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_4064394
_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_absolute_configuration ad
_chemical_formula_moiety         'C40 H16 Cl12 N6 Re, F6 P'
_chemical_formula_sum            'C40 H16 Cl12 F6 N6 P Re'
_chemical_formula_weight         1337.16
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.2773(2)
_cell_length_b                   17.1955(2)
_cell_length_c                   18.9925(3)
_cell_measurement_reflns_used    11514
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      71.5469
_cell_measurement_theta_min      3.4644
_cell_volume                     4662.76(11)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
1 omega  -69.00  -24.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
-        0.0000  -77.0000  120.0000 45

2 omega  -11.00   29.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
-        0.0000  -77.0000  120.0000 40

3 omega  -89.00  -54.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
-      -55.0000  125.0000  -60.0000 35

4 omega  -63.00   15.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
-      -55.0000   37.0000   90.0000 78

5 omega   73.00   98.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
-       55.0000  125.0000    0.0000 25

6 omega   77.00  121.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
-       55.0000  125.0000   60.0000 44

7 omega   74.00  105.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
-       55.0000  125.0000  -30.0000 31

8 omega   37.00   72.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -25.0000  150.0000 35

9 omega   37.00   62.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -25.0000 -150.0000 25

10 omega   42.00   69.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -25.0000  120.0000 27

11 omega   38.00  117.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -88.0000  -63.0000 79

12 omega   38.00   70.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -25.0000 -180.0000 32

13 omega   45.00   72.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -25.0000   90.0000 27

14 omega   40.00   67.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -25.0000    0.0000 27

15 omega   50.00   81.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -50.0000   90.0000 31

16 omega   40.00   82.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -50.0000  -30.0000 42

17 omega  112.00  139.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -88.0000  -30.0000 27

18 omega   41.00   54.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -50.0000 -180.0000 13
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.1069587
_diffrn_orient_matrix_UB_12      0.0110051
_diffrn_orient_matrix_UB_13      0.0017412
_diffrn_orient_matrix_UB_21      0.0042808
_diffrn_orient_matrix_UB_22      0.0150062
_diffrn_orient_matrix_UB_23      0.0799511
_diffrn_orient_matrix_UB_31      0.0127452
_diffrn_orient_matrix_UB_32      0.0876306
_diffrn_orient_matrix_UB_33      -0.0140648
_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  0.0289
_diffrn_reflns_av_unetI/netI     0.0250
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            12224
_diffrn_reflns_theta_full        66.99
_diffrn_reflns_theta_max         66.99
_diffrn_reflns_theta_min         3.47
_exptl_absorpt_coefficient_mu    12.318
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.36438
_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    red
_exptl_crystal_density_diffrn    1.905
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2584
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.342
_refine_diff_density_min         -1.435
_refine_diff_density_rms         0.099
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.000(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     596
_refine_ls_number_reflns         7557
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0355
_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^)+(0.0557P)^2^+14.2904P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0904
_refine_ls_wR_factor_ref         0.0922
_reflns_number_gt                7248
_reflns_number_total             7557
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200074t_si_002.cif
_cod_data_source_block           4
_cod_database_code               4064394