Self-Assembly of Selenium-Bridged Rhenium(I)-Based Metalla Rectangles: Synthesis, Characterization, and Molecular Recognition Studies
Manimaran, Bala.; Vanitha, A.; Karthikeyan, M.; Ramakrishna, Buthanapalli; Mobin, Shaikh M.; Organometallics 33 (2014) 465–; doi:10.1021/om400673f

data_4082351
_publ_section_title
;
 Self-Assembly of Selenium-Bridged Rhenium(I)-Based Metalla Rectangles:
 Synthesis, Characterization, and Molecular Recognition Studies
;
_journal_issue                   2
_journal_name_full               Organometallics
_journal_page_first              465
_journal_paper_doi               10.1021/om400673f
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C60 H44 N4 O12 Re4 Se4, 2(C18 H12)'
_chemical_formula_sum            'C96 H68 N4 O12 Re4 Se4'
_chemical_formula_weight         2530.18
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-11-22
_audit_creation_method
;
  Olex2 1.2
  (compiled 2012.05.09 svn.r2324, GUI svn.r4230)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 93.4932(16)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.7322(3)
_cell_length_b                   12.9415(2)
_cell_length_c                   19.7673(3)
_cell_measurement_reflns_used    10117
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      29.1097
_cell_measurement_theta_min      2.8088
_cell_volume                     4272.45(12)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_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, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector_area_resol_mean 15.9821
_diffrn_measured_fraction_theta_full 0.9981
_diffrn_measured_fraction_theta_max 0.9825
_diffrn_measurement_details
;
  1 omega  -89.00  -51.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.3397 -179.0000  -90.0000 38

  2 omega  -38.00   52.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.3397   19.0000  150.0000 90

  3 omega  -90.00   21.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.3397  -19.0000  120.0000 111

  4 omega  -90.00   -2.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.3397  -19.0000  -30.0000 88
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0171646000
_diffrn_orient_matrix_UB_12      0.0335986000
_diffrn_orient_matrix_UB_13      0.0234840000
_diffrn_orient_matrix_UB_21      0.0317843000
_diffrn_orient_matrix_UB_22      -0.0111941000
_diffrn_orient_matrix_UB_23      0.0242583000
_diffrn_orient_matrix_UB_31      0.0223483000
_diffrn_orient_matrix_UB_32      0.0418295000
_diffrn_orient_matrix_UB_33      -0.0123259000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0467
_diffrn_reflns_av_unetI/netI     0.0427
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            23524
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.81
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    7.417
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.42260
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            block
_exptl_crystal_density_diffrn    1.967
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2408
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.16
_refine_diff_density_max         2.816
_refine_diff_density_min         -2.011
_refine_diff_density_rms         0.199
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     529
_refine_ls_number_reflns         7520
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0353
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0588P)^2^+3.8482P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0885
_refine_ls_wR_factor_ref         0.0956
_reflns_number_gt                6443
_reflns_number_total             7520
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400673f_si_002.cif
_cod_data_source_block           1b.triphenylene
_cod_original_cell_volume        4272.47(13)
_cod_database_code               4082351
_chemical_oxdiff_formula         'C21 H12 O21 N6 Re2 Se2'
_chemical_oxdiff_usercomment     '120 K'
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32