Synergistic ligand effect for the construction of titanium-oxo clusters with planar chirality and high solution stability.
Ding, Qing-Rong; Xu, Gui-Lan; Zhang, Jian; Zhang, Lei; Dalton transactions (Cambridge, England : 2003) 49 (2020) 4030–4033; doi:10.1039/d0dt00197j

data_7703964
_publ_section_title
;
 Synergistic ligand effect for the construction of titanium-oxo clusters
 with planar chirality and high solution stability.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4030
_journal_page_last               4033
_journal_paper_doi               10.1039/d0dt00197j
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C62 H110 N6 O30 Ti9'
_chemical_formula_sum            'C62 H110 N6 O30 Ti9'
_chemical_formula_weight         1850.65
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-08-05
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2020-02-21 deposited with the CCDC.	2020-02-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.4809(5)
_cell_length_b                   24.6175(6)
_cell_length_c                   25.6441(7)
_cell_measurement_reflns_used    15376
_cell_measurement_temperature    100.0(3)
_cell_measurement_theta_max      73.2780
_cell_measurement_theta_min      3.4070
_cell_volume                     8510.4(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3468
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.989
_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   -112.00 -16.00   1.00    1.00    --  -41.54 -57.00 120.00   96
  2  \w    -65.00  32.00   1.00    1.00    --  -41.54  57.00 -90.00   97
  3  \w    -33.00  30.00   1.00    1.00    --   41.54 -38.00 -30.00   63
  4  \w     73.00  98.00   1.00    1.00    --   41.54-125.00-120.00   25
  5  \w      8.00  75.00   1.00    1.00    --   41.54 -99.00  30.00   67
  6  \w     38.00  65.00   1.00    1.00    --   41.54 -38.00 -30.00   27
  7  \w     28.00  74.00   1.00    1.00    --  104.65 -30.00 120.00   46
  8  \w     77.00 107.00   1.00    1.00    --  104.65 -94.00 -90.00   30
  9  \w    129.00 177.00   1.00    1.00    --  104.65 125.00-150.00   48
 10  \w     84.00 176.00   1.00    1.00    --  104.65  30.00 -60.00   92
 11  \w     35.00 100.00   1.00    1.00    --  104.65 -94.00   0.00   65
 12  \w     87.00 178.00   1.00    1.00    --  104.65  45.00-120.00   91
 13  \w     35.00 133.00   1.00    1.00    --  104.65 -61.00-180.00   98
 14  \w     32.00  57.00   1.00    1.00    --  104.65-125.00 120.00   25
 15  \w     87.00 118.00   1.00    1.00    --  104.65-125.00 120.00   31
 16  \w     44.00  99.00   1.00    1.00    --  104.65 -45.00 -30.00   55
 17  \w    120.00 162.00   1.00    1.00    --  104.65 125.00  60.00   42
 18  \w     86.00 118.00   1.00    1.00    --  104.65-125.00-120.00   32
 19  \w     22.00  97.00   1.00    1.00    --  104.65 -94.00 150.00   75
 20  \w     51.00 157.00   1.00    1.00    --  104.65 -15.00-120.00  106
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1127855000
_diffrn_orient_matrix_UB_12      0.0041585000
_diffrn_orient_matrix_UB_13      -0.0086035000
_diffrn_orient_matrix_UB_21      -0.0169226000
_diffrn_orient_matrix_UB_22      -0.0432447000
_diffrn_orient_matrix_UB_23      0.0424831000
_diffrn_orient_matrix_UB_31      -0.0059709000
_diffrn_orient_matrix_UB_32      0.0450724000
_diffrn_orient_matrix_UB_33      0.0416317000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0804
_diffrn_reflns_av_unetI/netI     0.0678
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            64659
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.751
_diffrn_reflns_theta_min         2.488
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.469
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.07518
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.444
_exptl_crystal_description       block
_exptl_crystal_F_000             3848
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.753
_refine_diff_density_min         -0.661
_refine_diff_density_rms         0.100
_refine_ls_abs_structure_details
;
 Flack x determined using 5670 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.031(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     994
_refine_ls_number_reflns         16847
_refine_ls_number_restraints     738
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0651
_refine_ls_R_factor_gt           0.0523
_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^)+(0.0630P)^2^+6.1220P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1251
_refine_ls_wR_factor_ref         0.1370
_reflns_Friedel_coverage         0.818
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.969
_reflns_number_gt                14473
_reflns_number_total             16847
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00197j2.cif
_cod_data_source_block           PTC-68B
_cod_database_code               7703964
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         'Ti C O H N'
_reflns_odcompleteness_completeness 99.98
_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. Uiso/Uaniso restraints and constraints
C01A \\sim C01B \\sim C01C \\sim C01D \\sim C01E \\sim C01F \\sim C01G \\sim
C01H \\sim C01I \\sim C01J \\sim C01K \\sim C01L \\sim C01M \\sim C01N \\sim
C01O \\sim C01P \\sim C01Q \\sim C01R \\sim C01S \\sim C01T \\sim C01U \\sim
C01V \\sim C01W \\sim C01X \\sim C01Y \\sim C01Z \\sim C020 \\sim C021 \\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: within 3.8A with
sigma of 0.005 and sigma for terminal atoms of 0.01
C021 \\sim O00Y \\sim C02Z \\sim C02V: within 3.8A with sigma of 0.01 and sigma
for terminal atoms of 0.02
Uanis(C02Z) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3.a Ternary CH refined with riding coordinates:
 C01Q(H01Q), C01R(H01R), C01X(H01X), C021(H021), C022(H022), C027(H027),
 C029(H029), C02B(H02P), C02D(H02T), C02E(H02U), C02G(H02Y), C02Q(H7AA)
3.b Aromatic/amide H refined with riding coordinates:
 C01G(H01G), C01J(H01J), C01O(H01O), C01P(H01P), C01V(H01V), C01W(H01W),
 C020(H020), C024(H024)
3.c Idealised Me refined as rotating group:
 C01L(H01A,H01B,H01C), C01S(H01D,H01E,H01F), C01T(H01H,H01I,H01K), C01Y(H01L,
 H01M,H01N), C01Z(H01S,H01T,H01U), C023(H02A,H02B,H02C), C025(H02D,H02E,H02F),
 C026(H02G,H02H,H02I), C028(H02J,H02K,H02L), C02A(H02M,H02N,H02O), C02C(H02Q,
 H02R,H02S), C02F(H02V,H02W,H02X), C02H(H02Z,H,HA), C02I(H02,HB,HC), C02J(H0AA,
 HD,HE), C02K(H1AA,HF,HG), C02L(H2AA,HH,HI), C02M(H3AA,HJ,HK), C02N(H4AA,HL,HM),
  C02O(H5AA,HN,HO), C02P(H6AA,HP,HQ), C02R(H8AA,HR,HS), C02S(H9AA,HT,HU),
 C02T(H0BA,HV,HW), C02U(H1BA,HX,HY), C02V(H2BA,HZ,H7BA), C02W(H3BA,H8BA,H9BA),
 C02X(H4BA,H0CA,H1CA), C02Y(H5BA,H2CA,H3CA), C02Z(H6BA,H4CA,H5CA)
;
_shelx_res_checksum              22469
_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 9.448
_oxdiff_exptl_absorpt_empirical_full_min 0.564