#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:32:58 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179850 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/46/7014606.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_7014606
loop_
_publ_author_name
'Huang, Hui'
'Hughes, Russell P.'
'Rheingold, Arnold L.'
_publ_section_title
;
 Synthesis and structural characterization of group 6 transition metal
 complexes with terminal fluoromethylidyne (CF) ligands; a DFT/NBO/NRT
 comparison of bonding characteristics of terminal NO, CF and CH
 ligands.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              47
_journal_page_last               55
_journal_paper_doi               10.1039/c0dt01006e
_journal_volume                  40
_journal_year                    2011
_chemical_formula_sum            'C8 H5 F O2 W'
_chemical_formula_weight         335.97
_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                 95.3340(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   5.8048(4)
_cell_length_b                   19.8293(12)
_cell_length_c                   7.0601(4)
_cell_measurement_reflns_used    289
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.23
_cell_measurement_theta_min      5.35
_cell_volume                     809.13(9)
_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, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.932
_diffrn_measurement_device_type  'CCD detector'
_diffrn_measurement_method       'phi and omega 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  0.0238
_diffrn_reflns_av_sigmaI/netI    0.0232
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            7596
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.21
_diffrn_reflns_theta_min         2.05
_exptl_absorpt_coefficient_mu    14.243
_exptl_absorpt_correction_T_max  0.736
_exptl_absorpt_correction_T_min  0.434
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.758
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             608
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.620
_refine_diff_density_min         -1.999
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     109
_refine_ls_number_reflns         1866
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0257
_refine_ls_R_factor_gt           0.0206
_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)+(0.0080P)²+2.8153P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0371
_refine_ls_wR_factor_ref         0.0387
_reflns_number_gt                1658
_reflns_number_total             1866
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            C0DT01006E.TXT
_cod_data_source_block           rph438
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7014606
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
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C -0.1440(7) 0.4371(2) 0.7430(6) 0.0223(9) Uani 1 1 d . . .
H1 H -0.2680 0.4485 0.8112 0.027 Uiso 1 1 calc R . .
C2 C 0.0602(7) 0.4737(2) 0.7399(6) 0.0212(9) Uani 1 1 d . . .
H2 H 0.0954 0.5135 0.8060 0.025 Uiso 1 1 calc R . .
C3 C 0.2047(8) 0.4406(2) 0.6204(6) 0.0248(9) Uani 1 1 d . . .
H3 H 0.3507 0.4547 0.5931 0.030 Uiso 1 1 calc R . .
C4 C 0.0877(9) 0.3820(2) 0.5494(6) 0.0289(11) Uani 1 1 d . . .
H4 H 0.1446 0.3506 0.4676 0.035 Uiso 1 1 calc R . .
C5 C -0.1310(8) 0.3791(2) 0.6236(6) 0.0258(10) Uani 1 1 d . . .
H5 H -0.2436 0.3460 0.5996 0.031 Uiso 1 1 calc R . .
C6 C 0.3431(7) 0.2886(2) 0.8736(5) 0.0194(8) Uani 1 1 d . . .
C7 C 0.3657(7) 0.4010(2) 1.0873(5) 0.0199(9) Uani 1 1 d . . .
C8 C -0.0257(7) 0.3237(2) 1.0584(5) 0.0190(8) Uani 1 1 d . . .
O1 O 0.4594(5) 0.23819(14) 0.8686(4) 0.0307(7) Uani 0.67 1 d P A 1
F1A F 0.4594(5) 0.23819(14) 0.8686(4) 0.0307(7) Uani 0.33 1 d P A 2
O2 O 0.4985(5) 0.42168(15) 1.2175(4) 0.0327(7) Uani 0.67 1 d P A 1
F1B F 0.4985(5) 0.42168(15) 1.2175(4) 0.0327(7) Uani 0.33 1 d P A 2
F1 F -0.1453(5) 0.29653(15) 1.1649(4) 0.0314(7) Uani 0.33 1 d P A 1
O3 O -0.1453(5) 0.29653(15) 1.1649(4) 0.0314(7) Uani 0.67 1 d P A 2
W1 W 0.15746(3) 0.368731(8) 0.88166(2) 0.01924(6) Uani 1 1 d . A .
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'
W W -0.8490 6.8722 '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 C1 C5 108.5(4) . . ?
C2 C1 W1 72.9(2) . . ?
C5 C1 W1 72.8(2) . . ?
C2 C1 H1 125.7 . . ?
C5 C1 H1 125.7 . . ?
W1 C1 H1 120.4 . . ?
C1 C2 C3 108.9(4) . . ?
C1 C2 W1 72.8(2) . . ?
C3 C2 W1 73.1(2) . . ?
C1 C2 H2 125.6 . . ?
C3 C2 H2 125.6 . . ?
W1 C2 H2 120.3 . . ?
C2 C3 C4 107.6(4) . . ?
C2 C3 W1 72.2(2) . . ?
C4 C3 W1 72.3(2) . . ?
C2 C3 H3 126.2 . . ?
C4 C3 H3 126.2 . . ?
W1 C3 H3 121.1 . . ?
C3 C4 C5 108.6(4) . . ?
C3 C4 W1 72.9(2) . . ?
C5 C4 W1 72.8(2) . . ?
C3 C4 H4 125.7 . . ?
C5 C4 H4 125.7 . . ?
W1 C4 H4 120.3 . . ?
C4 C5 C1 106.4(4) . . ?
C4 C5 W1 72.2(2) . . ?
C1 C5 W1 71.9(2) . . ?
C4 C5 H5 126.8 . . ?
C1 C5 H5 126.8 . . ?
W1 C5 H5 121.0 . . ?
O1 C6 W1 179.9(4) . . ?
O2 C7 W1 179.7(4) . . ?
F1 C8 W1 178.0(3) . . ?
C7 W1 C6 89.01(17) . . ?
C7 W1 C8 90.66(17) . . ?
C6 W1 C8 88.89(17) . . ?
C7 W1 C1 121.06(16) . . ?
C6 W1 C1 149.37(15) . . ?
C8 W1 C1 95.89(16) . . ?
C7 W1 C2 97.84(16) . . ?
C6 W1 C2 146.11(16) . . ?
C8 W1 C2 123.96(16) . . ?
C1 W1 C2 34.36(14) . . ?
C7 W1 C4 139.14(17) . . ?
C6 W1 C4 96.17(15) . . ?
C8 W1 C4 129.81(17) . . ?
C1 W1 C4 57.98(15) . . ?
C2 W1 C4 57.75(14) . . ?
C7 W1 C5 155.27(16) . . ?
C6 W1 C5 114.03(16) . . ?
C8 W1 C5 98.32(16) . . ?
C1 W1 C5 35.35(15) . . ?
C2 W1 C5 58.11(14) . . ?
C4 W1 C5 34.97(16) . . ?
C7 W1 C3 106.22(16) . . ?
C6 W1 C3 111.62(16) . . ?
C8 W1 C3 153.16(16) . . ?
C1 W1 C3 57.62(15) . . ?
C2 W1 C3 34.64(15) . . ?
C4 W1 C3 34.83(15) . . ?
C5 W1 C3 58.18(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
C1 C2 1.391(6) . ?
C1 C5 1.433(6) . ?
C1 W1 2.354(4) . ?
C1 H1 0.9300 . ?
C2 C3 1.406(6) . ?
C2 W1 2.355(4) . ?
C2 H2 0.9300 . ?
C3 C4 1.414(6) . ?
C3 W1 2.367(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.419(7) . ?
C4 W1 2.358(4) . ?
C4 H4 0.9300 . ?
C5 W1 2.366(4) . ?
C5 H5 0.9300 . ?
C6 O1 1.208(5) . ?
C6 W1 1.924(4) . ?
C7 O2 1.215(5) . ?
C7 W1 1.911(4) . ?
C8 F1 1.198(5) . ?
C8 W1 1.932(4) . ?
