Near-Infrared Emitters: Stepwise Assembly of Two Heteropolynuclear Clusters with Tunable Ag(I):Zn(II) Ratio.
Wang, Zhi; Zhuang, Gui-Lin; Deng, Yong-Kai; Feng, Zhen-Yu; Cao, Zhao-Zhen; Kurmoo, Mohamedally; Tung, Chen-Ho; Sun, Di; Inorganic chemistry 55 (2016) 4757–4763; doi:10.1021/acs.inorgchem.6b00044

data_4347344
_publ_section_title
;
 Near-Infrared Emitters: Stepwise Assembly of Two Heteropolynuclear
 Clusters with Tunable Ag(I):Zn(II) Ratio.
;
_journal_issue                   10
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4757
_journal_page_last               4763
_journal_paper_doi               10.1021/acs.inorgchem.6b00044
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety
'C113 H81 Ag9 N10 O21 S9 Zn4, C30 H24 N6 Zn, 2(C10 H8 N2)'
_chemical_formula_sum            'C163 H121 Ag9 N20 O21 S9 Zn5'
_chemical_formula_weight         4282.01
_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   mixed
_audit_creation_date             2016-03-13
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                107.385(4)
_cell_angle_beta                 104.141(3)
_cell_angle_gamma                105.049(4)
_cell_formula_units_Z            2
_cell_length_a                   20.2213(9)
_cell_length_b                   20.5331(12)
_cell_length_c                   26.3995(12)
_cell_measurement_reflns_used    6128
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      67.532
_cell_measurement_theta_min      2.417
_cell_volume                     9465.5(9)
_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-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.940
_diffrn_measured_fraction_theta_max 0.940
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1521
_diffrn_reflns_av_unetI/netI     0.2001
_diffrn_reflns_Laue_measured_fraction_full 0.940
_diffrn_reflns_Laue_measured_fraction_max 0.940
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            83805
_diffrn_reflns_point_group_measured_fraction_full 0.940
_diffrn_reflns_point_group_measured_fraction_max 0.940
_diffrn_reflns_theta_full        64.999
_diffrn_reflns_theta_max         64.999
_diffrn_reflns_theta_min         1.871
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.393
_exptl_absorpt_correction_T_max  0.6509
_exptl_absorpt_correction_T_min  0.4247
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.502
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4248
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.218
_refine_diff_density_min         -1.366
_refine_diff_density_rms         0.184
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.865
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1950
_refine_ls_number_reflns         30270
_refine_ls_number_restraints     300
_refine_ls_restrained_S_all      0.861
_refine_ls_R_factor_all          0.1815
_refine_ls_R_factor_gt           0.0941
_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^)+(0.1253P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2185
_refine_ls_wR_factor_ref         0.2578
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12300
_reflns_number_total             30270
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00044_si_002.cif
_cod_data_source_block           Ag9Zn4
_cod_database_code               4347344
_shelx_estimated_absorpt_t_max   0.651
_shelx_estimated_absorpt_t_min   0.425
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
N10 \\sim C103 \\sim C102 \\sim C99 \\sim C100 \\sim C101 \\sim C98 \\sim C96
\\sim C97 \\sim C95 \\sim C94 \\sim N9: within 1.7A with sigma of 0.004 and
sigma for terminal atoms of 0.08
N8 \\sim C93 \\sim C92 \\sim C91 \\sim C90 \\sim C89 \\sim C88 \\sim N7 \\sim
C84 \\sim C85 \\sim C86 \\sim C87: within 1.7A with sigma of 0.004 and sigma
for terminal atoms of 0.08
C143 \\sim C142 \\sim C141 \\sim C140 \\sim C139 \\sim N15 \\sim N16 \\sim C138
\\sim C137 \\sim C136 \\sim C135 \\sim C134: within 1.7A with sigma of 0.004
and sigma for terminal atoms of 0.08
C126 \\sim C127 \\sim C128 \\sim N13 \\sim N14 \\sim C130 \\sim C129 \\sim C124
\\sim C131 \\sim C133 \\sim C125: within 1.7A with sigma of 0.002 and sigma for
terminal atoms of 0.08
3.a Riding coordinates:
 O17(H17)
3.b Rotating group:
 O3(H3A,H3B), O6(H6A,H6B)
3.c Aromatic/amide H refined with riding coordinates:
 C84(H84), C85(H85), C86(H86), C87(H87), C97(H97), C96(H96), C95(H95),
 C94(H94), C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10),
 C13(H13), C14(H14), C15(H15), C16(H16), C20(H20), C21(H21), C22(H22), C23(H23),
  C26(H26), C27(H27), C28(H28), C29(H29), C34(H34), C35(H35), C36(H36),
 C37(H37), C42(H42), C43(H43), C44(H44), C45(H45), C48(H48), C49(H49), C50(H50),
  C51(H51), C56(H56), C57(H57), C58(H58), C59(H59), C63(H63), C64(H64),
 C65(H65), C66(H66), C70(H70), C71(H71), C72(H72), C73(H73), C74(H74), C75(H75),
  C76(H76), C77(H77), C80(H80), C81(H81), C82(H82), C83(H83), C93(H93),
 C90(H90), C91(H91), C92(H92), C103(H103), C102(H102), C101(H101), C100(H100),
 C104(H104), C105(H105), C106(H106), C107(H107), C110(H110), C111(H111),
 C112(H112), C113(H113), C137(H137), C134(H134), C135(H135), C136(H136),
 C140(H140), C141(H141), C142(H142), C143(H143), C144(H144), C145(H145),
 C146(H146), C147(H147), C150(H150), C151(H151), C152(H152), C153(H153),
 C154(H154), C155(H155), C156(H156), C157(H157), C160(H160), C161(H161),
 C162(H162), C163(H163), C114(H114), C115(H115), C116(H116), C117(H117),
 C120(H120), C121(H121), C122(H122), C123(H123), C130(H130), C131(H131),
 C132(H132), C133(H133), C126(H126), C127(H127), C124(H124), C125(H125)
3.d Fitted hexagon refined as free rotating group:
 N7(C84,C85,C86,C87,C88), N9(C98,C97,C96,C95,C94), C93(N8,C89,C90,C91,C92),
 C103(C102,C101,C100,C99,N10), C137(C138,N16,C134,C135,C136), C139(C140,C141,
 C142,C143,N15), N13(C129,C130,C131,C132,C133), C126(C127,C128,N14,C124,C125)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'