Novel Six-Coordinate Oxorhenium "3 + 2" Mixed-Ligand Complexes Carrying the SNS/PO Donor Atom Set: Synthesis and Characterization
Berthold Nock; Theodosia Maina; Francesco Tisato; Minas Papadopoulos; Catherine P. Raptopoulou; Aris Terzis; Efstratios Chiotellis; Inorganic Chemistry 38 (1999) 4197–4202; doi:10.1021/ic9905796

data_4322482
_publ_section_title
;
 Novel Six-Coordinate Oxorhenium "3 + 2" Mixed-Ligand Complexes Carrying
 the SNS/PO Donor Atom Set: Synthesis and Characterization
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4197
_journal_page_last               4202
_journal_paper_doi               10.1021/ic9905796
_journal_volume                  38
_journal_year                    1999
_chemical_formula_analytical
'[ReO{SCH2CH2N(C2H5)CH2CH2S}{P(C6H5)2O(C6H4)}].0.4C2H5OH.0.3CH3OH'
_chemical_formula_sum            'C25.1 H30.6 N O2.7 P Re S2'
_chemical_formula_weight         670.83
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 93.36(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.960(7)
_cell_length_b                   10.187(4)
_cell_length_c                   17.910(8)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298
_cell_measurement_theta_max      11.7
_cell_measurement_theta_min      5.4
_cell_volume                     2725(2)
_computing_cell_refinement
'Program LEAST (UCLA Crystallographic package, C.E.Strouse, 1994)'
_computing_data_collection
'Program COLLECT (UCLA Crystallographic package, C.E.Strouse, 1994)'
_computing_data_reduction
'Program REDUCE (UCLA Crystallographic package, C.E.Strouse, 1994)'
_computing_molecular_graphics    ORTEP
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298
_diffrn_measurement_device
'Crystal Logic Dual Goniometer diffractometer'
_diffrn_measurement_method       'theta-2theta 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  0.0382
_diffrn_reflns_av_sigmaI/netI    0.0534
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            2771
_diffrn_reflns_theta_max         20.99
_diffrn_reflns_theta_min         2.28
_diffrn_standards_decay_%        2.9
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.696
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.76
_exptl_absorpt_correction_type   'psi-scan empirical'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.635
_exptl_crystal_density_meas      1.61
_exptl_crystal_density_method    'floating method'
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             1327
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.772
_refine_diff_density_min         -0.609
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.104
_refine_ls_goodness_of_fit_obs   1.115
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         2666
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.104
_refine_ls_restrained_S_obs      1.115
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_obs          0.0335
_refine_ls_shift/esd_max         0.506
_refine_ls_shift/esd_mean        0.024
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0280P)^2^+16.0442P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0951
_refine_ls_wR_factor_obs         0.0855
_reflns_number_observed          2173
_reflns_number_total             2666
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9905796_1.cif
_cod_data_source_block           shel93
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0280P)^2^+16.0442P] 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^)+(0.0280P)^2^+16.0442P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4322482