#------------------------------------------------------------------------------
#$Date: 2016-03-23 22:19:03 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179476 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/73/4337360.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_4337360
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         'F7 Pa, 2(H4 N)'
_chemical_formula_sum            'F7 H8 N2 Pa'
_chemical_formula_weight         400.08
_chemical_melting_point          ?
_chemical_name_common            'diammonium heptafluoroprotactinate(V)'
_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_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                 90.606(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.1003(10)
_cell_length_b                   6.8966(9)
_cell_length_c                   11.8834(15)
_cell_measurement_reflns_used    8751
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.43
_cell_measurement_theta_min      2.51
_cell_volume                     663.82(15)
_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 0.949
_diffrn_measurement_device_type  'BRUKER APEX II'
_diffrn_measurement_method       '0.5 deg w/ scans'
_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  0.0217
_diffrn_reflns_av_sigmaI/netI    0.0172
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8751
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         30.43
_diffrn_reflns_theta_min         2.51
_exptl_absorpt_coefficient_mu    23.563
_exptl_absorpt_correction_T_max  0.1090
_exptl_absorpt_correction_T_min  0.0477
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    4.003
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             704
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.456
_refine_diff_density_min         -1.586
_refine_diff_density_rms         0.196
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.238
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     123
_refine_ls_number_reflns         1909
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.235
_refine_ls_R_factor_all          0.0179
_refine_ls_R_factor_gt           0.0171
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0298P)²+0.7427P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0537
_refine_ls_wR_factor_ref         0.0544
_reflns_number_gt                1835
_reflns_number_total             1909
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic402877a_si_001.cif
_cod_data_source_block           NH4-PaF7
_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      'P 21/c'
_cod_database_code               4337360
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_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 0.252259(11) 0.02153(2) 0.505344(9) 0.01466(7) Uani 1 1 d .
F1 F 0.0075(2) 0.1612(3) 0.54343(17) 0.0195(4) Uani 1 1 d .
F2 F 0.2876(2) 0.1587(3) 0.67246(16) 0.0207(4) Uani 1 1 d .
F3 F 0.4995(2) 0.0746(3) 0.40735(17) 0.0195(4) Uani 1 1 d .
F4 F 0.3150(2) -0.2450(3) 0.42456(18) 0.0220(4) Uani 1 1 d .
F5 F 0.2971(3) 0.3289(3) 0.48201(17) 0.0207(4) Uani 1 1 d .
F6 F 0.1867(2) -0.1936(3) 0.63316(17) 0.0204(4) Uani 1 1 d .
F7 F 0.1727(2) 0.0782(3) 0.33610(17) 0.0208(4) Uani 1 1 d .
N1 N 0.0585(5) 0.0131(5) 0.8316(4) 0.0204(7) Uani 1 1 d D
N2 N 0.5530(5) 0.0303(5) 0.8288(3) 0.0210(7) Uani 1 1 d D
H5 H 0.481(5) 0.027(6) 0.880(3) 0.021(11) Uiso 1 1 d D
H6 H 0.629(5) 0.115(6) 0.833(4) 0.031(13) Uiso 1 1 d D
H2 H 0.004(6) 0.099(6) 0.867(4) 0.045(15) Uiso 1 1 d D
H3 H 0.100(9) -0.065(9) 0.879(5) 0.08(2) Uiso 1 1 d D
H7 H 0.526(10) 0.063(12) 0.762(3) 0.07(3) Uiso 1 1 d D
H1 H 0.016(10) -0.067(11) 0.784(6) 0.07(3) Uiso 1 1 d D
H4 H 0.139(7) 0.049(11) 0.791(6) 0.08(3) Uiso 1 1 d D
H8 H 0.612(8) -0.072(7) 0.835(6) 0.054(19) Uiso 1 1 d 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 0.01426(9) 0.01438(10) 0.01534(9) -0.00016(3) 0.00000(5) 0.00012(3)
F1 0.0156(8) 0.0181(9) 0.0250(10) -0.0034(7) 0.0020(7) -0.0002(7)
F2 0.0228(9) 0.0193(10) 0.0202(9) -0.0013(7) 0.0005(7) -0.0009(8)
F3 0.0168(8) 0.0225(10) 0.0192(9) 0.0023(7) 0.0004(7) -0.0003(7)
F4 0.0207(9) 0.0190(10) 0.0264(10) -0.0035(8) 0.0002(7) 0.0003(7)
F5 0.0234(9) 0.0177(10) 0.0212(9) 0.0011(7) -0.0004(7) -0.0022(8)
F6 0.0193(9) 0.0202(10) 0.0217(9) 0.0029(7) 0.0008(7) -0.0005(7)
F7 0.0201(9) 0.0230(11) 0.0192(9) 0.0006(8) -0.0016(7) -0.0017(8)
N1 0.0234(18) 0.0167(15) 0.0210(17) -0.0017(11) -0.0005(13) -0.0002(11)
N2 0.0226(17) 0.0199(16) 0.0205(17) -0.0009(12) -0.0012(13) 0.0019(12)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
N N 0.0061 0.0033 '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'
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
F4 Pa1 F7 78.80(8) . .
F4 Pa1 F5 137.91(8) . .
F7 Pa1 F5 75.57(8) . .
F4 Pa1 F6 77.86(7) . .
F7 Pa1 F6 134.53(8) . .
F5 Pa1 F6 142.37(7) . .
F4 Pa1 F2 137.80(8) . .
F7 Pa1 F2 143.00(7) . .
F5 Pa1 F2 71.15(8) . .
F6 Pa1 F2 72.42(8) . .
F4 Pa1 F1 132.18(7) . .
F7 Pa1 F1 81.60(7) . .
F5 Pa1 F1 75.92(8) . .
F6 Pa1 F1 86.00(7) . .
F2 Pa1 F1 75.11(7) . .
F4 Pa1 F3 75.47(7) . 3_656
F7 Pa1 F3 135.59(7) . 3_656
F5 Pa1 F3 100.88(7) . 3_656
F6 Pa1 F3 73.47(7) . 3_656
F2 Pa1 F3 67.84(7) . 3_656
F1 Pa1 F3 141.50(7) . 3_656
F4 Pa1 F3 72.78(7) . .
F7 Pa1 F3 75.91(7) . .
F5 Pa1 F3 68.95(8) . .
F6 Pa1 F3 131.37(7) . .
F2 Pa1 F3 105.93(7) . .
F1 Pa1 F3 141.89(7) . .
F3 Pa1 F3 62.21(8) 3_656 .
F4 Pa1 F1 70.61(7) . 3_556
F7 Pa1 F1 68.42(7) . 3_556
F5 Pa1 F1 126.94(7) . 3_556
F6 Pa1 F1 67.19(7) . 3_556
F2 Pa1 F1 121.35(7) . 3_556
F1 Pa1 F1 61.65(8) . 3_556
F3 Pa1 F1 132.12(7) 3_656 3_556
F3 Pa1 F1 132.64(6) . 3_556
F4 Pa1 Pa1 71.37(5) . 3_656
F7 Pa1 Pa1 105.90(5) . 3_656
F5 Pa1 Pa1 84.26(6) . 3_656
F6 Pa1 Pa1 102.75(5) . 3_656
F2 Pa1 Pa1 86.59(5) . 3_656
F1 Pa1 Pa1 156.43(5) . 3_656
F3 Pa1 Pa1 31.16(5) 3_656 3_656
F3 Pa1 Pa1 31.05(5) . 3_656
F1 Pa1 Pa1 141.92(4) 3_556 3_656
F4 Pa1 Pa1 99.54(5) . 3_556
F7 Pa1 Pa1 72.18(5) . 3_556
F5 Pa1 Pa1 103.59(6) . 3_556
F6 Pa1 Pa1 73.96(5) . 3_556
F2 Pa1 Pa1 100.25(5) . 3_556
F1 Pa1 Pa1 32.69(5) . 3_556
F3 Pa1 Pa1 147.37(5) 3_656 3_556
F3 Pa1 Pa1 148.06(5) . 3_556
F1 Pa1 Pa1 28.96(4) 3_556 3_556
Pa1 Pa1 Pa1 170.880(8) 3_656 3_556
Pa1 F1 Pa1 118.35(8) . 3_556
Pa1 F3 Pa1 117.78(8) 3_656 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pa1 F4 2.138(2) .
Pa1 F7 2.141(2) .
Pa1 F5 2.169(2) .
Pa1 F6 2.193(2) .
Pa1 F2 2.216(2) .
Pa1 F1 2.2547(18) .
Pa1 F3 2.3484(19) 3_656
Pa1 F3 2.3560(19) .
Pa1 F1 2.5150(18) 3_556
Pa1 Pa1 4.0279(5) 3_656
Pa1 Pa1 4.0981(5) 3_556
F1 Pa1 2.5150(18) 3_556
F3 Pa1 2.3483(19) 3_656
