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_4322484
_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(CH2CH2SCH2CH3)CH2CH2S}{P(C6H5)2O(C6H4)}'
_chemical_formula_sum            'C26 H31 N O2 P Re S3'
_chemical_formula_weight         702.87
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 93.69(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.013(3)
_cell_length_b                   29.03(1)
_cell_length_c                   10.186(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298
_cell_measurement_theta_max      11.6
_cell_measurement_theta_min      5.3
_cell_volume                     2659.6(16)
_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  0.0285
_diffrn_reflns_av_sigmaI/netI    0.0448
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4978
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.12
_diffrn_standards_decay_%        -1.8
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.889
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.40
_exptl_absorpt_correction_type   'psi-scan empirical'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.755
_exptl_crystal_density_meas      1.73
_exptl_crystal_density_method    'floating method'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.825
_refine_diff_density_min         -2.342
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.102
_refine_ls_goodness_of_fit_obs   1.114
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         4663
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.108
_refine_ls_restrained_S_obs      1.114
_refine_ls_R_factor_all          0.0501
_refine_ls_R_factor_obs          0.0449
_refine_ls_shift/esd_max         0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0449P)^2^+19.4309P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1257
_refine_ls_wR_factor_obs         0.1196
_reflns_number_observed          4211
_reflns_number_total             4665
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9905796_3.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^)+(0.0449P)^2^+19.4309P] 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^)+(0.0449P)^2^+19.4309P] 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        2659(2)
_cod_database_code               4322484