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_7703963
_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                   13.6676(2)
_cell_length_b                   25.0164(4)
_cell_length_c                   25.7877(3)
_cell_measurement_reflns_used    36997
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.9010
_cell_measurement_theta_min      2.1880
_cell_volume                     8817.2(2)
_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 16.2083
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0521
_diffrn_reflns_av_unetI/netI     0.0422
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            52627
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        24.994
_diffrn_reflns_theta_max         24.994
_diffrn_reflns_theta_min         2.319
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.844
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.32142
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46c (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_description       block
_exptl_crystal_F_000             3848
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.305
_refine_diff_density_min         -0.980
_refine_diff_density_rms         0.072
_refine_ls_abs_structure_details
;
 Flack x determined using 5374 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.093(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     928
_refine_ls_number_reflns         15338
_refine_ls_number_restraints     731
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0561
_refine_ls_R_factor_gt           0.0486
_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^)+(0.0790P)^2^+4.9280P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1283
_refine_ls_wR_factor_ref         0.1333
_reflns_Friedel_coverage         0.814
_reflns_Friedel_fraction_full    0.978
_reflns_Friedel_fraction_max     0.978
_reflns_number_gt                13626
_reflns_number_total             15338
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00197j2.cif
_cod_data_source_block           PTC-68R
_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               7703963
_shelx_shelxl_version_number     2018/1
_oxdiff_exptl_absorpt_empirical_full_min 0.220
_oxdiff_exptl_absorpt_empirical_full_max 4.101
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_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. Restrained distances
 C2-C6
 1.5 with sigma of 0.01
 H16B-H30
 2.45 with sigma of 0.01
 C30-C33
 1.5 with sigma of 0.01
3. Rigid bond restraints
 C1, C31
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 O26, C31
 with sigma for 1-2 distances of 0.0008 and sigma for 1-3 distances of 0.0004
4. Uiso/Uaniso restraints and constraints
C31 \\sim O26 \\sim C20 \\sim C1: within 3.8A with sigma of 0.01 and sigma for
terminal atoms of 0.02
C62 \\sim C61 \\sim C60 \\sim C59 \\sim C58 \\sim C57 \\sim C56 \\sim C55 \\sim
C54 \\sim C53 \\sim C52 \\sim C51 \\sim C50 \\sim C49 \\sim C48 \\sim C47 \\sim
C46 \\sim C45 \\sim C44 \\sim C43 \\sim C42 \\sim C41 \\sim C40 \\sim C39 \\sim
C38 \\sim C37 \\sim C36 \\sim C35 \\sim C34 \\sim C33 \\sim C32 \\sim C31 \\sim
C30 \\sim C29 \\sim C28 \\sim C27 \\sim C26 \\sim C25 \\sim C24 \\sim C23 \\sim
C22 \\sim C21 \\sim C20 \\sim C19 \\sim C18 \\sim C17 \\sim C16 \\sim C15 \\sim
C14 \\sim C13 \\sim C12 \\sim C11 \\sim C10 \\sim C9 \\sim C8 \\sim C7 \\sim C6
\\sim C5 \\sim C4 \\sim C3 \\sim C2 \\sim C1: within 3.8A with sigma of 0.005
and sigma for terminal atoms of 0.01
Uanis(C1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O5) = Uanis(C6) = Uanis(C2) = Uanis(C3)
Uanis(C31) = Uanis(C20) = Uanis(C1)
Uanis(C30) = Uanis(C16)
5.a Ternary CH refined with riding coordinates:
 C41(H41), C34(H34), C31(H31), C30(H30), C28(H28), C27(H27), C26(H26),
 C25(H25), C23(H23), C12(H12), C6(H6), C5(H5)
5.b Me refined with riding coordinates:
 C48(H48A,H48B,H48C), C46(H46A,H46B,H46C), C43(H43A,H43B,H43C), C42(H42A,H42B,
 H42C), C40(H40A,H40B,H40C), C39(H39A,H39B,H39C), C37(H37A,H37B,H37C), C33(H33A,
 H33B,H33C), C32(H32A,H32B,H32C), C29(H29A,H29B,H29C), C24(H24A,H24B,H24C),
 C22(H22A,H22B,H22C), C21(H21A,H21B,H21C), C20(H20A,H20B,H20C), C19(H19A,H19B,
 H19C), C18(H18A,H18B,H18C), C17(H17A,H17B,H17C), C16(H16A,H16B,H16C), C15(H15A,
 H15B,H15C), C14(H14A,H14B,H14C), C13(H13A,H13B,H13C), C11(H11A,H11B,H11C),
 C10(H10A,H10B,H10C), C9(H9A,H9B,H9C), C8(H8A,H8B,H8C), C7(H7A,H7B,H7C), C4(H4A,
 H4B,H4C), C3(H3A,H3B,H3C), C2(H2A,H2B,H2C), C1(H1A,H1B,H1C)
5.c Aromatic/amide H refined with riding coordinates:
 C62(H62), C59(H59), C58(H58), C57(H57), C49(H49), C47(H47), C44(H44), C36(H36)
;
_shelx_res_checksum              67908
_olex2_submission_special_instructions 'No special instructions were received'