _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.256 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 76 _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.08 _refine_diff_density_max 0.443 _refine_diff_density_min -0.218 _refine_diff_density_rms 0.046 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881, 122 Friedel pairs' _refine_ls_abs_structure_Flack 0.05(14) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.176 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 10 _refine_ls_number_reflns 307 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.176 _refine_ls_R_factor_all 0.0154 _refine_ls_R_factor_gt 0.0154 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0052P)^2^+0.0100P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0296 _refine_ls_wR_factor_ref 0.0296 _reflns_number_gt 307 _reflns_number_total 307 _reflns_threshold_expression >2\s(I) _[local]_cod_data_source_file jp306665a_si_001.cif _[local]_cod_data_source_block zrbh4_0m _[local]_cod_chemical_formula_sum_orig 'B4 H16 Zr1' _cod_database_code 1508533 _refine_friedel_coverage 0.660 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'z, x, y' 'z, -x, -y' '-z, -x, y' '-z, x, -y' 'y, z, x' '-y, z, -x' 'y, -z, -x' '-y, -z, x' 'y, x, z' '-y, -x, z' 'y, -x, -z' '-y, x, -z' 'x, z, y' '-x, z, -y' '-x, -z, y' 'x, -z, -y' 'z, y, x' 'z, -y, -x' '-z, y, -x' '-z, -y, x' 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 Zr1 Zr 1 1 1 0.01664(6) Uani 1 24 d S B1 B 0.7714(2) 0.7714(2) 0.7714(2) 0.0284(4) Uani 1 6 d S H1 H 0.956(4) 0.748(2) 0.748(2) 0.046(6) Uiso 1 2 d S H2 H 0.668(3) 0.668(3) 0.668(3) 0.040(9) Uiso 1 6 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 Zr1 0.01664(6) 0.01664(6) 0.01664(6) 0 0 0 B1 0.0284(4) 0.0284(4) 0.0284(4) -0.0047(4) -0.0047(4) -0.0047(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -2.9673 0.5597 '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 B1 Zr1 B1 109.5 . 4_577 B1 Zr1 B1 109.5 . 2_775 B1 Zr1 B1 109.5 4_577 2_775 B1 Zr1 B1 109.5 . 3_757 B1 Zr1 B1 109.5 4_577 3_757 B1 Zr1 B1 109.4710(10) 2_775 3_757 B1 Zr1 H1 28.3(6) . . B1 Zr1 H1 137.7(6) 4_577 . B1 Zr1 H1 94.0(4) 2_775 . B1 Zr1 H1 94.0(4) 3_757 . Zr1 B1 H1 64.9(10) . . Zr1 B1 H2 180.0(9) . . H1 B1 H2 115.1(10) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Zr1 B1 2.312(2) . Zr1 B1 2.312(2) 4_577 Zr1 B1 2.312(2) 2_775 Zr1 B1 2.312(2) 3_757 Zr1 H1 2.096(18) . B1 H1 1.10(2) . B1 H2 1.05(4) . _journal_paper_doi 10.1021/jp306665a