Rhenabenzenes and Unexpected Coupling Products from the Reactions of Rhenacyclobutadienes with Ethoxyethyne
Lin, Ran; Lee, Ka-Ho; Sung, Herman H. Y.; Williams, Ian D.; Lin, Zhenyang; Jia, Guochen; Organometallics 34 (2015) 167–; doi:10.1021/om501034e

data_4085147
_publ_section_title
;
 Rhenabenzenes and Unexpected Coupling Products from the Reactions of
 Rhenacyclobutadienes with Ethoxyethyne
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              167
_journal_paper_doi               10.1021/om501034e
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C26 H23 O8 Re'
_chemical_formula_sum            'C26 H23 O8 Re'
_chemical_formula_weight         649.64
_chemical_name_systematic
;
 ? 
;
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-05-16
_audit_creation_method
;
  Olex2 1.2-beta
  (compiled May  9 2012 12:37:22, GUI svn.r4230)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 106.562(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   21.2127(7)
_cell_length_b                   8.8364(2)
_cell_length_c                   27.3229(9)
_cell_measurement_reflns_used    6403
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      74.8390
_cell_measurement_theta_min      5.2470
_cell_volume                     4909.0(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100.0(2)
_diffrn_detector_area_resol_mean 10.3587
_diffrn_measured_fraction_theta_full 0.9903
_diffrn_measured_fraction_theta_max 0.6694
_diffrn_measurement_details
;
  1 omega   45.00   98.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  -45.0000  -60.0000 53

  2 omega -107.00  -12.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.9453  -57.0000  120.0000 95

  3 omega  -96.00  -35.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.9453  125.0000   60.0000 61

  4 omega   27.00   82.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       40.9453  -99.0000  -60.0000 55

  5 omega   37.00   85.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  -45.0000 -120.0000 48

  6 omega   26.00  107.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  -94.0000 -120.0000 81

  7 omega   80.00  175.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703   61.0000   60.0000 95

  8 omega   32.00  113.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703 -111.0000 -180.0000 81

  9 omega -117.00  -15.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.9453  -37.0000    0.0000 102

 10 omega -120.00   -7.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.9453  -77.0000  -60.0000 113

 11 omega   49.00   83.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703   15.0000  -60.0000 34
;
_diffrn_measurement_device       'kappa diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0208968000
_diffrn_orient_matrix_UB_12      -0.1309814000
_diffrn_orient_matrix_UB_13      -0.0292660000
_diffrn_orient_matrix_UB_21      -0.0728284000
_diffrn_orient_matrix_UB_22      -0.0356130000
_diffrn_orient_matrix_UB_23      -0.0265657000
_diffrn_orient_matrix_UB_31      0.0012904000
_diffrn_orient_matrix_UB_32      0.1094346000
_diffrn_orient_matrix_UB_33      -0.0435327000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0366
_diffrn_reflns_av_unetI/netI     0.0403
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            10023
_diffrn_reflns_theta_full        66.50
_diffrn_reflns_theta_max         67.98
_diffrn_reflns_theta_min         4.35
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           0.80
_diffrn_source_power             0.040
_diffrn_source_target            Cu
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    10.101
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52064
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.758
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2544
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.624
_refine_diff_density_min         -1.270
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     319
_refine_ls_number_reflns         4407
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0314
_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/[\s^2^(Fo^2^)+(0.0540P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0811
_refine_ls_wR_factor_ref         0.0844
_reflns_number_gt                3927
_reflns_number_total             4407
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om501034e_si_003.cif
_cod_data_source_block           cpd10_ran31cult
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/home/saulius/struct/COD-crude-data--automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2935 2014-11-11 08:27:57Z andrius 

 Adding full bibliography for 4085145--4085148.cif.
;
_cod_original_sg_symbol_H-M      I2/a
_cod_database_code               4085147
_reflns_odcompleteness_completeness 99.03
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13