Chair-Boat Form Transformation of Piperazine-Containing Ligand toward the Preparation of Dirhenium Metallacycles
Chung-Chou Lee; Shu-Chun Hsu; Long-Li Lai; Kuang-Lieh Lu; Inorganic Chemistry 48 (2009) 6329–6331; doi:10.1021/ic900040a

data_4302605
_publ_section_title
;
Chair-Boat Form Transformation of Piperazine-Containing Ligand toward the
Preparation of Dirhenium Metallacycles
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6329
_journal_page_last               6331
_journal_paper_doi               10.1021/ic900040a
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C56.5 H54 N8 O6 Re2'
_chemical_formula_weight         1313.48
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                89.21(3)
_cell_angle_beta                 88.11(3)
_cell_angle_gamma                85.64(3)
_cell_formula_units_Z            2
_cell_length_a                   11.285(2)
_cell_length_b                   13.528(3)
_cell_length_c                   17.562(4)
_cell_measurement_reflns_used    23255
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      2.037
_cell_volume                     2671.7(10)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 19'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_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  0.0692
_diffrn_reflns_av_sigmaI/netI    0.0533
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            33702
_diffrn_reflns_theta_full        25.37
_diffrn_reflns_theta_max         25.37
_diffrn_reflns_theta_min         2.12
_exptl_absorpt_coefficient_mu    4.584
_exptl_absorpt_correction_T_max  0.765
_exptl_absorpt_correction_T_min  0.5697
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            pale-yellow
_exptl_crystal_density_diffrn    1.633
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1294
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.509
_refine_diff_density_min         -2.350
_refine_diff_density_rms         0.184
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     655
_refine_ls_number_reflns         9768
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0383
_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^)+(0.0649P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0960
_refine_ls_wR_factor_ref         0.1042
_reflns_number_gt                7805
_reflns_number_total             9768
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic900040a_si_001_2.cif
_cod_data_source_block           cpd2
_cod_original_cell_volume        2671.8(9)
_cod_original_formula_sum        'C56.50 H54 N8 O6 Re2'
_cod_database_code               4302605