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_7703962
_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     direct
_audit_creation_date             2020-02-20
_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                   13.686(2)
_cell_length_b                   25.029(4)
_cell_length_c                   25.781(5)
_cell_measurement_reflns_used    29481
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.5204
_cell_measurement_theta_min      2.8584
_cell_volume                     8831(3)
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_collection       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0310
_diffrn_reflns_av_unetI/netI     0.0291
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            66134
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         2.859
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.843
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8166
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
?
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.392
_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         1.263
_refine_diff_density_min         -2.140
_refine_diff_density_rms         0.091
_refine_ls_abs_structure_details
;
 Flack x determined using 7084 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.207(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     964
_refine_ls_number_reflns         17301
_refine_ls_number_restraints     773
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0637
_refine_ls_R_factor_gt           0.0618
_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^)+(0.0960P)^2^+14.3460P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1646
_refine_ls_wR_factor_ref         0.1669
_reflns_Friedel_coverage         0.836
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                16645
_reflns_number_total             17301
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00197j2.cif
_cod_data_source_block           PTC-68A
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/current/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_database_code               7703962
_shelx_shelxl_version_number     2018/1
_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. Rigid bond restraints
 C7
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O00U, C02A
 with sigma for 1-2 distances of 0.0008 and sigma for 1-3 distances of 0.0004
 C1, C02N
 with sigma for 1-2 distances of 0.0008 and sigma for 1-3 distances of 0.0004
 O00W, C02D
 with sigma for 1-2 distances of 0.0008 and sigma for 1-3 distances of 0.0004
 C3, C02D
 with sigma for 1-2 distances of 0.0008 and sigma for 1-3 distances of 0.0004
 C02D, C02S
 with sigma for 1-2 distances of 0.0008 and sigma for 1-3 distances of 0.0004
 C02A, C02W
 with sigma for 1-2 distances of 0.0008 and sigma for 1-3 distances of 0.0004
 C02E, C02N
 with sigma for 1-2 distances of 0.0008 and sigma for 1-3 distances of 0.0004
 Ti04, O011
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0002
 Ti09, O00W
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0002
 Ti05, O00T
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0002
 Ti08, O00U
 with sigma for 1-2 distances of 0.0008 and sigma for 1-3 distances of 0.0004
3. 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 C1 \\sim C3 \\sim C7: within 3.8A with sigma
of 0.005 and sigma for terminal atoms of 0.01
C02L \\sim O00T \\sim C02U \\sim C02F: within 3.8A with sigma of 0.005 and
sigma for terminal atoms of 0.01
Uanis(C7) \\sim Ueq, Uanis(C02W) \\sim Ueq: with sigma of 0.0001 and sigma for
terminal atoms of 0.0002
Uanis(C7) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C02A) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C02N) \\sim Ueq: with sigma of 0.0001 and sigma for terminal atoms of
0.0002
Uanis(C02L) \\sim Ueq: with sigma of 0.0001 and sigma for terminal atoms of
0.0002
Uanis(C02D) \\sim Ueq, Uanis(C02S) \\sim Ueq, Uanis(C3) \\sim Ueq: with sigma
of 0.001 and sigma for terminal atoms of 0.002
Uanis(C02A) = Uanis(C7)
Uanis(O00T) = Uanis(C02L)
Uanis(O011) = Uanis(C02N)
Uanis(C02F) = Uanis(C02L)
Uanis(C02U) = Uanis(C02L) = Uanis(O00T) = Uanis(C02F)
4.a Ternary CH refined with riding coordinates:
 C01O(H01O), C01W(H01W), C021(H021), C024(H024), C026(H026), C027(H027),
 C028(H028), C02A(H02M), C02C(H02Q), C02D(H02R), C02N(H3AA)
4.b Aromatic/amide H refined with riding coordinates:
 C01K(H01K), C01N(H01N), C01Q(H01Q), C01R(H01R), C01U(H01U), C01V(H01V),
 C01Z(H01Z), C020(H020)
4.c Idealised Me refined as rotating group:
 C01P(H01A,H01B,H01C), C01S(H01D,H01E,H01F), C01T(H01G,H01H,H01I), C01X(H01J,
 H01L,H01M), C01Y(H01P,H01S,H01T), C022(H02A,H02B,H02C), C023(H02D,H02E,H02F),
 C025(H02G,H02H,H02I), C029(H02J,H02K,H02L), C02B(H02N,H02O,H02P), C02E(H02S,
 H02T,H02U), C02F(H02V,H02W,H02X), C02G(H02Y,H,HA), C02H(H02Z,HB,HC), C02I(H02,
 HD,HE), C02J(H0AA,HF,HG), C02K(H1AA,HH,HI), C02M(H2AA,HJ,HK), C02O(H4AA,HL,HM),
  C02P(H5AA,HN,HO), C02Q(H6AA,HP,HQ), C02R(H7AA,HR,HS), C02S(H8AA,HT,HU),
 C02T(H9AA,HV,HW), C02U(H0BA,HX,HY), C02V(H1BA,HZ,H3BA), C02W(H2BA,H4BA,H5BA),
 C1(H1A,H1B,H1C), C3(H3A,H3B,H3C), C7(H7A,H7B,H7C)
;
_shelx_res_checksum              57595
_shelx_fab_checksum              49036
_olex2_submission_special_instructions 'No special instructions were received'