#------------------------------------------------------------------------------
#$Date: 2016-03-25 08:57:24 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179712 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/14/7001456.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_7001456
loop_
_publ_author_name
'Kühnel, Moritz F.'
'Lentz, Dieter'
_publ_section_title
;
 Hydrometalation of fluoroallenes
;
_journal_issue                   24
_journal_name_full               'Dalton Transactions'
_journal_page_first              4747
_journal_page_last               4755
_journal_paper_doi               10.1039/b903300a
_journal_year                    2009
_chemical_formula_moiety         'C13 H11 Cl F4 W'
_chemical_formula_sum            'C13 H11 Cl F4 W'
_chemical_formula_weight         462.52
_chemical_melting_point          448
_chemical_name_common
;Bis(cyclopentadienyl)(1-difluoromethyl-2,2-
difluorovinyl)chlorotungsten
;
_chemical_name_systematic
;
Bis(cyclopentadienyl)(1-difluoromethyl-2,2-difluorovinyl)chlorotungsten
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.970(3)
_cell_length_b                   10.859(2)
_cell_length_c                   8.7092(18)
_cell_measurement_reflns_used    982
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.51
_cell_measurement_theta_min      3.00
_cell_volume                     1226.6(4)
_computing_cell_refinement       'SAINT (Bruker-AXS)'
_computing_data_collection       'SMART (Bruker-AXS)'
_computing_data_reduction        'SAINT (Bruker-AXS)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'SMART-CCD Bruker-AXS'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0365
_diffrn_reflns_av_sigmaI/netI    0.0137
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            28238
_diffrn_reflns_theta_full        30.53
_diffrn_reflns_theta_max         30.53
_diffrn_reflns_theta_min         2.82
_exptl_absorpt_coefficient_mu    9.665
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker-AXS)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.504
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.480
_refine_diff_density_min         -1.913
_refine_diff_density_rms         0.194
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.287
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     97
_refine_ls_number_reflns         1966
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.287
_refine_ls_R_factor_all          0.0166
_refine_ls_R_factor_gt           0.0156
_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)+(0.0171P)²+1.3597P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0413
_refine_ls_wR_factor_ref         0.0417
_reflns_number_gt                1900
_reflns_number_total             1966
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b903300a.txt
_cod_data_source_block           mo52
_cod_original_cell_volume        1226.7(4)
_cod_original_sg_symbol_H-M      Pnma
_cod_database_code               7001456
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.378700(8) 0.2500 0.178908(12) 0.01217(5) Uani 1 2 d S . .
Cl1 Cl 0.55757(6) 0.2500 0.07832(10) 0.02768(18) Uani 1 2 d S . .
C2R C 0.2651(2) 0.0964(3) 0.2194(4) 0.0313(5) Uani 1 1 d . . .
H2R H 0.1947 0.1101 0.1944 0.038 Uiso 1 1 calc R . .
C3R C 0.3417(3) 0.0426(2) 0.1233(3) 0.0325(6) Uani 1 1 d . . .
H3R H 0.3306 0.0124 0.0223 0.039 Uiso 1 1 calc R . .
C4R C 0.4349(2) 0.0414(2) 0.2012(3) 0.0316(6) Uani 1 1 d . . .
H4R H 0.4979 0.0092 0.1623 0.038 Uiso 1 1 calc R . .
C5R C 0.4216(2) 0.0956(3) 0.3475(3) 0.0296(5) Uani 1 1 d . . .
H5R H 0.4735 0.1094 0.4225 0.036 Uiso 1 1 calc R . .
C1R C 0.3149(2) 0.1255(3) 0.3601(3) 0.0288(5) Uani 1 1 d . . .
H1R H 0.2824 0.1594 0.4482 0.035 Uiso 1 1 calc R . .
C2 C 0.3297(3) 0.2500 -0.0661(4) 0.0222(6) Uani 1 2 d S . .
C3 C 0.4027(3) 0.2500 -0.1980(4) 0.0269(7) Uani 1 2 d S . .
H1 H 0.4752 0.2500 -0.1589 0.032 Uiso 1 2 calc SR . .
C1 C 0.2324(3) 0.2500 -0.1101(5) 0.0373(10) Uani 1 2 d S . .
F1 F 0.38770(17) 0.1495(2) -0.2926(2) 0.0481(5) Uani 1 1 d . . .
F2 F 0.1970(2) 0.2500 -0.2537(3) 0.0492(7) Uani 1 2 d S . .
F3 F 0.1502(2) 0.2500 -0.0179(4) 0.0698(12) Uani 1 2 d S . .
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 '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'
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
C2 W1 C1R 124.79(10) . 7_565 ?
C2 W1 C1R 124.79(10) . . ?
C1R W1 C1R 74.36(15) 7_565 . ?
C2 W1 C2R 87.89(10) . 7_565 ?
C1R W1 C2R 36.89(11) 7_565 7_565 ?
C1R W1 C2R 95.44(11) . 7_565 ?
C2 W1 C2R 87.89(10) . . ?
C1R W1 C2R 95.44(11) 7_565 . ?
C1R W1 C2R 36.89(11) . . ?
C2R W1 C2R 95.49(15) 7_565 . ?
C2 W1 C5R 132.99(7) . 7_565 ?
C1R W1 C5R 36.65(11) 7_565 7_565 ?
C1R W1 C5R 94.58(11) . 7_565 ?
C2R W1 C5R 61.21(11) 7_565 7_565 ?
C2R W1 C5R 126.78(11) . 7_565 ?
C2 W1 C5R 132.99(7) . . ?
C1R W1 C5R 94.58(11) 7_565 . ?
C1R W1 C5R 36.65(11) . . ?
C2R W1 C5R 126.78(11) 7_565 . ?
C2R W1 C5R 61.21(11) . . ?
C5R W1 C5R 93.74(15) 7_565 . ?
C2 W1 C3R 75.20(8) . . ?
C1R W1 C3R 130.39(11) 7_565 . ?
C1R W1 C3R 59.42(10) . . ?
C2R W1 C3R 127.38(11) 7_565 . ?
C2R W1 C3R 35.93(10) . . ?
C5R W1 C3R 151.58(10) 7_565 . ?
C5R W1 C3R 58.84(11) . . ?
C2 W1 C3R 75.20(8) . 7_565 ?
C1R W1 C3R 59.42(10) 7_565 7_565 ?
C1R W1 C3R 130.39(11) . 7_565 ?
C2R W1 C3R 35.93(10) 7_565 7_565 ?
C2R W1 C3R 127.38(11) . 7_565 ?
C5R W1 C3R 58.84(11) 7_565 7_565 ?
C5R W1 C3R 151.58(10) . 7_565 ?
C3R W1 C3R 146.30(16) . 7_565 ?
C2 W1 C4R 99.50(8) . 7_565 ?
C1R W1 C4R 58.83(10) 7_565 7_565 ?
C1R W1 C4R 128.99(10) . 7_565 ?
C2R W1 C4R 58.99(11) 7_565 7_565 ?
C2R W1 C4R 152.78(11) . 7_565 ?
C5R W1 C4R 35.08(10) 7_565 7_565 ?
C5R W1 C4R 124.50(11) . 7_565 ?
C3R W1 C4R 170.78(10) . 7_565 ?
C3R W1 C4R 34.01(11) 7_565 7_565 ?
C2 W1 C4R 99.50(8) . . ?
C1R W1 C4R 128.99(10) 7_565 . ?
C1R W1 C4R 58.83(10) . . ?
C2R W1 C4R 152.78(11) 7_565 . ?
C2R W1 C4R 58.99(11) . . ?
C5R W1 C4R 124.50(11) 7_565 . ?
C5R W1 C4R 35.08(10) . . ?
C3R W1 C4R 34.01(11) . . ?
C3R W1 C4R 170.78(10) 7_565 . ?
C4R W1 C4R 143.15(16) 7_565 . ?
C2 W1 Cl1 85.90(10) . . ?
C1R W1 Cl1 126.55(8) 7_565 . ?
C1R W1 Cl1 126.55(8) . . ?
C2R W1 Cl1 131.84(8) 7_565 . ?
C2R W1 Cl1 131.84(8) . . ?
C5R W1 Cl1 89.94(8) 7_565 . ?
C5R W1 Cl1 89.94(8) . . ?
C3R W1 Cl1 96.79(8) . . ?
C3R W1 Cl1 96.79(8) 7_565 . ?
C4R W1 Cl1 75.10(8) 7_565 . ?
C4R W1 Cl1 75.10(8) . . ?
C1R C2R C3R 106.3(3) . . ?
C1R C2R W1 70.91(14) . . ?
C3R C2R W1 75.88(15) . . ?
C4R C3R C2R 109.0(3) . . ?
C4R C3R W1 74.35(15) . . ?
C2R C3R W1 68.19(14) . . ?
C3R C4R C5R 109.3(3) . . ?
C3R C4R W1 71.64(15) . . ?
C5R C4R W1 68.95(15) . . ?
C4R C5R C1R 106.4(3) . . ?
C4R C5R W1 75.97(15) . . ?
C1R C5R W1 69.36(14) . . ?
C2R C1R C5R 108.9(2) . . ?
C2R C1R W1 72.19(15) . . ?
C5R C1R W1 73.99(14) . . ?
C1 C2 C3 112.6(3) . . ?
C1 C2 W1 123.5(3) . . ?
C3 C2 W1 123.9(3) . . ?
F1 C3 F1 104.4(3) . 7_565 ?
F1 C3 C2 111.8(2) . . ?
F1 C3 C2 111.8(2) 7_565 . ?
C2 C1 F2 127.0(4) . . ?
C2 C1 F3 126.1(4) . . ?
F2 C1 F3 106.8(3) . . ?
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
W1 C2 2.226(3) . ?
W1 C1R 2.236(2) 7_565 ?
W1 C1R 2.236(2) . ?
W1 C2R 2.253(3) 7_565 ?
W1 C2R 2.253(3) . ?
W1 C5R 2.297(2) 7_565 ?
W1 C5R 2.297(2) . ?
W1 C3R 2.354(3) . ?
W1 C3R 2.354(3) 7_565 ?
W1 C4R 2.388(3) 7_565 ?
W1 C4R 2.388(3) . ?
W1 Cl1 2.4798(9) . ?
C2R C1R 1.421(4) . ?
C2R C3R 1.424(4) . ?
C3R C4R 1.387(5) . ?
C4R C5R 1.415(4) . ?
C5R C1R 1.426(4) . ?
C2 C1 1.319(5) . ?
C2 C3 1.489(5) . ?
C3 F1 1.381(3) . ?
C3 F1 1.381(3) 7_565 ?
C1 F2 1.333(5) . ?
C1 F3 1.334(5) . ?
