Synthesis, Functionalization, Characterization, and Photophysical Study of Carbonyl-Containing Isocyano Rhenium(I) Diimine Complexes
Apple Wai-Yi Cheung; Larry Tso-Lun Lo; Chi-Chiu Ko; Shek-Man Yiu; Inorganic Chemistry 50 (2011) 4798–4810; doi:10.1021/ic102429t

data_4325170
_publ_section_title
;
 Synthesis, Functionalization, Characterization, and Photophysical Study
 of Carbonyl-Containing Isocyano Rhenium(I) Diimine Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4798
_journal_page_last               4810
_journal_paper_doi               10.1021/ic102429t
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C40 H36 Cl3 N5 O Re, F6 P'
_chemical_formula_sum            'C40 H36 Cl3 F6 N5 O P Re'
_chemical_formula_weight         1040.26
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.219(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.4834(4)
_cell_length_b                   23.0100(7)
_cell_length_c                   14.6848(7)
_cell_measurement_reflns_used    24733
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      71.6592
_cell_measurement_theta_min      3.5826
_cell_volume                     4865.1(3)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_molecular_graphics
;
OLEX2: a complete structure solution, refinement and analysis program. 
Dolomanov et al., J. Appl. Cryst. (2009). 42, 339-341
;
_computing_publication_material
;
OLEX2: a complete structure solution, refinement and analysis program. 
Dolomanov et al., J. Appl. Cryst. (2009). 42, 339-341
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 16.127
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
1 omega    5.00   61.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
-        0.0000 -137.0000   40.0000 56

2 omega  -55.00   16.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
-        0.0000  -37.0000 -180.0000 71

3 omega   73.00  126.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
-       55.0000  125.0000 -180.0000 53

4 omega   78.00  116.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
-       55.0000  125.0000  150.0000 38

5 omega   87.00  122.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
-       55.0000  125.0000   90.0000 35

6 omega  -71.00    9.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
-      -64.0000   25.0000 -120.0000 80

7 omega -134.00 -108.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
-      -64.0000 -137.0000 -139.0000 26

8 omega -134.00  -96.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
-      -64.0000 -137.0000   76.0000 38

9 omega -134.00  -73.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
-      -64.0000  -50.0000  120.0000 61

10 omega   54.00   81.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -50.0000 -180.0000 27

11 omega  129.00  177.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000   50.0000  -60.0000 48

12 omega   82.00  109.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000   77.0000  -30.0000 27

13 omega   41.00   71.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -25.0000  -90.0000 30

14 omega   51.00   78.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -50.0000   90.0000 27

15 omega   55.00   80.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -50.0000  150.0000 25

16 omega  150.00  177.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000   25.0000  -90.0000 27

17 omega   38.00   65.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -25.0000 -150.0000 27

18 omega   39.00   64.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -44.0000   84.0000 25

19 omega  127.00  176.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  111.0000  -60.0000 49

20 omega   80.00  128.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000   25.0000  -90.0000 48

21 omega   39.00   70.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -25.0000  -30.0000 31

22 omega   37.00   71.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -25.0000 -120.0000 34

23 omega   38.00   67.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -25.0000  -60.0000 29

24 omega   37.00   62.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -25.0000    0.0000 25

25 omega  144.00  171.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000   77.0000  -30.0000 27

26 omega  121.00  178.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000   25.0000    0.0000 57

27 omega  -70.00   -5.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
-        0.0000  -77.0000  150.0000 65

28 omega -125.00  -81.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
-      -55.0000  -77.0000   90.0000 44

29 omega  -66.00  -40.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
-      -55.0000  -77.0000   90.0000 26

30 omega   -3.00   46.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
-       55.0000  -77.0000  120.0000 49

31 omega   73.00   98.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
-       55.0000  125.0000  120.0000 25

32 omega   79.00  120.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
-       55.0000  125.0000    0.0000 41

33 omega -133.00 -107.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
-      -64.0000 -137.0000 -103.0000 26

34 omega  -81.00  -44.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
-      -64.0000   50.0000    0.0000 37

35 omega -127.00  -69.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
-      -64.0000  137.0000  140.0000 58

36 omega   42.00   81.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -50.0000   60.0000 39

37 omega   44.00   83.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -50.0000  -30.0000 39

38 omega   44.00   70.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -25.0000    0.0000 26

39 omega   85.00  111.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -88.0000  155.0000 26

40 omega   96.00  143.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -88.0000    5.0000 47

41 omega   54.00   83.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -50.0000 -150.0000 29

42 omega   37.00   62.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -25.0000  150.0000 25

43 omega  104.00  146.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -88.0000  176.0000 42

44 omega   43.00   69.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -50.0000  -90.0000 26

45 omega  111.00  137.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000   50.0000  -90.0000 26

46 omega   37.00   65.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -25.0000   30.0000 28

47 omega   42.00  139.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -88.0000   76.0000 97

48 omega   56.00  146.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -88.0000 -131.0000 90

49 omega  143.00  162.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000   50.0000 -180.0000 19
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.1004616
_diffrn_orient_matrix_UB_12      0.0210921
_diffrn_orient_matrix_UB_13      -0.0253893
_diffrn_orient_matrix_UB_21      0.0335544
_diffrn_orient_matrix_UB_22      0.0635858
_diffrn_orient_matrix_UB_23      0.0063444
_diffrn_orient_matrix_UB_31      0.0151278
_diffrn_orient_matrix_UB_32      -0.0012958
_diffrn_orient_matrix_UB_33      -0.1021475
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'Enhance Ultra (Cu) X-ray Source'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0687
_diffrn_reflns_av_sigmaI/netI    0.0377
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            35595
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         67.00
_diffrn_reflns_theta_min         3.59
_exptl_absorpt_coefficient_mu    7.200
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.38926
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.420
_exptl_crystal_description       plate
_exptl_crystal_F_000             2056
_exptl_crystal_size_max          0.90
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         4.494
_refine_diff_density_min         -2.818
_refine_diff_density_rms         0.176
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     520
_refine_ls_number_reflns         8653
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0568
_refine_ls_R_factor_gt           0.0524
_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^)+(0.1086P)^2^+9.4857P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1463
_refine_ls_wR_factor_ref         0.1497
_reflns_number_gt                7835
_reflns_number_total             8653
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic102429t_si_004.cif
_cod_data_source_block           072010A_APPLE
_cod_database_code               4325170