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_4337672
_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         'C28 H20 Cl2 N4 O2 Re S, C0.25 Cl0.5, F6 P'
_chemical_formula_sum            'C28.25 H20.5 Cl2.5 F6 N4 O2 P Re S'
_chemical_formula_weight         899.84
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-07-17
_audit_creation_method
;
  Olex2 1.1
  (compiled 2011.08.18 svn.r1932, GUI svn.r3819)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 112.302(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.2744(7)
_cell_length_b                   9.8309(3)
_cell_length_c                   20.7285(7)
_cell_measurement_reflns_used    6872
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      71.5173
_cell_measurement_theta_min      4.2163
_cell_volume                     3256.9(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_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 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_details
;
  1 omega  -20.00   23.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   37.0000  150.0000 43

  2 omega   39.00   66.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   37.0000  150.0000 27

  3 omega  -24.00   31.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -99.0000    0.0000 55

  4 omega   98.00  125.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000  125.0000 -150.0000 27

  5 omega   -9.00   75.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000  -57.0000  120.0000 84

  6 omega   90.00  117.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000   88.0000 -110.0000 27

  7 omega  -71.00    7.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000   25.0000  -30.0000 78

  8 omega -137.00  -30.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000  -25.0000  -30.0000 107

  9 omega   53.00   90.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000 -111.0000  150.0000 37

 10 omega   38.00   66.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -37.0000   60.0000 28

 11 omega   37.00   69.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000    0.0000 32

 12 omega   41.00   68.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000   60.0000 27

 13 omega   38.00   65.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -37.0000  -60.0000 27

 14 omega   41.00   69.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -37.0000  150.0000 28

 15 omega   38.00   65.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000  120.0000 27

 16 omega   45.00   80.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -50.0000  -90.0000 35

 17 omega   90.00  125.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000   63.0000   30.0000 35

 18 omega   37.00   62.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000 -150.0000 25

 19 omega  135.00  178.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000   63.0000   30.0000 43

 20 omega   53.00   78.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000 -111.0000    0.0000 25

 21 omega   38.00   67.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -37.0000 -120.0000 29

 22 omega   37.00   70.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000   90.0000 33

 23 omega   44.00   80.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -50.0000  -30.0000 36

 24 omega   42.00  130.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -63.0000  120.0000 88
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0565268000
_diffrn_orient_matrix_UB_12      -0.0564194000
_diffrn_orient_matrix_UB_13      -0.0718016000
_diffrn_orient_matrix_UB_21      -0.0778380000
_diffrn_orient_matrix_UB_22      0.0279785000
_diffrn_orient_matrix_UB_23      0.0172884000
_diffrn_orient_matrix_UB_31      -0.0071700000
_diffrn_orient_matrix_UB_32      0.1433167000
_diffrn_orient_matrix_UB_33      -0.0316435000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0279
_diffrn_reflns_av_unetI/netI     0.0314
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            13664
_diffrn_reflns_theta_full        71.65
_diffrn_reflns_theta_max         71.65
_diffrn_reflns_theta_min         4.39
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_diffrn_source_current           n/a
_diffrn_source_voltage           n/a
_exptl_absorpt_coefficient_mu    10.868
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.21895
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.835
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1746
_exptl_crystal_size_max          0.61
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.01
_refine_diff_density_max         3.686
_refine_diff_density_min         -1.690
_refine_diff_density_rms         0.162
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     414
_refine_ls_number_reflns         6230
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0580
_refine_ls_R_factor_gt           0.0541
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0693P)^2^+25.0248P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1416
_refine_ls_wR_factor_ref         0.1450
_reflns_number_gt                5759
_reflns_number_total             6230
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4028145_si_002.cif
_cod_data_source_block           070913a_on
_cod_original_formula_sum        'C28.25 H20.50 Cl2.50 F6 N4 O2 P Re S'
_cod_database_code               4337672
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13