Preparation of a Family of Hexanuclear Rhenium Cluster Complexes Containing 5-(Phenyl)tetrazol-2-yl Ligands and Alkylation of 5-Substituted Tetrazolate Ligands
Jessica L. Durham; Joan N. Tirado; Stanley A. Knott; Meghan K. Oh; Robert McDonald; Lisa F. Szczepura; Inorganic Chemistry 51 (2012) 7825–7836; doi:10.1021/ic300877r

data_4329737
_publ_contact_author_address
;  Department of Chemistry
   Campus Box 4160
   Illinois State University
   Normal, IL 61790-4160
;
_publ_contact_author_email       lfszcze@ilstu.edu
_publ_contact_author_name        'Lisa F. Szczepura'
_publ_contact_author_phone       309-438-2359
_publ_section_title
;
 Preparation of a Family of Hexanuclear Rhenium Cluster Complexes
 Containing 5-(Phenyl)tetrazol-2-yl Ligands and Alkylation of
 5-Substituted Tetrazolate Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7825
_journal_page_last               7836
_journal_paper_doi               10.1021/ic300877r
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C37 H81 N5 P5 Re6 Se8, B F4'
_chemical_formula_sum            'C37 H81 B F4 N5 P5 Re6 Se8'
_chemical_formula_weight         2586.61
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.2743(17)
_cell_length_b                   19.7358(14)
_cell_length_c                   12.2496(8)
_cell_measurement_reflns_used    7736
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      25.64
_cell_measurement_theta_min      2.22
_cell_volume                     6110.2(7)
_computing_cell_refinement       'Bruker SAINT (Bruker, 1997)'
_computing_data_collection       'Bruker SMART (Bruker, 1997)'
_computing_data_reduction        'Bruker SAINT (Bruker, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL (Bruker, 1997)'
_computing_publication_material  'Bruker SHELXTL (Bruker, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'DIRDIF-2008 (Beurskens et al., 2008)'
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type
'Bruker PLATFORM diffractometer/SMART 1000 CCD area detector'
_diffrn_measurement_method       '\w scans'
_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  0.0519
_diffrn_reflns_av_sigmaI/netI    0.0440
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            43320
_diffrn_reflns_theta_full        25.70
_diffrn_reflns_theta_max         25.70
_diffrn_reflns_theta_min         1.61
_exptl_absorpt_coefficient_mu    16.780
_exptl_absorpt_correction_T_max  0.4326
_exptl_absorpt_correction_T_min  0.0607
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.812
_exptl_crystal_description       prism
_exptl_crystal_F_000             4704
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.913
_refine_diff_density_min         -0.682
_refine_diff_density_rms         0.150
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.017(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     590
_refine_ls_number_reflns         11582
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      0.991
_refine_ls_R_factor_all          0.0345
_refine_ls_R_factor_gt           0.0254
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0186P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0492
_refine_ls_wR_factor_ref         0.0519
_reflns_number_gt                10137
_reflns_number_total             11582
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic300877r_si_002_3.cif
_cod_data_source_block           6
_cod_database_code               4329737