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_7131400
_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
'2(C48 H20.5 F26 N2 O0.5 Sn0.5 Tc0.5), 2(C3.5 H4), C2 H4 O0.5'
_chemical_formula_sum            'C105 H53 F52 N4 O1.5 Sn Tc'
_chemical_formula_weight         2599.20
_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                94.762(7)
_cell_angle_beta                 96.185(10)
_cell_angle_gamma                94.402(12)
_cell_formula_units_Z            4
_cell_length_a                   14.727(5)
_cell_length_b                   15.583(9)
_cell_length_c                   50.04(3)
_cell_measurement_reflns_used    9948
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.78
_cell_measurement_theta_min      2.20
_cell_volume                     11335(10)
_computing_cell_refinement       'APEX 3'
_computing_data_collection       'APEX 3'
_computing_data_reduction        'APEX 3'
_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_area_resol_mean 10.42
_diffrn_detector_type            'PHOTON 100'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'Bruker D8 Venture Duo'
_diffrn_measurement_device_type  'D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1169
_diffrn_reflns_av_unetI/netI     0.0887
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       63
_diffrn_reflns_limit_l_min       -63
_diffrn_reflns_number            355824
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.077
_diffrn_reflns_theta_min         1.885
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.476
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6942
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1021 before and 0.0742 after correction.
The Ratio of minimum to maximum transmission is 0.9312.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_description       plate
_exptl_crystal_F_000             5136
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.091
_refine_diff_density_min         -1.542
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2806
_refine_ls_number_reflns         49591
_refine_ls_number_restraints     4139
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.1403
_refine_ls_R_factor_gt           0.1000
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0779P)^2^+93.5693P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2248
_refine_ls_wR_factor_ref         0.2450
_reflns_Friedel_coverage         0.000
_reflns_number_gt                33993
_reflns_number_total             49591
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc00946g2.cif
_cod_data_source_block           Tctin
_cod_depositor_comments
'Adding full bibliography for 7131398--7131400.cif.'
_cod_original_cell_volume        11336(10)
_cod_original_formula_sum        'C105 H53 F52 N4 O1.50 Sn Tc'
_cod_database_code               7131400
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.991
_shelx_estimated_absorpt_t_min   0.870
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 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
 F4-F5 \\sim F5-F6 \\sim F6-F4
 with sigma of 0.02
 F4A-F5A \\sim F5A-F6A \\sim F6A-F4A
 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
 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
 F13-F14 \\sim F14-F15 \\sim F15-F13
 with sigma of 0.02
 F13A-F14A \\sim F14A-F15A \\sim F15A-F13A
 with sigma of 0.02
 F19-F20 \\sim F20-F21 \\sim F21-F19
 with sigma of 0.02
 F19A-F20A \\sim F20A-F21A \\sim F21A-F19A
 with sigma of 0.02
 F16-F17 \\sim F17-F18 \\sim F18-F16
 with sigma of 0.02
 F16A-F17A \\sim F17A-F18A \\sim F18A-F16A
 with sigma of 0.02
 C07V-C087 \\sim C07Y-C31
 with sigma of 0.02
 F22-F23 \\sim F23-F24 \\sim F24-F22
 with sigma of 0.02
 F22A-F23A \\sim F23A-F24A \\sim F24A-F22A
 with sigma of 0.02
 F37-F38 \\sim F38-F39 \\sim F39-F37
 with sigma of 0.02
 F37A-F38A \\sim F38A-F39A \\sim F39A-F37A
 with sigma of 0.02
 F31-F32 \\sim F32-F33 \\sim F33-F31
 with sigma of 0.02
 F31A-F32A \\sim F32A-F33A \\sim F33A-F31A
 with sigma of 0.02
 F34-F35 \\sim F35-F36 \\sim F36-F34
 with sigma of 0.02
 F34A-F35A \\sim F35A-F36A \\sim F36A-F34A
 with sigma of 0.02
 F28-F29 \\sim F29-F30 \\sim F30-F28
 with sigma of 0.02
 F28A-F29A \\sim F29A-F30A \\sim F30A-F28A
 with sigma of 0.02
 F27-F26 \\sim F26-F42 \\sim F42-F27
 with sigma of 0.02
 C15A-F27 \\sim C15A-F26 \\sim C15A-F42
 with sigma of 0.02
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. 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(F13) = Uanis(F14) = Uanis(F15) = Uanis(F13A) = Uanis(F14A) = Uanis(F15A)
Uanis(F19) = Uanis(F20) = Uanis(F21) = Uanis(F19A) = Uanis(F20A) = Uanis(F21A)
Uanis(F16) = Uanis(F17) = Uanis(F18) = Uanis(F16A) = Uanis(F17A) = Uanis(F18A)
Uanis(F22) = Uanis(F23) = Uanis(F24) = Uanis(F22A) = Uanis(F23A) = Uanis(F24A)
Uanis(F37) = Uanis(F38) = Uanis(F39) = Uanis(F37A) = Uanis(F38A) = Uanis(F39A)
Uanis(F31) = Uanis(F32) = Uanis(F33) = Uanis(F31A) = Uanis(F32A) = Uanis(F33A)
Uanis(F34) = Uanis(F35) = Uanis(F36) = Uanis(F34A) = Uanis(F35A) = Uanis(F36A)
Uanis(F28) = Uanis(F29) = Uanis(F30) = Uanis(F28A) = Uanis(F29A) = Uanis(F30A)
Uanis(C12A) = Uanis(C19A) = Uanis(C13A) = Uanis(C14A) = Uanis(C16A) =
Uanis(C17A) = Uanis(C18A) = Uanis(F41) = Uanis(F25) = Uanis(F40) = Uanis(C15A)
= Uanis(F27) = Uanis(F26) = Uanis(F42)
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Same fragment restrains
{C6, C7, C8, C9, C10, C11, C12, C13, C14, C15, C16, C17, C18, C19, C20, C21,
C22, C23, C24, C25, C26, C27} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C6A, C7A, C8A, C9A, C10A, C11A, C12A, C13A, C14A, C15A, C16A, C17A, C18A,
C19A, C20A, C21A, C22A, C23A, C24A, C25A, C26A, C27A}
7. Others
 Sof(F1A)=Sof(F2A)=Sof(F3A)=1-FVAR(1)
 Sof(F2)=Sof(F1)=Sof(F3)=FVAR(1)
 Sof(F5A)=Sof(F4A)=Sof(F6A)=1-FVAR(2)
 Sof(F5)=Sof(F4)=Sof(F6)=FVAR(2)
 Sof(F7A)=Sof(F8A)=Sof(F9A)=1-FVAR(3)
 Sof(F9)=Sof(F8)=Sof(F7)=FVAR(3)
 Sof(F10A)=Sof(F12A)=Sof(F11A)=1-FVAR(4)
 Sof(F11)=Sof(F12)=Sof(F10)=FVAR(4)
 Sof(F15A)=Sof(F13A)=Sof(F14A)=1-FVAR(5)
 Sof(F15)=Sof(F14)=Sof(F13)=FVAR(5)
 Sof(F21A)=Sof(F19A)=Sof(F20A)=1-FVAR(6)
 Sof(F21)=Sof(F19)=Sof(F20)=FVAR(6)
 Sof(F17A)=Sof(F16A)=Sof(F18A)=1-FVAR(7)
 Sof(F17)=Sof(F16)=Sof(F18)=FVAR(7)
 Sof(F22A)=Sof(F23A)=Sof(F24A)=1-FVAR(8)
 Sof(F22)=Sof(F24)=Sof(F23)=FVAR(8)
 Sof(F38A)=Sof(F39A)=Sof(F37A)=1-FVAR(9)
 Sof(F39)=Sof(F38)=Sof(F37)=FVAR(9)
 Sof(F33A)=Sof(F31A)=Sof(F32A)=1-FVAR(10)
 Sof(F32)=Sof(F31)=Sof(F33)=FVAR(10)
 Sof(F35A)=Sof(F34A)=Sof(F36A)=1-FVAR(11)
 Sof(F35)=Sof(F36)=Sof(F34)=FVAR(11)
 Sof(F28A)=Sof(F30A)=Sof(F29A)=1-FVAR(12)
 Sof(F30)=Sof(F28)=Sof(F29)=FVAR(12)
8.a Secondary CH2 refined with riding coordinates:
 C33(H33a,H33b), C36(H36a,H36b), C35(H35a,H35b), C34(H34a,H34b)
8.b Me refined with riding coordinates:
 C08E(H08a,H08b,H08c), C47(H47a,H47b,H47c)
8.c Aromatic/amide H refined with riding coordinates:
 C01M(H01M), C024(H024), C025(H025), C028(H028), C02G(H02G), C02L(H02L),
 C02R(H02R), C033(H033), C038(H038), C03B(H03B), C03L(H03L), C03M(H03M),
 C03O(H03O), C03R(H03R), C03Z(H03Z), C041(H041), C042(H042), C04I(H04I),
 C04M(H04M), C04O(H04O), C04S(H04S), C04T(H04T), C04X(H04X), C054(H054),
 C056(H056), C058(H058), C059(H059), C05B(H05B), C05C(H05C), C05J(H05J),
 C05K(H05K), C05M(H05M), C05S(H05S), C05T(H05T), C065(H065), C06A(H06A),
 C06B(H06B), C06D(H06D), C06J(H06J), C06P(H06P), C06T(H06T), C06Y(H06Y),
 C071(H071), C075(H075), C07A(H07A), C07C(H07C), C07G(H07G), C07R(H07R),
 C07S(H07S), C07U(H07U), C084(H084), C088(H088), C08G(H08G), C08H(H08H),
 C08O(H08O), C08P(H08P), C08R(H08R), C095(H095), C8(H8), C10(H10), C13(H13),
 C16(H16), C19(H19), C21(H21), C24(H24), C27(H27), C8A(H8A), C10A(H10A),
 C13A(H13A), C16A(H16A), C19A(H19A), C21A(H21A), C24A(H24A), C27A(H27A)
8.d Idealised Me refined as rotating group:
 C28(H28d,H28e,H28f), C30(H30d,H30e,H30f), C29(H29d,H29e,H29f), C29A(H29a,H29b,
 H29c), C28A(H28a,H28b,H28c), C30A(H30a,H30b,H30c)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              16572
_shelx_hkl_checksum              63581
_shelx_fab_checksum              83432
_olex2_submission_special_instructions 'No special instructions were received'