Uncommon Anionic Dioxorhenium(V) and Neutral Monooxorhenium(V) Mixed-Ligand Complexes Containing Heterofunctionalized Phosphine Ligands: Syntheses and Structural Characterization
Cristina Bolzati; Francesco Tisato; Fiorenzo Refosco; Giuliano Bandoli; Alessandro Dolmella; Inorganic Chemistry 35 (1996) 6221–6229; doi:10.1021/ic960404l

data_4323940
_publ_section_title
;
 Uncommon Anionic Dioxorhenium(V) and Neutral Monooxorhenium(V)
 Mixed-Ligand Complexes Containing Heterofunctionalized Phosphine Ligands:
 Syntheses and Structural Characterization
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6221
_journal_page_last               6229
_journal_paper_doi               10.1021/ic960404l
_journal_volume                  35
_journal_year                    1996
_chemical_formula_sum            'C62.5 H52.5 As O5 P2 Re'
_chemical_formula_weight         1206.60
_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   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                82.64(4)
_cell_angle_beta                 81.16(4)
_cell_angle_gamma                62.27(3)
_cell_formula_units_Z            2
_cell_length_a                   12.679(7)
_cell_length_b                   13.082(7)
_cell_length_c                   19.649(8)
_cell_measurement_reflns_used    50
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14
_cell_measurement_theta_min      9
_cell_volume                     2845(3)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Nicolet R3m/V automated diffractometer '
_diffrn_measurement_method       'omega-2 theta'
_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  0.0529
_diffrn_reflns_av_sigmaI/netI    0.1070
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3898
_diffrn_reflns_theta_max         18.04
_diffrn_reflns_theta_min         2.01
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 100
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    2.816
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.76
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            pale_yellow
_exptl_crystal_density_diffrn    1.409
_exptl_crystal_F_000             1211
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.969
_refine_ls_goodness_of_fit_obs   1.077
_refine_ls_matrix_type           full
_refine_ls_number_parameters     252
_refine_ls_number_reflns         3890
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.969
_refine_ls_restrained_S_obs      1.077
_refine_ls_R_factor_all          0.0969
_refine_ls_R_factor_obs          0.0634
_refine_ls_shift/esd_max         -0.048
_refine_ls_shift/esd_mean        0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1709
_refine_ls_wR_factor_obs         0.1534
_reflns_number_observed          2598
_reflns_number_total             3890
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic960404l_2.cif
_cod_data_source_block           4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2844.6(25)
_cod_original_formula_sum        'C62.50 H52.50 As O5 P2 Re'
_cod_database_code               4323940