#------------------------------------------------------------------------------
#$Date: 2014-07-05 05:18:45 +0300 (Sat, 05 Jul 2014) $
#$Revision: 119000 $
#$URL: file:///home/coder/svn-repositories/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 ReO~3~-related phases. III. \g-ZrF~4~,
a high-pressure form of zirconium tetrafluoride, and a comparison of
MX~4~ 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+0.001xFc^2^\l^3^/sin(2\q)]^-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/[\s^2^(Fo^2^)+(0.0110P)^2^+3.0227P] where P=(Fo^2^+2Fc^2^)/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)
_iucr_refine_instructions_details
;
TITL Compound ZrF4 gamma P 21/
CELL 0.7107 5.554 5.639 7.973 90.00 105.98 90.00
ZERR 1. 0.002 0.002 0.003 0. 0.05 0.
LATT 1
SYMM -X , Y+.50, -Z+.50
SFAC ZR F
UNIT 4 16
LIST 4
ACTA
L.S. 14
BOND
FMAP -2
PLAN 20
REM WGHT 0.100000
REM WGHT 0.026000 4.892100
REM WGHT 0.021500 4.419200
REM WGHT 0.024000 4.330101
REM WGHT 0.021600 4.003800
REM WGHT 0.011500 3.024500
WGHT 0.011000 3.022700
EXTI 0.007635
FVAR 0.75642
ZR1 1 0.787605 0.166273 0.829541 11.00000 0.00892 0.00843 =
0.00833 0.00002 0.00380 0.00007
F1 2 1.141717 0.157789 1.020499 11.00000 0.01507 0.01201 =
0.01417 0.00107 0.00235 0.00024
F2 2 1.005438 -0.042019 0.709011 11.00000 0.01710 0.01398 =
0.01373 0.00098 0.00491 0.00497
F3 2 0.482703 -0.043815 0.734701 11.00000 0.01573 0.01340 =
0.01605 0.00130 0.00539 -0.00484
F4 2 0.686471 0.261350 1.047561 11.00000 0.01504 0.01862 =
0.01036 -0.00056 0.00435 0.00187
HKLF 4
REM Compound ZrF4 gamma P 21/
REM R1 = 0.0261 for 513 Fo > 4sig(Fo) and 0.0270 for all 541 data
REM 47 parameters refined using 0 restraints
END
WGHT 0.0111 3.0199
REM Highest difference peak 1.336, deepest hole -0.723, 1-sigma level 0.193
Q1 1 0.5433 0.1470 0.8234 11.00000 0.05 1.34
Q2 1 0.9999 0.1540 0.8314 11.00000 0.05 1.30
Q3 1 0.8577 0.0283 0.6806 11.00000 0.05 1.03
Q4 1 1.1875 0.1869 0.8240 11.00000 0.05 1.01
Q5 1 0.3717 0.1877 0.8380 11.00000 0.05 0.91
Q6 1 0.6121 0.0267 0.6960 11.00000 0.05 0.90
Q7 1 0.7055 0.1442 0.8959 11.00000 0.05 -0.72
Q8 1 0.7152 0.4984 1.1451 11.00000 0.05 -0.62
Q9 1 0.3571 0.0259 0.6775 11.00000 0.05 0.62
Q10 1 1.1990 0.4208 0.9730 11.00000 0.05 -0.58
Q11 1 1.1167 0.0272 0.6943 11.00000 0.05 0.56
Q12 1 0.5090 0.2021 0.8986 11.00000 0.05 -0.54
Q13 1 0.4686 0.0423 0.6578 11.00000 0.05 -0.54
Q14 1 0.5061 -0.2595 0.7315 11.00000 0.05 -0.52
Q15 1 0.8918 0.1460 0.7449 11.00000 0.05 -0.51
Q16 1 0.3943 0.0745 0.7958 11.00000 0.05 -0.50
Q17 1 1.0294 -0.1214 0.7869 11.00000 0.05 0.49
Q18 1 0.8484 0.3604 1.1254 11.00000 0.05 -0.49
Q19 1 0.9095 0.2461 0.9582 11.00000 0.05 0.48
Q20 1 0.7463 0.2804 0.7651 11.00000 0.05 -0.47
;
_[local]_cod_data_source_file ov3051sup1.cf
_[local]_cod_data_source_block I
_[local]_cod_cif_authors_sg_H-M 'P 21/c'
_cod_original_cell_volume 240.06(15)
_cod_database_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_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Zr1 0.0089(3) 0.0084(3) 0.0083(3) 0.00007(19) 0.00380(19) 0.00002(18)
F1 0.0151(16) 0.0120(16) 0.0142(15) 0.0002(13) 0.0024(13) 0.0011(13)
F2 0.0171(16) 0.0140(18) 0.0137(16) 0.0050(13) 0.0049(13) 0.0010(13)
F3 0.0157(16) 0.0134(18) 0.0161(16) -0.0048(13) 0.0054(13) 0.0013(13)
F4 0.0150(16) 0.0186(17) 0.0104(15) 0.0019(14) 0.0043(13) -0.0006(13)
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
_cod_database_fobs_code 2019609