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_7056113
_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         '2(C46 H36 Ag N4 O4), 2(F6 P)'
_chemical_formula_sum            'C92 H72 Ag2 F12 N8 O8 P2'
_chemical_formula_weight         1923.25
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-06-04
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2017-03-29 deposited with the CCDC.
2017-04-19 downloaded from the CCDC.
;
_cell_angle_alpha                78.0530(10)
_cell_angle_beta                 83.1270(10)
_cell_angle_gamma                62.7450(10)
_cell_formula_units_Z            2
_cell_length_a                   15.1732(11)
_cell_length_b                   15.5680(11)
_cell_length_c                   22.2494(16)
_cell_measurement_reflns_used    9771
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.34
_cell_measurement_theta_min      2.37
_cell_volume                     4569.1(6)
_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      173.15
_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  0.0261
_diffrn_reflns_av_unetI/netI     0.0453
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            26585
_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         1.494
_exptl_absorpt_coefficient_mu    0.546
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5786
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1247 before and 0.0378 after correction.
The Ratio of minimum to maximum transmission is 0.7759.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.398
_exptl_crystal_description       block
_exptl_crystal_F_000             1952
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.16
_platon_squeeze_details
;
 ?
;
_refine_diff_density_max         3.120
_refine_diff_density_min         -1.249
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.156
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1105
_refine_ls_number_reflns         16089
_refine_ls_number_restraints     517
_refine_ls_restrained_S_all      1.210
_refine_ls_R_factor_all          0.1152
_refine_ls_R_factor_gt           0.0949
_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^)+(0.1684P)^2^+8.8106P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2722
_refine_ls_wR_factor_ref         0.2908
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12025
_reflns_number_total             16089
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nj00276a2.cif
_cod_data_source_block           n1311120c
_cod_database_code               7056113
_shelx_estimated_absorpt_t_max   0.918
_shelx_estimated_absorpt_t_min   0.908
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C53-C47
 1.53 with sigma of 0.01
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
Uanis(C31) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(Ag2) \\sim Ueq, Uanis(F1) \\sim Ueq, Uanis(F7) \\sim Ueq, Uanis(F8) \\sim
Ueq, Uanis(N5) \\sim Ueq, Uanis(N7) \\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(C45)
\\sim Ueq, Uanis(C50) \\sim Ueq, Uanis(C54) \\sim Ueq, Uanis(C56) \\sim Ueq,
Uanis(C59) \\sim Ueq, Uanis(C60) \\sim Ueq, Uanis(C66) \\sim Ueq, Uanis(C68)
\\sim Ueq, Uanis(C70) \\sim Ueq, Uanis(C71) \\sim Ueq, Uanis(C77) \\sim Ueq,
Uanis(C78) \\sim Ueq, Uanis(C81) \\sim Ueq, Uanis(C83) \\sim Ueq, Uanis(C84)
\\sim Ueq, Uanis(C85) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C53) \\sim Ueq, Uanis(N5) \\sim Ueq, Uanis(C47) \\sim Ueq, Uanis(C52)
\\sim Ueq, Uanis(C51) \\sim Ueq: with sigma of 0.005 and sigma for terminal
atoms of 0.01
5.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C15(H15A,H15B), C16(H16A,H16B), C31(H31A,H31B), C32(H32A,H32B),
 C40(H40A,H40B), C53(H53A,H53B), C61(H61A,H61B), C62(H62A,H62B), C77(H77A,H77B),
  C78(H78A,H78B), C86(H86A,H86B)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C11(H11), C12(H12), C13(H13),
 C14(H14), C21(H21), C22(H22), C23(H23), C24(H24), C29(H29), C30(H30), C35(H35),
  C36(H36), C37(H37), C38(H38), C42(H42), C43(H43), C44(H44), C45(H45),
 C46(H46), C48(H48), C49(H49), C50(H50), C51(H51), C52(H52), C56(H56), C57(H57),
  C58(H58), C59(H59), C67(H67), C68(H68), C69(H69), C70(H70), C75(H75),
 C76(H76), C81(H81), C82(H82), C83(H83), C84(H84), C88(H88), C89(H89), C90(H90),
  C91(H91), C92(H92)
5.c Fitted hexagon refined as free rotating group:
 C47(C48,C49,C50,C51,C52)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'