Luminescent Rhenium(I) Phenanthroline Complexes with a Benzoxazol-2-ylidene Ligand: Synthesis, Characterization, and Photophysical Study
Ko, Chi-Chiu; Ng, Chi-On; Yiu, Shek-Man; Organometallics 31 (2012) 7074–; doi:10.1021/om300526e

data_4079151
_publ_section_title
;
 Luminescent Rhenium(I) Phenanthroline Complexes with a
 Benzoxazol-2-ylidene Ligand: Synthesis, Characterization, and
 Photophysical Study
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              7074
_journal_paper_doi               10.1021/om300526e
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C34 H26 N3 O3 P Re, F6 P, C3 H6 O1'
_chemical_formula_sum            'C37 H32 F6 N3 O4 P2 Re'
_chemical_formula_weight         944.80
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2011-11-10
_audit_creation_method
;
  Olex2 1.1
  (compiled 2011.08.18 svn.r1932, GUI svn.r3819)
;
_audit_update_record
;
2012-01-21 # Formatted by publCIF
;
_cell_angle_alpha                90.00(2)
_cell_angle_beta                 100.859(2)
_cell_angle_gamma                90.00(2)
_cell_formula_units_Z            4
_cell_length_a                   10.9257(2)
_cell_length_b                   20.0094(3)
_cell_length_c                   17.2111(3)
_cell_measurement_reflns_used    8777
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      71.6456
_cell_measurement_theta_min      3.4200
_cell_volume                     3695.26(11)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_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      133.1
_diffrn_detector_area_resol_mean 16.1270
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
  1 omega  -37.00  -10.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -62.0000  -98.0000 27

  2 omega   15.00   68.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   37.0000 -180.0000 53

  3 omega  -68.00  -42.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -62.0000  -98.0000 26

  4 omega   77.00  121.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000  125.0000   90.0000 44

  5 omega  -12.00   71.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000  -37.0000   90.0000 83

  6 omega   76.00  125.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000  125.0000    0.0000 49

  7 omega   81.00  109.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000  125.0000 -150.0000 28

  8 omega  -11.00   69.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000  -37.0000  -30.0000 80

  9 omega  101.00  176.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000   50.0000 -120.0000 75

 10 omega   39.00   72.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000  -90.0000 33

 11 omega   50.00   76.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -50.0000    0.0000 26

 12 omega  142.00  168.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000   77.0000  150.0000 26

 13 omega  107.00  133.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000   77.0000  150.0000 26

 14 omega   40.00   66.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000  150.0000 26

 15 omega   38.00   71.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000 -150.0000 33

 16 omega   42.00   78.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -50.0000  -90.0000 36

 17 omega  122.00  172.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000   50.0000  -60.0000 50

 18 omega   38.00   63.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000  -60.0000 25

 19 omega   47.00   72.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -50.0000   60.0000 25

 20 omega   50.00   83.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -50.0000   90.0000 33

 21 omega   37.00   64.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000   60.0000 27

 22 omega   37.00   67.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000 -120.0000 30

 23 omega   42.00  129.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -62.0000  141.0000 87
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.1114109000
_diffrn_orient_matrix_UB_12      0.0481595000
_diffrn_orient_matrix_UB_13      0.0051563000
_diffrn_orient_matrix_UB_21      0.0267844000
_diffrn_orient_matrix_UB_22      -0.0280072000
_diffrn_orient_matrix_UB_23      -0.0785520000
_diffrn_orient_matrix_UB_31      -0.0865355000
_diffrn_orient_matrix_UB_32      0.0530858000
_diffrn_orient_matrix_UB_33      -0.0459523000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0209
_diffrn_reflns_av_unetI/netI     0.0232
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            14170
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         67.00
_diffrn_reflns_theta_min         3.42
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_diffrn_source_current           n/a
_diffrn_source_voltage           n/a
_exptl_absorpt_coefficient_mu    7.905
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.39078
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.698
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1864
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.890
_refine_diff_density_min         -0.893
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     753
_refine_ls_number_reflns         6581
_refine_ls_number_restraints     563
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0245
_refine_ls_R_factor_gt           0.0228
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0342P)^2^+2.0313P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0573
_refine_ls_wR_factor_ref         0.0584
_reflns_number_gt                6198
_reflns_number_total             6581
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300526e_si_002.cif
_cod_data_source_block           5_(101911a_on)
_cod_database_code               4079151
_chemical_oxdiff_formula         'C11 H10 S O2'
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13