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_7044948
_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         'C21 H39 N O12 P Ti3'
_chemical_formula_sum            'C21 H39 N O12 P Ti3'
_chemical_formula_weight         672.20
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-11-28
_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
_cell_angle_beta                 99.380(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.9697(7)
_cell_length_b                   14.2366(6)
_cell_length_c                   16.8559(8)
_cell_measurement_reflns_used    5271
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      29.2650
_cell_measurement_theta_min      3.5580
_cell_volume                     3070.7(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  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3503
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.962
_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    -44.00  36.00   1.00    3.28    --   11.76 -38.00 -60.00   80
  2  \w    -22.00  81.00   1.00    3.28    --   11.76  19.00 150.00  103
;
_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      0.0391694000
_diffrn_orient_matrix_UB_12      -0.0149322000
_diffrn_orient_matrix_UB_13      0.0318976000
_diffrn_orient_matrix_UB_21      0.0123330000
_diffrn_orient_matrix_UB_22      -0.0381421000
_diffrn_orient_matrix_UB_23      -0.0238458000
_diffrn_orient_matrix_UB_31      0.0372912000
_diffrn_orient_matrix_UB_32      0.0282950000
_diffrn_orient_matrix_UB_33      -0.0152717000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0238
_diffrn_reflns_av_unetI/netI     0.0376
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13998
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         3.405
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.868
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83097
_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            colorless
_exptl_crystal_density_diffrn    1.454
_exptl_crystal_description       prism
_exptl_crystal_F_000             1396
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.878
_refine_diff_density_min         -0.477
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     378
_refine_ls_number_reflns         6783
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0511
_refine_ls_R_factor_gt           0.0389
_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^)+(0.0487P)^2^+1.8099P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1012
_refine_ls_wR_factor_ref         0.1078
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5568
_reflns_number_total             6783
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04204c2.cif
_cod_data_source_block           PTC-75
_cod_depositor_comments
'Adding full bibliography for 7044948--7044951.cif.'
_cod_database_code               7044948
_shelxl_version_number           2013-2
_reflns_odcompleteness_completeness 99.63
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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. Same fragment restrains
{O1, C1B, C2B, C3B} sigma for 1-2: 0.02, 1-3: 0.04
as
{O1, C1A, C2A, C3A}
3. Others
 Sof(C1B)=Sof(H1B)=Sof(C2B)=Sof(H2BA)=Sof(H2BB)=Sof(H2BC)=Sof(C3B)=Sof(H3BA)=
 Sof(H3BB)=Sof(H3BC)=1-FVAR(1)
 Sof(C1A)=Sof(H1A)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(H2AC)=Sof(C3A)=Sof(H3AA)=
 Sof(H3AB)=Sof(H3AC)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C1A(H1A), C1B(H1B), C00J(H00J), C00L(H00L), C00M(H00M), C00W(H00W)
4.b Aromatic/amide H refined with riding coordinates:
 C00N(H00N), C00O(H00O), C1AA(H1AA), C00T(H00T)
4.c Idealised Me refined as rotating group:
 C2A(H2AA,H2AB,H2AC), C3A(H3AA,H3AB,H3AC), C2B(H2BA,H2BB,H2BC), C3B(H3BA,H3BB,
 H3BC), C00Q(H00A,H00B,H00C), C00R(H00D,H00E,H00F), C00S(H00G,H00H,H00I),
 C00U(H00K,H00P,H00Q), C00V(H00R,H00S,H00U), C00X(H00V,H00X,H00Y), C00Z(H00Z,H,
 HA), C011(H01A,H01B,H01C)
;
_shelx_res_checksum              96967
_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 1.318
_oxdiff_exptl_absorpt_empirical_full_min 0.775