[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_7044202
_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         'C38 H28 F6 N3 O5 P2 Tc, C0.5 H2 O0.5, O0.25'
_chemical_formula_sum            'C38.5 H30 F6 N3 O5.75 P2 Tc'
_chemical_formula_weight         900.59
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 98.96
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.863(2)
_cell_length_b                   10.6900(10)
_cell_length_c                   29.057(2)
_cell_measurement_reflns_used    9967
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      0.7450
_cell_measurement_theta_min      0.7138
_cell_volume                     7628.7(11)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0727
_diffrn_reflns_av_unetI/netI     0.0404
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            116573
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.290
_diffrn_reflns_theta_min         2.237
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.541
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.568
_exptl_crystal_description       needle
_exptl_crystal_F_000             3640
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.484
_refine_diff_density_min         -1.142
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     515
_refine_ls_number_reflns         9338
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.0727
_refine_ls_R_factor_gt           0.0503
_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^)+(0.0331P)^2^+54.5908P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1039
_refine_ls_wR_factor_ref         0.1125
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7402
_reflns_number_total             9338
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03084c1.cif
_cod_data_source_block           tcnopypph2tfa
_cod_original_formula_sum        'C38.50 H30 F6 N3 O5.75 P2 Tc'
_cod_database_code               7044202
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.774
_shelx_estimated_absorpt_t_max   0.989
_shelx_res_checksum              62807