Synthesis and Spectroscopic and Structural Characterization of Oxamidato-Bridged Rhenium(I) Supramolecular Rectangles with Ester Functionalization
Nagarajaprakash, R.; Divya, D.; Ramakrishna, Buthanapalli; Manimaran, Bala.; Organometallics 33 (2014) 1367–; doi:10.1021/om400776m

data_4082762
_publ_section_title
;
 Synthesis and Spectroscopic and Structural Characterization of
 Oxamidato-Bridged Rhenium(I) Supramolecular Rectangles with Ester
 Functionalization
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1367
_journal_paper_doi               10.1021/om400776m
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C68 H60 N8 O24 Re4'
_chemical_formula_sum            'C68 H60 N8 O24 Re4'
_chemical_formula_weight         2118.04
_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             2012-12-12
_audit_creation_method
;
  Olex2 1.2
  (compiled Dec  5 2012 16:17:34, GUI svn.r4385)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 103.877(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.1723(5)
_cell_length_b                   11.5645(4)
_cell_length_c                   21.2154(8)
_cell_measurement_reflns_used    6998
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      29.2816
_cell_measurement_theta_min      2.5732
_cell_volume                     3613.8(2)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_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      150.0
_diffrn_detector_area_resol_mean 15.9821
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega   -1.00   86.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9803   37.0000  -30.0000 87

  2 omega   38.00   71.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9803  179.0000 -180.0000 33

  3 omega  -52.00   43.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9803  -37.0000  150.0000 95

  4 omega   34.00   59.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9803  179.0000   60.0000 25
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0449681000
_diffrn_orient_matrix_UB_12      -0.0022732000
_diffrn_orient_matrix_UB_13      -0.0041796000
_diffrn_orient_matrix_UB_21      -0.0100638000
_diffrn_orient_matrix_UB_22      0.0459811000
_diffrn_orient_matrix_UB_23      -0.0227271000
_diffrn_orient_matrix_UB_31      0.0139445000
_diffrn_orient_matrix_UB_32      0.0405250000
_diffrn_orient_matrix_UB_33      0.0255406000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0481
_diffrn_reflns_av_unetI/netI     0.0859
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            14721
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.58
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.760
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51828
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.946
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2032
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.423
_refine_diff_density_min         -1.577
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.945
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     462
_refine_ls_number_reflns         6357
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.945
_refine_ls_R_factor_all          0.0677
_refine_ls_R_factor_gt           0.0404
_refine_ls_shift/su_max          0.074
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0099P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0555
_refine_ls_wR_factor_ref         0.0605
_reflns_number_gt                4652
_reflns_number_total             6357
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400776m_si_001.cif
_cod_data_source_block           1
_cod_database_code               4082762
_chemical_oxdiff_formula         'C60 H60 N8 O24 Re4'
_chemical_oxdiff_usercomment     '150 K, ORANGE'
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  {H14A,H14B} of C14, {H15A,H15B} of C15, {H37A,H37B} of C37, {H36A,H36B} of
  C36, {H35A,H35B} of C35, {H41A,H41B} of C41, {H40A,H40B} of C40, {H39A,H39B}
  of C39, {H11A,H11B} of C11, H27 of C27, H24 of C24, H28 of C28, H25 of C25,
  H32 of C32, H33 of C33, H30 of C30, {H10A,H10B} of C10, H21 of C21, H17 of
  C17, {H9A,H9B} of C9, H20 of C20, H18 of C18, H29 of C29, {H13A,H13B} of C13
 At 1.5 times of:
  {H38A,H38B,H38C} of C38, {H42A,H42B,H42C} of C42, {H16A,H16B,H16C} of C16,
  {H12A,H12B,H12C} of C12
2. Uiso/Uaniso restraints and constraints
Uanis(C16) = Uanis(C38)
Uanis(C40) = Uanis(C10)
Uanis(C11) = Uanis(C41)
Uanis(C42) = Uanis(C12)
Uanis(C13) = Uanis(C35) = Uanis(C14) = Uanis(C36) = Uanis(C15) = Uanis(C37)
Uanis(C2) = Uanis(O2)
Uanis(C4) = Uanis(O4)
Uanis(N1) = Uanis(O14) = Uanis(N5) = Uanis(O7) = Uanis(N2) = Uanis(O13) = Uanis(N6) = Uanis(O8) = Uanis(C8) = Uanis(C7)
3. Others
 Sof(O7)=Sof(N2)=Sof(O8)=Sof(N1)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(C13)=Sof(H13A)=
 Sof(H13B)=Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(H16C)=
 Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(H12C)=Sof(C11)=Sof(H11A)=Sof(H11B)=1-Sof(N2)=
 1-Sof(N2)=1-Sof(N2)=1-Sof(N2)=1-Sof(N2)=1-Sof(N2)=1-Sof(N2)=1-Sof(N2)=1-
 Sof(N2)=1-Sof(N2)=1-Sof(N2)=1-Sof(N2)=1-Sof(N2)=1-Sof(N2)=1-Sof(N2)=1-Sof(N2)=
 1-Sof(N2)=1-Sof(N2)=1-Sof(N2)=1-Sof(N2)=1-Sof(N2)=1-Sof(N2)=Sof(C15)=Sof(H15A)=
 Sof(H15B)=Sof(C14)=Sof(H14A)=Sof(H14B)=1-Sof(N2)=1-Sof(N2)=1-Sof(N2)=1-Sof(N2)=
 1-Sof(N2)=1-Sof(N2)=1-Sof(N2)=1-Sof(N2)
4.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C13(H13A,H13B), C10(H10A,H10B), C11(H11A,H11B), C39(H39A,H39B),
 C40(H40A,H40B), C41(H41A,H41B), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B),
  C15(H15A,H15B), C14(H14A,H14B)
4.b Aromatic/amide H refined with riding coordinates:
 C21(H21), C17(H17), C20(H20), C18(H18), C29(H29), C27(H27), C24(H24),
 C28(H28), C25(H25), C32(H32), C33(H33), C30(H30)
4.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C12(H12A,H12B,H12C), C42(H42A,H42B,H42C), C38(H38A,H38B,
 H38C)
;