#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/96/2019609.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2019609
loop_
_publ_author_name
'Laval, Jean-Paul'
_publ_section_title
;
 Crystal chemistry of anion-excess ReO₃-related phases. III. γ-ZrF₄,
 a high-pressure form of zirconium tetrafluoride, and a comparison of
 MX₄ structure types
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229614014338
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          'Zr F4'
_chemical_formula_moiety         'F4 Zr'
_chemical_formula_sum            'F4 Zr'
_chemical_formula_weight         167.22
_chemical_name_systematic
;
Zirconium tetrafluoride
;
_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_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 105.98(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   5.554(2)
_cell_length_b                   5.639(2)
_cell_length_c                   7.973(3)
_cell_measurement_temperature    293(2)
_cell_volume                     240.06(16)
_computing_cell_refinement       'DIRAX/LSQ (Duisenberg & Schreurs, 2000)'
_computing_data_collection       'COLLECT (Nonius, 2004)'
_computing_data_reduction        'EvalCCD (Duisenberg et al., 2003)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material
'SHELXL97 (Sheldrick, 2008) and publCIF (Westrip, 2010)'
_computing_structure_refinement
'SHELXL97 (Sheldrick, 2008) and WinGX (Farrugia, 2012)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0466
_diffrn_reflns_av_sigmaI/netI    0.0203
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            5384
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         5.26
_exptl_absorpt_coefficient_mu    4.459
_exptl_absorpt_correction_T_max  0.976
_exptl_absorpt_correction_T_min  0.920
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2004)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    4.627
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             304
_exptl_crystal_size_max          0.014
_exptl_crystal_size_mid          0.011
_exptl_crystal_size_min          0.010
_refine_diff_density_max         1.336
_refine_diff_density_min         -0.723
_refine_ls_extinction_coef       0.008(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.289
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     47
_refine_ls_number_reflns         541
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.289
_refine_ls_R_factor_all          0.0270
_refine_ls_R_factor_gt           0.0261
_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/[σ²(Fo²)+(0.0110P)²+3.0227P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0705
_refine_ls_wR_factor_ref         0.0708
_reflns_number_gt                513
_reflns_number_total             541
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ov3051sup1.cf
_cod_data_source_block           I
_cod_original_cell_volume        240.06(15)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2019609
_cod_database_fobs_code          2019609
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_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_symmetry_multiplicity
Zr Zr1 0.78760(9) 0.16627(9) 0.82954(6) 0.0083(2) Uani d 1 1
F F1 1.1417(6) 0.1578(6) 1.0205(4) 0.0141(7) Uani d 1 1
F F2 1.0054(6) -0.0420(6) 0.7090(4) 0.0148(7) Uani d 1 1
F F3 0.4827(6) -0.0438(6) 0.7347(4) 0.0149(7) Uani d 1 1
F F4 0.6865(6) 0.2614(7) 1.0476(4) 0.0145(7) Uani d 1 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Zr Zr -2.9673 0.5597 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
F3 Zr1 F4 . . 94.21(14)
F3 Zr1 F2 . 2_756 147.57(13)
F4 Zr1 F2 . 2_756 102.20(14)
F3 Zr1 F2 . . 91.70(14)
F4 Zr1 F2 . . 149.95(14)
F2 Zr1 F2 2_756 . 87.89(5)
F3 Zr1 F1 . . 139.71(13)
F4 Zr1 F1 . . 79.25(14)
F2 Zr1 F1 2_756 . 71.58(13)
F2 Zr1 F1 . . 77.27(13)
F3 Zr1 F1 . 3_757 73.67(14)
F4 Zr1 F1 . 3_757 78.54(14)
F2 Zr1 F1 2_756 3_757 136.74(13)
F2 Zr1 F1 . 3_757 74.94(13)
F1 Zr1 F1 . 3_757 66.05(15)
F3 Zr1 F3 . 2_656 84.29(4)
F4 Zr1 F3 . 2_656 70.75(14)
F2 Zr1 F3 2_756 2_656 75.23(14)
F2 Zr1 F3 . 2_656 139.23(13)
F1 Zr1 F3 . 2_656 128.64(13)
F1 Zr1 F3 3_757 2_656 140.53(13)
F3 Zr1 F4 . 4_565 77.06(14)
F4 Zr1 F4 . 4_565 140.28(13)
F2 Zr1 F4 2_756 4_565 72.42(13)
F2 Zr1 F4 . 4_565 69.71(13)
F1 Zr1 F4 . 4_565 131.31(13)
F1 Zr1 F4 3_757 4_565 132.76(14)
F3 Zr1 F4 2_656 4_565 69.86(13)
F3 Zr1 Zr1 . 3_757 106.44(11)
F4 Zr1 Zr1 . 3_757 76.72(10)
F2 Zr1 Zr1 2_756 3_757 104.48(10)
F2 Zr1 Zr1 . 3_757 73.35(9)
F1 Zr1 Zr1 . 3_757 33.28(9)
F1 Zr1 Zr1 3_757 3_757 32.77(9)
F3 Zr1 Zr1 2_656 3_757 146.44(9)
F4 Zr1 Zr1 4_565 3_757 143.00(10)
Zr1 F1 Zr1 . 3_757 113.95(15)
Zr1 F2 Zr1 2_746 . 157.34(18)
Zr1 F3 Zr1 . 2_646 166.34(19)
Zr1 F4 Zr1 . 4_566 150.07(18)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Zr1 F3 . 2.034(3) y
Zr1 F4 . 2.040(3) y
Zr1 F2 2_756 2.078(3) y
Zr1 F2 . 2.099(3) y
Zr1 F1 . 2.131(4) y
Zr1 F1 3_757 2.160(3) y
Zr1 F3 2_656 2.183(3) y
Zr1 F4 4_565 2.200(3) y
Zr1 Zr1 3_757 3.597(2) y
F1 Zr1 3_757 2.160(3) no
F2 Zr1 2_746 2.078(3) no
F3 Zr1 2_646 2.183(3) no
F4 Zr1 4_566 2.200(3) no
