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_7044950
_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 H53 Br0.33 Cu0.33 N O13 P Ti3'
_chemical_formula_sum            'C27 H46 Br0.33 Cu0.33 N O13 P Ti3'
_chemical_formula_weight         815.13
_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
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-11-27
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-12-01 deposited with the CCDC.
2017-12-05 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   19.0415(6)
_cell_length_b                   19.0415(6)
_cell_length_c                   20.0613(6)
_cell_measurement_reflns_used    5654
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      74.0530
_cell_measurement_theta_min      4.6380
_cell_volume                     6299.3(3)
_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(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3503
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_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     39.00  66.00   1.00    1.00    --   40.84-125.00-120.00   27
  2  \w     26.00  68.00   1.00    3.96    --  108.54 -95.00 -90.00   42
  3  \w     42.00 134.00   1.00    3.96    --  108.54 -61.00  60.00   92
  4  \w    131.00 177.00   1.00    3.96    --  108.54  45.00 -90.00   46
  5  \w     81.00 171.00   1.00    3.96    --  108.54  30.00-180.00   90
  6  \w   -120.00 -16.00   1.00    1.00    --  -40.84 -19.00-120.00  104
;
_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      -0.0621302000
_diffrn_orient_matrix_UB_12      -0.0745277000
_diffrn_orient_matrix_UB_13      -0.0398146000
_diffrn_orient_matrix_UB_21      0.0693360000
_diffrn_orient_matrix_UB_22      0.0023575000
_diffrn_orient_matrix_UB_23      -0.0411958000
_diffrn_orient_matrix_UB_31      0.0074202000
_diffrn_orient_matrix_UB_32      -0.0564492000
_diffrn_orient_matrix_UB_33      0.0511190000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0415
_diffrn_reflns_av_unetI/netI     0.0596
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15147
_diffrn_reflns_theta_full        74.37
_diffrn_reflns_theta_max         74.37
_diffrn_reflns_theta_min         3.47
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.088
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.12578
_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    1.289
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2528
_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         1.388
_refine_diff_density_min         -1.107
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     426
_refine_ls_number_reflns         8349
_refine_ls_number_restraints     237
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0937
_refine_ls_R_factor_gt           0.0808
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1710P)^2^+1.7620P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2314
_refine_ls_wR_factor_ref         0.2480
_reflns_number_gt                6622
_reflns_number_total             8349
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7dt04204c2.cif
_cod_data_source_block           PTC-77
_cod_depositor_comments
'Adding full bibliography for 7044948--7044951.cif.'
_cod_database_code               7044950
_chemical_oxdiff_formula         COPTi
_reflns_odcompleteness_completeness 99.97
_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. Restrained distances
 C2-C016
 1.45 with sigma of 0.02
 C1-C016
 1.45 with sigma of 0.02
 C1-C2
 2.5 with sigma of 0.02
3. Rigid bond restraints
 C016
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
C016: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C00J \\sim C00K \\sim C00L \\sim C00M \\sim C00N \\sim C00O \\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 C014 \\sim C015 \\sim
C016 \\sim C017 \\sim C3 \\sim C4 \\sim C1 \\sim C2: within 3.8A with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C016) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5.a Ternary CH refined with riding coordinates:
 C00S(H00S), C00T(H00T), C00U(H00U), C00V(H00V), C00Z(H00Z), C011(H011),
 C016(H016)
5.b Aromatic/amide H refined with riding coordinates:
 C00K(H00K), C00L(H00L), C00M(H00M), C00N(H00N)
5.c Idealised Me refined as rotating group:
 C00R(H00A,H00B,H00C), C00W(H00D,H00E,H00F), C00X(H00G,H00H,H00I), C00Y(H00J,
 H00O,H00P), C010(H01A,H01B,H01C), C012(H01D,H01E,H01F), C013(H01G,H01H,H01I),
 C014(H01J,H01K,H01L), C015(H01M,H01N,H01O), C017(H01P,H01Q,H01R), C3(H3A,H3B,
 H3C), C4(H4A,H4B,H4C), C1(H1A,H1B,H1C), C2(H2A,H2B,H2C)
;
_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 4.480
_oxdiff_exptl_absorpt_empirical_full_min 0.377