#------------------------------------------------------------------------------
#$Date: 2016-03-25 08:57:24 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179712 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/14/7001460.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_7001460
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         'C11 H6 F4 Mo O3'
_chemical_formula_sum            'C11 H6 F4 Mo O3'
_chemical_formula_weight         358.10
_chemical_melting_point          336
_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                 93.838(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.0792(11)
_cell_length_b                   12.7380(18)
_cell_length_c                   11.6673(18)
_cell_measurement_reflns_used    983
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.46
_cell_measurement_theta_min      2.97
_cell_volume                     1198.0(3)
_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 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'SMART-CCD Bruker-AXS'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0220
_diffrn_reflns_av_sigmaI/netI    0.0196
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14540
_diffrn_reflns_theta_full        30.52
_diffrn_reflns_theta_max         30.52
_diffrn_reflns_theta_min         2.37
_exptl_absorpt_coefficient_mu    1.146
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker-AXS)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.985
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.358
_refine_diff_density_min         -0.627
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         3634
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0315
_refine_ls_R_factor_gt           0.0242
_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)+(0.0376P)²+0.8010P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0653
_refine_ls_wR_factor_ref         0.0701
_reflns_number_gt                3122
_reflns_number_total             3634
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b903300a.txt
_cod_data_source_block           mor12m
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7001460
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
Mo1 Mo 0.172436(17) 0.221070(12) 0.303300(13) 0.02135(6) Uani 1 1 d . . .
C1 C -0.0775(3) 0.3751(2) 0.4136(2) 0.0445(6) Uani 1 1 d . . .
C2 C -0.0278(3) 0.34271(17) 0.3154(2) 0.0309(4) Uani 1 1 d . . .
C3 C -0.1334(3) 0.3824(2) 0.2145(2) 0.0392(5) Uani 1 1 d . . .
H1 H -0.2384 0.4129 0.2409 0.047 Uiso 1 1 calc R . .
C1O C 0.1758(3) 0.27691(19) 0.1429(2) 0.0356(5) Uani 1 1 d . . .
C2O C 0.4131(3) 0.2169(2) 0.2740(2) 0.0437(6) Uani 1 1 d . . .
C3O C 0.2824(3) 0.32671(18) 0.41027(19) 0.0343(4) Uani 1 1 d . . .
C1R C 0.0629(3) 0.11035(17) 0.4387(2) 0.0342(4) Uani 1 1 d . . .
H1R H 0.0474 0.1343 0.5144 0.041 Uiso 1 1 calc R . .
C2R C 0.2087(3) 0.06491(18) 0.4002(2) 0.0355(5) Uani 1 1 d . . .
H2R H 0.3087 0.0523 0.4457 0.043 Uiso 1 1 calc R . .
C3R C 0.1796(3) 0.04150(19) 0.2816(2) 0.0405(5) Uani 1 1 d . . .
H3R H 0.2569 0.0108 0.2337 0.049 Uiso 1 1 calc R . .
C4R C 0.0151(3) 0.07196(19) 0.2475(2) 0.0407(5) Uani 1 1 d . . .
H4R H -0.0377 0.0653 0.1726 0.049 Uiso 1 1 calc R . .
C5R C -0.0560(3) 0.11374(18) 0.3440(2) 0.0383(5) Uani 1 1 d . . .
H5R H -0.1659 0.1400 0.3455 0.046 Uiso 1 1 calc R . .
F2 F -0.0102(2) 0.35052(15) 0.51701(14) 0.0584(4) Uani 1 1 d . . .
F1 F -0.2088(3) 0.43597(18) 0.4312(2) 0.0824(7) Uani 1 1 d . . .
F3 F -0.0495(2) 0.45728(14) 0.15591(16) 0.0595(5) Uani 1 1 d . . .
F4 F -0.16943(18) 0.30495(13) 0.13656(14) 0.0453(3) Uani 1 1 d . . .
O1 O 0.1818(3) 0.30066(19) 0.04916(16) 0.0541(5) Uani 1 1 d . . .
O2 O 0.5512(2) 0.2167(2) 0.2596(2) 0.0711(8) Uani 1 1 d . . .
O3 O 0.3516(3) 0.38461(16) 0.47034(17) 0.0531(5) 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'
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'
Mo Mo -1.6832 0.6857 '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
C2O Mo1 C3O 74.22(10) . . ?
C2O Mo1 C1O 77.03(11) . . ?
C3O Mo1 C1O 108.09(10) . . ?
C2O Mo1 C2 137.81(10) . . ?
C3O Mo1 C2 77.82(9) . . ?
C1O Mo1 C2 82.47(9) . . ?
C2O Mo1 C2R 88.14(10) . . ?
C3O Mo1 C2R 103.80(9) . . ?
C1O Mo1 C2R 139.26(9) . . ?
C2 Mo1 C2R 129.32(8) . . ?
C2O Mo1 C3R 85.58(11) . . ?
C3O Mo1 C3R 136.28(9) . . ?
C1O Mo1 C3R 104.37(10) . . ?
C2 Mo1 C3R 135.57(8) . . ?
C2R Mo1 C3R 35.94(8) . . ?
C2O Mo1 C1R 121.14(10) . . ?
C3O Mo1 C1R 99.01(9) . . ?
C1O Mo1 C1R 151.09(9) . . ?
C2 Mo1 C1R 93.82(8) . . ?
C2R Mo1 C1R 35.51(8) . . ?
C3R Mo1 C1R 59.19(9) . . ?
C2O Mo1 C4R 116.45(11) . . ?
C3O Mo1 C4R 157.50(9) . . ?
C1O Mo1 C4R 93.95(9) . . ?
C2 Mo1 C4R 101.28(9) . . ?
C2R Mo1 C4R 59.07(8) . . ?
C3R Mo1 C4R 35.40(9) . . ?
C1R Mo1 C4R 58.50(9) . . ?
C2O Mo1 C5R 143.03(10) . . ?
C3O Mo1 C5R 125.57(9) . . ?
C1O Mo1 C5R 116.82(9) . . ?
C2 Mo1 C5R 79.16(8) . . ?
C2R Mo1 C5R 58.49(8) . . ?
C3R Mo1 C5R 58.31(9) . . ?
C1R Mo1 C5R 34.99(8) . . ?
C4R Mo1 C5R 34.54(9) . . ?
C2 C1 F2 126.3(2) . . ?
C2 C1 F1 127.5(3) . . ?
F2 C1 F1 106.1(2) . . ?
C1 C2 C3 113.1(2) . . ?
C1 C2 Mo1 122.45(18) . . ?
C3 C2 Mo1 123.90(16) . . ?
F4 C3 F3 105.1(2) . . ?
F4 C3 C2 111.52(19) . . ?
F3 C3 C2 110.5(2) . . ?
O1 C1O Mo1 174.4(2) . . ?
O2 C2O Mo1 178.1(3) . . ?
O3 C3O Mo1 176.9(2) . . ?
C5R C1R C2R 107.5(2) . . ?
C5R C1R Mo1 73.83(13) . . ?
C2R C1R Mo1 70.75(13) . . ?
C1R C2R C3R 108.0(2) . . ?
C1R C2R Mo1 73.74(12) . . ?
C3R C2R Mo1 72.24(13) . . ?
C4R C3R C2R 107.9(2) . . ?
C4R C3R Mo1 74.25(14) . . ?
C2R C3R Mo1 71.82(13) . . ?
C5R C4R C3R 107.8(2) . . ?
C5R C4R Mo1 73.39(13) . . ?
C3R C4R Mo1 70.35(13) . . ?
C4R C5R C1R 108.8(2) . . ?
C4R C5R Mo1 72.06(13) . . ?
C1R C5R Mo1 71.18(12) . . ?
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
Mo1 C2O 1.997(2) . ?
Mo1 C3O 2.002(2) . ?
Mo1 C1O 2.004(2) . ?
Mo1 C2 2.252(2) . ?
Mo1 C2R 2.297(2) . ?
Mo1 C3R 2.302(2) . ?
Mo1 C1R 2.336(2) . ?
Mo1 C4R 2.353(2) . ?
Mo1 C5R 2.370(2) . ?
C1 C2 1.305(3) . ?
C1 F2 1.327(3) . ?
C1 F1 1.341(3) . ?
C2 C3 1.495(3) . ?
C3 F4 1.360(3) . ?
C3 F3 1.378(3) . ?
C1O O1 1.139(3) . ?
C2O O2 1.140(3) . ?
C3O O3 1.138(3) . ?
C1R C5R 1.415(3) . ?
C1R C2R 1.413(3) . ?
C2R C3R 1.419(3) . ?
C3R C4R 1.416(3) . ?
C4R C5R 1.402(4) . ?
