#------------------------------------------------------------------------------
#$Date: 2015-12-09 13:43:51 +0100 (Wed 09 de Dec de 2015) $
#$Revision: 171047 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/18/7221866.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_7221866
loop_
_publ_author_name
'Yeon, Jeongho'
'Felder, Justin B.'
'Smith, Mark D.'
'Morrison, Gregory'
'zur Loye, Hans-Conrad'
_publ_section_title
;
 Synthetic strategies for new vanadium oxyfluorides containing novel
 building blocks: structures of V(iv) and V(v) containing Sr4V3O5F13,
 Pb7V4O8F18, Pb2VO2F5, and Pb2VOF6
;
_journal_issue                   44
_journal_name_full               CrystEngComm
_journal_page_first              8428
_journal_paper_doi               10.1039/C5CE01464F
_journal_volume                  17
_journal_year                    2015
_chemical_formula_moiety         'F6 O Pb2 V'
_chemical_formula_sum            'F6 O Pb2 V'
_chemical_formula_weight         595.32
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 92.019(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   5.6675(4)
_cell_length_b                   15.7931(12)
_cell_length_c                   12.9995(9)
_cell_measurement_reflns_used    7192
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.578
_cell_measurement_theta_min      2.580
_cell_volume                     1162.83(15)
_computing_cell_refinement       'SAINT-Plus Version 6.45 (Bruker, 2001)'
_computing_data_collection       'SMART Version 5.631 (Bruker, 2001)'
_computing_data_reduction        'SAINT-Plus Version 6.45 (Bruker, 2001)'
_computing_molecular_graphics    various
_computing_publication_material  various
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker SMART APEX CCD diffractometer'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0423
_diffrn_reflns_av_unetI/netI     0.0326
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11443
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.578
_diffrn_reflns_theta_min         2.579
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    59.401
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.1914
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS Version 2.05 (Bruker, 2001)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    6.801
_exptl_crystal_description       tablet
_exptl_crystal_F_000             1992
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.040
_refine_diff_density_max         3.405
_refine_diff_density_min         -1.646
_refine_diff_density_rms         0.406
_refine_ls_extinction_coef       0.00108(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     93
_refine_ls_number_reflns         2120
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0293
_refine_ls_R_factor_gt           0.0260
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0242P)²+9.5236P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0564
_refine_ls_wR_factor_ref         0.0577
_reflns_number_gt                1963
_reflns_number_total             2120
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5ce01464f1.cif
_cod_data_source_block           Pb2VOF6
_cod_depositor_comments
'Adding full bibliography for 7221863--7221866.cif.'
_cod_database_code               7221866
_shelx_space_group_comment
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;
_shelx_estimated_absorpt_t_min   0.066
_shelx_estimated_absorpt_t_max   0.200
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Pb1 Pb 0.21077(4) 0.01143(2) 0.62502(2) 0.00942(7) Uani 1 1 d . . .
Pb2 Pb 0.27257(4) 0.17245(2) 0.35773(2) 0.00933(7) Uani 1 1 d . . .
V1 V 0.20791(18) 0.32501(6) 0.08999(8) 0.00929(19) Uani 1 1 d . . .
F1 F 0.2520(7) 0.2288(2) 0.1785(3) 0.0152(7) Uani 1 1 d . . .
F2 F -0.1078(7) 0.3339(2) 0.1311(3) 0.0142(7) Uani 1 1 d . . .
F3 F 0.1095(6) 0.3952(2) -0.0271(3) 0.0127(7) Uani 1 1 d . . .
F4 F 0.4590(6) 0.2755(2) 0.0098(3) 0.0119(7) Uani 1 1 d . . .
F5 F 0.1209(6) 0.0568(2) 0.4514(3) 0.0124(7) Uani 1 1 d . . .
F6 F 0.0000 0.0820(3) 0.2500 0.0122(9) Uani 1 2 d S T P
F7 F 0.5000 0.0789(3) 0.2500 0.0127(10) Uani 1 2 d S T P
O1 O 0.3447(8) 0.3972(3) 0.1574(3) 0.0122(8) Uani 1 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 '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'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 '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
F5 Pb1 F5 66.50(14) 5_556 .
F5 Pb1 F3 77.33(12) 5_556 4_545
F5 Pb1 F3 79.38(12) . 4_545
F5 Pb1 F6 67.39(9) 5_556 5_556
F5 Pb1 F6 133.49(8) . 5_556
F3 Pb1 F6 96.30(12) 4_545 5_556
F5 Pb1 O1 71.91(13) 5_556 8_456
F5 Pb1 O1 80.87(13) . 8_456
F3 Pb1 O1 148.12(13) 4_545 8_456
F6 Pb1 O1 79.66(12) 5_556 8_456
F5 Pb1 F2 137.48(12) 5_556 8_556
F5 Pb1 F2 79.79(12) . 8_556
F3 Pb1 F2 122.22(12) 4_545 8_556
F6 Pb1 F2 135.32(12) 5_556 8_556
O1 Pb1 F2 78.02(13) 8_456 8_556
F5 Pb1 F7 118.31(12) 5_556 5_656
F5 Pb1 F7 146.36(9) . 5_656
F3 Pb1 F7 70.26(11) 4_545 5_656
F6 Pb1 F7 65.91(5) 5_556 5_656
O1 Pb1 F7 132.78(10) 8_456 5_656
F2 Pb1 F7 104.15(12) 8_556 5_656
F5 Pb1 Pb1 33.64(8) 5_556 5_556
F5 Pb1 Pb1 32.85(8) . 5_556
F3 Pb1 Pb1 76.05(9) 4_545 5_556
F6 Pb1 Pb1 100.85(2) 5_556 5_556
O1 Pb1 Pb1 73.76(10) 8_456 5_556
F2 Pb1 Pb1 109.20(9) 8_556 5_556
F7 Pb1 Pb1 141.58(9) 5_656 5_556
F5 Pb1 Pb2 32.28(8) 5_556 5_556
F5 Pb1 Pb2 98.39(8) . 5_556
F3 Pb1 Pb2 77.61(8) 4_545 5_556
F6 Pb1 Pb2 36.90(5) 5_556 5_556
O1 Pb1 Pb2 80.83(10) 8_456 5_556
F2 Pb1 Pb2 158.79(8) 8_556 5_556
F7 Pb1 Pb2 89.13(8) 5_656 5_556
Pb1 Pb1 Pb2 65.667(7) 5_556 5_556
F5 Pb2 F7 92.10(13) . .
F5 Pb2 F1 138.44(12) . .
F7 Pb2 F1 71.77(11) . .
F5 Pb2 F6 67.63(11) . .
F7 Pb2 F6 70.13(6) . .
F1 Pb2 F6 70.86(11) . .
F5 Pb2 F3 70.25(11) . 8_556
F7 Pb2 F3 71.97(8) . 8_556
F1 Pb2 F3 133.67(12) . 8_556
F6 Pb2 F3 120.85(12) . 8_556
F5 Pb2 F2 124.25(12) . 2
F7 Pb2 F2 142.05(12) . 2
F1 Pb2 F2 73.18(12) . 2
F6 Pb2 F2 111.04(12) . 2
F3 Pb2 F2 126.72(12) 8_556 2
F5 Pb2 F4 109.43(11) . 2_655
F7 Pb2 F4 114.95(8) . 2_655
F1 Pb2 F4 112.11(12) . 2_655
F6 Pb2 F4 174.55(7) . 2_655
F3 Pb2 F4 60.79(10) 8_556 2_655
F2 Pb2 F4 66.44(11) 2 2_655
F5 Pb2 F4 67.49(11) . 8_456
F7 Pb2 F4 159.57(12) . 8_456
F1 Pb2 F4 122.68(11) . 8_456
F6 Pb2 F4 99.59(8) . 8_456
F3 Pb2 F4 100.56(10) 8_556 8_456
F2 Pb2 F4 57.64(11) 2 8_456
F4 Pb2 F4 74.97(11) 2_655 8_456
F5 Pb2 F1 132.58(12) . 2_655
F7 Pb2 F1 65.02(10) . 2_655
F1 Pb2 F1 75.60(14) . 2_655
F6 Pb2 F1 130.25(7) . 2_655
F3 Pb2 F1 63.42(11) 8_556 2_655
F2 Pb2 F1 92.53(11) 2 2_655
F4 Pb2 F1 55.17(10) 2_655 2_655
F4 Pb2 F1 129.57(10) 8_456 2_655
F5 Pb2 Pb2 129.29(9) . 2_655
F7 Pb2 Pb2 37.33(9) . 2_655
F1 Pb2 Pb2 48.28(9) . 2_655
F6 Pb2 Pb2 90.503(8) . 2_655
F3 Pb2 Pb2 85.56(8) 8_556 2_655
F2 Pb2 Pb2 106.08(8) 2 2_655
F4 Pb2 Pb2 94.84(7) 2_655 2_655
F4 Pb2 Pb2 163.08(7) 8_456 2_655
F1 Pb2 Pb2 40.04(7) 2_655 2_655
O1 V1 F2 103.6(2) . .
O1 V1 F1 100.6(2) . .
F2 V1 F1 89.63(16) . .
O1 V1 F3 98.10(19) . .
F2 V1 F3 86.06(16) . .
F1 V1 F3 161.32(17) . .
O1 V1 F4 103.1(2) . .
F2 V1 F4 153.33(16) . .
F1 V1 F4 85.49(16) . .
F3 V1 F4 90.23(16) . .
O1 V1 F4 176.02(19) . 7
F2 V1 F4 80.29(15) . 7
F1 V1 F4 80.15(15) . 7
F3 V1 F4 81.21(14) . 7
F4 V1 F4 73.04(16) . 7
V1 F1 Pb2 147.62(19) . .
V1 F1 Pb2 104.38(15) . 2_655
Pb2 F1 Pb2 91.68(11) . 2_655
V1 F2 Pb1 115.45(16) . 8_455
V1 F2 Pb2 106.02(15) . 2
Pb1 F2 Pb2 137.02(16) 8_455 2
V1 F3 Pb1 135.42(18) . 4
V1 F3 Pb2 113.48(15) . 8_455
Pb1 F3 Pb2 108.34(13) 4 8_455
V1 F4 V1 106.96(16) . 7
V1 F4 Pb2 107.19(14) . 2_655
V1 F4 Pb2 98.89(13) 7 2_655
V1 F4 Pb2 138.04(17) . 8
V1 F4 Pb2 93.70(12) 7 8
Pb2 F4 Pb2 105.03(11) 2_655 8
Pb1 F5 Pb2 115.71(14) 5_556 .
Pb1 F5 Pb1 113.50(14) 5_556 .
Pb2 F5 Pb1 129.95(15) . .
Pb2 F6 Pb2 110.23(19) . 2
Pb2 F6 Pb1 113.432(8) . 6
Pb2 F6 Pb1 105.705(9) 2 6
Pb2 F6 Pb1 105.705(9) . 5_556
Pb2 F6 Pb1 113.431(9) 2 5_556
Pb1 F6 Pb1 108.49(18) 6 5_556
Pb2 F7 Pb2 105.34(19) 2_655 .
Pb2 F7 Pb1 107.415(11) 2_655 6
Pb2 F7 Pb1 110.298(11) . 6
Pb2 F7 Pb1 110.298(11) 2_655 5_656
Pb2 F7 Pb1 107.415(11) . 5_656
Pb1 F7 Pb1 115.61(18) 6 5_656
V1 O1 Pb1 132.8(2) . 8
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 F5 2.356(4) 5_556
Pb1 F5 2.406(3) .
Pb1 F3 2.474(3) 4_545
Pb1 F6 2.526(3) 5_556
Pb1 O1 2.574(4) 8_456
Pb1 F2 2.651(3) 8_556
Pb1 F7 2.679(3) 5_656
Pb1 Pb1 3.9820(5) 5_556
Pb1 Pb2 4.0039(4) 5_556
Pb2 F5 2.373(3) .
Pb2 F7 2.435(3) .
Pb2 F1 2.493(4) .
Pb2 F6 2.497(3) .
Pb2 F3 2.613(4) 8_556
Pb2 F2 2.720(3) 2
Pb2 F4 2.783(4) 2_655
Pb2 F4 2.826(3) 8_456
Pb2 F1 2.892(4) 2_655
Pb2 Pb2 3.8729(5) 2_655
V1 O1 1.619(4) .
V1 F2 1.890(4) .
V1 F1 1.917(4) .
V1 F3 1.949(4) .
V1 F4 1.957(4) .
V1 F4 2.238(4) 7
F1 Pb2 2.892(4) 2_655
F2 Pb1 2.651(3) 8_455
F2 Pb2 2.721(3) 2
F3 Pb1 2.474(3) 4
F3 Pb2 2.613(4) 8_455
F4 V1 2.238(4) 7
F4 Pb2 2.783(4) 2_655
F4 Pb2 2.826(3) 8
F5 Pb1 2.356(3) 5_556
F6 Pb2 2.497(3) 2
F6 Pb1 2.526(3) 6
F6 Pb1 2.526(3) 5_556
F7 Pb2 2.435(3) 2_655
F7 Pb1 2.679(3) 6
F7 Pb1 2.679(3) 5_656
O1 Pb1 2.574(4) 8
