Hexacarbonyltechnetium(I) perchlorate
Gurzhiy, V. V.; Miroslavov, A. E.; Sidorenko, G. V.; Lumpov, A. A.; Krivovichev, S. V.; Suglobov, D. N.; Acta Crystallographica Section E 64 (2008) m1145–; doi:10.1107/S1600536808025208

data_2219320
_publ_section_title
;
 Hexacarbonyltechnetium(I) perchlorate
;
_journal_coeditor_code           FJ2134
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1145
_journal_paper_doi               10.1107/S1600536808025208
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '[Tc (C O)6] Cl O4'
_chemical_formula_moiety         'C6 O6 Tc +, Cl O4 -'
_chemical_formula_sum            'C6 Cl O10 Tc'
_chemical_formula_weight         366.419
_chemical_name_systematic
;
Hexacarbonyltechnetium(I) perchlorate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 112.56(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.227(4)
_cell_length_b                   6.8002(18)
_cell_length_c                   13.616(3)
_cell_measurement_reflns_used    5446
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.61
_cell_measurement_theta_min      2.02
_cell_volume                     1131.0(5)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2007)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2007)'
_computing_data_reduction        'X-RED (Stoe & Cie, 2005)'
_computing_molecular_graphics    'ATOMS (Dowty, 2000)'
_computing_publication_material  'publCIF (Westrip, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXL97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Stoe IPDS-2'
_diffrn_measurement_method       'rotation method'
_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  0.0348
_diffrn_reflns_av_sigmaI/netI    0.0256
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            4935
_diffrn_reflns_theta_full        29.22
_diffrn_reflns_theta_max         29.22
_diffrn_reflns_theta_min         3.24
_exptl_absorpt_coefficient_mu    1.553
_exptl_absorpt_correction_T_max  0.7233
_exptl_absorpt_correction_T_min  0.6199
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   '(X-RED and X-SHAPE; Stoe & Cie, 2005)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.152
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             704
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.317
_refine_diff_density_min         -0.444
_refine_ls_extinction_coef       0.0043(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_matrix_type           full
_refine_ls_number_parameters     99
_refine_ls_number_reflns         1508
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0305
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0289P)^2^+1.543P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0613
_refine_ls_wR_factor_ref         0.0670
_reflns_number_gt                1224
_reflns_number_total             1508
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fj2134.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2219320
_cod_database_fobs_code          2219320