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#$Date: 2022-04-06 02:09:10 +0300 (Wed, 06 Apr 2022) $
#$Revision: 274364 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/99/7709929.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_7709929
loop_
_publ_author_name
'González-López, Vianney'
'Resendiz-Lara, Diego'
'Rosas-Sánchez, Alfredo'
'Ledesma-Olvera, Lydia G.'
'Daran, Jean-Claude'
'Barquera-Lozada, Jose Enrique'
'López-Cortés, Jose G.'
'Ortega-Alfaro, M. Carmen'
_publ_section_title
;
 Iodine-promoted insertion of the oxygen atom from water in
 η4-vinylketene[Fe(CO)3] complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00674J
_journal_year                    2022
_chemical_formula_moiety         'C19 H11 Cl Fe O4'
_chemical_formula_sum            'C19 H11 Cl Fe O4'
_chemical_formula_weight         394.58
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2021-02-04 deposited with the CCDC.	2022-04-05 downloaded from the CCDC.
;
_cell_angle_alpha                104.201(2)
_cell_angle_beta                 98.461(2)
_cell_angle_gamma                95.747(2)
_cell_formula_units_Z            2
_cell_length_a                   6.5931(2)
_cell_length_b                   8.5797(2)
_cell_length_c                   15.3443(4)
_cell_measurement_reflns_used    15193
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.2890
_cell_measurement_theta_min      3.9110
_cell_volume                     823.85(4)
_computing_cell_refinement       CrysAlisPro
_computing_data_collection
'CrysAlisPro (Rigaku Oxford Diffraction, 2016)'
_computing_data_reduction        CrysAlisPro
_computing_molecular_graphics
'ORTEPIII (Burnett & Johnson, 1996); ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  SHELXL-2015
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXt (Sheldrick, 2015)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1978
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_av_unetI/netI     0.0155
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            33334
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.400
_diffrn_reflns_theta_max         26.369
_diffrn_reflns_theta_min         3.143
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.102
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.732
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
CrysAlisPro (Rigaku Oxford Diffraction, 2015)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.591
_exptl_crystal_description       box
_exptl_crystal_F_000             400
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.514
_refine_diff_density_min         -0.527
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         3369
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0349
_refine_ls_R_factor_gt           0.0325
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0479P)²+0.6642P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0894
_refine_ls_wR_factor_ref         0.0920
_reflns_number_gt                3181
_reflns_number_total             3369
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2dt00674j2.cif
_cod_data_source_block           3g
_cod_database_code               7709929
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.609
_shelx_estimated_absorpt_t_max   0.898
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe Fe 0.55721(4) 0.48999(3) 0.77418(2) 0.02326(11) Uani 1 1 d . . . . .
Cl1 Cl -0.25150(10) 0.02710(7) 0.37651(4) 0.04297(16) Uani 1 1 d . . . . .
O11 O 0.7641(3) 0.5702(2) 0.96492(12) 0.0490(5) Uani 1 1 d . . . . .
O12 O 0.1571(3) 0.3649(3) 0.81767(13) 0.0506(5) Uani 1 1 d . . . . .
O13 O 0.7140(3) 0.1819(2) 0.70910(13) 0.0427(4) Uani 1 1 d . . . . .
O1 O 0.9554(3) 0.6708(2) 0.75886(14) 0.0471(4) Uani 1 1 d . . . . .
C1 C 0.4452(3) 0.4941(2) 0.63325(13) 0.0250(4) Uani 1 1 d . . . . .
H1 H 0.581768 0.470498 0.629146 0.030 Uiso 1 1 calc R U . . .
C2 C 0.4209(3) 0.6367(2) 0.69786(13) 0.0245(4) Uani 1 1 d . . . . .
H2 H 0.288334 0.670217 0.700171 0.029 Uiso 1 1 calc R U . . .
C3 C 0.5980(3) 0.7282(2) 0.75885(14) 0.0261(4) Uani 1 1 d . . . . .
C4 C 0.7748(3) 0.6415(2) 0.75541(14) 0.0241(4) Uani 1 1 d . . . . .
C11 C 0.6803(3) 0.5367(2) 0.89109(15) 0.0310(4) Uani 1 1 d . . . . .
C12 C 0.3065(3) 0.4129(3) 0.79912(15) 0.0335(5) Uani 1 1 d . . . . .
C13 C 0.6518(3) 0.2998(3) 0.73488(14) 0.0286(4) Uani 1 1 d . . . . .
C31 C 0.6039(3) 0.8850(2) 0.82732(14) 0.0279(4) Uani 1 1 d . . . . .
C32 C 0.4236(4) 0.9476(3) 0.84589(15) 0.0328(5) Uani 1 1 d . . . . .
H32 H 0.292905 0.888623 0.814366 0.039 Uiso 1 1 calc R U . . .
C33 C 0.4321(4) 1.0947(3) 0.90972(16) 0.0392(5) Uani 1 1 d . . . . .
H33 H 0.307591 1.136127 0.921370 0.047 Uiso 1 1 calc R U . . .
C34 C 0.6206(4) 1.1812(3) 0.95640(17) 0.0436(6) Uani 1 1 d . . . . .
H34 H 0.626402 1.281561 1.000648 0.052 Uiso 1 1 calc R U . . .
C35 C 0.7995(5) 1.1214(3) 0.9385(2) 0.0540(7) Uani 1 1 d . . . . .
H35 H 0.929523 1.181166 0.970294 0.065 Uiso 1 1 calc R U . . .
C36 C 0.7930(4) 0.9741(3) 0.87429(19) 0.0452(6) Uani 1 1 d . . . . .
H36 H 0.918286 0.934313 0.862488 0.054 Uiso 1 1 calc R U . . .
C111 C 0.2707(3) 0.3796(2) 0.57179(13) 0.0241(4) Uani 1 1 d . . . . .
C112 C 0.3061(3) 0.2771(3) 0.49167(14) 0.0283(4) Uani 1 1 d . . . . .
H112 H 0.442608 0.281338 0.478543 0.034 Uiso 1 1 calc R U . . .
C113 C 0.1480(4) 0.1692(3) 0.43045(14) 0.0322(5) Uani 1 1 d . . . . .
H113 H 0.174760 0.101250 0.375614 0.039 Uiso 1 1 calc R U . . .
C114 C -0.0492(3) 0.1624(2) 0.45081(14) 0.0295(4) Uani 1 1 d . . . . .
C115 C -0.0902(3) 0.2614(3) 0.53008(15) 0.0337(5) Uani 1 1 d . . . . .
H115 H -0.226641 0.254779 0.543298 0.040 Uiso 1 1 calc R U . . .
C116 C 0.0689(3) 0.3704(3) 0.59018(14) 0.0297(4) Uani 1 1 d . . . . .
H116 H 0.040586 0.439504 0.644329 0.036 Uiso 1 1 calc R U . . .
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'
Fe Fe 0.3463 0.8444 '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'
Cl Cl 0.1484 0.1585 '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
C11 Fe C13 97.80(10) . . ?
C11 Fe C12 92.71(10) . . ?
C13 Fe C12 99.31(10) . . ?
C11 Fe C4 88.06(9) . . ?
C13 Fe C4 101.05(9) . . ?
C12 Fe C4 159.34(10) . . ?
C11 Fe C2 130.88(9) . . ?
C13 Fe C2 129.18(9) . . ?
C12 Fe C2 92.79(9) . . ?
C4 Fe C2 71.48(8) . . ?
C11 Fe C3 97.33(9) . . ?
C13 Fe C3 138.71(9) . . ?
C12 Fe C3 118.07(9) . . ?
C4 Fe C3 41.54(8) . . ?
C2 Fe C3 39.16(8) . . ?
C11 Fe C1 165.51(9) . . ?
C13 Fe C1 90.94(9) . . ?
C12 Fe C1 97.27(8) . . ?
C4 Fe C1 78.90(8) . . ?
C2 Fe C1 38.41(8) . . ?
C3 Fe C1 68.70(8) . . ?
C2 C1 C111 123.80(18) . . ?
C2 C1 Fe 67.30(11) . . ?
C111 C1 Fe 123.95(13) . . ?
C2 C1 H1 118.1 . . ?
C111 C1 H1 118.1 . . ?
Fe C1 H1 79.4 . . ?
C3 C2 C1 118.51(18) . . ?
C3 C2 Fe 70.84(11) . . ?
C1 C2 Fe 74.29(12) . . ?
C3 C2 H2 120.7 . . ?
C1 C2 H2 120.7 . . ?
Fe C2 H2 125.9 . . ?
C2 C3 C4 111.65(18) . . ?
C2 C3 C31 125.95(18) . . ?
C4 C3 C31 122.00(18) . . ?
C2 C3 Fe 69.99(11) . . ?
C4 C3 Fe 62.92(11) . . ?
C31 C3 Fe 129.25(14) . . ?
O1 C4 C3 138.1(2) . . ?
O1 C4 Fe 144.52(18) . . ?
C3 C4 Fe 75.54(11) . . ?
O11 C11 Fe 177.5(2) . . ?
O12 C12 Fe 177.2(2) . . ?
O13 C13 Fe 178.4(2) . . ?
C36 C31 C32 118.3(2) . . ?
C36 C31 C3 120.0(2) . . ?
C32 C31 C3 121.67(19) . . ?
C33 C32 C31 120.9(2) . . ?
C33 C32 H32 119.6 . . ?
C31 C32 H32 119.6 . . ?
C34 C33 C32 120.2(2) . . ?
C34 C33 H33 119.9 . . ?
C32 C33 H33 119.9 . . ?
C35 C34 C33 119.5(2) . . ?
C35 C34 H34 120.3 . . ?
C33 C34 H34 120.3 . . ?
C34 C35 C36 120.8(2) . . ?
C34 C35 H35 119.6 . . ?
C36 C35 H35 119.6 . . ?
C35 C36 C31 120.3(2) . . ?
C35 C36 H36 119.9 . . ?
C31 C36 H36 119.9 . . ?
C112 C111 C116 118.12(19) . . ?
C112 C111 C1 119.19(18) . . ?
C116 C111 C1 122.69(18) . . ?
C113 C112 C111 121.9(2) . . ?
C113 C112 H112 119.1 . . ?
C111 C112 H112 119.1 . . ?
C114 C113 C112 118.6(2) . . ?
C114 C113 H113 120.7 . . ?
C112 C113 H113 120.7 . . ?
C113 C114 C115 121.22(19) . . ?
C113 C114 Cl1 120.10(17) . . ?
C115 C114 Cl1 118.68(17) . . ?
C114 C115 C116 119.6(2) . . ?
C114 C115 H115 120.2 . . ?
C116 C115 H115 120.2 . . ?
C115 C116 C111 120.6(2) . . ?
C115 C116 H116 119.7 . . ?
C111 C116 H116 119.7 . . ?
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
Fe C11 1.786(2) . ?
Fe C13 1.802(2) . ?
Fe C12 1.846(2) . ?
Fe C4 1.9397(19) . ?
Fe C2 2.0985(19) . ?
Fe C3 2.110(2) . ?
Fe C1 2.190(2) . ?
Cl1 C114 1.738(2) . ?
O11 C11 1.138(3) . ?
O12 C12 1.132(3) . ?
O13 C13 1.132(3) . ?
O1 C4 1.183(3) . ?
C1 C2 1.413(3) . ?
C1 C111 1.476(3) . ?
C1 H1 0.9500 . ?
C2 C3 1.410(3) . ?
C2 H2 0.9500 . ?
C3 C4 1.445(3) . ?
C3 C31 1.483(3) . ?
C31 C36 1.390(3) . ?
C31 C32 1.391(3) . ?
C32 C33 1.385(3) . ?
C32 H32 0.9500 . ?
C33 C34 1.379(4) . ?
C33 H33 0.9500 . ?
C34 C35 1.370(4) . ?
C34 H34 0.9500 . ?
C35 C36 1.390(4) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C111 C112 1.391(3) . ?
C111 C116 1.399(3) . ?
C112 C113 1.385(3) . ?
C112 H112 0.9500 . ?
C113 C114 1.380(3) . ?
C113 H113 0.9500 . ?
C114 C115 1.382(3) . ?
C115 C116 1.386(3) . ?
C115 H115 0.9500 . ?
C116 H116 0.9500 . ?
