Synthesis, spectroscopic characterization and X-ray crystal structures of mononuclear and binuclear oxidorhenium(V) complexes containing indazolyl moieties
B. Machura; M. Wolff; J. Palion; E. Benoist; Inorganica Chimica Acta 404 (2013) 144–154; doi:

data_1517756
_publ_section_title
;
 Synthesis, spectroscopic characterization and X-ray crystal structures of
 mononuclear and binuclear oxidorhenium(V) complexes containing indazolyl
 moieties
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              144
_journal_page_last               154
_journal_volume                  404
_journal_year                    2013
_chemical_formula_moiety         'C50 H40 Cl2 N4 O3 P2 Re2'
_chemical_formula_sum            'C50 H40 Cl2 N4 O3 P2 Re2'
_chemical_formula_weight         1250.10
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 109.690(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.3583(7)
_cell_length_b                   18.9687(7)
_cell_length_c                   11.4532(5)
_cell_measurement_reflns_used    5848
_cell_measurement_temperature    295.0(2)
_cell_measurement_theta_max      29.2545
_cell_measurement_theta_min      3.6066
_cell_volume                     2323.3(2)
_computing_cell_refinement       'CrysAlis RED v. 1.163 (UNIL IC & KUMA 2000)'
_computing_data_collection       'CrysAlis CCD v. 1.163 (UNIL IC & KUMA 2000)'
_computing_data_reduction        'CrysAlis RED v. 1.163 (UNIL IC & KUMA 2000)'
_computing_molecular_graphics
;XP in SHELXTL/PC (Sheldrick, 1990b)
 ORTEP-3 W v. 1.062 (Farrugia 1997)
;
_computing_publication_material
;SHELXL-97 (Sheldrick, 1997) and
 PLATON (Spek, 1990)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295.0(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0304
_diffrn_reflns_av_sigmaI/netI    0.0534
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            13609
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.61
_exptl_absorpt_coefficient_mu    5.436
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61016
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'CrysAlis RED, (2005)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.787
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1212
_exptl_crystal_size_max          0.189
_exptl_crystal_size_mid          0.073
_exptl_crystal_size_min          0.019
_refine_diff_density_max         2.196
_refine_diff_density_min         -1.131
_refine_diff_density_rms         0.113
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.020(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     568
_refine_ls_number_reflns         7498
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0375
_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^)+(0.0308P)^2^+2.7856P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0728
_refine_ls_wR_factor_ref         0.0759
_reflns_number_gt                6898
_reflns_number_total             7498
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2013-404-144-154-1.cif
_cod_data_source_block           ren276a
_cod_original_cell_volume        2323.31(19)
_cod_original_sg_symbol_H-M      P21
_cod_database_code               1517756