Ligand dependent assembly of trinuclear titanium-oxo units into coordination tetrahedra and capsules.
Fan, Xi; Narayanam, Nagaraju; Gao, Meiyan; Zhang, Lei; Zhang, Jian; Dalton transactions (Cambridge, England : 2003) 47 (2018) 663–665; doi:10.1039/c7dt04204c

data_7044951
_publ_section_title
;
 Ligand dependent assembly of trinuclear titanium-oxo units into
 coordination tetrahedra and capsules.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              663
_journal_page_last               665
_journal_paper_doi               10.1039/c7dt04204c
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C27 H49 Cl0.33 Cu0.33 N O13 P Ti3'
_chemical_formula_sum            'C27 H49 Cl0.33 Cu0.33 N O13 P Ti3'
_chemical_formula_weight         803.34
_space_group_crystal_system      trigonal
_space_group_IT_number           147
_space_group_name_Hall           '-P 3'
_space_group_name_H-M_alt        'P -3'
_symmetry_space_group_name_Hall  '-P 3'
_symmetry_space_group_name_H-M   'P -3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-11-24
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_audit_update_record
;
2017-12-01 deposited with the CCDC.
2017-12-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   18.9783(12)
_cell_length_b                   18.9783(12)
_cell_length_c                   19.9218(9)
_cell_measurement_reflns_used    4511
_cell_measurement_temperature    100.00(13)
_cell_measurement_theta_max      74.1470
_cell_measurement_theta_min      4.6680
_cell_volume                     6214.0(6)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_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      100.00(13)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3503
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.965
_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     24.00  54.00   1.00    1.57    --   40.72-125.00-120.00   30
  2  \w     35.00  62.00   1.00    1.57    --   40.72-125.00  90.00   27
  3  \w     63.00 174.00   1.00    6.29    --  108.54  15.00  30.00  111
  4  \w    109.00 172.00   1.00    6.29    --  108.54  45.00  60.00   63
  5  \w    105.00 154.00   1.00    6.29    --  108.54 125.00 -30.00   49
  6  \w    106.00 156.00   1.00    6.29    --  108.54 125.00 -60.00   50
  7  \w    -93.00  -6.00   1.00    1.57    --  -40.72 125.00-120.00   87
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0300545000
_diffrn_orient_matrix_UB_12      -0.0442087000
_diffrn_orient_matrix_UB_13      0.0467048000
_diffrn_orient_matrix_UB_21      -0.0784601000
_diffrn_orient_matrix_UB_22      -0.0811017000
_diffrn_orient_matrix_UB_23      -0.0139464000
_diffrn_orient_matrix_UB_31      0.0416058000
_diffrn_orient_matrix_UB_32      -0.0153854000
_diffrn_orient_matrix_UB_33      -0.0601288000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0554
_diffrn_reflns_av_unetI/netI     0.0729
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            15005
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.413
_diffrn_reflns_theta_min         3.486
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.993
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.27549
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_description       prism
_exptl_crystal_F_000             2510
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_platon_squeeze_details
;
;
_refine_diff_density_max         1.203
_refine_diff_density_min         -1.211
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     425
_refine_ls_number_reflns         8193
_refine_ls_number_restraints     244
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.1574
_refine_ls_R_factor_gt           0.1342
_refine_ls_shift/su_max          0.049
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1250P)^2^+65.4400P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3239
_refine_ls_wR_factor_ref         0.3378
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6087
_reflns_number_total             8193
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04204c2.cif
_cod_data_source_block           PTC-76
_cod_depositor_comments
'Adding full bibliography for 7044948--7044951.cif.'
_cod_original_cell_volume        6214.0(8)
_cod_database_code               7044951
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         COTi
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.13
_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
 O00I, C00X
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C2, C5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C012, C018
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O00Q, C2
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
3. Uiso/Uaniso restraints and constraints
C00J \\sim C00K \\sim C00L \\sim C00M \\sim C00N \\sim C00P \\sim C00R \\sim
C00S \\sim C00T \\sim C00U \\sim C00V \\sim C00W \\sim C00X \\sim C00Y \\sim
C00Z \\sim C010 \\sim C011 \\sim C012 \\sim C013 \\sim C015 \\sim C016 \\sim
C017 \\sim C018 \\sim C2 \\sim C5 \\sim C15 \\sim C3: within 3.8A with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(O00Q) \\sim Ueq, Uanis(C2) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4.a Ternary CH refined with riding coordinates:
 C00S(H00S), C00T(H00T), C00V(H00V), C00X(H00X), C010(H010), C012(H012)
4.b Aromatic/amide H refined with riding coordinates:
 C00J(H00J), C00M(H00M), C00N(H00N), C00P(H00P)
4.c Idealised Me refined as rotating group:
 C00R(H00A,H00B,H00C), C00U(H00D,H00E,H00F), C00W(H00G,H00H,H00I), C00Y(H00K,
 H00L,H00O), C00Z(H00Q,H00R,H00U), C011(H01A,H01B,H01C), C013(H01D,H01E,H01F),
 C015(H01G,H01H,H01I), C016(H01J,H01K,H01L), C017(H01M,H01N,H01O), C018(H01P,
 H01Q,H01R), C5(H5A,H5B,H5C), C3(H3A,H3B,H3C)
;
_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 2.131
_oxdiff_exptl_absorpt_empirical_full_min 0.663