A Series of [3 + 2] Cycloaddition Products from the Reaction of Rhenium Oxo Complexes with Diphenyl Ketene
Michael Middleditch; James C. Anderson; Alexander J. Blake; Clare Wilson; Inorganic Chemistry 46 (2007) 2797–2804; doi:10.1021/ic062290b

data_4307803
_publ_section_title
;
A Series of [3 + 2] Cycloaddition Products from the Reaction of Rhenium Oxo
Complexes with Diphenyl Ketene
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2797
_journal_page_last               2804
_journal_paper_doi               10.1021/ic062290b
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         'C23 H20 B N4 O3 Re, 0.63(C4 H8 O)'
_chemical_formula_sum            'C25.5 H25 B N4 O3.63 Re'
_chemical_formula_weight         686.53
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'enCIFer editing of SHELXL97 CIF output'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.758(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.1042(10)
_cell_length_b                   8.3461(6)
_cell_length_c                   21.8796(14)
_cell_measurement_reflns_used    11474
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.3
_cell_volume                     2757.9(3)
_computing_cell_refinement       'Bruker SAINT version 6.36a (Bruker, 2002)'
_computing_data_collection       'Bruker SMART version 5.624 (Bruker, 2001)'
_computing_data_reduction        'Bruker SAINT; Bruker SHELXTL (Bruker, 2001)'
_computing_molecular_graphics    ' ?'
_computing_publication_material
'enCIFer(Allen et al.,2004);PLATON(Spek,2003)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker SMART1000 CCD area detector'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.046
_diffrn_reflns_av_sigmaI/netI    0.029
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            25010
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         1.86
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.450
_exptl_absorpt_correction_T_max  0.164
_exptl_absorpt_correction_T_min  0.081
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SHELXTL; Bruker, 2001)'
_exptl_crystal_colour            'royal blue'
_exptl_crystal_density_diffrn    1.653
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tablet
_exptl_crystal_F_000             1348
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
 PLATON SQUEEZE identified 2.5 molecules of diffuse THF solvent
 per unit cell. These molecules are included in the cell
 contents and in the calculation of formula weight, density, etc.
;
_refine_diff_density_max         1.42
_refine_diff_density_min         -1.04
_refine_diff_density_rms         0.11
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.07
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     288
_refine_ls_number_reflns         6228
_refine_ls_number_restraints     96
_refine_ls_restrained_S_all      1.06
_refine_ls_R_factor_all          0.0393
_refine_ls_R_factor_gt           0.0302
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.036P)^2^+1.720P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0683
_refine_ls_wR_factor_ref         0.0704
_reflns_number_gt                5191
_reflns_number_total             6228
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic062290bsi20061201_094724_1.cif
_cod_data_source_block           9
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        2757.9(5)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C25.50 H25 B N4 O3.63 Re'
_cod_database_code               4307803