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_7704827
_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         'C74 H132 Ag4 N2 O39 Ti8'
_chemical_formula_sum            'C70 H124 Ag4 N2 O39 Ti8'
_chemical_formula_weight         2432.38
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-04-10
_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                 100.439(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.5445(3)
_cell_length_b                   27.2039(6)
_cell_length_c                   25.2746(6)
_cell_measurement_reflns_used    5129
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      65.9750
_cell_measurement_theta_min      4.4610
_cell_volume                     10511.0(4)
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_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 0.992
_diffrn_measured_fraction_theta_max 0.985
_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    -33.00  17.00   1.00    1.50    --    0.00  77.00 -30.00   50
  2  \w    -77.00 -52.00   1.00    1.50    --    0.00 178.00 -60.00   25
  3  \w     18.00  68.00   1.00    1.50    --    0.00  77.00 -30.00   50
  4  \w     13.00  70.00   1.00    5.00    --   53.22 -38.00-180.00   57
  5  \w      9.00 121.00   1.00    5.00    --   53.22  19.00-180.00  112
  6  \w     -5.00  86.00   1.00    5.00    --   53.22 -77.00   0.00   91
  7  \w     56.00  94.00   1.00    5.00    --   53.22-129.00 -33.00   38
  8  \w     82.00 176.00   1.00    1.00    --  106.44  63.00-120.00   94
  9  \w     70.00 112.00   1.00    1.00    --  106.44-111.00 150.00   42
 10  \w     36.00 132.00   1.00    1.00    --  106.44 -50.00  90.00   96
 11  \w    103.00 147.00   1.00    1.00    --  106.44 -91.00  90.00   44
 12  \w     89.00 162.00   1.00    1.00    --  106.44  63.00-180.00   73
 13  \w     33.00  86.00   1.00    1.00    --  106.44 -91.00  90.00   53
 14  \w    115.00 161.00   1.00    1.00    --  106.44  50.00-150.00   46
 15  \w     64.00 151.00   1.00    1.00    --  106.44 178.00   0.00   87
;
_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      0.0026717000
_diffrn_orient_matrix_UB_12      0.0565299000
_diffrn_orient_matrix_UB_13      -0.0030353000
_diffrn_orient_matrix_UB_21      0.0273222000
_diffrn_orient_matrix_UB_22      0.0025839000
_diffrn_orient_matrix_UB_23      0.0616541000
_diffrn_orient_matrix_UB_31      0.0969558000
_diffrn_orient_matrix_UB_32      -0.0023010000
_diffrn_orient_matrix_UB_33      -0.0055938000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0383
_diffrn_reflns_av_unetI/netI     0.0516
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            18708
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.481
_diffrn_reflns_theta_min         3.507
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.362
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.46809
_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 light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.537
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             4936
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.767
_refine_diff_density_min         -0.925
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     565
_refine_ls_number_reflns         9525
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0850
_refine_ls_R_factor_gt           0.0617
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0900P)^2^+53.3330P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1625
_refine_ls_wR_factor_ref         0.1823
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7046
_reflns_number_total             9525
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02396e2.cif
_cod_data_source_block           hsm
_cod_depositor_comments
'Adding full bibliography for 7704826--7704827.cif.'
_cod_database_code               7704827
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         TiAgCONH
_shelx_estimated_absorpt_t_max   0.727
_shelx_estimated_absorpt_t_min   0.221
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     64.99
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C014(H01A,H01B,H01C), C015(H01D,H01E,H01F), C016(H01G,H01H,H01I), C019(H01J,
 H01K,H01L), C01A(H01M,H01N,H01O), C01C(H01P,H01Q,H01R), C01D(H01S,H01T,H01U),
 C01E(H01V,H01W,H01X), C01F(H01Y,H,HA), C01G(H01Z,HB,HC), C01H(H01,HD,HE),
 C01J(H0AA,HF,HG), C01K(H1AA,HH,HI), C01P(H2AA,HJ,HK), C01Q(H3AA,HL,HM),
 C01R(H4AA,HN,HO), C6AA(H6AA,H6AB,H6AC), C12(H12A,H12B,H12C), C6(H6A,H6B,H6C),
 C7(H7A,H7B,H7C), C1(H1A,H1B,H1C), C2(H2A,H2B,H2C)
;
_shelx_res_checksum              60940
_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 2.021
_oxdiff_exptl_absorpt_empirical_full_min 0.626