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_4346452
_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_absolute_configuration unk
_chemical_formula_moiety         'C80 H60 N8 O16 Re4'
_chemical_formula_sum            'C80 H60 N8 O16 Re4'
_chemical_formula_weight         2134.16
_space_group_crystal_system      orthorhombic
_space_group_IT_number           34
_space_group_name_Hall           'P 2 -2n'
_space_group_name_H-M_alt        'P n n 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-08-29
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   23.0606(16)
_cell_length_b                   22.355(2)
_cell_length_c                   12.2692(7)
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.7780
_cell_measurement_theta_min      3.6400
_cell_volume                     6325.0(8)
_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(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0691
_diffrn_reflns_av_unetI/netI     0.1016
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            24207
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.87
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.859
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.72582
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
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    1.121
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2048
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.756
_refine_diff_density_min         -2.045
_refine_diff_density_rms         0.156
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.972
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     319
_refine_ls_number_reflns         9413
_refine_ls_number_restraints     453
_refine_ls_restrained_S_all      0.957
_refine_ls_R_factor_all          0.1103
_refine_ls_R_factor_gt           0.0722
_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^)+(0.1130P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1869
_refine_ls_wR_factor_ref         0.2051
_reflns_number_gt                5749
_reflns_number_total             9413
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b01543_si_002.cif
_cod_data_source_block           4
_cod_original_cell_volume        6324.9(8)
_cod_database_code               4346452
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 O5-C2AA
 1.19 with sigma of 0.02
 O6-C6
 1.1 with sigma of 0.02
 O3-C3
 1.19 with sigma of 0.02
 O2-C1AA
 1.17 with sigma of 0.02
 C40-C31
 1.31 with sigma of 0.02
3. 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
4. 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(C9) = Uanis(C8) = Uanis(C7) = Uanis(C12) = Uanis(C11) = Uanis(C10)
Uanis(C15) = Uanis(C16) = Uanis(C17) = Uanis(C18) = Uanis(C19) = Uanis(C20)
Uanis(C23) = Uanis(C28) = Uanis(C27) = Uanis(C26) = Uanis(C25) = Uanis(C24)
Uanis(O2) = Uanis(C1AA)
Uanis(O3) = Uanis(C3)
Uanis(O6) = Uanis(C6)
5.a Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C13(H13A,H13B), C14(H14A,H14B), C22(H22A,H22B)
5.b Aromatic/amide H refined with riding coordinates:
 C34(H34), C35(H35), C37(H37), C38(H38), C39(H39), C8(H8), C11(H11), C5(H5),
 C1(H1), C2(H2), C3AA(H3AA), C20(H20), C19(H19), C18(H18), C17(H17), C16(H16),
 C40(H40), C28(H28), C27(H27), C26(H26), C25(H25), C24(H24)
5.c Fitted hexagon refined as free rotating group:
 N4(C34,C35,C36,C37,C38), C8(C7,C12,C11,C10,C9), C31(C5,C1,N3,C2,C3AA),
 C15(C20,C19,C18,C17,C16), C23(C28,C27,C26,C25,C24)
;
_olex2_submission_special_instructions 'No special instructions were received'