#------------------------------------------------------------------------------
#$Date: 2016-03-25 08:57:24 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179712 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/14/7001458.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_7001458
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 H8 F2 Mo O3'
_chemical_formula_sum            'C11 H8 F2 Mo O3'
_chemical_formula_weight         322.11
_chemical_name_common
;Cyclopentadienyl(2,2-difluoro-1-
methylvinyl)tricarbonylmolybdenum
;
_chemical_name_systematic
;
Cyclopentadienyl(2,2-difluoro-1-methylvinyl)tricarbonylmolybdenum
;
_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                 95.309(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.084(2)
_cell_length_b                   8.951(2)
_cell_length_c                   11.548(2)
_cell_measurement_reflns_used    806
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.12
_cell_measurement_theta_min      2.67
_cell_volume                     1140.8(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 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     0.71069
_diffrn_reflns_av_R_equivalents  0.0226
_diffrn_reflns_av_sigmaI/netI    0.0339
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7686
_diffrn_reflns_theta_full        30.49
_diffrn_reflns_theta_max         30.49
_diffrn_reflns_theta_min         2.44
_exptl_absorpt_coefficient_mu    1.168
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker-AXS)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.875
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.889
_refine_diff_density_min         -0.450
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         3439
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_gt           0.0272
_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)+(0.0264P)²+0.5270P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0568
_refine_ls_wR_factor_ref         0.0636
_reflns_number_gt                2625
_reflns_number_total             3439
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b903300a.txt
_cod_data_source_block           mo13m
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7001458
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 0.723381(17) 0.29097(2) 0.467649(16) 0.02143(6) Uani 1 1 d . . .
F1 F 0.93239(17) 0.4182(2) 0.80177(15) 0.0584(5) Uani 1 1 d . . .
F2 F 0.96707(16) 0.4472(3) 0.62339(17) 0.0635(6) Uani 1 1 d . . .
O3 O 0.78387(19) 0.6341(2) 0.47324(17) 0.0439(5) Uani 1 1 d . . .
C3O C 0.7598(2) 0.5100(3) 0.4741(2) 0.0303(5) Uani 1 1 d . . .
O1 O 0.47528(19) 0.2272(3) 0.5680(2) 0.0601(6) Uani 1 1 d . . .
C2 C 0.7796(3) 0.3357(3) 0.6576(2) 0.0337(6) Uani 1 1 d . . .
O2 O 0.5236(2) 0.4207(3) 0.2844(2) 0.0576(6) Uani 1 1 d . . .
C1R C 0.7665(3) 0.0342(3) 0.4521(3) 0.0415(7) Uani 1 1 d . . .
H1R H 0.7217 -0.0385 0.4865 0.050 Uiso 1 1 calc R . .
C5R C 0.8720(3) 0.1021(3) 0.5023(3) 0.0444(7) Uani 1 1 d . . .
H5R H 0.9093 0.0828 0.5763 0.053 Uiso 1 1 calc R . .
C2R C 0.7400(3) 0.0948(3) 0.3404(2) 0.0414(7) Uani 1 1 d . . .
H2R H 0.6740 0.0701 0.2883 0.050 Uiso 1 1 calc R . .
C4R C 0.9125(2) 0.2048(4) 0.4219(3) 0.0465(8) Uani 1 1 d . . .
H4R H 0.9808 0.2651 0.4335 0.056 Uiso 1 1 calc R . .
C1 C 0.8844(3) 0.3959(3) 0.6898(2) 0.0412(7) Uani 1 1 d . . .
C3R C 0.8314(3) 0.2001(4) 0.3212(3) 0.0455(7) Uani 1 1 d . . .
H3R H 0.8367 0.2560 0.2540 0.055 Uiso 1 1 calc R . .
C1O C 0.5672(3) 0.2551(3) 0.5357(2) 0.0387(6) Uani 1 1 d . . .
C2O C 0.5974(3) 0.3748(3) 0.3509(2) 0.0380(6) Uani 1 1 d . . .
C3 C 0.7069(3) 0.2853(4) 0.7549(2) 0.0598(10) Uani 1 1 d . . .
H3 H 0.7535 0.3004 0.8282 0.090 Uiso 1 1 calc R . .
H2 H 0.6877 0.1812 0.7454 0.090 Uiso 1 1 calc R . .
H1 H 0.6334 0.3422 0.7528 0.090 Uiso 1 1 calc R . .
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
C1O Mo1 C2O 75.40(12) . . ?
C1O Mo1 C3O 108.83(11) . . ?
C2O Mo1 C3O 77.48(11) . . ?
C1O Mo1 C2 79.48(11) . . ?
C2O Mo1 C2 134.60(11) . . ?
C3O Mo1 C2 75.74(10) . . ?
C1O Mo1 C2R 104.59(11) . . ?
C2O Mo1 C2R 87.02(11) . . ?
C3O Mo1 C2R 137.84(10) . . ?
C2 Mo1 C2R 136.19(10) . . ?
C1O Mo1 C3R 139.51(12) . . ?
C2O Mo1 C3R 90.89(12) . . ?
C3O Mo1 C3R 104.84(11) . . ?
C2 Mo1 C3R 131.16(11) . . ?
C2R Mo1 C3R 35.72(11) . . ?
C1O Mo1 C4R 149.93(12) . . ?
C2O Mo1 C4R 123.84(12) . . ?
C3O Mo1 C4R 98.59(11) . . ?
C2 Mo1 C4R 96.04(11) . . ?
C2R Mo1 C4R 58.63(11) . . ?
C3R Mo1 C4R 35.12(11) . . ?
C1O Mo1 C1R 93.60(11) . . ?
C2O Mo1 C1R 116.69(11) . . ?
C3O Mo1 C1R 156.34(10) . . ?
C2 Mo1 C1R 101.94(10) . . ?
C2R Mo1 C1R 35.03(10) . . ?
C3R Mo1 C1R 58.53(10) . . ?
C4R Mo1 C1R 57.94(11) . . ?
C1O Mo1 C5R 115.74(12) . . ?
C2O Mo1 C5R 144.57(11) . . ?
C3O Mo1 C5R 123.93(11) . . ?
C2 Mo1 C5R 80.63(10) . . ?
C2R Mo1 C5R 57.95(10) . . ?
C3R Mo1 C5R 58.17(11) . . ?
C4R Mo1 C5R 34.85(11) . . ?
C1R Mo1 C5R 34.33(10) . . ?
O3 C3O Mo1 176.6(2) . . ?
C1 C2 C3 115.7(3) . . ?
C1 C2 Mo1 120.6(2) . . ?
C3 C2 Mo1 123.4(2) . . ?
C5R C1R C2R 108.0(3) . . ?
C5R C1R Mo1 73.25(16) . . ?
C2R C1R Mo1 70.53(16) . . ?
C1R C5R C4R 108.4(3) . . ?
C1R C5R Mo1 72.42(16) . . ?
C4R C5R Mo1 71.42(16) . . ?
C1R C2R C3R 108.0(3) . . ?
C1R C2R Mo1 74.45(16) . . ?
C3R C2R Mo1 72.16(15) . . ?
C3R C4R C5R 107.9(3) . . ?
C3R C4R Mo1 71.25(15) . . ?
C5R C4R Mo1 73.73(15) . . ?
C2 C1 F2 128.5(3) . . ?
C2 C1 F1 126.1(3) . . ?
F2 C1 F1 105.4(2) . . ?
C4R C3R C2R 107.7(3) . . ?
C4R C3R Mo1 73.63(15) . . ?
C2R C3R Mo1 72.12(15) . . ?
O1 C1O Mo1 174.8(3) . . ?
O2 C2O Mo1 178.7(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
Mo1 C1O 1.993(3) . ?
Mo1 C2O 1.996(3) . ?
Mo1 C3O 2.002(3) . ?
Mo1 C2 2.260(3) . ?
Mo1 C2R 2.308(3) . ?
Mo1 C3R 2.308(3) . ?
Mo1 C4R 2.339(3) . ?
Mo1 C1R 2.358(3) . ?
Mo1 C5R 2.369(3) . ?
F1 C1 1.367(3) . ?
F2 C1 1.330(3) . ?
O3 C3O 1.142(3) . ?
O1 C1O 1.144(3) . ?
C2 C1 1.302(4) . ?
C2 C3 1.510(4) . ?
O2 C2O 1.146(3) . ?
C1R C5R 1.395(4) . ?
C1R C2R 1.405(4) . ?
C5R C4R 1.410(4) . ?
C2R C3R 1.416(4) . ?
C4R C3R 1.402(5) . ?
