#------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/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_paper_doi               10.1021/jp306665a
_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 φ- and ω-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/[σ²(Fo²)+(0.0052P)²+0.0100P] where P=(Fo²+2Fc²)/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     >2σ(I)
_cod_data_source_file            jp306665a_si_001.cif
_cod_data_source_block           zrbh4_0m
_cod_original_formula_sum        'B4 H16 Zr1'
_cod_database_code               1508533
#BEGIN Tags that were not found in dictionaries:
_refine_friedel_coverage         0.660
#END Tags that were not found in dictionaries
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) .
