Macrometallocycle binuclear NHC silver(I) complexes: synthesis, structure and recognition for o-phenylenediamine
Liu, Qingxiang; Wei, Deng-Che; Zhao, Dong-Xue; Sun, Xiao-Feng; Zhao, Zhi-Xiang; Yan, Jing; New J. Chem. 41 (2017) 4843–4852; doi:10.1039/C7NJ00276A

data_7056114
_publ_section_title
;
 Macrometallocycle binuclear NHC silver(I) complexes: synthesis, structure
 and recognition for o-phenylenediamine
;
_journal_issue                   12
_journal_name_full               'New J. Chem.'
_journal_page_first              4843
_journal_page_last               4852
_journal_paper_doi               10.1039/C7NJ00276A
_journal_volume                  41
_journal_year                    2017
_chemical_formula_moiety         '0.5(C152 H128 Ag4 N16 O16), 2(F6 P)'
_chemical_formula_sum            'C76 H64 Ag2 F12 N8 O8 P2'
_chemical_formula_weight         1723.03
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-10-25
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2017-03-29 deposited with the CCDC.
2017-04-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.4540(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.1719(4)
_cell_length_b                   11.2926(4)
_cell_length_c                   28.5875(10)
_cell_measurement_reflns_used    7179
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.37
_cell_measurement_theta_min      2.31
_cell_volume                     3567.4(2)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0304
_diffrn_reflns_av_unetI/netI     0.0300
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            20079
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.009
_diffrn_reflns_theta_max         25.009
_diffrn_reflns_theta_min         1.440
_exptl_absorpt_coefficient_mu    0.689
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6769
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0819 before and 0.0335 after correction.
The Ratio of minimum to maximum transmission is 0.9077.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.604
_exptl_crystal_description       block
_exptl_crystal_F_000             1744
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.473
_refine_diff_density_min         -1.544
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     620
_refine_ls_number_reflns         6287
_refine_ls_number_restraints     467
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0693
_refine_ls_R_factor_gt           0.0600
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0580P)^2^+20.6740P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1420
_refine_ls_wR_factor_ref         0.1498
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5413
_reflns_number_total             6287
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nj00276a2.cif
_cod_data_source_block           n130823a
_cod_database_code               7056114
_shelx_estimated_absorpt_t_max   0.904
_shelx_estimated_absorpt_t_min   0.886
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Restrained distances
 C24'-C25 = C18-C19 = C18-C19'
 1.5 with sigma of 0.01
 C1-C7 = C1'-C7 = C32-C33 = C32-C33' = C24-C25
 1.5 with sigma of 0.01
 F3'-F4' = F3'-F5' = F3'-F6' = F4'-F5' = F4'-F6'
 2.23 with sigma of 0.001
 P1'-F1' = P1'-F2' = P1'-F3' = P1'-F4' = P1'-F5' = P1'-F6'
 1.57 with sigma of 0.01
 F3-F4 = F3-F5 = F3-F6 = F4-F5 = F4-F6
 2.23 with sigma of 0.001
 F1-F2 = F1-F4 = F1-F5 = F1-F6 = F2-F3 = F2-F5 = F2-F6
 2.23 with sigma of 0.001
 P1-F1 = P1-F2 = P1-F3 = P1-F4 = P1-F5 = P1-F6
 1.57 with sigma of 0.01
 F1'-F2' \\sim F1'-F4' \\sim F1'-F5' \\sim F1'-F6' \\sim F2'-F3' \\sim F2'-F5'
\\sim F2'-F6'
 with sigma of 0.001
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6: within 2A with sigma of 0.001
and sigma for terminal atoms of 0.002
C1' \\sim C2' \\sim C3' \\sim C4' \\sim C5' \\sim C6': within 2A with sigma of
0.001 and sigma for terminal atoms of 0.002
C33' \\sim C34' \\sim C35' \\sim C36' \\sim C37' \\sim C38': within 2A with
sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C1') \\sim Ueq, Uanis(C1) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.002
Uanis(O3) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C23)
\\sim Ueq, Uanis(C20') \\sim Ueq, Uanis(C21') \\sim Ueq, Uanis(C22') \\sim Ueq,
Uanis(C23') \\sim Ueq, Uanis(C20) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.002
Uanis(C36') \\sim Ueq, Uanis(C36) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.002
Uanis(C38) = Uanis(C38')
Uanis(C37) = Uanis(C37')
Uanis(C36) = Uanis(C36')
Uanis(C35) = Uanis(C35')
Uanis(C34) = Uanis(C34')
Uanis(C33) = Uanis(C33')
Uanis(C20) = Uanis(C20')
Uanis(C21) = Uanis(C21')
Uanis(C22) = Uanis(C22')
Uanis(C23) = Uanis(C23')
5. Others
 Sof(P1')=Sof(F1')=Sof(F2')=Sof(F3')=Sof(F4')=Sof(F5')=Sof(F6')=1-FVAR(1)
 Sof(P1)=Sof(F1)=Sof(F2)=Sof(F3)=Sof(F4)=Sof(F5)=Sof(F6)=FVAR(1)
 Sof(C1')=Sof(C2')=Sof(H2')=Sof(C3')=Sof(H3')=Sof(C4')=Sof(H4')=Sof(C5')=
 Sof(H5')=Sof(C6')=Sof(H6')=Sof(H7BC)=Sof(H7BD)=1-FVAR(2)
 Sof(C1)=Sof(C2)=Sof(H2)=Sof(C3)=Sof(H3)=Sof(C4)=Sof(H4)=Sof(C5)=Sof(H5)=
 Sof(C6)=Sof(H6)=Sof(H7AA)=Sof(H7AB)=FVAR(2)
 Sof(C19')=Sof(C20')=Sof(H20')=Sof(C21')=Sof(H21')=Sof(C22')=Sof(H22')=
 Sof(C23')=Sof(H23')=Sof(C24')=1-FVAR(3)
 Sof(C19)=Sof(C20)=Sof(H20)=Sof(C21)=Sof(H21)=Sof(C22)=Sof(H22)=Sof(C23)=
 Sof(H23)=Sof(C24)=FVAR(3)
 Sof(H32C)=Sof(H32D)=Sof(C33')=Sof(C34')=Sof(H34')=Sof(C35')=Sof(H35')=
 Sof(C36')=Sof(H36')=Sof(C37')=Sof(H37')=Sof(C38')=Sof(H38')=1-FVAR(4)
 Sof(H32A)=Sof(H32B)=Sof(C33)=Sof(C34)=Sof(H34)=Sof(C35)=Sof(H35)=Sof(C36)=
 Sof(H36)=Sof(C37)=Sof(H37)=Sof(C38)=Sof(H38)=FVAR(4)
6.a Secondary CH2 refined with riding coordinates:
 C7(H7AA,H7AB), C7(H7BC,H7BD), C11(H11A,H11B), C12(H12A,H12B), C27(H27A,H27B),
 C28(H28A,H28B), C32(H32A,H32B), C32(H32C,H32D)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C2'(H2'), C3'(H3'), C4'(H4'),
 C5'(H5'), C6'(H6'), C9(H9), C10(H10), C14(H14), C15(H15), C20(H20), C21(H21),
 C22(H22), C23(H23), C20'(H20'), C21'(H21'), C22'(H22'), C23'(H23'), C30(H30),
 C31(H31), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38), C34'(H34'),
 C35'(H35'), C36'(H36'), C37'(H37'), C38'(H38')
6.c Fitted hexagon refined as free rotating group:
 C1(C2,C3,C4,C5,C6), C19(C20,C21,C22,C23,C24), C33(C34,C35,C36,C37,C38)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'