#------------------------------------------------------------------------------
#$Date: 2016-03-23 21:19:03 +0100 (Wed 23 de Mar de 2016) $
#$Revision: 179476 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/73/4337365.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_4337365
loop_
_publ_author_name
'De Sio, Stéphanie M'
'Wilson, Richard E.'
_publ_section_title
;
 Structural and spectroscopic studies of fluoroprotactinates.
;
_journal_issue                   3
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1750
_journal_page_last               1755
_journal_paper_doi               10.1021/ic402877a
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'F8 Pa, 2(C4 H12 N), 2(O) '
_chemical_formula_sum            'C8 H28 F8 N2 O2 Pa'
_chemical_formula_weight         567.32
_chemical_melting_point          ?
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 104.92
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.1001(5)
_cell_length_b                   9.0563(3)
_cell_length_c                   12.9862(4)
_cell_measurement_reflns_used    3085
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.06
_cell_measurement_theta_min      2.65
_cell_volume                     1716.00(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_device_type  'BRUKER APEX II'
_diffrn_measurement_method       '0.5 deg w/ scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0322
_diffrn_reflns_av_sigmaI/netI    0.0245
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14711
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         33.06
_diffrn_reflns_theta_min         2.65
_exptl_absorpt_coefficient_mu    9.167
_exptl_absorpt_correction_T_max  0.4609
_exptl_absorpt_correction_T_min  0.1871
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.196
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1076
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.135
_refine_diff_density_min         -1.389
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.236
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     100
_refine_ls_number_reflns         3085
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.236
_refine_ls_R_factor_all          0.0198
_refine_ls_R_factor_gt           0.0184
_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)+(0.0099P)²+4.8859P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0439
_refine_ls_wR_factor_ref         0.0443
_reflns_number_gt                2979
_reflns_number_total             3085
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic402877a_si_001.cif
_cod_data_source_block           (Me4N)2(H3O)PaF8
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4337365
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Pa1 Pa 0.5000 0.350570(13) 0.2500 0.01095(4) Uani 1 2 d S
F1 F 0.41931(14) 0.1888(2) 0.14829(16) 0.0334(4) Uani 1 1 d .
F2 F 0.39600(15) 0.5160(3) 0.22999(16) 0.0411(5) Uani 1 1 d .
F3 F 0.59579(15) 0.2651(3) 0.16337(18) 0.0502(7) Uani 1 1 d .
F4 F 0.46602(16) 0.4608(3) 0.08006(17) 0.0466(6) Uani 1 1 d .
N1 N 0.35474(16) 0.8457(3) 0.3597(2) 0.0200(4) Uani 1 1 d .
C1 C 0.45694(19) 0.8353(3) 0.3955(3) 0.0252(6) Uani 1 1 d .
H1A H 0.4778 0.7520 0.3596 0.038 Uiso 1 1 calc R
H1B H 0.4759 0.8201 0.4727 0.038 Uiso 1 1 calc R
H1C H 0.4840 0.9269 0.3774 0.038 Uiso 1 1 calc R
C2 C 0.3131(2) 0.7057(3) 0.3872(3) 0.0252(6) Uani 1 1 d .
H2A H 0.2463 0.7111 0.3612 0.038 Uiso 1 1 calc R
H2B H 0.3301 0.6924 0.4647 0.038 Uiso 1 1 calc R
H2C H 0.3358 0.6219 0.3536 0.038 Uiso 1 1 calc R
C3 C 0.3228(2) 0.9707(4) 0.4157(3) 0.0305(7) Uani 1 1 d .
H3A H 0.3493 1.0632 0.3982 0.046 Uiso 1 1 calc R
H3B H 0.3424 0.9543 0.4929 0.046 Uiso 1 1 calc R
H3C H 0.2558 0.9768 0.3929 0.046 Uiso 1 1 calc R
C4 C 0.3260(2) 0.8709(4) 0.2422(3) 0.0287(6) Uani 1 1 d .
H4A H 0.2591 0.8782 0.2187 0.043 Uiso 1 1 calc R
H4B H 0.3467 0.7882 0.2056 0.043 Uiso 1 1 calc R
H4C H 0.3534 0.9628 0.2250 0.043 Uiso 1 1 calc R
O1 O 0.66893(17) 0.3258(3) -0.0022(2) 0.0359(6) Uani 1 1 d .
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
Pa1 0.01141(5) 0.01134(5) 0.01051(5) 0.000 0.00356(4) 0.000
F1 0.0379(11) 0.0248(9) 0.0319(10) -0.0104(8) -0.0013(8) -0.0089(8)
F2 0.0450(12) 0.0518(13) 0.0269(10) 0.0037(9) 0.0098(9) 0.0319(10)
F3 0.0314(11) 0.0865(19) 0.0375(12) -0.0136(13) 0.0176(9) 0.0163(12)
F4 0.0421(12) 0.0711(17) 0.0307(11) -0.0093(11) 0.0166(9) -0.0118(12)
N1 0.0170(10) 0.0192(10) 0.0244(11) 0.0051(9) 0.0065(8) 0.0035(8)
C1 0.0166(12) 0.0284(15) 0.0307(15) 0.0047(12) 0.0061(11) 0.0022(10)
C2 0.0243(13) 0.0220(13) 0.0312(15) 0.0060(11) 0.0104(12) -0.0014(11)
C3 0.0317(15) 0.0250(15) 0.0370(17) 0.0041(12) 0.0127(13) 0.0097(12)
C4 0.0278(14) 0.0323(16) 0.0240(14) 0.0106(12) 0.0032(12) 0.0036(12)
O1 0.0276(11) 0.0340(13) 0.0506(16) 0.0052(11) 0.0181(11) 0.0079(9)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Pa Pa -8.0334 9.2807 '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
F1 Pa1 F1 93.22(11) 2_655 .
F1 Pa1 F2 147.32(8) 2_655 .
F1 Pa1 F2 96.97(9) . .
F1 Pa1 F2 96.97(9) 2_655 2_655
F1 Pa1 F2 147.32(8) . 2_655
F2 Pa1 F2 91.00(14) . 2_655
F1 Pa1 F3 77.67(9) 2_655 2_655
F1 Pa1 F3 74.20(9) . 2_655
F2 Pa1 F3 75.43(10) . 2_655
F2 Pa1 F3 138.35(9) 2_655 2_655
F1 Pa1 F3 74.20(9) 2_655 .
F1 Pa1 F3 77.67(9) . .
F2 Pa1 F3 138.35(9) . .
F2 Pa1 F3 75.43(10) 2_655 .
F3 Pa1 F3 138.58(16) 2_655 .
F1 Pa1 F4 76.05(8) 2_655 2_655
F1 Pa1 F4 145.45(9) . 2_655
F2 Pa1 F4 78.04(8) . 2_655
F2 Pa1 F4 67.22(8) 2_655 2_655
F3 Pa1 F4 71.45(9) 2_655 2_655
F3 Pa1 F4 128.16(8) . 2_655
F1 Pa1 F4 145.45(9) 2_655 .
F1 Pa1 F4 76.05(8) . .
F2 Pa1 F4 67.23(8) . .
F2 Pa1 F4 78.04(8) 2_655 .
F3 Pa1 F4 128.16(8) 2_655 .
F3 Pa1 F4 71.45(9) . .
F4 Pa1 F4 129.83(13) 2_655 .
C3 N1 C4 109.7(2) . .
C3 N1 C1 109.5(2) . .
C4 N1 C1 109.4(2) . .
C3 N1 C2 108.6(2) . .
C4 N1 C2 110.1(2) . .
C1 N1 C2 109.6(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pa1 F1 2.1320(18) 2_655
Pa1 F1 2.1321(18) .
Pa1 F2 2.1371(19) .
Pa1 F2 2.1371(19) 2_655
Pa1 F3 2.1898(19) 2_655
Pa1 F3 2.1898(19) .
Pa1 F4 2.355(2) 2_655
Pa1 F4 2.355(2) .
N1 C3 1.492(4) .
N1 C4 1.492(4) .
N1 C1 1.496(4) .
N1 C2 1.498(4) .
