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_4337673
_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 H19 Cl2 N5 O2 Re, F6 P'
_chemical_formula_sum            'C28 H19 Cl2 F6 N5 O2 P Re'
_chemical_formula_weight         859.55
_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             2013-05-24
_audit_creation_method
;
  Olex2 1.1
  (compiled 2011.08.18 svn.r1932, GUI svn.r3819)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 119.867(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   24.796(2)
_cell_length_b                   14.7810(5)
_cell_length_c                   18.781(3)
_cell_measurement_reflns_used    6626
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      29.0897
_cell_measurement_theta_min      2.8228
_cell_volume                     5969.2(14)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -95.00  -37.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.4430  178.0000  150.0000 58

  2 omega  -72.00  -42.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.4430  -57.0000   30.0000 30

  3 omega  -92.00  -51.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.4430 -178.0000   90.0000 41

  4 omega  -38.00   49.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.4430   57.0000    0.0000 87

  5 omega   -4.00   48.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.4430   57.0000  120.0000 52

  6 omega  -16.00    9.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9899  102.0000  146.0000 25
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0033675000
_diffrn_orient_matrix_UB_12      0.0460501000
_diffrn_orient_matrix_UB_13      -0.0059099000
_diffrn_orient_matrix_UB_21      -0.0375901000
_diffrn_orient_matrix_UB_22      0.0075215000
_diffrn_orient_matrix_UB_23      -0.0205844000
_diffrn_orient_matrix_UB_31      0.0112113000
_diffrn_orient_matrix_UB_32      0.0112185000
_diffrn_orient_matrix_UB_33      0.0379386000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0279
_diffrn_reflns_av_unetI/netI     0.0320
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            13785
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.83
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_source_current           n/a
_diffrn_source_voltage           n/a
_exptl_absorpt_coefficient_mu    4.379
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.21558
_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            orange
_exptl_crystal_density_diffrn    1.913
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3328
_exptl_crystal_size_max          0.81
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.278
_refine_diff_density_min         -1.513
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         5265
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0361
_refine_ls_R_factor_gt           0.0283
_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^)+(0.0435P)^2^+19.8567P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0727
_refine_ls_wR_factor_ref         0.0792
_reflns_number_gt                4590
_reflns_number_total             5265
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4028145_si_002.cif
_cod_data_source_block           052213a_on
_cod_original_cell_volume        5969.4(11)
_cod_database_code               4337673
_chemical_oxdiff_formula         'C11 H10 S O2'
_reflns_odcompleteness_completeness 99.72
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30