Geometrically Controlled Selective Formation of Nitrido Technetium(V) Asymmetrical Heterocomplexes with Bidentate Ligands
Cristina Bolzati; Alessandra Boschi; Adriano Duatti; Sushumna Prakash; Licia Uccelli; Fiorenzo Refosco; Francesco Tisato; Giuliano Bandoli; Journal of the American Chemical Society 122 (2000) 4510–4511; doi:10.1021/ja993834u

data_4115995
_publ_section_title
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 Geometrically Controlled Selective Formation of Nitrido Technetium(V)
 Asymmetrical Heterocomplexes with Bidentate Ligands
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_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4510
_journal_page_last               4511
_journal_paper_doi               10.1021/ja993834u
_journal_volume                  122
_journal_year                    2000
_chemical_formula_sum            'C28 H28 Cl2 N O P2 Tc'
_chemical_formula_weight         625.35
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_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                   20.049(6)
_cell_length_b                   13.635(3)
_cell_length_c                   20.125(6)
_cell_measurement_reflns_used    50
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      13.9
_cell_measurement_theta_min      8.8
_cell_volume                     5502(3)
_computing_cell_refinement       'P3/P4-PC Vers.4.27 (1991)'
_computing_data_collection       'P3/P4-PC Vers.4.27 (1991)'
_computing_data_reduction        'P3/P4-PC Vers.4.27 (1991)'
_computing_molecular_graphics    'SHELXTL/PC,Vers.5.03 (Sheldrick, 1994)'
_computing_publication_material  'SHELXTL/PC,Vers.5.03 (Sheldrick, 1994)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXTL/PC,Vers.5.03 (Sheldrick, 1994)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens-Nicolet R3m/V '
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0588
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            3608
_diffrn_reflns_theta_max         22.55
_diffrn_reflns_theta_min         2.52
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 150
_diffrn_standards_number         three
_exptl_absorpt_coefficient_mu    0.856
_exptl_absorpt_correction_T_max  0.769
_exptl_absorpt_correction_T_min  0.488
_exptl_absorpt_correction_type   psi-scans
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_description       parallelepipeds
_exptl_crystal_F_000             2544
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.617
_refine_diff_density_min         -0.594
_refine_diff_density_rms         0.088
_refine_ls_extinction_coef       0.00000(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.036
_refine_ls_goodness_of_fit_obs   1.071
_refine_ls_hydrogen_treatment    'riding model '
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         3607
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_restrained_S_obs      1.071
_refine_ls_R_factor_all          0.0774
_refine_ls_R_factor_obs          0.0452
_refine_ls_shift/esd_max         -1.514
_refine_ls_shift/esd_mean        0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0595P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1145
_refine_ls_wR_factor_obs         0.0976
_reflns_number_observed          2549
_reflns_number_total             3608
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja993834u.cif
_cod_data_source_block           tcndua
_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^)+(0.0595P)^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^)+(0.0595P)^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_original_cell_volume        5501.7(26)
_cod_database_code               4115995