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_4085148
_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         'C32 H7 N O8 Re'
_chemical_formula_sum            'C32 H27 N O8 Re'
_chemical_formula_weight         739.75
_chemical_name_systematic
;
 ? 
;
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-06-19
_audit_creation_method
;
  Olex2 1.2-beta
  (compiled May  9 2012 12:37:22, GUI svn.r4230)
;
_cell_angle_alpha                79.342(4)
_cell_angle_beta                 88.070(4)
_cell_angle_gamma                76.320(4)
_cell_formula_units_Z            2
_cell_length_a                   7.5891(4)
_cell_length_b                   9.1757(5)
_cell_length_c                   22.2233(10)
_cell_measurement_reflns_used    4430
_cell_measurement_temperature    99.96(17)
_cell_measurement_theta_max      74.7580
_cell_measurement_theta_min      5.0520
_cell_volume                     1477.60(13)
_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
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
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    'J. Appl. Cryst. (2007) 40, 786-790'
_diffrn_ambient_temperature      99.96(17)
_diffrn_detector_area_resol_mean 10.3587
_diffrn_measured_fraction_theta_full 0.9841
_diffrn_measured_fraction_theta_max 0.5266
_diffrn_measurement_details
;
  1 omega   59.00   96.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  178.0000  -60.0000 37

  2 omega  -47.00   12.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.6953   37.0000    0.0000 59

  3 omega -110.00   -7.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.6953  -19.0000    0.0000 103

  4 omega  -47.00   35.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.6953   37.0000 -180.0000 82

  5 omega   95.00  121.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       40.6953  164.0000  165.0000 26

  6 omega   24.00   97.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       40.6953 -125.0000  -60.0000 73

  7 omega   80.00  172.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703   30.0000   90.0000 92

  8 omega   37.00   73.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  -30.0000 -180.0000 36

  9 omega   38.00  144.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  -77.0000  -30.0000 106

 10 omega   87.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703   45.0000  150.0000 91

 11 omega  116.00  151.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  178.0000  -60.0000 35

 12 omega   36.00  138.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  -61.0000   90.0000 102

 13 omega   36.00  115.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703 -111.0000  -60.0000 79

 14 omega   41.00   66.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  -30.0000  -30.0000 25

 15 omega   43.00   87.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  -30.0000 -120.0000 44
;
_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      0.0515060000
_diffrn_orient_matrix_UB_12      -0.0521282000
_diffrn_orient_matrix_UB_13      -0.0616042000
_diffrn_orient_matrix_UB_21      0.1492849000
_diffrn_orient_matrix_UB_22      -0.1332138000
_diffrn_orient_matrix_UB_23      0.0325173000
_diffrn_orient_matrix_UB_31      -0.1367875000
_diffrn_orient_matrix_UB_32      -0.1020861000
_diffrn_orient_matrix_UB_33      0.0111591000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0569
_diffrn_reflns_av_unetI/netI     0.0687
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            7802
_diffrn_reflns_theta_full        66.50
_diffrn_reflns_theta_max         67.00
_diffrn_reflns_theta_min         5.05
_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    8.487
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.11974
_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            orange
_exptl_crystal_density_diffrn    1.663
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             730
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.776
_refine_diff_density_min         -3.444
_refine_diff_density_rms         0.204
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     359
_refine_ls_number_reflns         5075
_refine_ls_number_restraints     219
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0752
_refine_ls_R_factor_gt           0.0658
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0945P)^2^+13.6995P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1589
_refine_ls_wR_factor_ref         0.1662
_reflns_number_gt                4569
_reflns_number_total             5075
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om501034e_si_003.cif
_cod_data_source_block           cpd12_ran43cult
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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      P-1
_cod_database_code               4085148
_reflns_odcompleteness_completeness 98.41
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13