Synthesis and structural characterization of new oxorhenium and oxotechnetium complexes with XN2S-tetradentate semi-rigid ligands (X = O, S, N)
Le Gal, Julien; Tisato, Francesco; Bandoli, Giuliano; Gressier, Marie; Jaud, Joël; Michaud, Sandra; Dartiguenave, Michèle; Benoist, Eric; Dalton Transactions  (2005) 3800–; doi:10.1039/b508661b

data_7008805
_publ_section_title
;
 Synthesis and structural characterization of new oxorhenium and
 oxotechnetium complexes with XN2S-tetradentate semi-rigid ligands (X =
 O, S, N)
;
_journal_issue                   23
_journal_name_full               'Dalton Transactions'
_journal_page_first              3800
_journal_paper_doi               10.1039/b508661b
_journal_year                    2005
_chemical_formula_sum            'C26 H44 N3 O4 S Tc'
_chemical_formula_weight         592.70
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.32(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.114(2)
_cell_length_b                   18.383(4)
_cell_length_c                   17.360(4)
_cell_measurement_reflns_used    50
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      8.6
_cell_measurement_theta_min      6.1
_cell_volume                     2907.8(11)
_computing_cell_refinement       'P3/P4 vers.4.27 (Nicolet, 1991)'
_computing_data_collection       'P3/P4 vers.4.27 (Nicolet, 1991)'
_computing_data_reduction        'P3/P4 vers.4.27 (Nicolet, 1991)'
_computing_molecular_graphics    'SHELXTL NT vers.5.10 (Bruker, 1999)'
_computing_publication_material  'SHELXTL NT vers.5.10 (Bruker, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXTL NT vers.5.10 (Bruker, 1999)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.890
_diffrn_measured_fraction_theta_max 0.890
_diffrn_measurement_device_type  'Nicolet R3m/V diffractometer'
_diffrn_measurement_method       omega-2theta
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0585
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7250
_diffrn_reflns_theta_full        29.55
_diffrn_reflns_theta_max         29.55
_diffrn_reflns_theta_min         3.53
_diffrn_standards_decay_%        'no decay'
_diffrn_standards_interval_count 150
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.601
_exptl_absorpt_correction_T_max  0.562
_exptl_absorpt_correction_T_min  0.345
_exptl_absorpt_correction_type   'psi-scan method'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.354
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.758
_refine_diff_density_min         -0.684
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.881
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     315
_refine_ls_number_reflns         7250
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.881
_refine_ls_R_factor_all          0.0900
_refine_ls_R_factor_gt           0.0454
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0613P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1064
_refine_ls_wR_factor_ref         0.1286
_reflns_number_gt                3700
_reflns_number_total             7250
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b508661b.txt
_cod_data_source_block           '[TcO(Ph-ON2S)]-'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'heavy-atom method' was changed
to 'heavy'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_cell_volume        2908(1)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7008805