#------------------------------------------------------------------------------
#$Date: 2016-03-23 21:34:49 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179452 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/49/4334979.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_4334979
loop_
_publ_author_name
'Tobias Böttcher'
'Bassem S. Bassil'
'Lyuben Zhechkov'
'Gerd-Volker Röschenthaler'
_publ_section_title
;
 Phosphorus(V) Complexes with Acyclic Monoaminocarbene Ligands via
 Oxidative Addition
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5651
_journal_page_last               5653
_journal_paper_doi               10.1021/ic400756z
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C3 H7 F5 N P'
_chemical_formula_weight         183.06
_chemical_name_systematic
; 
 ? 
;
_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                 93.561(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.123(3)
_cell_length_b                   8.0657(17)
_cell_length_c                   11.628(2)
_cell_measurement_reflns_used    8864
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.48
_cell_measurement_theta_min      2.89
_cell_volume                     1322.0(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω 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  0.0428
_diffrn_reflns_av_sigmaI/netI    0.0110
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            129339
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         3.44
_exptl_absorpt_coefficient_mu    0.439
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6817
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.840
_exptl_crystal_description       block
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.709
_refine_diff_density_min         -0.545
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         3999
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_gt           0.0302
_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)+(0.0400P)²+0.8000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0780
_refine_ls_wR_factor_ref         0.0814
_reflns_number_gt                3696
_reflns_number_total             3999
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400756z_si_002.cif
_cod_data_source_block           try
_cod_database_code               4334979
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
C1A C 0.41504(7) 0.40634(14) 0.11717(9) 0.01745(19) Uani 1 1 d
H11A H 0.4627(11) 0.357(2) 0.1679(14) 0.022(4) Uiso 1 1 d
C1 C -0.02620(8) 0.13126(14) 0.17297(10) 0.0199(2) Uani 1 1 d
H11 H -0.0495(12) 0.060(2) 0.2306(15) 0.028(4) Uiso 1 1 d
C2A C 0.40187(10) 0.13460(15) 0.03635(12) 0.0257(2) Uani 1 1 d
H23A H 0.4535(12) 0.115(2) 0.0931(16) 0.029(4) Uiso 1 1 d
H22A H 0.4201(14) 0.112(3) -0.0390(19) 0.046(5) Uiso 1 1 d
H21A H 0.3492(14) 0.073(3) 0.0504(17) 0.039(5) Uiso 1 1 d
C2 C -0.07688(9) 0.30367(19) 0.00802(12) 0.0290(3) Uani 1 1 d
H23 H -0.0185(14) 0.298(2) -0.0125(17) 0.035(5) Uiso 1 1 d
H22 H -0.0929(15) 0.410(3) 0.0337(19) 0.049(6) Uiso 1 1 d
H21 H -0.1233(15) 0.274(3) -0.051(2) 0.050(6) Uiso 1 1 d
C3A C 0.30132(9) 0.35913(18) -0.04725(11) 0.0259(2) Uani 1 1 d
H33A H 0.3171(15) 0.314(3) -0.115(2) 0.054(6) Uiso 1 1 d
H32A H 0.2933(14) 0.472(3) -0.0580(17) 0.043(5) Uiso 1 1 d
H31A H 0.2439(16) 0.309(3) -0.030(2) 0.053(6) Uiso 1 1 d
C3 C -0.19211(8) 0.15744(17) 0.12204(13) 0.0267(2) Uani 1 1 d
H33 H -0.2195(13) 0.251(2) 0.1471(16) 0.034(5) Uiso 1 1 d
H32 H -0.1958(13) 0.074(2) 0.1772(16) 0.034(5) Uiso 1 1 d
H31 H -0.2199(13) 0.123(2) 0.0528(18) 0.037(5) Uiso 1 1 d
N1A N 0.37569(6) 0.31111(12) 0.04074(8) 0.01802(17) Uani 1 1 d
N1 N -0.09138(6) 0.19203(11) 0.10488(8) 0.01737(17) Uani 1 1 d
P1A P 0.39288(2) 0.62792(4) 0.15111(3) 0.01868(7) Uani 1 1 d
P1 P 0.10516(2) 0.15780(4) 0.17894(2) 0.02069(8) Uani 1 1 d
F1A F 0.37869(7) 0.81559(10) 0.18891(8) 0.03512(19) Uani 1 1 d
F1 F 0.21770(5) 0.17514(13) 0.19070(7) 0.0355(2) Uani 1 1 d
F2A F 0.50664(5) 0.64861(10) 0.17278(7) 0.02725(16) Uani 1 1 d
F2 F 0.11363(7) -0.03417(12) 0.21454(9) 0.0448(2) Uani 1 1 d
F3A F 0.27994(5) 0.60563(10) 0.12971(7) 0.02707(16) Uani 1 1 d
F3 F 0.09873(6) 0.20882(16) 0.31261(7) 0.0450(3) Uani 1 1 d
F4A F 0.38643(5) 0.56931(9) 0.28347(6) 0.02501(15) Uani 1 1 d
F4 F 0.09597(5) 0.35138(9) 0.14447(8) 0.02847(17) Uani 1 1 d
F5A F 0.40037(6) 0.68338(10) 0.01894(7) 0.02885(17) Uani 1 1 d
F5 F 0.10928(5) 0.10988(10) 0.04556(6) 0.02543(15) 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
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'
F F 0.0171 0.0103 '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'
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
N1A C1A P1A 130.87(8)
N1 C1 P1 131.12(9)
C1A N1A C3A 125.94(10)
C1A N1A C2A 120.45(10)
C3A N1A C2A 113.59(10)
C1 N1 C2 125.69(10)
C1 N1 C3 120.57(10)
C2 N1 C3 113.69(10)
F1A P1A F5A 90.93(5)
F1A P1A F3A 90.48(5)
F5A P1A F3A 90.38(4)
F1A P1A F4A 89.99(5)
F5A P1A F4A 178.99(4)
F3A P1A F4A 90.04(4)
F1A P1A F2A 89.99(5)
F5A P1A F2A 89.80(5)
F3A P1A F2A 179.50(4)
F4A P1A F2A 89.78(4)
F1A P1A C1A 175.70(5)
F5A P1A C1A 92.44(5)
F3A P1A C1A 92.18(4)
F4A P1A C1A 86.63(4)
F2A P1A C1A 87.34(4)
F1 P1 F5 90.47(4)
F1 P1 F2 90.26(5)
F5 P1 F2 90.59(5)
F1 P1 F4 90.04(5)
F5 P1 F4 90.01(4)
F2 P1 F4 179.32(5)
F1 P1 F3 90.60(5)
F5 P1 F3 178.60(5)
F2 P1 F3 90.30(6)
F4 P1 F3 89.09(6)
F1 P1 C1 176.82(5)
F5 P1 C1 91.84(5)
F2 P1 C1 87.53(5)
F4 P1 C1 92.14(5)
F3 P1 C1 87.12(5)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
C1A N1A 1.2756(14)
C1A P1A 1.8609(12)
C1 N1 1.2744(15)
C1 P1 1.8644(12)
C2A N1A 1.4726(15)
C2 N1 1.4662(15)
C3A N1A 1.4720(15)
C3 N1 1.4753(14)
P1A F1A 1.5924(9)
P1A F5A 1.6104(8)
P1A F3A 1.6090(8)
P1A F4A 1.6179(8)
P1A F2A 1.6194(8)
P1 F1 1.5930(8)
P1 F5 1.6029(8)
P1 F2 1.6054(10)
P1 F4 1.6152(9)
P1 F3 1.6159(9)
