A twist on a classic scaffold: rational design of a new bimetallic platform.
Rumi, Sultana P.; Zakharov, Lev N.; Desnoyer, Addison N.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 18828–18833; doi:10.1039/d4dt01840k

data_7716786
_publ_section_title
;
 A twist on a classic scaffold: rational design of a new bimetallic
 platform.
;
_journal_issue                   47
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              18828
_journal_page_last               18833
_journal_paper_doi               10.1039/d4dt01840k
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C50 H114 N8 O2 Si4 Ti2'
_chemical_formula_sum            'C50 H114 N8 O2 Si4 Ti2'
_chemical_formula_weight         1067.65
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2024-06-19
_audit_creation_method
;
Olex2 1.5
(compiled 2024.01.12 svn.r2f8d729c for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-06-24 deposited with the CCDC.	2024-07-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.737(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.8754(3)
_cell_length_b                   13.7638(2)
_cell_length_c                   18.1998(3)
_cell_measurement_reflns_used    9890
_cell_measurement_temperature    172.99(10)
_cell_measurement_theta_max      75.5610
_cell_measurement_theta_min      4.1370
_cell_volume                     3228.62(11)
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      172.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.957
_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    -51.00  -9.00   1.00    2.00    --  -47.14 120.00 158.00   42
  2  \w    -81.00 -54.00   1.00    2.00    --  -47.14 120.00 158.00   27
  3  \w   -119.00 -68.00   1.00    2.00    --  -47.14-153.00 -83.00   51
  4  \w     37.00  62.00   1.00    2.00    --   47.14-120.00  74.00   25
  5  \w   -138.00-101.00   1.00   10.00    --  -86.25-120.00  74.00   37
  6  \w     99.00 164.00   1.00   10.00    --  104.22 120.00 158.00   65
  7  \w     90.00 115.00   1.00   10.00    --  104.22-153.00 -83.00   25
  8  \w     98.00 123.00   1.00   10.00    --  104.22 153.00 -43.00   25
  9  \w     46.00  71.00   1.00   10.00    --  104.22-120.00  74.00   25
 10  \w   -119.00 -85.00   1.00    2.00    --  -47.14 -77.00 -60.00   34
 11  \w   -117.00 -92.00   1.00    2.00    --  -47.14 -77.00 -90.00   25
 12  \w     87.00 118.00   1.00    2.00    --   47.14  77.00  90.00   31
 13  \w     92.00 117.00   1.00    2.00    --   47.14  77.00-150.00   25
 14  \w     86.00 112.00   1.00    2.00    --   47.14  77.00 -30.00   26
 15  \w     86.00 113.00   1.00    2.00    --   47.14  77.00  60.00   27
 16  \w     86.00 112.00   1.00    2.00    --   47.14  77.00  30.00   26
 17  \w    -51.00 -16.00   1.00   10.00    --  -86.25  45.00 -90.00   35
 18  \w    -49.00 -17.00   1.00   10.00    --  -86.25  45.00   0.00   32
 19  \w   -157.00-109.00   1.00   10.00    --  -86.25 -94.00 -60.00   48
 20  \w   -125.00-100.00   1.00   10.00    --  -86.25-153.00 -83.00   25
 21  \w    -45.00 -19.00   1.00   10.00    --  -86.25  45.00 -60.00   26
 22  \w    -49.00 -20.00   1.00   10.00    --  -86.25  45.00 -30.00   29
 23  \w     92.00 176.00   1.00   10.00    --  104.22  45.00 -30.00   84
 24  \w     45.00  70.00   1.00   10.00    --  104.22 -61.00 150.00   25
 25  \w     32.00  70.00   1.00   10.00    --  104.22 -61.00  90.00   38
 26  \w     77.00 107.00   1.00   10.00    --  104.22-125.00 120.00   30
 27  \w     32.00  64.00   1.00   10.00    --  104.22 -61.00 120.00   32
 28  \w     35.00 102.00   1.00   10.00    --  104.22 -94.00-180.00   67
 29  \w     38.00  70.00   1.00   10.00    --  104.22-125.00 120.00   32
 30  \w     32.00 106.00   1.00   10.00    --  104.22 -94.00  90.00   74
 31  \w     42.00 100.00   1.00   10.00    --  104.22 -77.00  90.00   58
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1055659000
_diffrn_orient_matrix_UB_12      0.0501091000
_diffrn_orient_matrix_UB_13      -0.0419050000
_diffrn_orient_matrix_UB_21      -0.0548960000
_diffrn_orient_matrix_UB_22      -0.0991707000
_diffrn_orient_matrix_UB_23      -0.0105855000
_diffrn_orient_matrix_UB_31      -0.0120631000
_diffrn_orient_matrix_UB_32      0.0131550000
_diffrn_orient_matrix_UB_33      0.0802109000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0442
_diffrn_reflns_av_unetI/netI     0.0395
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            25746
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.885
_diffrn_reflns_theta_min         3.429
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.112
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56181
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.098
_exptl_crystal_description       block
_exptl_crystal_F_000             1172
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.430
_refine_diff_density_min         -0.330
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         6443
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0616
_refine_ls_R_factor_gt           0.0470
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0288P)^2^+4.6180P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1001
_refine_ls_wR_factor_ref         0.1193
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5425
_reflns_number_total             6443
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01840k2.cif
_cod_data_source_block           and12_auto
_cod_depositor_comments
'Adding full bibliography for 7716783--7716789.cif.'
_cod_original_cell_volume        3228.59(11)
_cod_database_code               7716786
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         C21H60H8Si4Ti2
_shelx_estimated_absorpt_t_max   0.886
_shelx_estimated_absorpt_t_min   0.455
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5A,H5B), C2(H2A,H2B), C1(H1A,H1B), C22(H22A,H22B), C25(H25A,
 H25B), C24(H24A,H24B), C23(H23A,H23B)
2.b Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C13(H13A,H13B,
 H13C), C6(H6A,H6B,H6C), C12(H12A,H12B,H12C), C9(H9A,H9B,H9C), C7(H7A,H7B,H7C),
 C11(H11A,H11B,H11C), C10(H10A,H10B,H10C), C26A(H26A,H26B,H26C)
;
_shelx_res_checksum              50260
_shelx_hkl_checksum              998
_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 2.053
_oxdiff_exptl_absorpt_empirical_full_min 0.680