{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_7124952
_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         'C29 H25 N O Tc P'
_chemical_formula_sum            'C29 H25 N O P Tc'
_chemical_formula_weight         532.47
_chemical_name_common            ' [Tc(NO)(Cp)(Ph)(PPh3)]'
_chemical_name_systematic
;        
hapto5-cyclopentadienylphenyl
triphenylphosphinenitrosyl technetium(I)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 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                 112.89(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.179(1)
_cell_length_b                   13.937(1)
_cell_length_c                   10.048(7)
_cell_measurement_reflns_used    9603
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.92
_cell_measurement_theta_min      2.56
_cell_volume                     1184.2(9)
_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 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_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  0.0220
_diffrn_reflns_av_unetI/netI     0.0135
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            46079
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.909
_diffrn_reflns_theta_min         2.408
_exptl_absorpt_coefficient_mu    0.698
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6948
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5
(Bruker, 2014)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.493
_exptl_crystal_description       block
_exptl_crystal_F_000             544
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.274
_refine_diff_density_min         -0.412
_refine_diff_density_rms         0.048
_refine_ls_abs_structure_details
;
 Flack x determined using 2640 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.006(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.714
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         5631
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.714
_refine_ls_R_factor_all          0.0144
_refine_ls_R_factor_gt           0.0141
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0261P)^2^+1.1186P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0358
_refine_ls_wR_factor_ref         0.0361
_reflns_Friedel_coverage         0.918
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                5576
_reflns_number_total             5631
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc05811f2.cif
_cod_data_source_block           TcNOCpPPh3_Phenyl
_cod_original_cell_volume        1184.2(17)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7124952
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.845
_shelx_estimated_absorpt_t_max   0.921
_shelx_res_checksum              43652