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_7056116
_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         'C80 H72 Ag2 N8 O8, 0.5(C H2 Cl2), 2(F6 P)'
_chemical_formula_sum            'C80.5 H73 Ag2 Cl F12 N8 O8 P2'
_chemical_formula_weight         1821.59
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 97.327(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.458(3)
_cell_length_b                   14.898(3)
_cell_length_c                   37.068(6)
_cell_measurement_reflns_used    9920
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.71
_cell_measurement_theta_min      2.46
_cell_volume                     7919(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0247
_diffrn_reflns_av_unetI/netI     0.0279
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            40239
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.009
_diffrn_reflns_theta_max         25.009
_diffrn_reflns_theta_min         1.108
_exptl_absorpt_coefficient_mu    0.658
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6604
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1246 before and 0.0368 after correction.
The Ratio of minimum to maximum transmission is 0.8856.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.528
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3700
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.250
_refine_diff_density_min         -1.004
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1036
_refine_ls_number_reflns         13957
_refine_ls_number_restraints     71
_refine_ls_restrained_S_all      1.193
_refine_ls_R_factor_all          0.0730
_refine_ls_R_factor_gt           0.0596
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0934P)^2^+23.7293P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1683
_refine_ls_wR_factor_ref         0.1823
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11246
_reflns_number_total             13957
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nj00276a2.cif
_cod_data_source_block           n130305a
_cod_original_cell_volume        7920(2)
_cod_original_formula_sum        'C80.50 H73 Ag2 Cl F12 N8 O8 P2'
_cod_database_code               7056116
_shelx_estimated_absorpt_t_max   0.902
_shelx_estimated_absorpt_t_min   0.837
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 Cl1-Cl2
 2.55 with sigma of 0.01
 Cl1-C81 = Cl2-C81
 1.78 with sigma of 0.01
 C69-C68
 1.46 with sigma of 0.01
3. Rigid bond restraints
 P1, F4
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 P2, F7
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 P2, F8
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 P2, F9
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 P2, F10
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 P2, F11
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 P2, F12
 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(C81) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F4) \\sim Ueq, Uanis(F8) \\sim Ueq, Uanis(F9) \\sim Ueq, Uanis(F11) \\sim
Ueq, Uanis(F12) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C43) \\sim Ueq,
Uanis(C44) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.002
Uanis(F7) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.002
5. Others
 Fixed Sof: Cl1(0.5) Cl2(0.5) C81(0.5) H81A(0.5) H81B(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C28(H28A,H28B),
 C29(H29A,H29B), C30(H30A,H30B), C34(H34A,H34B), C47(H47A,H47B), C51(H51A,H51B),
  C52(H52A,H52B), C53(H53A,H53B), C68(H68A,H68B), C69(H69A,H69B), C70(H70A,
 H70B), C74(H74A,H74B), C81(H81A,H81B)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C18(H18), C19(H19),
 C20(H20), C21(H21), C26(H26), C27(H27), C31(H31), C32(H32), C36(H36), C37(H37),
  C38(H38), C39(H39), C40(H40), C42(H42), C43(H43), C44(H44), C45(H45),
 C46(H46), C49(H49), C50(H50), C55(H55), C56(H56), C61(H61), C62(H62), C63(H63),
  C64(H64), C72(H72), C73(H73), C76(H76), C77(H77), C78(H78), C79(H79), C80(H80)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'