[TcII(NO)(trifluoroacetate)4F]2- - Synthesis and Reactions
Balasekaran, Samundeeswari Mariappan; Hagenbach, Adelheid; Drees, Markus; Abram, Ulrich; Dalton Trans.  (2017) –; doi:10.1039/C7DT03084C

data_7044203
_publ_section_title
;
 [TcII(NO)(trifluoroacetate)4F]2- - Synthesis and Reactions
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT03084C
_journal_year                    2017
_chemical_formula_moiety         'C8 F13 N O9 Tc, Cs, C16 H36 N'
_chemical_formula_sum            'C24 H36 Cs F13 N2 O9 Tc'
_chemical_formula_weight         974.46
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-07-24 deposited with the CCDC.
2017-09-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.870(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.7160(10)
_cell_length_b                   9.6050(10)
_cell_length_c                   28.907(2)
_cell_measurement_reflns_used    6422
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.43
_cell_measurement_theta_min      3.33
_cell_volume                     3736.4(6)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_molecular_graphics    Ortep
_computing_publication_material  WingX
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0930
_diffrn_reflns_av_unetI/netI     0.1519
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            15306
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         3.325
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.456
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            pale-green
_exptl_crystal_density_diffrn    1.732
_exptl_crystal_description       plate
_exptl_crystal_F_000             1924
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.533
_refine_diff_density_min         -0.437
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.847
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     455
_refine_ls_number_reflns         6539
_refine_ls_number_restraints     88
_refine_ls_restrained_S_all      0.865
_refine_ls_R_factor_all          0.1336
_refine_ls_R_factor_gt           0.0516
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0263P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0810
_refine_ls_wR_factor_ref         0.0967
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3098
_reflns_number_total             6539
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03084c1.cif
_cod_data_source_block           tcnotfa4
_cod_database_code               7044203
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              88093