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_7700766
_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         'C140 H112 Ag2 O38 P2 Ti8, 2(C2 H3 N)'
_chemical_formula_sum            'C144 H118 Ag2 N2 O38 P2 Ti8'
_chemical_formula_weight         3145.28
_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
_audit_creation_date             2019-07-11
_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                67.905(6)
_cell_angle_beta                 82.025(5)
_cell_angle_gamma                65.532(6)
_cell_formula_units_Z            1
_cell_length_a                   14.2246(9)
_cell_length_b                   15.4590(9)
_cell_length_c                   18.8915(11)
_cell_measurement_reflns_used    7061
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      72.0470
_cell_measurement_theta_min      4.9230
_cell_volume                     3502.7(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_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 0.975
_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     13.00  60.00   1.00    5.84    --    0.00  57.00-150.00   47
  2  \w    -68.00 -34.00   1.00    5.84    --    0.00 178.00-120.00   34
  3  \w     10.00  42.00   1.00    5.84    --    0.00 -99.00 -30.00   32
  4  \w     34.00  66.00   1.00    5.84    --    0.00  77.00 120.00   32
  5  \w    -30.00  30.00   1.00    5.84    --    0.00  77.00 120.00   60
  6  \w     27.00 124.00   1.00   23.34    --   54.94  77.00 -90.00   97
  7  \w     90.00 125.00   1.00   23.34    --   54.94 156.00 150.00   35
  8  \w     24.00 110.00   1.00   23.34    --   54.94-125.00 150.00   86
  9  \w     17.00 128.00   1.00   23.34    --   54.94  19.00  60.00  111
 10  \w     30.00  66.00   1.00   23.34    --   54.94 -57.00 -90.00   36
 11  \w     37.00  62.00   1.00   23.34    --   54.94  57.00-180.00   25
 12  \w    -13.00  70.00   1.00   23.34    --   54.94 -57.00 150.00   83
 13  \w    -12.00  24.00   1.00   23.34    --   54.94 -57.00  60.00   36
 14  \w     41.00  67.00   1.00    5.00    --  109.89-111.00 120.00   26
 15  \w     40.00 115.00   1.00    5.00    --  109.89-111.00  90.00   75
 16  \w     90.00 115.00   1.00    5.00    --  109.89-111.00-180.00   25
 17  \w     40.00 133.00   1.00    5.00    --  109.89 -38.00 -90.00   93
 18  \w     98.00 133.00   1.00    5.00    --  109.89 -77.00 -90.00   35
 19  \w     43.00 135.00   1.00    5.00    --  109.89 -38.00  60.00   92
 20  \w     63.00 101.00   1.00    5.00    --  109.89-111.00 -90.00   38
 21  \w    113.00 139.00   1.00    5.00    --  109.89 111.00-120.00   26
 22  \w    102.00 128.00   1.00    5.00    --  109.89 111.00 150.00   26
 23  \w    136.00 177.00   1.00    5.00    --  109.89  64.00-150.00   41
 24  \w     48.00 130.00   1.00    5.00    --  109.89 -50.00-180.00   82
 25  \w     63.00 105.00   1.00    5.00    --  109.89-111.00   0.00   42
 26  \w     88.00 128.00   1.00    5.00    --  109.89  64.00-150.00   40
 27  \w     56.00 131.00   1.00    5.00    --  109.89 -77.00  90.00   75
 28  \w     56.00  91.00   1.00    5.00    --  109.89 -77.00 -90.00   35
 29  \w     38.00 176.00   1.00    5.00    --  109.89  12.00 -30.00  138
;
_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      0.0548186000
_diffrn_orient_matrix_UB_12      -0.1079054000
_diffrn_orient_matrix_UB_13      0.0578876000
_diffrn_orient_matrix_UB_21      0.0257484000
_diffrn_orient_matrix_UB_22      -0.0428413000
_diffrn_orient_matrix_UB_23      -0.0651230000
_diffrn_orient_matrix_UB_31      0.1024505000
_diffrn_orient_matrix_UB_32      0.0148637000
_diffrn_orient_matrix_UB_33      -0.0125386000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_av_unetI/netI     0.0489
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            24469
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.141
_diffrn_reflns_theta_min         3.414
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.746
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.31481
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.27b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.491
_exptl_crystal_description       block
_exptl_crystal_F_000             1600
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.920
_refine_diff_density_min         -1.076
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     875
_refine_ls_number_reflns         13449
_refine_ls_number_restraints     79
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0642
_refine_ls_R_factor_gt           0.0506
_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^)+(0.0702P)^2^+2.7852P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1316
_refine_ls_wR_factor_ref         0.1434
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10810
_reflns_number_total             13449
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02508a2.cif
_cod_data_source_block           6
_cod_depositor_comments
'Adding full bibliography for 7700762--7700767.cif.'
_cod_database_code               7700766
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C H O N P Ag Ti'
_shelx_estimated_absorpt_t_max   0.376
_shelx_estimated_absorpt_t_min   0.263
_reflns_odcompleteness_completeness 99.85
_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-C71
 1.15 with sigma of 0.01
 C71-C72
 1.47 with sigma of 0.01
3. Rigid bond restraints
 C4, C5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C3, C4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C5, C6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C54, C56
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C51, C52
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(O14) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C32)
\\sim Ueq, Uanis(C47) \\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(C67) \\sim Ueq,
Uanis(C2) \\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C54) \\sim Ueq, Uanis(C71)
\\sim Ueq, Uanis(N1) \\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), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42), C44(H44),
  C46(H46), C47(H47), C48(H48), C51(H51), C52(H52), C53(H53), C55(H55),
 C58(H58), C60(H60), C61(H61), C62(H62), C66(H66), C67(H67), C68(H68), C69(H69),
  C70(H70)
5.b Fitted hexagon refined as free rotating group:
 C30(C31,C32,C33,C34,C35)
5.c Idealised Me refined as rotating group:
 C49(H49A,H49B,H49C), C56(H56A,H56B,H56C), C63(H63A,H63B,H63C), C72(H72A,H72B,
 H72C)
;
_shelx_res_checksum              78035
_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 2.639
_oxdiff_exptl_absorpt_empirical_full_min 0.647