#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:26:56 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179328 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/25/4322579.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_4322579
loop_
_publ_author_name
'Shaun E. Landau'
'Robert H. Morris'
'Alan J. Lough'
_publ_section_title
;
 Acidic Dicationic Iron(II) Dihydrogen Complexes and Compounds Related by
 H2 Substitution
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6060
_journal_page_last               6068
_journal_paper_doi               10.1021/ic990876a
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C10 H26 B2 F8 P2'
_chemical_formula_weight         381.87
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 100.432(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.5997(3)
_cell_length_b                   16.4115(9)
_cell_length_c                   8.2463(3)
_cell_measurement_temperature    100.0(1)
_cell_volume                     878.40(7)
_computing_cell_refinement       'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'KappaCCD server software (Nonius, 1997)'
_computing_data_reduction        'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL V5.1'
_computing_publication_material  'Bruker SHELXTL V5.1'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100.0(1)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Nonius Kappa-CCD'
_diffrn_measurement_method       'φ scans and ω scans with κ offsets'
_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  0.051
_diffrn_reflns_av_sigmaI/netI    0.0531
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            6601
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         4.36
_exptl_absorpt_coefficient_mu    0.313
_exptl_absorpt_correction_T_max  0.9693
_exptl_absorpt_correction_T_min  0.9258
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Denzo-SMN (Otwinowski & Minor, 1997)'
_exptl_crystal_density_diffrn    1.444
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             396
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.312
_refine_diff_density_min         -0.355
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     104
_refine_ls_number_reflns         2007
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_gt           0.0354
_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)+(0.0491P)²+0.0332P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0911
_refine_ls_wR_factor_ref         0.0964
_reflns_number_gt                1565
_reflns_number_total             2007
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic990876a_4.cif
_cod_data_source_block           k9949_[H2(depe)][BF4]2
_cod_database_code               4322579
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.18836(6) 0.41024(2) 0.66053(5) 0.02027(14) Uani 1 1 d . . .
H1P H 0.364(2) 0.4466(10) 0.661(2) 0.022(4) Uiso 1 1 d . . .
C1 C 0.0015(2) 0.45321(9) 0.49744(19) 0.0235(4) Uani 1 1 d . . .
H1A H 0.0329 0.4353 0.3900 0.028 Uiso 1 1 calc R . .
H1B H -0.1368 0.4323 0.5061 0.028 Uiso 1 1 calc R . .
C2 C 0.1139(3) 0.42742(11) 0.8563(2) 0.0311(4) Uani 1 1 d . . .
H2A H 0.2305 0.4133 0.9453 0.037 Uiso 1 1 calc R . .
H2B H 0.0827 0.4860 0.8669 0.037 Uiso 1 1 calc R . .
C3 C -0.0735(3) 0.37736(12) 0.8774(3) 0.0426(5) Uani 1 1 d . . .
H3A H -0.1087 0.3887 0.9856 0.064 Uiso 1 1 calc R . .
H3B H -0.0424 0.3193 0.8694 0.064 Uiso 1 1 calc R . .
H3C H -0.1902 0.3918 0.7908 0.064 Uiso 1 1 calc R . .
C4 C 0.2154(2) 0.30357(10) 0.62671(19) 0.0231(4) Uani 1 1 d . . .
H4A H 0.0822 0.2761 0.6284 0.028 Uiso 1 1 calc R . .
H4B H 0.2512 0.2950 0.5165 0.028 Uiso 1 1 calc R . .
C5 C 0.3821(3) 0.26551(11) 0.7580(2) 0.0340(4) Uani 1 1 d . . .
H5A H 0.3930 0.2072 0.7356 0.051 Uiso 1 1 calc R . .
H5B H 0.3455 0.2729 0.8671 0.051 Uiso 1 1 calc R . .
H5C H 0.5145 0.2920 0.7555 0.051 Uiso 1 1 calc R . .
F1 F 0.65939(19) 0.54052(7) 0.71534(19) 0.0591(4) Uani 1 1 d . . .
F2 F 0.44691(17) 0.63201(8) 0.56655(13) 0.0528(4) Uani 1 1 d . . .
F3 F 0.66143(16) 0.67187(6) 0.79780(13) 0.0394(3) Uani 1 1 d . . .
F4 F 0.38681(16) 0.59003(6) 0.81475(13) 0.0348(3) Uani 1 1 d . . .
B1 B 0.5380(3) 0.60875(12) 0.7245(2) 0.0260(4) 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
P1 0.0198(2) 0.0201(2) 0.0203(2) 0.00058(16) 0.00216(15) -0.00103(15)
C1 0.0223(8) 0.0245(9) 0.0223(7) 0.0005(6) 0.0001(6) -0.0008(6)
C2 0.0471(11) 0.0250(9) 0.0218(8) -0.0005(7) 0.0081(8) -0.0008(8)
C3 0.0602(13) 0.0308(10) 0.0456(11) -0.0018(9) 0.0327(10) -0.0038(9)
C4 0.0239(8) 0.0212(8) 0.0244(8) -0.0001(7) 0.0045(7) -0.0013(6)
C5 0.0312(9) 0.0263(9) 0.0408(10) 0.0038(8) -0.0036(8) 0.0032(7)
F1 0.0455(7) 0.0374(7) 0.1023(11) -0.0156(7) 0.0345(7) 0.0039(5)
F2 0.0398(7) 0.0895(11) 0.0267(6) 0.0106(6) -0.0006(5) -0.0252(6)
F3 0.0398(6) 0.0342(6) 0.0409(6) -0.0029(5) -0.0017(5) -0.0112(5)
F4 0.0356(6) 0.0371(6) 0.0359(6) 0.0052(5) 0.0179(5) -0.0003(4)
B1 0.0252(9) 0.0270(10) 0.0259(9) -0.0019(8) 0.0045(7) -0.0030(7)
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'
B B 0.0013 0.0007 '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'
P P 0.1023 0.0942 '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
_geom_angle_publ_flag
C4 P1 C2 110.24(8) . . ?
C4 P1 C1 110.01(7) . . ?
C2 P1 C1 110.46(8) . . ?
C1 C1 P1 112.49(14) 3_566 . ?
C3 C2 P1 112.30(13) . . ?
C5 C4 P1 111.64(11) . . ?
F4 B1 F2 109.55(14) . . ?
F4 B1 F1 109.27(15) . . ?
F2 B1 F1 109.16(16) . . ?
F4 B1 F3 110.79(15) . . ?
F2 B1 F3 108.94(15) . . ?
F1 B1 F3 109.10(15) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1 C4 1.7867(16) . ?
P1 C2 1.7926(17) . ?
P1 C1 1.7960(15) . ?
C1 C1 1.537(3) 3_566 ?
C2 C3 1.521(3) . ?
C4 C5 1.530(2) . ?
F1 B1 1.387(2) . ?
F2 B1 1.385(2) . ?
F3 B1 1.387(2) . ?
F4 B1 1.383(2) . ?
