Synthesis and Characterization of Six-Coordinate "3 + 2" Mixed-Ligand Oxorhenium Complexes with theo-Diphenylphosphinophenolato Ligand and Tridentate Coligands of Different N and S Donor Atom Combinations
Berthold Nock; Theodosia Maina; Francesco Tisato; Minas Papadopoulos; Catherine P. Raptopoulou; Aris Terzis; Efstratios Chiotellis; Inorganic Chemistry 39 (2000) 2178–2184; doi:10.1021/ic991341k

data_4320950
_publ_section_title
;
 Synthesis and Characterization of Six-Coordinate "3 + 2" Mixed-Ligand
 Oxorhenium Complexes with theo-Diphenylphosphinophenolato Ligand and
 Tridentate Coligands of Different N and S Donor Atom Combinations
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2178
_journal_page_last               2184
_journal_paper_doi               10.1021/ic991341k
_journal_volume                  39
_journal_year                    2000
_chemical_formula_analytical
ReO{[C2H5SCH2CH2NCH2CH2S][o-C6H4P(C6H5)2]}.0.25CH3OH
_chemical_formula_sum            'C24.25 H28 N O2.25 P Re S2'
_chemical_formula_weight         650.80
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           79
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I 4'
_symmetry_space_group_name_H-M   'I 4'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   24.00(1)
_cell_length_b                   24.00(1)
_cell_length_c                   8.693(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298
_cell_measurement_theta_max      11.7
_cell_measurement_theta_min      5.4
_cell_volume                     5007(4)
_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  0.0240
_diffrn_reflns_av_sigmaI/netI    0.0562
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            3722
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.40
_diffrn_standards_decay_%        -2.9
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    5.105
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.83
_exptl_absorpt_correction_type   'psi-scan empirical'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.726
_exptl_crystal_density_meas      1.70
_exptl_crystal_density_method    'floating method'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2564
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.820
_refine_diff_density_min         -0.882
_refine_diff_density_rms         0.126
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.03(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.076
_refine_ls_goodness_of_fit_obs   1.077
_refine_ls_matrix_type           full
_refine_ls_number_parameters     296
_refine_ls_number_reflns         3540
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.076
_refine_ls_restrained_S_obs      1.077
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_obs          0.0378
_refine_ls_shift/esd_max         0.023
_refine_ls_shift/esd_mean        0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0307P)^2^+54.6138P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0993
_refine_ls_wR_factor_obs         0.0899
_reflns_number_observed          2944
_reflns_number_total             3540
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic991341k_4.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^)+(0.0307P)^2^+54.6138P] 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^)+(0.0307P)^2^+54.6138P] 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        5009(1)
_cod_database_code               4320950