Heterometallic Ag<sub>2</sub>Ti<sub>10</sub> and Ag<sub>4</sub>Ti<sub>8</sub>-oxo clusters with different silver doping models: synthesis, structure, and theoretical studies.
Hou, Simin; Li, Qiaohong; Ding, Qing-Rong; Kang, Yao; Zhang, Jian; Zhang, Lei; Dalton transactions (Cambridge, England : 2003) 49 (2020) 11005–11009; doi:10.1039/d0dt02396e

data_7704826
_publ_section_title
;
 Heterometallic Ag<sub>2</sub>Ti<sub>10</sub> and
 Ag<sub>4</sub>Ti<sub>8</sub>-oxo clusters with different silver doping
 models: synthesis, structure, and theoretical studies.
;
_journal_issue                   31
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11005
_journal_page_last               11009
_journal_paper_doi               10.1039/d0dt02396e
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C132 H86 Ag2 O58 Ti10'
_chemical_formula_sum            'C132 H86 Ag2 O58 Ti10'
_chemical_formula_weight         3294.74
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2020-03-03
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2020-03-25 deposited with the CCDC.	2020-07-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.069(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.4863(2)
_cell_length_b                   45.3078(6)
_cell_length_c                   19.2032(3)
_cell_measurement_reflns_used    16065
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      69.6630
_cell_measurement_theta_min      4.2650
_cell_volume                     13124.9(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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_environment      N~2~
_diffrn_ambient_temperature      100.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2083
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.979
_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    -21.00  69.00   1.00    1.80    --    0.00  57.00-180.00   90
  2  \w     37.00  65.00   1.00    1.80    --    0.00  38.00 -30.00   28
  3  \w    -19.00   7.00   1.00    1.80    --    0.00  38.00 -30.00   26
  4  \w     30.00  84.00   1.00    7.21    --   54.00-125.00 -90.00   54
  5  \w     11.00 127.00   1.00    7.21    --   54.00  19.00   0.00  116
  6  \w     -5.00  74.00   1.00    7.21    --   54.00 -57.00  90.00   79
  7  \w     29.00  66.00   1.00    7.21    --   54.00-125.00  30.00   37
  8  \w     71.00 106.00   1.00    7.21    --  108.00-111.00   0.00   35
  9  \w     82.00 174.00   1.00    7.21    --  108.00  77.00 -60.00   92
 10  \w     42.00  85.00   1.00    7.21    --  108.00-111.00 -30.00   43
 11  \w     97.00 169.00   1.00    7.21    --  108.00  63.00   0.00   72
 12  \w     50.00 143.00   1.00    7.21    --  108.00 -91.00 150.00   93
 13  \w    115.00 170.00   1.00    7.21    --  108.00 109.00-123.00   55
 14  \w     81.00 171.00   1.00    7.21    --  108.00  77.00 -90.00   90
 15  \w    115.00 173.00   1.00    7.21    --  108.00  63.00 -30.00   58
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0269127000
_diffrn_orient_matrix_UB_12      0.0327990000
_diffrn_orient_matrix_UB_13      0.0052693000
_diffrn_orient_matrix_UB_21      -0.0529244000
_diffrn_orient_matrix_UB_22      0.0049706000
_diffrn_orient_matrix_UB_23      -0.0772765000
_diffrn_orient_matrix_UB_31      -0.0830122000
_diffrn_orient_matrix_UB_32      0.0074846000
_diffrn_orient_matrix_UB_33      0.0280898000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0647
_diffrn_reflns_av_unetI/netI     0.0806
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -55
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            51803
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.484
_diffrn_reflns_theta_min         3.462
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.075
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.02587
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear reddish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.667
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             6624
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.201
_refine_diff_density_min         -1.543
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1839
_refine_ls_number_reflns         24602
_refine_ls_number_restraints     784
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.1214
_refine_ls_R_factor_gt           0.0899
_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^)+(0.1200P)^2^+73.9101P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2289
_refine_ls_wR_factor_ref         0.2544
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17960
_reflns_number_total             24602
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02396e2.cif
_cod_data_source_block           a
_cod_depositor_comments
'Adding full bibliography for 7704826--7704827.cif.'
_cod_database_code               7704826
_shelx_shelxl_version_number     2017/1
_reflns_odcompleteness_completeness 99.68
_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, All O(H) groups
2. Restrained distances
 O01Y-H01Y
 0.85 with sigma of 0.01
 C05L-C05N
 1.5 with sigma of 0.02
 C04U-H01Y
 1.87382 with sigma of 0.02
 Ti08-H01Y
 2.362503 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C01Z \\sim C020 \\sim C022 \\sim C023 \\sim C024 \\sim C025 \\sim C026 \\sim
C027 \\sim C028 \\sim C029 \\sim C02A \\sim C02B \\sim C02C \\sim C02D \\sim
C02E \\sim C02F \\sim C02G \\sim C02H \\sim C02I \\sim C02J \\sim C02K \\sim
C02L \\sim C02M \\sim C02N \\sim C02O \\sim C02P \\sim C02Q \\sim C02R \\sim
C02S \\sim C02T \\sim C02U \\sim C02V \\sim C02W \\sim C02X \\sim C02Y \\sim
C02Z \\sim C030 \\sim C031 \\sim C032 \\sim C033 \\sim C034 \\sim C035 \\sim
C036 \\sim C037 \\sim C038 \\sim C039 \\sim C03A \\sim C03B \\sim C03C \\sim
C03D \\sim C03E \\sim C03F \\sim C03G \\sim C03H \\sim C03I \\sim C03J \\sim
C03K \\sim C03L \\sim C03M \\sim C03N \\sim C03O \\sim C03P \\sim C03Q \\sim
C03R \\sim C03S \\sim C03T \\sim C03U \\sim C03V \\sim C03W \\sim C03X \\sim
C03Y \\sim C03Z \\sim C040 \\sim C041 \\sim C042 \\sim C043 \\sim C044 \\sim
C045 \\sim C046 \\sim C047 \\sim C048 \\sim C049 \\sim C04A \\sim C04B \\sim
C04C \\sim C04D \\sim C04E \\sim C04F \\sim C04G \\sim C04H \\sim C04I \\sim
C04J \\sim C04K \\sim C04L \\sim C04M \\sim C04N \\sim C04O \\sim C04P \\sim
C04Q \\sim C04R \\sim C04S \\sim C04T \\sim C04U \\sim C04V \\sim C04W \\sim
C04X \\sim C04Y \\sim C04Z \\sim C050 \\sim C051 \\sim C052 \\sim C053 \\sim
C054 \\sim C055 \\sim C056 \\sim C057 \\sim C059 \\sim C05A \\sim C05B \\sim
C05C \\sim C05D \\sim C05E \\sim C05F \\sim C05G \\sim C05H \\sim C05I \\sim
C05J \\sim C05K \\sim C05L \\sim C05M \\sim C05N \\sim C06A: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
4. Others
 Sof(Ag1A)=1-FVAR(1)
 Sof(Ag1)=FVAR(1)
 Sof(Ag2A)=1-FVAR(2)
 Sof(Ag2)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 C05L(H05n)
5.b Me refined with riding coordinates:
 C05N(H05r,H05s,H05t), C06A(H06a,H06b,H06c)
5.c Aromatic/amide H refined with riding coordinates:
 C02C(H02C), C02F(H02F), C02J(H02J), C02P(H02P), C02Q(H02Q), C02R(H02R),
 C02W(H02W), C02X(H02X), C02Z(H02Z), C030(H030), C035(H035), C036(H036),
 C03B(H03B), C03C(H03C), C03E(H03E), C03H(H03H), C03M(H03M), C03N(H03N),
 C03O(H03O), C03P(H03P), C03Q(H03Q), C03S(H03S), C03U(H03U), C03V(H03V),
 C03Y(H03Y), C040(H040), C041(H041), C042(H042), C043(H043), C046(H046),
 C047(H047), C048(H048), C049(H049), C04A(H04A), C04B(H04B), C04C(H04C),
 C04E(H04E), C04F(H04F), C04G(H04G), C04I(H04I), C04J(H04J), C04K(H04K),
 C04L(H04L), C04M(H04M), C04N(H04N), C04P(H04P), C04Q(H04Q), C04R(H04R),
 C04S(H04S), C04T(H04T), C04V(H04V), C04W(H04W), C04Y(H04Y), C04Z(H04Z),
 C050(H050), C052(H052), C053(H053), C054(H054), C055(H055), C056(H056),
 C057(H057), C059(H059), C05A(H05A), C05B(H05B), C05C(H05C), C05D(H05D),
 C05F(H05h), C05G(H05i), C05H(H05j), C05I(H05k), C05J(H05l), C05K(H05m)
5.d Idealised Me refined as rotating group:
 C05E(H05e,H05f,H05g), C05M(H05o,H05p,H05q)
;
_shelx_res_checksum              60785
_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 27.241
_oxdiff_exptl_absorpt_empirical_full_min 0.412