Synthesis, Characterization, and Photophysical and Emission Solvatochromic Study of Rhenium(I) Tetra(isocyano) Diimine Complexes
Ko, Chi-Chiu; Siu, Jacky Wai-Kit; Cheung, Apple Wai-Yi; Yiu, Shek-Man; Organometallics 30 (2011) 2701–; doi:10.1021/om200074t

data_4064396
_publ_section_title
;
 Synthesis, Characterization, and Photophysical and Emission
 Solvatochromic Study of Rhenium(I) Tetra(isocyano) Diimine Complexes
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              2701
_journal_paper_doi               10.1021/om200074t
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         'C37 H25 Cl4 N7 Re, F6 P'
_chemical_formula_sum            'C37 H25 Cl4 F6 N7 P Re'
_chemical_formula_weight         1040.61
_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
_atom_sites_solution_secondary   difmap
_audit_creation_date             2011-01-11
_audit_creation_method
;
  Olex2 1.1
  (compiled 2010.09.30 svn.r1450, GUI svn.r3284)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 93.2027(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.71954(19)
_cell_length_b                   21.3547(3)
_cell_length_c                   25.3961(4)
_cell_measurement_reflns_used    33471
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      71.5012
_cell_measurement_theta_min      3.4832
_cell_volume                     7970.3(2)
_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
;
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  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133.0
_diffrn_detector_area_resol_mean 16.127
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details
;
1 omega  -29.00    5.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
-        0.0000  -81.0000    5.0000 34

2 omega  -70.00   26.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
-        0.0000  -37.0000   30.0000 96

3 omega   76.00  126.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
-       55.0000  125.0000 -150.0000 50

4 omega   23.00   55.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
-       55.0000  -37.0000    0.0000 32

5 omega   73.00  122.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
-       55.0000  125.0000  120.0000 49

6 omega -134.00  -44.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
-      -64.0000  -50.0000 -120.0000 90

7 omega -113.00  -29.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
-      -64.0000  111.0000   60.0000 84

8 omega   43.00   79.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -50.0000  -90.0000 36

9 omega   44.00   69.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -25.0000  -30.0000 25

10 omega   41.00   82.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -50.0000    0.0000 41

11 omega   38.00   72.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -25.0000   60.0000 34

12 omega   49.00   75.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -50.0000  -60.0000 26

13 omega   42.00   67.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -25.0000  -90.0000 25

14 omega   45.00   74.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -50.0000 -180.0000 29

15 omega  107.00  132.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  179.0000   60.0000 25

16 omega   86.00  175.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000   77.0000   60.0000 89

17 omega   39.00  131.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -81.0000 -174.0000 92

18 omega   37.00   70.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -25.0000    0.0000 33

19 omega   89.00  169.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000   48.0000  103.0000 80

20 omega   79.00  151.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  111.0000  -30.0000 72

21 omega  -70.00   30.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
-        0.0000  -77.0000 -120.0000 100

22 omega  -30.00   70.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
-        0.0000   77.0000 -180.0000 100

23 omega -125.00  -25.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
-      -55.0000  -77.0000  150.0000 100

24 omega   25.00  125.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
-       55.0000   77.0000   30.0000 100

25 omega  -94.00    6.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
-      -64.0000   77.0000  -90.0000 100

26 omega -134.00  -42.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
-      -64.0000  -50.0000 -150.0000 92

27 omega -134.00  -42.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
-      -64.0000  -50.0000  -30.0000 92

28 omega -134.00  -42.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
-      -64.0000  -50.0000   60.0000 92

29 omega   76.00  178.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000   25.0000 -180.0000 102

30 omega   88.00  178.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000   50.0000  -30.0000 90

31 omega   76.00  178.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000   25.0000  -90.0000 102

32 omega   80.00  178.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000   77.0000   30.0000 98

33 omega   37.00   72.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -25.0000   30.0000 35

34 omega   40.00   83.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -50.0000  -30.0000 43

35 omega   39.00  142.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -81.0000   51.0000 103

36 omega   37.00   72.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -25.0000   90.0000 35

37 omega  -26.00   72.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
-        0.0000   37.0000  -60.0000 98

38 omega  -26.00   72.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
-        0.0000   37.0000   90.0000 98

39 omega -125.00  -25.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
-      -55.0000  -77.0000  -60.0000 100

40 omega   73.00  126.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
-       55.0000  125.0000  -60.0000 53

41 omega   80.00  102.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000   77.0000 -180.0000 22
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0797676
_diffrn_orient_matrix_UB_12      0.0237718
_diffrn_orient_matrix_UB_13      -0.0313219
_diffrn_orient_matrix_UB_21      0.0562491
_diffrn_orient_matrix_UB_22      -0.0579865
_diffrn_orient_matrix_UB_23      0.0174406
_diffrn_orient_matrix_UB_31      -0.0381628
_diffrn_orient_matrix_UB_32      -0.0357199
_diffrn_orient_matrix_UB_33      -0.0490757
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0536
_diffrn_reflns_av_unetI/netI     0.0207
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            43954
_diffrn_reflns_theta_full        71.64
_diffrn_reflns_theta_max         71.64
_diffrn_reflns_theta_min         3.49
_exptl_absorpt_coefficient_mu    9.393
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.06657
_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_primary    yellow
_exptl_crystal_density_diffrn    1.734
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rect. Prism'
_exptl_crystal_F_000             4064
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.500
_refine_diff_density_min         -1.746
_refine_diff_density_rms         0.117
_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     759
_refine_ls_number_reflns         7711
_refine_ls_number_restraints     531
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0350
_refine_ls_R_factor_gt           0.0337
_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^)+(0.0564P)^2^+35.4486P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0925
_refine_ls_wR_factor_ref         0.0934
_reflns_number_gt                7368
_reflns_number_total             7711
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200074t_si_002.cif
_cod_data_source_block           12
_cod_original_cell_volume        7970.32(19)
_cod_database_code               4064396