Synthesis, characterization, and photophysical study of luminescent rhenium(i) diimine complexes with various types of N-heterocyclic carbene ligands.
Ng, Chi-On; Yiu, Shek-Man; Ko, Chi-Chiu; Inorganic chemistry 53 (2014) 3022–3031; doi:10.1021/ic4028145

data_4337668
_publ_section_title
;
 Synthesis, characterization, and photophysical study of luminescent
 rhenium(i) diimine complexes with various types of N-heterocyclic carbene
 ligands.
;
_journal_issue                   6
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3022
_journal_page_last               3031
_journal_paper_doi               10.1021/ic4028145
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C17 H10 Br N2 O5 Re, 0.38(C H Cl3)'
_chemical_formula_sum            'C17.38 H10.38 Br Cl1.13 N2 O5 Re'
_chemical_formula_weight         633.14
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-02-02
_audit_creation_method
;
  Olex2 1.1
  (compiled 2011.08.18 svn.r1932, GUI svn.r3819)
;
_cell_angle_alpha                110.622(4)
_cell_angle_beta                 102.013(4)
_cell_angle_gamma                90.398(3)
_cell_formula_units_Z            4
_cell_length_a                   10.9098(5)
_cell_length_b                   14.1254(5)
_cell_length_c                   14.4369(6)
_cell_measurement_reflns_used    9635
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      71.6564
_cell_measurement_theta_min      3.3526
_cell_volume                     2028.81(16)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_detector_area_resol_mean 16.1270
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
  1 omega   25.00   50.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000 -122.0000   34.0000 25

  2 omega  -15.00   25.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -37.0000  -30.0000 40

  3 omega   16.00   56.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   77.0000  120.0000 40

  4 omega  -70.00  -34.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -37.0000  -30.0000 36

  5 omega  -22.00   12.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   77.0000  120.0000 34

  6 omega -111.00  -22.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -55.0000  125.0000    0.0000 89

  7 omega   28.00  125.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000   77.0000 -150.0000 97

  8 omega   84.00  114.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000  122.0000  145.0000 30

  9 omega   44.00  113.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000   77.0000   90.0000 69

 10 omega   26.00  118.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000   77.0000  150.0000 92

 11 omega  -83.00    0.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000   50.0000    0.0000 83

 12 omega -134.00 -109.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000 -149.0000   81.0000 25

 13 omega  130.00  157.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000   50.0000   60.0000 27

 14 omega   37.00   67.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000  -30.0000 30

 15 omega   83.00  165.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000   77.0000 -120.0000 82

 16 omega   89.00  177.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000   50.0000  -60.0000 88

 17 omega   40.00   78.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -50.0000  150.0000 38

 18 omega   39.00  115.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -88.0000   37.0000 76

 19 omega  122.00  146.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -88.0000  -15.0000 24

 20 omega   46.00   71.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000    0.0000 25

 21 omega   41.00   72.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -50.0000   30.0000 31

 22 omega   38.00  146.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -88.0000  149.0000 108

 23 omega   42.00   69.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000   60.0000 27

 24 omega   48.00   83.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -50.0000  120.0000 35

 25 omega   40.00   83.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -50.0000 -120.0000 43

 26 omega  106.00  170.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  111.0000    0.0000 64

 27 omega   41.00   67.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000  -60.0000 26

 28 omega   90.00  117.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000   50.0000   60.0000 27

 29 omega   98.00  174.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000   25.0000    0.0000 76

 30 omega   50.00   75.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -50.0000  -90.0000 25

 31 omega   75.00  127.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -88.0000 -109.0000 52

 32 omega   46.00   81.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -50.0000  -60.0000 35

 33 omega   76.00  101.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -88.0000  -15.0000 25

 34 omega   94.00  119.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -88.0000  -84.0000 25
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0480612000
_diffrn_orient_matrix_UB_12      -0.1116474000
_diffrn_orient_matrix_UB_13      -0.0286068000
_diffrn_orient_matrix_UB_21      0.0348135000
_diffrn_orient_matrix_UB_22      0.0122577000
_diffrn_orient_matrix_UB_23      0.1128599000
_diffrn_orient_matrix_UB_31      -0.1323271000
_diffrn_orient_matrix_UB_32      0.0326309000
_diffrn_orient_matrix_UB_33      0.0113458000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0349
_diffrn_reflns_av_unetI/netI     0.0320
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13213
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         67.00
_diffrn_reflns_theta_min         3.36
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_diffrn_source_current           n/a
_diffrn_source_voltage           n/a
_exptl_absorpt_coefficient_mu    15.665
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.14282
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.073
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1191
_exptl_crystal_size_max          0.71
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         2.970
_refine_diff_density_min         -2.991
_refine_diff_density_rms         0.304
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     541
_refine_ls_number_reflns         7174
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0475
_refine_ls_R_factor_gt           0.0456
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1061P)^2^+7.8962P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1429
_refine_ls_wR_factor_ref         0.1446
_reflns_number_gt                6881
_reflns_number_total             7174
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4028145_si_002.cif
_cod_data_source_block           011212a_on
_cod_original_cell_volume        2028.80(14)
_cod_database_code               4337668
_chemical_oxdiff_formula         'C11 H10 S O2'
_reflns_odcompleteness_completeness 99.37
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13