Does [TcF(CO)5] exist? The crystal and molecular structure of [Tc(CO)3(OH)0.49F0.51]4·[Tc(CO)5(BF4)].
Stepanova, E. S.; Gurzhiy, V. V.; Tyupina, M. Yu; Miroslavov, A. E.; Sidorenko, G. V.; Lumpov, A. A.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 8428–8432; doi:10.1039/c6dt00958a

data_7038978
_publ_section_title
;
 Does [TcF(CO)5] exist? The crystal and molecular structure of
 [Tc(CO)3(OH)0.49F0.51]4&#x00B7;[Tc(CO)5(BF4)].
;
_journal_issue                   20
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8428
_journal_page_last               8432
_journal_paper_doi               10.1039/c6dt00958a
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C12 H1.96 F2.04 O13.96 Tc4, B C5 F4 O5 Tc'
_chemical_formula_sum            'C17 H1.96 B F6.04 O18.96 Tc5'
_chemical_formula_weight         1125.07
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_audit_creation_date             2015-11-06
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-03-11 deposited with the CCDC.
2016-04-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.553(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.0520(15)
_cell_length_b                   9.0526(10)
_cell_length_c                   26.357(3)
_cell_measurement_reflns_used    9542
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      31.16
_cell_measurement_theta_min      2.30
_cell_volume                     3315.5(6)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.926
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.710
_diffrn_reflns_av_R_equivalents  0.0464
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_Laue_measured_fraction_full 0.926
_diffrn_reflns_Laue_measured_fraction_max 0.947
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            18206
_diffrn_reflns_point_group_measured_fraction_full 0.926
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_theta_full        25.214
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         1.464
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.139
_exptl_absorpt_correction_T_max  0.3155
_exptl_absorpt_correction_T_min  0.1969
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Bruker, 2007'
_exptl_crystal_colour            'translucent colorless'
_exptl_crystal_density_diffrn    2.254
_exptl_crystal_description       prism
_exptl_crystal_F_000             2120
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_platon_squeeze_details
;
The unit cell contains disordered dichloromethane 
molecules which have been treated as a diffuse
contribution to the overall scattering
without specific atom positions by SQUEEZE/PLATON.
The total approximate amount of solvent molecules
in the structural model have been calculated taking
into account the Electron Count of 88 and a Total
Potential Solvent Accessible Void Volume of 312.5 e/A3.
;
_refine_diff_density_max         1.231
_refine_diff_density_min         -0.878
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     443
_refine_ls_number_reflns         5555
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0343
_refine_ls_R_factor_gt           0.0282
_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^)+(0.0387P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0691
_refine_ls_wR_factor_ref         0.0710
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4698
_reflns_number_total             5555
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt00958a2.cif
_cod_data_source_block           mo_tcco5f_0m
_cod_depositor_comments          'Adding full bibliography for 7038978.cif.'
_cod_original_cell_volume        3315.6(6)
_cod_database_code               7038978
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All O(H) groups
2. Shared sites
{F2, O2}
{F4, O4}
{F3, O3}
{F1, O1}
3. Restrained distances
 F4-H4 = F2-H2
 0.9 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(F2) = Uanis(O2)
Uanis(F1) = Uanis(O1)
Uanis(F3) = Uanis(O3)
Uanis(C51) = Uanis(O51)
Uanis(F4) = Uanis(O4)
5. Others
 Sof(O2)=Sof(H2)=1-FVAR(1)
 Sof(F2)=FVAR(1)
 Sof(O4)=Sof(H4)=1-FVAR(2)
 Sof(F4)=FVAR(2)
 Sof(O3)=Sof(H3)=1-FVAR(3)
 Sof(F3)=FVAR(3)
 Sof(O1)=Sof(H1)=1-FVAR(4)
 Sof(F1)=FVAR(4)
;