A new class of highly solvatochromic dicyano rhenate(I) diimine complexes ‒ synthesis, photophysics and photocatalysis
Larry Tso-Lun Lo; Sze-Wing Lai; Shek-Man Yiu; Chi-Chiu Ko; Chem.Commun. 49 (2013) 2311–; doi:10.1039/c3cc39189b

data_7108968
_publ_section_title
;
 A new class of highly solvatochromic dicyano rhenate(I) diimine complexes
 -- synthesis, photophysics and photocatalysis
;
_journal_name_full               Chem.Commun.
_journal_page_first              2311
_journal_paper_doi               10.1039/c3cc39189b
_journal_volume                  49
_journal_year                    2013
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C16 H8 N4 O2 Re, H2 O, C16 H36 N'
_chemical_formula_sum            'C32 H46 N5 O3 Re'
_chemical_formula_weight         734.94
_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             2012-12-08
_audit_creation_method
;
Olex2 1.1
(compiled 2011.08.18 svn.r1932, GUI svn.r3819)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.9402(2)
_cell_length_b                   15.3605(2)
_cell_length_c                   21.5569(3)
_cell_measurement_reflns_used    9491
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      71.3329
_cell_measurement_theta_min      3.5302
_cell_volume                     3291.45(9)
_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 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_details
;
1 omega -13.00 14.00 1.0000 6.0000
omega____ theta____ kappa____ phi______ frames
- 0.0000 57.0000 -60.0000 27
2 omega -19.00 29.00 1.0000 6.0000
omega____ theta____ kappa____ phi______ frames
- 0.0000 -99.0000 -180.0000 48
3 omega 24.00 55.00 1.0000 6.0000
omega____ theta____ kappa____ phi______ frames
- 0.0000 57.0000 -60.0000 31
4 omega -125.00 -25.00 1.0000 24.0000
omega____ theta____ kappa____ phi______ frames
- -55.0000 -77.0000 60.0000 100
5 omega 80.00 106.00 1.0000 24.0000
omega____ theta____ kappa____ phi______ frames
- 55.0000 109.0000 35.0000 26
6 omega 99.00 125.00 1.0000 24.0000
omega____ theta____ kappa____ phi______ frames
- 55.0000 109.0000 59.0000 26
7 omega 66.00 95.00 1.0000 24.0000
omega____ theta____ kappa____ phi______ frames
- 55.0000 -125.0000 -90.0000 29
8 omega 57.00 87.00 1.0000 48.0000
omega____ theta____ kappa____ phi______ frames
- 110.0000 -111.0000 30.0000 30
9 omega 38.00 63.00 1.0000 48.0000
omega____ theta____ kappa____ phi______ frames
- 110.0000 -37.0000 -150.0000 25
10 omega 49.00 79.00 1.0000 48.0000
omega____ theta____ kappa____ phi______ frames
- 110.0000 -50.0000 30.0000 30
11 omega 37.00 65.00 1.0000 48.0000
omega____ theta____ kappa____ phi______ frames
- 110.0000 -25.0000 -120.0000 28
12 omega 43.00 69.00 1.0000 48.0000
omega____ theta____ kappa____ phi______ frames
- 110.0000 -25.0000 -150.0000 26
13 omega 38.00 64.00 1.0000 48.0000
omega____ theta____ kappa____ phi______ frames
- 110.0000 -37.0000 -30.0000 26
14 omega 40.00 68.00 1.0000 48.0000
omega____ theta____ kappa____ phi______ frames
- 110.0000 -37.0000 -60.0000 28
15 omega 64.00 90.00 1.0000 48.0000
omega____ theta____ kappa____ phi______ frames
- 110.0000 -111.0000 90.0000 26
16 omega 41.00 68.00 1.0000 48.0000
omega____ theta____ kappa____ phi______ frames
- 110.0000 -109.0000 143.0000 27
17 omega 89.00 156.00 1.0000 48.0000
omega____ theta____ kappa____ phi______ frames
- 110.0000 25.0000 0.0000 67
18 omega -16.00 47.00 1.0000 6.0000
omega____ theta____ kappa____ phi______ frames
- 0.0000 -109.0000 120.0000 63
19 omega -25.00 42.00 1.0000 6.0000
omega____ theta____ kappa____ phi______ frames
- 0.0000 -99.0000 -60.0000 67
20 omega -125.00 -74.00 1.0000 24.0000
omega____ theta____ kappa____ phi______ frames
- -55.0000 -157.0000 -120.0000 51
21 omega -124.00 -34.00 1.0000 24.0000
omega____ theta____ kappa____ phi______ frames
- -55.0000 -57.0000 -180.0000 90
22 omega -124.00 -34.00 1.0000 24.0000
omega____ theta____ kappa____ phi______ frames
- -55.0000 -57.0000 -90.0000 90
23 omega 73.00 126.00 1.0000 24.0000
omega____ theta____ kappa____ phi______ frames
- 55.0000 125.0000 -90.0000 53
24 omega 40.00 83.00 1.0000 48.0000
omega____ theta____ kappa____ phi______ frames
- 110.0000 -50.0000 150.0000 43
25 omega 38.00 59.00 1.0000 48.0000
omega____ theta____ kappa____ phi______ frames
- 110.0000 -37.0000 0.0000 21
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0282515000
_diffrn_orient_matrix_UB_12      -0.0234082000
_diffrn_orient_matrix_UB_13      -0.0682869000
_diffrn_orient_matrix_UB_21      0.0271183000
_diffrn_orient_matrix_UB_22      0.0966556000
_diffrn_orient_matrix_UB_23      -0.0144047000
_diffrn_orient_matrix_UB_31      0.1498880000
_diffrn_orient_matrix_UB_32      -0.0130805000
_diffrn_orient_matrix_UB_33      0.0154787000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0367
_diffrn_reflns_av_unetI/netI     0.0268
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            12936
_diffrn_reflns_theta_full        71.47
_diffrn_reflns_theta_max         71.47
_diffrn_reflns_theta_min         3.53
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_diffrn_source_current           n/a
_diffrn_source_voltage           n/a
_exptl_absorpt_coefficient_mu    7.521
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.17921
_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            red
_exptl_crystal_density_diffrn    1.483
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.78
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.140
_refine_diff_density_min         -0.763
_refine_diff_density_rms         0.102
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.022(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         5694
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0299
_refine_ls_R_factor_gt           0.0297
_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^)+(0.0590P)^2^+3.6085P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0844
_refine_ls_wR_factor_ref         0.0847
_reflns_number_gt                5631
_reflns_number_total             5694
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc39189b.txt
_cod_data_source_block           100312a_larry
_cod_database_code               7108968
_chemical_oxdiff_formula         'C11 H10 S O2'
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13