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_4346451
_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         'C64 H57 N8 O16 Re4, C16 H10, C3 H7 N O'
_chemical_formula_sum            'C83 H76 N9 O17 Re4'
_chemical_formula_weight         2216.33
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 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            4
_cell_length_a                   21.9339(6)
_cell_length_b                   20.4623(4)
_cell_length_c                   20.0974(5)
_cell_measurement_temperature    153(4)
_cell_measurement_theta_max      29.0846
_cell_measurement_theta_min      3.4180
_cell_volume                     9020.1(4)
_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
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.905
_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  0.0668
_diffrn_reflns_av_unetI/netI     0.0783
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            62016
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.15
_diffrn_reflns_theta_min         3.42
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    5.416
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.32721
_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    1.632
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4292
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.24
_refine_diff_density_max         2.168
_refine_diff_density_min         -1.350
_refine_diff_density_rms         0.171
_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   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     940
_refine_ls_number_reflns         20910
_refine_ls_number_restraints     331
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0677
_refine_ls_R_factor_gt           0.0494
_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^)+(0.0636P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1139
_refine_ls_wR_factor_ref         0.1228
_reflns_number_gt                16781
_reflns_number_total             20910
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b01543_si_002.cif
_cod_data_source_block           3a
_cod_database_code               4346451
_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
2. Restrained distances
 C39-C40
 1.51 with sigma of 0.02
 N9-C82
 1.41 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
Uanis(C23) = Uanis(C24) = Uanis(C25) = Uanis(C26)
Uanis(C33) = Uanis(C34) = Uanis(C35) = Uanis(C36)
Uanis(C37) = Uanis(C38) = Uanis(C39) = Uanis(C40)
Uanis(C83) = Uanis(C82) = Uanis(C81) = Uanis(C20) = Uanis(C21) = Uanis(C22)
5.a Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B), C38(H38A,H38B), C21(H21A,H21B), C33(H33A,H33B), C23(H23A,
 H23B), C24(H24A,H24B), C34(H34A,H34B), C25(H25A,H25B), C39(H39A,H39B),
 C0AA(H0AA,H0AB)
5.b Aromatic/amide H refined with riding coordinates:
 C53(H53), C28(H28), C17(H17), C46(H46), C51(H51), C42(H42), C41(H41),
 C50(H50), C47(H47), C14(H14), C45(H45), C44(H44), C57(H57), C31(H31), C52(H52),
  C49(H49), C63(H63), C62(H62), C64(H64), C54(H54), C56(H56), C58(H58),
 C61(H61), C59(H59), C65(H65), C74(H74), C67(H67), C69(H69), C73(H73), C66(H66),
  C72(H72), C70(H70), C77(H77), C76(H76), C35(H35), C83(H83)
5.c Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C26(H26A,H26B,H26C), C36(H36A,H36B,H36C), C82(H82A,H82B,
 H82C), C81(H81A,H81B,H81C), C40(H40A,H40B,H40C)
;
_olex2_submission_special_instructions 'No special instructions were received'