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_4082763
_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         'C80 H52 N8 O24 Re4'
_chemical_formula_sum            'C80 H52 N8 O24 Re4'
_chemical_formula_weight         2254.10
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-12-15
_audit_creation_method
;
  Olex2 1.2
  (compiled Dec  5 2012 16:17:34, GUI svn.r4385)
;
_cell_angle_alpha                95.6181(19)
_cell_angle_beta                 95.4012(19)
_cell_angle_gamma                102.252(2)
_cell_formula_units_Z            1
_cell_length_a                   8.5728(2)
_cell_length_b                   12.9783(3)
_cell_length_c                   17.8728(4)
_cell_measurement_reflns_used    8398
_cell_measurement_temperature    150
_cell_measurement_theta_max      29.2681
_cell_measurement_theta_min      2.6466
_cell_volume                     1920.36(8)
_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
_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  -90.00  -61.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.3397  179.0000 -150.0000 29

  2 omega   -5.00   24.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9803   99.0000  -68.0000 29

  3 omega  -22.00   22.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9803   99.0000  175.0000 44

  4 omega   -7.00   75.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9803   37.0000   90.0000 82

  5 omega   38.00   95.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9803  179.0000  -60.0000 57

  6 omega  -37.00   81.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9803    0.0000 -150.0000 118

  7 omega   21.00   49.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9803  -77.0000   60.0000 28

  8 omega   -7.00   18.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9803   37.0000 -180.0000 25

  9 omega  -54.00   92.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9803    0.0000    0.0000 146
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0028612000
_diffrn_orient_matrix_UB_12      -0.0441206000
_diffrn_orient_matrix_UB_13      0.0201669000
_diffrn_orient_matrix_UB_21      0.0406394000
_diffrn_orient_matrix_UB_22      0.0349173000
_diffrn_orient_matrix_UB_23      0.0322551000
_diffrn_orient_matrix_UB_31      -0.0749016000
_diffrn_orient_matrix_UB_32      0.0029255000
_diffrn_orient_matrix_UB_33      0.0128698000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0606
_diffrn_reflns_av_unetI/netI     0.0884
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            18568
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.65
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.368
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.40251
_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_colour            'metallic light yellow'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.949
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.22
_refine_diff_density_max         4.872
_refine_diff_density_min         -2.570
_refine_diff_density_rms         0.188
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     517
_refine_ls_number_reflns         6758
_refine_ls_number_restraints     479
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0792
_refine_ls_R_factor_gt           0.0535
_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^)+(0.0482P)^2^+2.9127P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1151
_refine_ls_wR_factor_ref         0.1289
_reflns_number_gt                5007
_reflns_number_total             6758
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400776m_si_001.cif
_cod_data_source_block           4
_cod_database_code               4082763
_chemical_oxdiff_formula         'C72 H52 N8 O24 Re4'
_chemical_oxdiff_usercomment     '150 K, BROWN, PLATE'
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  H12 of C12, H14 of C14, H30 of C30, H13 of C13, H15 of C15, H19 of C19, H18
  of C18, H20 of C20, H21 of C21, H11 of C11, H39 of C39, H22 of C22, H37 of
  C37, H23 of C23, H26 of C26, {H9A,H9B} of C9, H27 of C27, H24 of C24, H36 of
  C36, {H16A,H16B} of C16, H40 of C40, H33 of C33, H32 of C32, H29 of C29
2. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C30) = Uanis(C31)
4.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C16(H16A,H16B)
4.b Aromatic/amide H refined with riding coordinates:
 C26(H26), C27(H27), C24(H24), C36(H36), C40(H40), C33(H33), C32(H32),
 C29(H29), C23(H23), C37(H37), C22(H22), C39(H39), C11(H11), C21(H21), C20(H20),
  C18(H18), C19(H19), C15(H15), C13(H13), C30(H30), C14(H14), C12(H12)
;