Amide-Functionalized Chalcogen-Bridged Flexible Tetranuclear Rhenacycles: Synthesis, Characterization, Solvent Effect on the Structure, and Guest Binding.
Karthikeyan, Muthuraman; Ramakrishna, Buthanapalli; Vellaiyadevan, Sivalingam; Divya, Dhanaraj; Manimaran, Bala; ACS omega 3 (2018) 3257–3266; doi:10.1021/acsomega.7b02075

data_4516185
_publ_section_title
;
 Amide-Functionalized Chalcogen-Bridged Flexible Tetranuclear Rhenacycles:
 Synthesis, Characterization, Solvent Effect on the Structure, and Guest
 Binding.
;
_journal_issue                   3
_journal_name_full               'ACS omega'
_journal_page_first              3257
_journal_page_last               3266
_journal_paper_doi               10.1021/acsomega.7b02075
_journal_volume                  3
_journal_year                    2018
_chemical_formula_moiety         'C90 H68 N8 O16 Re4 S4, 4(C3 H7 N O)'
_chemical_formula_sum            'C102 H96 N12 O20 Re4 S4'
_chemical_formula_weight         2682.95
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-04-12
_audit_creation_method
;
Olex2 1.2
(compiled 2013.11.15 svn.r2834 for OlexSys, GUI svn.r4720)
;
_cell_angle_alpha                92.133(4)
_cell_angle_beta                 101.334(4)
_cell_angle_gamma                106.648(4)
_cell_formula_units_Z            2
_cell_length_a                   14.9664(7)
_cell_length_b                   17.7611(8)
_cell_length_c                   22.4582(11)
_cell_measurement_reflns_used    19624
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      2.6839
_cell_volume                     5580.2(5)
_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      120.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0734
_diffrn_reflns_av_unetI/netI     0.1119
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            52650
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.59
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    4.467
_exptl_crystal_density_diffrn    1.597
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2632
_platon_squeeze_details
;
;
_refine_diff_density_max         1.939
_refine_diff_density_min         -1.477
_refine_diff_density_rms         0.177
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.957
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1243
_refine_ls_number_reflns         19624
_refine_ls_number_restraints     390
_refine_ls_restrained_S_all      0.952
_refine_ls_R_factor_all          0.0969
_refine_ls_R_factor_gt           0.0556
_refine_ls_shift/su_max          0.051
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0565P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1194
_refine_ls_wR_factor_ref         0.1349
_reflns_number_gt                12713
_reflns_number_total             19624
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ao7b02075_si_002.cif
_cod_data_source_block           7
_cod_database_code               4516185
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
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
Uanis(C103) = Uanis(C104) = Uanis(C100) = Uanis(C106) = Uanis(C108) =
Uanis(C99) = Uanis(C98) = Uanis(C102)
Uanis(C8) = Uanis(C9)
4.a Secondary CH2 refined with riding coordinates:
 C50(H50A,H50B), C25(H25A,H25B)
4.b Aromatic/amide H refined with riding coordinates:
 N2(H2), C16(H16), C56(H56), C74(H74), C49(H49), N6(H6), C23(H23), C61(H61),
 C52(H52), C13(H13), C21(H21), C62(H62), C20(H20), C17(H17), C24(H24), C58(H58),
  C14(H14), C71(H71), C48(H48), C38(H38), N3(H3), C81(H81), C35(H35), C85(H85),
 C94(H94), C39(H39), C42(H42), C59(H59), C86(H86), C36(H36), C41(H41), C53(H53),
  C70(H70), C45(H45), C91(H91), C73(H73), C88(H88), C82(H82), C95(H95),
 C78(H78), C89(H89), C37(H37), C34(H34), N7(H7), C46(H46), C55(H55), C27(H27),
 C30(H30), C31(H31), C28(H28), C101(H101), C79(H79), C92(H92), C105(H105),
 C107(H107), C97(H97)
4.c Idealised Me refined as rotating group:
 C75(H75A,H75B,H75C), C76(H76A,H76B,H76C), C96(H96A,H96B,H96C), C100(H10A,H10B,
 H10C), C83(H83A,H83B,H83C), C102(H10D,H10E,H10F), C104(H10G,H10H,H10I),
 C103(H10J,H10K,H10L), C108(H10M,H10N,H10O), C106(H10P,H10Q,H10R), C98(H98A,
 H98B,H98C), C99(H99A,H99B,H99C)
;