#------------------------------------------------------------------------------
#$Date: 2016-03-23 04:09:31 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179278 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/98/4319875.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_4319875
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            'C10 H15 O Re'
_chemical_formula_weight         337.42
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           114
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P -4 2n'
_symmetry_space_group_name_H-M   'P -4 21 c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.56890(10)
_cell_length_b                   16.56890(10)
_cell_length_c                   7.45200(10)
_cell_measurement_temperature    163(2)
_cell_volume                     2045.79(3)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      163(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       'ω 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  0.1240
_diffrn_reflns_av_sigmaI/netI    0.0733
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            9010
_diffrn_reflns_theta_max         23.22
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    11.832
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear lt. y'
_exptl_crystal_density_diffrn    2.191
_exptl_crystal_description       rectangular
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.708
_refine_diff_density_min         -2.480
_refine_diff_density_rms         0.378
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00
_refine_ls_extinction_coef       0.0035(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.087
_refine_ls_goodness_of_fit_obs   1.045
_refine_ls_matrix_type           full
_refine_ls_number_parameters     110
_refine_ls_number_reflns         1459
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.133
_refine_ls_restrained_S_obs      1.045
_refine_ls_R_factor_all          0.0511
_refine_ls_R_factor_obs          0.0349
_refine_ls_shift/esd_max         0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0156P)²+7.4015P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0681
_refine_ls_wR_factor_obs         0.0615
_reflns_number_observed          1403
_reflns_number_total             1460
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic0100931_2.cif
_cod_data_source_block           jrn1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0156P)^2^+7.4015P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0156P)^2^+7.4015P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4319875
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Re1 0.0133(2) 0.0142(2) 0.0223(3) 0.0007(2) 0.0031(2) -0.00129(12)
O1 0.027(4) 0.020(4) 0.031(5) 0.002(3) 0.007(3) -0.003(3)
C1 0.041(6) 0.016(5) 0.041(6) 0.005(6) 0.000(7) -0.009(4)
C2 0.023(5) 0.011(4) 0.031(5) 0.002(5) 0.002(6) -0.001(3)
C3 0.011(5) 0.016(5) 0.033(6) -0.002(4) 0.007(4) 0.002(4)
C4 0.025(5) 0.021(5) 0.033(7) -0.002(5) -0.010(5) 0.010(4)
C5 0.010(5) 0.023(5) 0.039(7) -0.007(5) -0.003(4) 0.003(3)
C6 0.022(5) 0.017(5) 0.032(7) -0.002(5) 0.001(5) 0.000(4)
C7 0.018(5) 0.013(5) 0.021(6) 0.001(4) 0.001(4) 0.003(4)
C8 0.025(5) 0.021(5) 0.024(6) 0.005(5) 0.000(6) 0.003(4)
C9 0.023(5) 0.050(7) 0.037(8) 0.000(6) 0.005(5) 0.014(4)
C10 0.022(5) 0.033(5) 0.014(6) 0.010(5) 0.004(5) 0.004(4)
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Re1 Re 0.23926(2) 0.46325(2) 0.94570(7) 0.0166(2) Uani 1 d . .
O1 O 0.2833(4) 0.4808(4) 0.7408(10) 0.026(2) Uani 1 d . .
C1 C 0.2318(6) 0.2646(5) 1.0573(19) 0.033(2) Uani 1 d . .
H1B H 0.1944(6) 0.2555(5) 0.9575(19) 0.049 Uiso 1 calc R .
H1C H 0.2038(6) 0.2554(5) 1.1712(19) 0.049 Uiso 1 calc R .
H1D H 0.2775(6) 0.2273(5) 1.0472(19) 0.049 Uiso 1 calc R .
C2 C 0.2623(5) 0.3502(5) 1.0510(16) 0.021(2) Uani 1 d . .
C3 C 0.3083(5) 0.4030(5) 1.1271(15) 0.020(2) Uani 1 d . .
C4 C 0.3677(6) 0.4273(6) 1.2663(17) 0.026(3) Uani 1 d . .
H4A H 0.4173(6) 0.3947(6) 1.2516(17) 0.032 Uiso 1 calc R .
H4B H 0.3450(6) 0.4153(6) 1.3863(17) 0.032 Uiso 1 calc R .
C5 C 0.3897(5) 0.5161(6) 1.2578(16) 0.024(2) Uani 1 d . .
H5A H 0.4178(5) 0.5271(6) 1.1431(16) 0.029 Uiso 1 calc R .
H5B H 0.4274(5) 0.5289(6) 1.3567(16) 0.029 Uiso 1 calc R .
C6 C 0.3152(6) 0.5717(6) 1.2722(15) 0.024(2) Uani 1 d . .
H6A H 0.2905(6) 0.5656(6) 1.3923(15) 0.028 Uiso 1 calc R .
H6B H 0.3323(6) 0.6286(6) 1.2584(15) 0.028 Uiso 1 calc R .
C7 C 0.2530(5) 0.5512(5) 1.1286(14) 0.017(2) Uani 1 d . .
C8 C 0.1819(5) 0.5605(5) 1.0618(18) 0.023(2) Uani 1 d . .
C9 C 0.1036(6) 0.6055(7) 1.0775(19) 0.037(3) Uani 1 d . .
H9A H 0.0665(6) 0.5873(7) 0.9833(19) 0.055 Uiso 1 calc R .
H9B H 0.1136(6) 0.6635(7) 1.0640(19) 0.055 Uiso 1 calc R .
H9C H 0.0796(6) 0.5951(7) 1.1954(19) 0.055 Uiso 1 calc R .
C10 C 0.1158(5) 0.4146(6) 0.9170(15) 0.023(2) Uani 1 d . .
H10A H 0.1155(5) 0.3723(6) 0.8252(15) 0.035 Uiso 1 calc R .
H10B H 0.0790(5) 0.4581(6) 0.8813(15) 0.035 Uiso 1 calc R .
H10C H 0.0980(5) 0.3919(6) 1.0319(15) 0.035 Uiso 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'
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
_geom_angle_publ_flag
O1 Re1 C7 115.6(4) . . ?
O1 Re1 C3 115.8(4) . . ?
C7 Re1 C3 80.9(4) . . ?
O1 Re1 C8 115.9(4) . . ?
C7 Re1 C8 36.9(4) . . ?
C3 Re1 C8 111.4(4) . . ?
O1 Re1 C2 114.4(4) . . ?
C7 Re1 C2 112.3(4) . . ?
C3 Re1 C2 36.7(4) . . ?
C8 Re1 C2 129.4(5) . . ?
O1 Re1 C10 111.7(4) . . ?
C7 Re1 C10 115.8(4) . . ?
C3 Re1 C10 114.0(3) . . ?
C8 Re1 C10 84.2(4) . . ?
C2 Re1 C10 82.9(3) . . ?
C3 C2 C1 145.3(11) . . ?
C3 C2 Re1 70.2(6) . . ?
C1 C2 Re1 143.5(7) . . ?
C2 C3 C4 151.8(10) . . ?
C2 C3 Re1 73.0(6) . . ?
C4 C3 Re1 134.7(6) . . ?
C3 C4 C5 113.1(9) . . ?
C4 C5 C6 112.6(8) . . ?
C7 C6 C5 111.1(8) . . ?
C8 C7 C6 149.7(10) . . ?
C8 C7 Re1 73.8(7) . . ?
C6 C7 Re1 135.6(6) . . ?
C7 C8 C9 145.1(12) . . ?
C7 C8 Re1 69.3(5) . . ?
C9 C8 Re1 145.0(8) . . ?
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
Re1 O1 1.717(7) . ?
Re1 C7 2.008(10) . ?
Re1 C3 2.033(11) . ?
Re1 C8 2.061(10) . ?
Re1 C2 2.066(8) . ?
Re1 C10 2.209(9) . ?
C1 C2 1.506(12) . ?
C2 C3 1.291(13) . ?
C3 C4 1.486(15) . ?
C4 C5 1.517(14) . ?
C5 C6 1.543(12) . ?
C6 C7 1.524(14) . ?
C7 C8 1.288(13) . ?
C8 C9 1.501(14) . ?
