Triethylammonium bis(oxalato)oxido(triphenylphosphane)rhenate(V)
Grimminger, Philipp; Klüfers, Peter; Acta Crystallographica Section E 63 (2007) m3188–m3188; doi:10.1107/S1600536807061879

data_2216432
_publ_section_title
;
 Triethylammonium bis(oxalato)oxido(triphenylphosphane)rhenate(V)
;
_journal_coeditor_code           EZ2113
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m3188
_journal_page_last               m3188
_journal_paper_doi               10.1107/S1600536807061879
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '(C6 H16 N) [Re (C2 O4)2 O (C18 H15 P)]'
_chemical_formula_moiety         'C6 H16 N +, C22 H15 O9 P Re -'
_chemical_formula_sum            'C28 H31 N O9 P Re'
_chemical_formula_weight         742.71
_chemical_name_common            ReO(oxalate)2(PPh3)
_chemical_name_systematic
;
Triethylammonium bis(oxalato)oxido(triphenylphosphane)rhenate(V)
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'form98_non/compatible with shelxl97-2'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   12.4146(2)
_cell_length_b                   15.3531(2)
_cell_length_c                   30.3448(5)
_cell_measurement_reflns_used    7243
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      3.134
_cell_volume                     5783.80(15)
_computing_cell_refinement       'Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'COLLECT (Nonius, 2004)'
_computing_data_reduction        'Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics
'ORTEPIII (Burnett & Johnson, 1996) and SCHAKAL99 (Keller, 1999)'
_computing_publication_material  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare <i>et al.</i>, 1999)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'CCD; rotation images; thick slices'
_diffrn_radiation_monochromator  'MONTEL, graded multilayered X-ray optics'
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0859
_diffrn_reflns_av_sigmaI/netI    0.0502
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            60925
_diffrn_reflns_theta_full        27.65
_diffrn_reflns_theta_max         27.65
_diffrn_reflns_theta_min         3.15
_exptl_absorpt_coefficient_mu    4.310
_exptl_absorpt_correction_T_max  0.772
_exptl_absorpt_correction_T_min  0.6312
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2001)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.706
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2944
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.084
_refine_diff_density_min         -0.566
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         6646
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0806
_refine_ls_R_factor_gt           0.0334
_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^)+(0.0284P)^2^+5.1452P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0657
_refine_ls_wR_factor_ref         0.0790
_reflns_number_gt                3895
_reflns_number_total             6646
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ez2113.cif
_cod_data_source_block           I
_cod_database_code               2216432
_cod_database_fobs_code          2216432