A series of silver doped butterfly-like Ti<sub>8</sub>Ag<sub>2</sub> clusters with two Ag ions panelled on a Ti<sub>8</sub> surface.
Yu, You-Zhu; Guo, Yao; Zhang, Yan-Ru; Liu, Min-Min; Feng, Ya-Ru; Geng, Cui-Huan; Zhang, Xian-Ming; Dalton transactions (Cambridge, England : 2003) 48 (2019) 13423–13429; doi:10.1039/c9dt02508a

data_7700762
_publ_section_title
;
 A series of silver doped butterfly-like Ti<sub>8</sub>Ag<sub>2</sub>
 clusters with two Ag ions panelled on a Ti<sub>8</sub> surface.
;
_journal_issue                   35
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13423
_journal_page_last               13429
_journal_paper_doi               10.1039/c9dt02508a
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C134 H100 Ag2 O38 P2 Ti8, 2(C2 H3 N)'
_chemical_formula_sum            'C138 H106 Ag2 N2 O38 P2 Ti8'
_chemical_formula_weight         3061.12
_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
_audit_creation_date             2019-07-17
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-07-17 deposited with the CCDC.    2019-08-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.723(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.2611(3)
_cell_length_b                   18.0847(5)
_cell_length_c                   26.3595(8)
_cell_measurement_reflns_used    4778
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      72.2210
_cell_measurement_theta_min      5.0520
_cell_volume                     6790.6(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0710
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -20.00  22.00   1.00    3.72    --    0.00  57.00-180.00   42
  2  \w    -74.00 -49.00   1.00    3.72    --    0.00 178.00   0.00   25
  3  \w    -72.00 -46.00   1.00    3.72    --    0.00 178.00 -60.00   26
  4  \w     39.00  68.00   1.00    3.72    --    0.00  57.00-180.00   29
  5  \w     35.00 124.00   1.00    3.89    --   55.26  57.00-180.00   89
  6  \w     50.00  76.00   1.00    3.89    --   55.26  57.00  30.00   26
  7  \w     39.00 124.00   1.00    3.89    --   55.26  57.00  60.00   85
  8  \w    -12.00  76.00   1.00    3.89    --   55.26 -57.00 -90.00   88
  9  \w    136.00 178.00   1.00    4.00    --  110.51  50.00  90.00   42
 10  \w     89.00 116.00   1.00    4.00    --  110.51  50.00  90.00   27
 11  \w     46.00  71.00   1.00    4.00    --  110.51-111.00-120.00   25
 12  \w     45.00 127.00   1.00    4.00    --  110.51 -64.00 -90.00   82
 13  \w     39.00 114.00   1.00    4.00    --  110.51-111.00  90.00   75
 14  \w     44.00 115.00   1.00    4.00    --  110.51-111.00 -60.00   71
 15  \w     89.00 116.00   1.00    4.00    --  110.51  25.00  90.00   27
 16  \w     56.00 123.00   1.00    4.00    --  110.51 -50.00  60.00   67
 17  \w     92.00 137.00   1.00    4.00    --  110.51  50.00 120.00   45
 18  \w     61.00 119.00   1.00    4.00    --  110.51 -92.00 150.00   58
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0386705000
_diffrn_orient_matrix_UB_12      -0.0631861000
_diffrn_orient_matrix_UB_13      0.0321800000
_diffrn_orient_matrix_UB_21      0.1006875000
_diffrn_orient_matrix_UB_22      -0.0201561000
_diffrn_orient_matrix_UB_23      0.0188575000
_diffrn_orient_matrix_UB_31      -0.0078015000
_diffrn_orient_matrix_UB_32      0.0535316000
_diffrn_orient_matrix_UB_33      0.0450472000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0388
_diffrn_reflns_av_unetI/netI     0.0589
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            26992
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.444
_diffrn_reflns_theta_min         3.950
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.943
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.32922
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.32a (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.497
_exptl_crystal_description       block
_exptl_crystal_F_000             3104
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.651
_refine_diff_density_min         -0.582
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     785
_refine_ls_number_reflns         13157
_refine_ls_number_restraints     673
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0806
_refine_ls_R_factor_gt           0.0511
_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^)+(0.0616P)^2^+3.3948P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1252
_refine_ls_wR_factor_ref         0.1458
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9115
_reflns_number_total             13157
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02508a2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7700762--7700767.cif.'
_cod_original_cell_volume        6790.7(3)
_cod_database_code               7700762
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C H O N P Ag Ti '
_shelx_estimated_absorpt_t_max   0.516
_shelx_estimated_absorpt_t_min   0.276
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N1-C69
 1.15 with sigma of 0.01
 C68-C69
 1.47 with sigma of 0.01
3. Rigid bond restraints
 O18, C61
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C6, C7
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C18, C19
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C1, C2, C3, C4, C5, C6, C7, C8, C9, C10, C11, C12, C13, C14, C15, C16, C17,
 C18, C19, C20, C21, C22, C23, C24, C25, C26, C27, C28, C29, C30, C31, C32, C33,
  C34, C35, C36, C37, C38, C39, C40, C41, C42, C43, C44, C45, C46, C47, C48,
 C49, C50, C51, C52, C53, C54, C55, C56, C57, C58, C59, C60, C61, C62, C63, C64,
  C65, C66, C67, C68, C69
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17
\\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25
\\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33
\\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41
\\sim C42 \\sim C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim C49
\\sim C50 \\sim C51 \\sim C52 \\sim C53 \\sim C54 \\sim C55 \\sim C56 \\sim C57
\\sim C58 \\sim C59 \\sim C60 \\sim C61 \\sim C62 \\sim C63 \\sim C64 \\sim C65
\\sim C66 \\sim C67 \\sim C68 \\sim C69: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C19) \\sim
Ueq, Uanis(C24) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C26) \\sim Ueq,
Uanis(C27) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C65)
\\sim Ueq, Uanis(C66) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.01
Uanis(O17) \\sim Ueq, Uanis(O19) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C23)
\\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(C55) \\sim Ueq,
Uanis(C62) \\sim Ueq, Uanis(C69) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.01
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C10(H10), C11(H11), C12(H12),
 C13(H13), C14(H14), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C24(H24),
  C25(H25), C26(H26), C27(H27), C28(H28), C31(H31), C32(H32), C33(H33),
 C34(H34), C35(H35), C37(H37), C38(H38), C39(H39), C40(H40), C41(H41), C43(H43),
  C44(H44), C45(H45), C46(H46), C47(H47), C49(H49), C50(H50), C51(H51),
 C52(H52), C53(H53), C56(H56), C57(H57), C58(H58), C59(H59), C60(H60), C63(H63),
  C64(H64), C65(H65), C66(H66), C67(H67)
5.b Fitted hexagon refined as free rotating group:
 C2(C3,C4,C5,C6,C7), C16(C17,C18,C19,C20,C21), C23(C24,C25,C26,C27,C28),
 C30(C31,C32,C33,C34,C35), C55(C56,C57,C58,C59,C60), C62(C63,C64,C65,C66,C67)
5.c Idealised Me refined as rotating group:
 C68(H68A,H68B,H68C)
;
_shelx_res_checksum              86767
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.410
_oxdiff_exptl_absorpt_empirical_full_min 0.733