#------------------------------------------------------------------------------
#$Date: 2016-03-26 21:17:49 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180472 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/41/7214125.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_7214125
loop_
_publ_author_name
'Hernández, José G.'
'Macdonald, Neil A. J.'
'Mottillo, Cristina'
'Butler, Ian S.'
'Friščić, Tomislav'
_publ_section_title
;
 A mechanochemical strategy for oxidative addition: remarkable yields and
 stereoselectivity in the halogenation of organometallic Re(i) complexes
;
_journal_issue                   3
_journal_name_full               'Green Chemistry'
_journal_page_first              1087
_journal_paper_doi               10.1039/c3gc42104j
_journal_volume                  16
_journal_year                    2014
_chemical_formula_moiety         'C7 H5 I2 O2 Re'
_chemical_formula_sum            'C7 H5 I2 O2 Re'
_chemical_formula_weight         561.11
_chemical_name_common            dia-CpRe(CO)2I2
_chemical_name_systematic
;
 dia-cyclopentadienyldiiododicarbonyl Re(III)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 107.669(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.389(5)
_cell_length_b                   9.290(4)
_cell_length_c                   9.128(4)
_cell_measurement_reflns_used    1680
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.24
_cell_measurement_theta_min      2.71
_cell_volume                     1081.8(8)
_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-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXL-2013 (Sheldrickm 2013)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0620
_diffrn_reflns_av_unetI/netI     0.0632
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            3268
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.343
_diffrn_reflns_theta_min         2.342
_exptl_absorpt_coefficient_mu    16.901
_exptl_absorpt_correction_T_max  0.03
_exptl_absorpt_correction_T_min  0.002
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Blessing, 1995)'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    3.445
_exptl_crystal_description       Plates
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.075
_refine_diff_density_min         -1.740
_refine_diff_density_rms         0.261
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     61
_refine_ls_number_reflns         1047
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0479
_refine_ls_R_factor_gt           0.0414
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0574P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1020
_refine_ls_wR_factor_ref         0.1076
_reflns_Friedel_coverage         0.000
_reflns_number_gt                915
_reflns_number_total             1047
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c3gc42104j.txt
_cod_data_source_block           dia-CpRe(CO)2I2
_cod_database_code               7214125
#BEGIN Tags that were not found in dictionaries:
_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.
;
_shelxl_version_number           2013-4
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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
Re1 Re 0.23217(4) 0.5000 0.23767(6) 0.0376(2) Uani 1 2 d S T P
I1 I 0.17540(12) 0.5000 -0.08024(11) 0.0699(4) Uani 1 2 d S T P
I2 I 0.13664(12) 0.5000 0.46692(14) 0.0798(5) Uani 1 2 d S T P
O1 O 0.0912(7) 0.2321(10) 0.1598(10) 0.076(3) Uani 1 1 d . . .
C1 C 0.1378(9) 0.3320(12) 0.1839(12) 0.051(3) Uani 1 1 d . . .
C3A C 0.3937(18) 0.5000 0.201(3) 0.117(11) Uani 1 2 d S T P
H3A H 0.4026 0.5000 0.1040 0.140 Uiso 1 2 calc R U P
C4A C 0.3854(10) 0.3805(16) 0.290(2) 0.105(7) Uani 1 1 d . . .
H4A H 0.3866 0.2844 0.2622 0.126 Uiso 1 1 calc R U .
C5A C 0.3755(13) 0.4298(15) 0.4232(19) 0.098(5) Uani 1 1 d . . .
H5A H 0.3695 0.3723 0.5035 0.117 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'
I I -0.4742 1.8119 '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'
Re Re -1.0185 7.2310 '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
C1 Re1 C1 104.5(6) 6_565 .
C1 Re1 C5A 107.2(5) 6_565 6_565
C1 Re1 C5A 139.1(5) . 6_565
C1 Re1 C5A 139.1(5) 6_565 .
C1 Re1 C5A 107.2(5) . .
C5A Re1 C5A 33.9(8) 6_565 .
C1 Re1 C4A 97.8(5) 6_565 6_565
C1 Re1 C4A 156.3(5) . 6_565
C5A Re1 C4A 34.8(6) 6_565 6_565
C5A Re1 C4A 57.7(6) . 6_565
C1 Re1 C4A 156.3(5) 6_565 .
C1 Re1 C4A 97.8(5) . .
C5A Re1 C4A 57.7(6) 6_565 .
C5A Re1 C4A 34.8(6) . .
C4A Re1 C4A 59.0(7) 6_565 .
C1 Re1 C3A 121.7(4) 6_565 .
C1 Re1 C3A 121.7(4) . .
C5A Re1 C3A 58.6(7) 6_565 .
C5A Re1 C3A 58.6(7) . .
C4A Re1 C3A 35.9(5) 6_565 .
C4A Re1 C3A 35.9(5) . .
C1 Re1 I2 77.3(3) 6_565 .
C1 Re1 I2 77.3(3) . .
C5A Re1 I2 85.1(5) 6_565 .
C5A Re1 I2 85.1(5) . .
C4A Re1 I2 116.1(5) 6_565 .
C4A Re1 I2 116.1(5) . .
C3A Re1 I2 141.8(6) . .
C1 Re1 I1 77.8(3) 6_565 .
C1 Re1 I1 77.8(3) . .
C5A Re1 I1 133.9(5) 6_565 .
C5A Re1 I1 133.9(5) . .
C4A Re1 I1 99.5(5) 6_565 .
C4A Re1 I1 99.5(5) . .
C3A Re1 I1 79.5(6) . .
I2 Re1 I1 138.67(5) . .
O1 C1 Re1 174.8(11) . .
C4A C3A C4A 105(2) 6_565 .
C4A C3A Re1 70.8(10) 6_565 .
C4A C3A Re1 70.8(10) . .
C4A C3A H3A 127.5 6_565 .
C4A C3A H3A 127.5 . .
Re1 C3A H3A 122.7 . .
C5A C4A C3A 107.6(14) . .
C5A C4A Re1 72.0(9) . .
C3A C4A Re1 73.3(11) . .
C5A C4A H4A 126.2 . .
C3A C4A H4A 126.2 . .
Re1 C4A H4A 120.3 . .
C5A C5A C4A 110.0(10) 6_565 .
C5A C5A Re1 73.0(4) 6_565 .
C4A C5A Re1 73.3(9) . .
C5A C5A H5A 125.0 6_565 .
C4A C5A H5A 125.0 . .
Re1 C5A H5A 120.3 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Re1 C1 1.974(11) 6_565
Re1 C1 1.974(11) .
Re1 C5A 2.237(14) 6_565
Re1 C5A 2.237(14) .
Re1 C4A 2.253(14) 6_565
Re1 C4A 2.253(14) .
Re1 C3A 2.29(2) .
Re1 I2 2.7640(15) .
Re1 I1 2.7676(16) .
O1 C1 1.102(13) .
C3A C4A 1.40(2) 6_565
C3A C4A 1.40(2) .
C3A H3A 0.9300 .
C4A C5A 1.34(3) .
C4A H4A 0.9300 .
C5A C5A 1.30(3) 6_565
C5A H5A 0.9300 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
C4A C3A C4A C5A -1(2) 6_565 .
Re1 C3A C4A C5A -64.3(12) . .
C4A C3A C4A Re1 63.0(14) 6_565 .
C3A C4A C5A C5A 0.8(15) . 6_565
Re1 C4A C5A C5A -64.3(4) . 6_565
C3A C4A C5A Re1 65.2(14) . .
