Synthesis, Structural Characterization, and Host-Guest Studies of Aminoquinonato-Bridged Re(I) Supramolecular Rectangles.
Govindarajan, R.; Nagarajaprakash, R.; Manimaran, Bala; Inorganic chemistry 54 (2015) 10686–10694; doi:10.1021/acs.inorgchem.5b01543

data_4346450
_publ_section_title
;
 Synthesis, Structural Characterization, and Host-Guest Studies of
 Aminoquinonato-Bridged Re(I) Supramolecular Rectangles.
;
_journal_issue                   22
_journal_name_full               'Inorganic chemistry'
_journal_page_first              10686
_journal_page_last               10694
_journal_paper_doi               10.1021/acs.inorgchem.5b01543
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C60 H56 N8 O16 Re4, 7(C3 H7 N O)'
_chemical_formula_sum            'C81 H105 N15 O23 Re4'
_chemical_formula_weight         2401.60
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-05-19
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 96.737(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.6254(9)
_cell_length_b                   14.1188(7)
_cell_length_c                   23.2687(11)
_cell_measurement_reflns_used    14650
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      29.0727
_cell_measurement_theta_min      4.3601
_cell_volume                     4771.6(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector_area_resol_mean 15.9821
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.859
_diffrn_measurement_details
;
  1 omega  -23.00   11.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.4960  -99.0000 -180.0000 34

  2 omega  -80.00   12.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.4960  -77.0000  -90.0000 92

  3 omega  -80.00    8.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.4960  -37.0000   30.0000 88

  4 omega  -89.00   -1.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.4960  -37.0000  120.0000 88

  5 omega  -46.00   50.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.4960   77.0000   30.0000 96

  6 omega  -43.00   43.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.4960   37.0000 -150.0000 86
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0099311000
_diffrn_orient_matrix_UB_12      -0.0310002000
_diffrn_orient_matrix_UB_13      0.0238924000
_diffrn_orient_matrix_UB_21      -0.0197161000
_diffrn_orient_matrix_UB_22      -0.0381913000
_diffrn_orient_matrix_UB_23      -0.0169638000
_diffrn_orient_matrix_UB_31      0.0435724000
_diffrn_orient_matrix_UB_32      -0.0101506000
_diffrn_orient_matrix_UB_33      -0.0091094000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0508
_diffrn_reflns_av_unetI/netI     0.0495
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            43475
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.14
_diffrn_reflns_theta_min         4.37
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.132
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.30279
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.672
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2360
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         3.708
_refine_diff_density_min         -1.340
_refine_diff_density_rms         0.194
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     552
_refine_ls_number_reflns         11041
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0560
_refine_ls_R_factor_gt           0.0375
_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^)+(0.0360P)^2^+24.3261P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0871
_refine_ls_wR_factor_ref         0.0965
_reflns_number_gt                8890
_reflns_number_total             11041
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b01543_si_002.cif
_cod_data_source_block           1
_cod_original_cell_volume        4771.7(4)
_cod_database_code               4346450
_reflns_odcompleteness_completeness 98.99
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Restrained distances
 N6-C34
 1.42 with sigma of 0.02
 O9-C33
 1.266 with sigma of 0.02
 O9-C33
 1.26 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O9) = Uanis(C33) = Uanis(N5) = Uanis(C32) = Uanis(C31)
Uanis(C40A) = Uanis(O12) = Uanis(C42) = Uanis(N8) = Uanis(C41) = Uanis(C40) =
Uanis(N8A) = Uanis(C42A) = Uanis(O12A)
4. Others
 Sof(H41D)=Sof(H41E)=Sof(H41F)=Sof(C40A)=Sof(H40D)=Sof(H40E)=Sof(H40F)=
 Sof(C42A)=Sof(H42A)=Sof(N8A)=Sof(O12A)=1-FVAR(1)
 Sof(O12)=Sof(N8)=Sof(H41A)=Sof(H41B)=Sof(H41C)=Sof(C42)=Sof(H42)=Sof(C40)=
 Sof(H40A)=Sof(H40B)=Sof(H40C)=FVAR(1)
 Fixed Sof: C33(0.5) H33(0.5) C31(0.5) H31A(0.5) H31B(0.5) H31C(0.5) O9(0.5)
 N5(0.5) C32(0.5) H32A(0.5) H32B(0.5) H32C(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C13(H13A,H13B), C14(H14A,H14B), C18(H18A,H18B), C19(H19A,
 H19B), C15(H15A,H15B)
5.b Me refined with riding coordinates:
 C41(H41A,H41B,H41C), C41(H41D,H41E,H41F)
5.c Aromatic/amide H refined with riding coordinates:
 C24(H24), C11(H11), C22(H22), C25(H25), C30(H30), C29(H29), C21(H21),
 C28(H28), C27(H27), C8(H8), C36(H36), C33(H33), C39(H39), C42(H42), C42A(H42A)
5.d Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C35(H35A,H35B,H35C), C20(H20A,H20B,H20C), C34(H34A,H34B,
 H34C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C31(H31A,H31B,H31C), C32(H32A,
 H32B,H32C), C40(H40A,H40B,H40C), C40A(H40D,H40E,H40F)
;
_olex2_submission_special_instructions 'No special instructions were received'