{Tc(NO)(Cp)(PPh3)}(+) - a novel technetium(i) core.
Ackermann, J.; Hagenbach, A.; Abram, U.; Chemical communications (Cambridge, England) 52 (2016) 10285–10288; doi:10.1039/c6cc05811f

data_7124953
_publ_section_title
;
 {Tc(NO)(Cp)(PPh3)}(+) - a novel technetium(i) core.
;
_journal_issue                   67
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              10285
_journal_page_last               10288
_journal_paper_doi               10.1039/c6cc05811f
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety         'C36 H30 Br3  N O3 P2 Tc, C0.5 H1 Cl1'
_chemical_formula_sum            'C36.5 H31 Br3 Cl N O3 P2 Tc'
_chemical_formula_weight         966.74
_chemical_name_common            '[Tc(NO)Br3(OPPh3)2]'
_chemical_name_systematic
;
Tribromidobistriphenylphosphine
oxid nitrosyl technetium(II)
;
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-07-14 deposited with the CCDC.
2016-07-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.550(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.5510(10)
_cell_length_b                   14.3940(10)
_cell_length_c                   44.488(4)
_cell_measurement_reflns_used    18145
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      24.37
_cell_measurement_theta_min      3.12
_cell_volume                     7967.5(11)
_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    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.1777
_diffrn_reflns_av_unetI/netI     0.1783
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            47263
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         3.152
_exptl_absorpt_coefficient_mu    3.552
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.612
_exptl_crystal_description       needle
_exptl_crystal_F_000             3808
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.668
_refine_diff_density_min         -0.968
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.867
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     881
_refine_ls_number_reflns         13834
_refine_ls_number_restraints     99
_refine_ls_restrained_S_all      0.866
_refine_ls_R_factor_all          0.1770
_refine_ls_R_factor_gt           0.0673
_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^)+(0.0671P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1388
_refine_ls_wR_factor_ref         0.1782
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5626
_reflns_number_total             13834
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc05811f2.cif
_cod_data_source_block           TcNOBr3OPPh3
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C36.50 H31 Br3 Cl N O3 P2 Tc'
_cod_database_code               7124953
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              70460