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_4323942
_publ_section_title
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 Uncommon Anionic Dioxorhenium(V) and Neutral Monooxorhenium(V)
 Mixed-Ligand Complexes Containing Heterofunctionalized Phosphine Ligands:
 Syntheses and Structural Characterization
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_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            'C36 H29 Cl N O2 P2 Re'
_chemical_formula_weight         791.19
_chemical_name_systematic
; 

 ? 

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_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.199(2)
_cell_length_b                   14.147(4)
_cell_length_c                   21.772(6)
_cell_measurement_reflns_used    50
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14
_cell_measurement_theta_min      9
_cell_volume                     3141.4(14)
_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  0.0218
_diffrn_reflns_av_sigmaI/netI    0.0478
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2363
_diffrn_reflns_theta_max         22.55
_diffrn_reflns_theta_min         2.36
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 100
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    4.089
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.83
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.673
_exptl_crystal_F_000             1560
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.45(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.832
_refine_ls_goodness_of_fit_obs   0.858
_refine_ls_matrix_type           full
_refine_ls_number_parameters     194
_refine_ls_number_reflns         2341
_refine_ls_number_restraints     B0
_refine_ls_restrained_S_all      2.700
_refine_ls_restrained_S_obs      0.858
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_obs          0.0391
_refine_ls_shift/esd_max         -0.018
_refine_ls_shift/esd_mean        0.002
_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         0.3335
_refine_ls_wR_factor_obs         0.1039
_reflns_number_observed          2060
_reflns_number_total             2351
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic960404l_4.cif
_cod_data_source_block           8
_cod_depositor_comments
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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 
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_cod_database_code               4323942