Na[Tc(CO)(CN<i>p</i>-F-Ar<sup>DArF2</sup>)<sub>4</sub>]: an isocyanide analogue of the elusive Na[Tc(CO)<sub>5</sub>].
Salsi, Federico; Hagenbach, Adelheid; Figueroa, Joshua S.; Abram, Ulrich; Chemical communications (Cambridge, England) 59 (2023) 4028–4031; doi:10.1039/d3cc00946g

data_7131399
_publ_section_title
;
 Na[Tc(CO)(CN<i>p</i>-F-Ar<sup>DArF2</sup>)<sub>4</sub>]: an isocyanide
 analogue of the elusive Na[Tc(CO)<sub>5</sub>].
;
_journal_issue                   27
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              4028
_journal_page_last               4031
_journal_paper_doi               10.1039/d3cc00946g
_journal_volume                  59
_journal_year                    2023
_chemical_formula_moiety         'C93 H32 F52 N4 O Tc'
_chemical_formula_sum            'C93 H32 F52 N4 O Tc'
_chemical_formula_weight         2307.22
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-12-21
_audit_creation_method
;
Olex2 1.3
(compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938)
;
_audit_update_record
;
2023-01-30 deposited with the CCDC.	2023-03-09 downloaded from the CCDC.
;
_cell_angle_alpha                84.718(19)
_cell_angle_beta                 86.25(2)
_cell_angle_gamma                73.327(19)
_cell_formula_units_Z            2
_cell_length_a                   14.324(10)
_cell_length_b                   15.260(9)
_cell_length_c                   21.510(14)
_cell_measurement_reflns_used    9090
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      26.09
_cell_measurement_theta_min      2.32
_cell_volume                     4481(5)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.3 (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'CMOS area detector'
_diffrn_detector_area_resol_mean 10.42
_diffrn_detector_type            'PHOTON 100'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'Bruker D8 Venture Duo'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'W/C multilayer mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~2,3~
_diffrn_reflns_av_R_equivalents  0.1044
_diffrn_reflns_av_unetI/netI     0.0497
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            178241
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.098
_diffrn_reflns_theta_min         2.052
_diffrn_source                   'micro-focus sealed tube'
_diffrn_source_target            Mo
_diffrn_source_type              'Incoatec I\mS 1.0'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.321
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6511
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0968 before and 0.0749 after correction.
The Ratio of minimum to maximum transmission is 0.8734.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.710
_exptl_crystal_description       plate
_exptl_crystal_F_000             2274
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.876
_refine_diff_density_min         -1.353
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1362
_refine_ls_number_reflns         19699
_refine_ls_number_restraints     50
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0997
_refine_ls_R_factor_gt           0.0807
_refine_ls_shift/su_max          0.036
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0713P)^2^+23.6311P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1893
_refine_ls_wR_factor_ref         0.2007
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15980
_reflns_number_total             19699
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc00946g2.cif
_cod_data_source_block           tchydride
_cod_depositor_comments
'Adding full bibliography for 7131398--7131400.cif.'
_cod_database_code               7131399
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.994
_shelx_estimated_absorpt_t_min   0.924
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 F2-C041 \\sim F2A-C041
 with sigma of 0.02
 F1-C041 \\sim F1A-C041
 with sigma of 0.02
 F3-C041 \\sim F3A-C041
 with sigma of 0.02
 F1-F2 \\sim F2-F3 \\sim F3-F1
 with sigma of 0.02
 F1A-F2A \\sim F2A-F3A \\sim F3A-F1A
 with sigma of 0.02
 F4A-F5A \\sim F5A-F6A \\sim F6A-F4A
 with sigma of 0.02
 F4-F5 \\sim F5-F6 \\sim F6-F4
 with sigma of 0.02
 F4-C047 \\sim F5-C047 \\sim F6-C047
 with sigma of 0.02
 F4A-C047 \\sim F5A-C047 \\sim F6A-C047
 with sigma of 0.02
 F9-C042 \\sim F8A-C042
 with sigma of 0.02
 F7-C042 \\sim F9A-C042
 with sigma of 0.02
 F8-C042 \\sim F7A-C042
 with sigma of 0.02
 F7-F8 \\sim F8-F9 \\sim F9-F7
 with sigma of 0.02
 F7A-F8A \\sim F8A-F9A \\sim F9A-F7A
 with sigma of 0.02
 F11-C040 \\sim F10A-C040
 with sigma of 0.02
 F10-C040 \\sim F12A-C040
 with sigma of 0.02
 F12-C040 \\sim F11A-C040
 with sigma of 0.02
 F10-F11 \\sim F11-F12 \\sim F12-F10
 with sigma of 0.02
 F10A-F11A \\sim F11A-F12A \\sim F12A-F10A
 with sigma of 0.02
 Tc-C3 \\sim Tc1A-C3
 with sigma of 0.02
 Tc-C2 \\sim Tc1A-C2
 with sigma of 0.02
 Tc-C5 \\sim Tc1A-C5
 with sigma of 0.02
 Tc-C4 \\sim Tc1A-C4
 with sigma of 0.02
 Tc-C1 \\sim Tc1A-C1A
 with sigma of 0.02
 O1-C1 \\sim O1A-C1A
 with sigma of 0.02
 Tc-O1 \\sim Tc1A-O1A
 with sigma of 0.04
 C3-C1 \\sim C3-C1A
 with sigma of 0.04
 C2-C1 \\sim C2-C1A
 with sigma of 0.04
 C5-C1 \\sim C5-C1A
 with sigma of 0.04
 C4-C1 \\sim C4-C1A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(F1) = Uanis(F2) = Uanis(F3) = Uanis(F1A) = Uanis(F2A) = Uanis(F3A)
Uanis(F4) = Uanis(F5) = Uanis(F6) = Uanis(F4A) = Uanis(F5A) = Uanis(F6A)
Uanis(F7) = Uanis(F8) = Uanis(F9) = Uanis(F7A) = Uanis(F8A) = Uanis(F9A)
Uanis(F10) = Uanis(F11) = Uanis(F12) = Uanis(F10A) = Uanis(F11A) = Uanis(F12A)
Uanis(Tc) = Uanis(Tc1A)
Uanis(C1A) = Uanis(C1)
Uanis(O1) = Uanis(O1A)
4. Others
 Sof(F6A)=Sof(F5A)=Sof(F4A)=1-FVAR(1)
 Sof(F5)=Sof(F4)=Sof(F6)=FVAR(1)
 Sof(F2A)=Sof(F3A)=Sof(F1A)=1-FVAR(2)
 Sof(F2)=Sof(F1)=Sof(F3)=FVAR(2)
 Sof(F7A)=Sof(F8A)=Sof(F9A)=1-FVAR(3)
 Sof(F9)=Sof(F7)=Sof(F8)=FVAR(3)
 Sof(F12A)=Sof(F10A)=Sof(F11A)=1-FVAR(4)
 Sof(F11)=Sof(F10)=Sof(F12)=FVAR(4)
 Sof(O1A)=Sof(C1A)=Sof(Tc1A)=1-FVAR(5)
 Sof(Tc)=Sof(O1)=Sof(C1)=FVAR(5)
5.a Aromatic/amide H refined with riding coordinates:
 C01C(H01C), C01P(H01P), C01T(H01T), C01U(H01U), C01X(H01X), C01Z(H01Z),
 C025(H025), C028(H028), C02B(H02B), C02C(H02C), C02H(H02H), C02K(H02K),
 C02N(H02N), C02O(H02O), C02R(H02R), C02T(H02T), C02V(H02V), C02Z(H02Z),
 C030(H030), C031(H031), C032(H032), C033(H033), C034(H034), C03F(H03F),
 C03G(H03G), C03J(H03J), C03K(H03K), C03N(H03N), C03Q(H03Q), C03X(H03X),
 C03Y(H03Y), C045(H045)
;
_shelx_res_checksum              8514
_shelx_hkl_checksum              30930
_olex2_submission_special_instructions 'No special instructions were received'