A stable silver metallacage with solvatochromic and mechanochromic behaviors for white LED fabrication
Lu, Zhixiang; Cheng, Yi; Fan, Wenwen; Yang, Shaoxiong; Liu, Xiaolan; Qin, Yu; Zhao, Ruidun; Zheng, Liyan; Zhang, Hongbin; Chemical Communications  (2019) –; doi:10.1039/C9CC03229K

data_7123659
_publ_section_title
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 A stable silver metallacage with solvatochromic and mechanochromic
 behaviors for white LED fabrication
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_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC03229K
_journal_year                    2019
_chemical_formula_moiety
'C108 H72 Ag4 N16, 2(N2 O6), 2(C4 H12 O2 S2), 29[H2O]'
_chemical_formula_sum            'C116 H98 Ag4 N20 O17 S4'
_chemical_formula_weight         2603.86
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-06-06
_audit_creation_method
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Olex2 1.3-dev
(compiled 2019.03.18 svn.r3573 for OlexSys, GUI svn.r5585)
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_audit_update_record
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2019-06-13 deposited with the CCDC.    2019-06-14 downloaded from the CCDC.
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_cell_angle_alpha                90
_cell_angle_beta                 94.433(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   20.3071(5)
_cell_length_b                   15.2401(3)
_cell_length_c                   22.2814(5)
_cell_measurement_reflns_used    9488
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      54.505
_cell_measurement_theta_min      3.061
_cell_volume                     6875.1(3)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      170.0
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.14
_diffrn_reflns_av_unetI/netI     0.2365
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            55494
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         55.057
_diffrn_reflns_theta_min         3.059
_exptl_absorpt_coefficient_mu    3.715
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.2289
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.2090 before and 0.1009 after correction.
The Ratio of minimum to maximum transmission is 0.3049.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.258
_exptl_crystal_description       block
_exptl_crystal_F_000             2644
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         4.699
_refine_diff_density_min         -2.668
_refine_diff_density_rms         0.306
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     713
_refine_ls_number_reflns         12987
_refine_ls_number_restraints     654
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.2270
_refine_ls_R_factor_gt           0.1868
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4155
_refine_ls_wR_factor_ref         0.4423
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5646
_reflns_number_total             12987
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc03229k2.cif
_cod_data_source_block           mjl18523_0m
_cod_database_code               7123659
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.929
_shelx_estimated_absorpt_t_min   0.836
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C54) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C48) \\sim Ueq, Uanis(C25)
\\sim Ueq, Uanis(C49) \\sim Ueq, Uanis(C29) \\sim Ueq: with sigma of 0.005 and
sigma for terminal atoms of 0.01
3. Rigid body (RIGU) restrains
 Ag02, Ag01, N5, N7, C48, C49, C28, C30, N6, C45, C50, C54, N8, C25, C29, C31,
 C43, C46, C51, C53, C24, C26, C34, C32, C44, C47, C52, C23, C27, C33, C42, C22,
  C41, C21, C38, C18, C37, C39, C17, C19, C36, C40, C16, C20, C35, C15, C1, C8,
 N3, N4, N1, N2, C7, C2, C14, C9, C6, C3, C13, C10, C5, C4, C12, C11
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N10, O1, O2, O3
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O5, N9, O6, O7
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 S1, O4, C58, C57, H58A, H58B, H58C, H57A, H57B, H57C
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 S2, O9, C56, C55
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Fixed U11: C5(0.056546) C6(0.056546)
 Fixed U12: C5(-0.007036) C6(-0.007036)
 Fixed U13: C5(-0.006797) C6(-0.006797)
 Fixed U22: C5(0.05691) C6(0.05691)
 Fixed U23: C5(0.00265) C6(0.00265)
 Fixed U33: C5(0.05844) C6(0.05844)
5.a Aromatic/amide H refined with riding coordinates:
 N1(H1), N4(H4), N6(H6), N8(H8), C3(H3), C4(H4A), C5(H5), C6(H6A), C10(H10),
 C11(H11), C12(H12), C13(H13), C16(H16), C17(H17), C19(H19), C20(H20), C23(H23),
  C24(H24), C26(H26), C27(H27), C31(H31), C32(H32), C33(H33), C34(H34),
 C36(H36), C37(H37), C39(H39), C40(H40), C43(H43), C44(H44), C46(H46), C47(H47),
  C50(H50), C51(H51), C52(H52), C53(H53)
5.b Idealised Me refined as rotating group:
 C58(H58A,H58B,H58C), C57(H57A,H57B,H57C), C56(H56A,H56B,H56C), C55(H55A,H55B,
 H55C)
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_smtbx_masks_special_details
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A solvent mask was calculated and 575 electrons were 
found in a volume of 1763\%A^3 in 1 void per UNIT CELL.
This is consistent with the presence of 
29[H2O] per Formula Unit which account for 580 electrons found in the cell.
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_smtbx_masks_void_probe_radius   1.5
_smtbx_masks_void_truncation_radius 1.5
_olex2_submission_special_instructions 'No special instructions were received'