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_4341230
_publ_section_title
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 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         'C33 H27 N4 O9 Re S, C H2 Cl2'
_chemical_formula_sum            'C34 H29 Cl2 N4 O9 Re S'
_chemical_formula_weight         926.77
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_audit_creation_date             2014-01-31
_audit_creation_method
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Olex2 1.2
(compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736)
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_cell_angle_alpha                116.910(3)
_cell_angle_beta                 102.629(2)
_cell_angle_gamma                92.489(2)
_cell_formula_units_Z            2
_cell_length_a                   10.8019(3)
_cell_length_b                   13.7644(3)
_cell_length_c                   13.8159(4)
_cell_measurement_reflns_used    17373
_cell_measurement_temperature    173.22(10)
_cell_measurement_theta_max      74.0780
_cell_measurement_theta_min      3.6473
_cell_volume                     1763.33(10)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
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_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
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_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
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_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      173.22(10)
_diffrn_detector_area_resol_mean 10.3281
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_av_unetI/netI     0.0260
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            34637
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.246
_diffrn_reflns_theta_min         3.650
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.205
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45439
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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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.
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_exptl_crystal_colour            'clear greenish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.745
_exptl_crystal_description       block
_exptl_crystal_F_000             916
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.312
_refine_diff_density_min         -0.521
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     468
_refine_ls_number_reflns         7064
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0293
_refine_ls_R_factor_gt           0.0258
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
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 w=1/[\s^2^(Fo^2^)+(0.0353P)^2^+1.3878P]
 where P=(Fo^2^+2Fc^2^)/3
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_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0630
_refine_ls_wR_factor_ref         0.0653
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6526
_reflns_number_total             7064
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic500917s_si_002.cif
_cod_data_source_block           10bTsO
_cod_depositor_comments
'Adding full bibliography for 4341223--4341230.cif.'
_cod_original_cell_volume        1763.34(9)
_cod_database_code               4341230
_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, All C(H,H,H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl1-C34 = Cl3A-C34 = Cl4A-C34 = Cl2-C34
 1.77 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(Cl1) = Uanis(Cl3A)
Uanis(Cl2) = Uanis(Cl4A)
4. Others
 Sof(H34C)=Sof(H34D)=Sof(Cl3A)=Sof(Cl4A)=1-FVAR(1)
 Sof(Cl1)=Sof(Cl2)=Sof(H34A)=Sof(H34B)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C18(H18A,H18B), C20(H20A,H20B), C34(H34A,H34B), C34(H34C,H34D)
5.b Aromatic/amide H refined with riding coordinates:
 N4(H4), C28(H28), C11(H11), C5(H5), C32(H32), C8(H8), C29(H29), C23(H23),
 C14(H14), C26(H26), C22(H22), C7(H7), C6(H6), C13(H13), C24(H24), C25(H25),
 C12(H12), C31(H31)
5.c Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C)
;
_shelx_res_checksum              53984
_shelx_hkl_checksum              37224