#------------------------------------------------------------------------------
#$Date: 2016-03-23 04:09:31 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179278 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/98/4319878.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_4319878
loop_
_publ_author_name
'Yi Han'
'C. Jeff Harlan'
'Philipp Stoessel'
'Brian J. Frost'
'Jack R. Norton'
'Susie Miller'
'Brian Bridgewater'
'Qiang Xu'
_publ_section_title
;
 Rhenium Oxo Complexes of a Chelating Diyne Ligand. Synthesis and Study of
 the Kinetics of Protonation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2942
_journal_page_last               2952
_journal_paper_doi               10.1021/ic0100931
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C12 H21 I O P Re'
_chemical_formula_weight         525.36
_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                 94.068(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.9812(16)
_cell_length_b                   18.417(3)
_cell_length_c                   9.7160(17)
_cell_measurement_temperature    228(2)
_cell_volume                     1603.0(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      228(2)
_diffrn_measured_fraction_theta_full 0.929
_diffrn_measured_fraction_theta_max 0.929
_diffrn_measurement_device_type  'CCD area 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  0.0265
_diffrn_reflns_av_sigmaI/netI    0.0272
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            11017
_diffrn_reflns_theta_full        28.13
_diffrn_reflns_theta_max         28.13
_diffrn_reflns_theta_min         2.21
_exptl_absorpt_coefficient_mu    9.588
_exptl_absorpt_correction_T_max  0.6457
_exptl_absorpt_correction_T_min  0.4473
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    2.177
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.872
_refine_diff_density_min         -0.526
_refine_diff_density_rms         0.106
_refine_ls_extinction_coef       0.00083(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     151
_refine_ls_number_reflns         3638
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0301
_refine_ls_R_factor_gt           0.0219
_refine_ls_shift/su_max          0.768
_refine_ls_shift/su_mean         0.018
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0171P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0415
_refine_ls_wR_factor_ref         0.0428
_reflns_number_gt                3114
_reflns_number_total             3638
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0100931_5.cif
_cod_data_source_block           jeps10
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4319878
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
Re Re 1.243546(16) 0.432947(8) 1.948283(13) 0.02735(6) Uani 1 1 d . . .
I I 0.67528(3) 0.323126(16) 1.40926(3) 0.04878(9) Uani 1 1 d . . .
P P 1.32216(12) 0.41933(5) 1.71711(9) 0.0335(2) Uani 1 1 d . . .
O O 1.2666(3) 0.52137(14) 1.9962(3) 0.0423(7) Uani 1 1 d . . .
C1 C 1.5528(5) 0.3221(2) 1.9754(5) 0.0484(11) Uani 1 1 d . . .
H1A H 1.6205 0.3191 2.0575 0.073 Uiso 1 1 calc R . .
H1B H 1.6011 0.3477 1.9035 0.073 Uiso 1 1 calc R . .
H1C H 1.5262 0.2735 1.9439 0.073 Uiso 1 1 calc R . .
C2 C 1.4159(4) 0.36187(19) 2.0078(4) 0.0345(9) Uani 1 1 d . . .
C3 C 1.3180(4) 0.3634(2) 2.0980(4) 0.0356(9) Uani 1 1 d . . .
C4 C 1.2543(5) 0.3341(2) 2.2228(4) 0.0505(11) Uani 1 1 d . . .
H4A H 1.3252 0.3423 2.3027 0.061 Uiso 1 1 calc R . .
H4B H 1.2407 0.2815 2.2121 0.061 Uiso 1 1 calc R . .
C5 C 1.1063(5) 0.3684(3) 2.2500(4) 0.0509(11) Uani 1 1 d . . .
H5A H 1.1219 0.4200 2.2707 0.061 Uiso 1 1 calc R . .
H5B H 1.0676 0.3455 2.3312 0.061 Uiso 1 1 calc R . .
C6 C 0.9912(5) 0.3609(2) 2.1282(4) 0.0470(10) Uani 1 1 d . . .
H6A H 0.9662 0.3095 2.1144 0.056 Uiso 1 1 calc R . .
H6B H 0.8999 0.3867 2.1487 0.056 Uiso 1 1 calc R . .
C7 C 1.0472(4) 0.39084(19) 1.9990(4) 0.0333(8) Uani 1 1 d . . .
C8 C 1.0339(4) 0.4004(2) 1.8684(4) 0.0355(9) Uani 1 1 d . . .
C9 C 0.9264(5) 0.3844(3) 1.7479(4) 0.0601(13) Uani 1 1 d . . .
H9A H 0.9745 0.3541 1.6826 0.090 Uiso 1 1 calc R . .
H9B H 0.8947 0.4296 1.7035 0.090 Uiso 1 1 calc R . .
H9C H 0.8401 0.3593 1.7793 0.090 Uiso 1 1 calc R . .
C11 C 1.3261(6) 0.3274(2) 1.6546(4) 0.0530(12) Uani 1 1 d . . .
H11A H 1.3717 0.3264 1.5670 0.080 Uiso 1 1 calc R . .
H11B H 1.2250 0.3088 1.6422 0.080 Uiso 1 1 calc R . .
H11C H 1.3838 0.2974 1.7210 0.080 Uiso 1 1 calc R . .
C12 C 1.5046(5) 0.4584(2) 1.7064(4) 0.0471(10) Uani 1 1 d . . .
H12A H 1.5704 0.4413 1.7830 0.071 Uiso 1 1 calc R . .
H12B H 1.4974 0.5109 1.7102 0.071 Uiso 1 1 calc R . .
H12C H 1.5443 0.4441 1.6202 0.071 Uiso 1 1 calc R . .
C13 C 1.2103(5) 0.4696(3) 1.5872(4) 0.0538(12) Uani 1 1 d . . .
H13A H 1.2033 0.5199 1.6157 0.081 Uiso 1 1 calc R . .
H13B H 1.1110 0.4487 1.5763 0.081 Uiso 1 1 calc R . .
H13C H 1.2565 0.4672 1.5001 0.081 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'
P P 0.1023 0.0942 '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'
I I -0.4742 1.8119 '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
O Re C3 112.49(14) . . ?
O Re C7 113.08(14) . . ?
C3 Re C7 80.24(15) . . ?
O Re C8 117.96(14) . . ?
C3 Re C8 109.38(16) . . ?
C7 Re C8 36.37(14) . . ?
O Re C2 116.91(14) . . ?
C3 Re C2 36.56(15) . . ?
C7 Re C2 109.66(15) . . ?
C8 Re C2 124.10(15) . . ?
O Re P 108.41(10) . . ?
C3 Re P 120.09(11) . . ?
C7 Re P 120.35(11) . . ?
C8 Re P 86.54(11) . . ?
C2 Re P 86.11(11) . . ?
C12 P C11 108.5(2) . . ?
C12 P C13 102.6(2) . . ?
C11 P C13 105.6(2) . . ?
C12 P Re 109.86(14) . . ?
C11 P Re 115.18(14) . . ?
C13 P Re 114.25(16) . . ?
C3 C2 C1 140.6(4) . . ?
C3 C2 Re 69.1(2) . . ?
C1 C2 Re 149.8(3) . . ?
C2 C3 C4 150.9(4) . . ?
C2 C3 Re 74.3(2) . . ?
C4 C3 Re 134.1(3) . . ?
C3 C4 C5 112.7(3) . . ?
C4 C5 C6 112.6(3) . . ?
C7 C6 C5 111.7(3) . . ?
C8 C7 C6 150.8(4) . . ?
C8 C7 Re 74.1(2) . . ?
C6 C7 Re 134.5(3) . . ?
C7 C8 C9 139.6(4) . . ?
C7 C8 Re 69.5(2) . . ?
C9 C8 Re 150.4(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
Re O 1.702(2) . ?
Re C3 2.016(4) . ?
Re C7 2.019(4) . ?
Re C8 2.074(4) . ?
Re C2 2.078(4) . ?
Re P 2.4148(10) . ?
P C12 1.799(4) . ?
P C11 1.801(4) . ?
P C13 1.811(4) . ?
C1 C2 1.484(5) . ?
C2 C3 1.285(5) . ?
C3 C4 1.479(5) . ?
C4 C5 1.512(6) . ?
C5 C6 1.521(5) . ?
C6 C7 1.490(5) . ?
C7 C8 1.278(5) . ?
C8 C9 1.493(5) . ?
