Rhenium and technetium tricarbonyl complexes of N-heterocyclic carbene ligands.
Chan, Chung Ying; Pellegrini, Paul A.; Greguric, Ivan; Barnard, Peter J.; Inorganic chemistry 53 (2014) 10862–10873; doi:10.1021/ic500917s

data_4341228
_publ_section_title
;
 Rhenium and technetium tricarbonyl complexes of N-heterocyclic carbene
 ligands.
;
_journal_issue                   20
_journal_name_full               'Inorganic chemistry'
_journal_page_first              10862
_journal_page_last               10873
_journal_paper_doi               10.1021/ic500917s
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C34 H20 N6 O10 Re2, 2(C2 H3 N)'
_chemical_formula_sum            'C34 H20 Cl2 N6 O10 Re2'
_chemical_formula_weight         1115.86
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-04-16
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_cell_angle_alpha                90
_cell_angle_beta                 111.912(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.3994(7)
_cell_length_b                   13.4274(4)
_cell_length_c                   14.0447(4)
_cell_measurement_reflns_used    7217
_cell_measurement_temperature    173
_cell_measurement_theta_max      30.3948
_cell_measurement_theta_min      2.9223
_cell_volume                     3919.0(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 10.3281
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0257
_diffrn_reflns_av_unetI/netI     0.0271
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11938
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.369
_diffrn_reflns_theta_min         3.007
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.369
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67060
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.891
_exptl_crystal_description       prism
_exptl_crystal_F_000             2120
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.092
_refine_diff_density_min         -0.622
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         4008
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0313
_refine_ls_R_factor_gt           0.0257
_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^)+(0.0248P)^2^+12.6940P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0588
_refine_ls_wR_factor_ref         0.0621
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3579
_reflns_number_total             4008
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic500917s_si_002.cif
_cod_data_source_block           9b
_cod_depositor_comments
'Adding full bibliography for 4341223--4341230.cif.'
_cod_database_code               4341228
_shelxl_version_number           2013-2
_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
 O1A-C1A = O1-C1 = O3-C3 = O3A-C3A = O2-C2 = O2A-C2A
 1.14 with sigma of 0.02
 O5-C17A = O5A-C17A
 1.23 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C18) = Uanis(C18A)
Uanis(C19) = Uanis(C19A)
Uanis(Re1) = Uanis(Re1A)
Uanis(C2) = Uanis(C2A)
Uanis(O2) = Uanis(O2A)
Uanis(C3) = Uanis(C3A)
Uanis(O3) = Uanis(O3A)
Uanis(C1) = Uanis(C1A)
Uanis(O1) = Uanis(O1A)
Uanis(N1) = Uanis(N1A)
Uanis(C8) = Uanis(C8A)
Uanis(C7) = Uanis(C7A)
Uanis(C6) = Uanis(C6A)
Uanis(C5) = Uanis(C5A)
Uanis(O4) = Uanis(O4A)
Uanis(O5) = Uanis(O5A)
Uiso(C4A) = Uiso(C4)
4. Others
 Sof(C18A)=Sof(C19A)=Sof(H19D)=Sof(H19E)=Sof(H19F)=1-FVAR(1)
 Sof(C18)=Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(H19C)=FVAR(1)
 Sof(Re1A)=Sof(C2A)=Sof(O2A)=Sof(C3A)=Sof(O3A)=Sof(C1A)=Sof(O1A)=Sof(N1A)=
 Sof(C5A)=Sof(H5A)=Sof(C6A)=Sof(H6A)=Sof(C7A)=Sof(H7A)=Sof(C8A)=Sof(H8A)=
 Sof(O4A)=1-FVAR(2)
 Sof(Re1)=Sof(O4)=Sof(N1)=Sof(C5)=Sof(H5)=Sof(C6)=Sof(H6)=Sof(C7)=Sof(H7)=
 Sof(C8)=Sof(H8)=Sof(C3)=Sof(O2)=Sof(O1)=Sof(C2)=Sof(O3)=Sof(C1)=FVAR(2)
 Sof(O5A)=1-FVAR(3)
 Sof(O5)=FVAR(3)
 Sof(C4)=1-FVAR(4)
 Sof(C4A)=FVAR(4)
5.a Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B)
5.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C13(H13), C14(H14), C12(H12), C5(H5), C6(H6), C7(H7), C8(H8),
 C5A(H5A), C6A(H6A), C7A(H7A), C8A(H8A)
5.c Fitted hexagon refined as free rotating group:
 N1(C4,C5,C6,C7,C8), N1A(C4A,C5A,C6A,C7A,C8A)
5.d Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C19A(H19D,H19E,H19F)
;
_shelx_res_checksum              31450
_shelx_hkl_checksum              77310
_olex2_exptl_crystal_mounting_method
'Crystals were removed from the crystallisation vial and immediately coated with Paratone oil on a glass slide. A suitable single crystal was mounted in Paratone oil on a glass fibre and cooled rapidly to 173 K in a stream of cold N2 using an Oxford low temperature device. '