C-H and H-H Activation at a Di-titanium Centre
Tsoureas, Nikolaos; Green, Jennifer; Cloke, Frederick Geoffrey; Chem. Commun.  (2017) –; doi:10.1039/C7CC07726B

data_7120817
_publ_section_title
;
 C-H and H-H Activation at a Di-titanium Centre
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC07726B
_journal_year                    2017
_chemical_formula_moiety         'C59 H104 N2 Si4 Ti2'
_chemical_formula_sum            'C59 H104 N2 Si4 Ti2'
_chemical_formula_weight         1049.60
_chemical_name_common            3
_chemical_name_systematic        3
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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   mixed
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2017-10-23 deposited with the CCDC.
2017-10-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.357(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.9788(8)
_cell_length_b                   13.1934(4)
_cell_length_c                   22.3687(7)
_cell_measurement_reflns_used    17855
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.7050
_cell_measurement_theta_min      2.1640
_cell_volume                     5997.9(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -78.00  73.00   1.00   70.00    --  -17.00  18.00-180.00  151
  2  \w   -100.00   2.00   1.00   70.00    --  -17.00 -72.00  60.00  102
  3  \w    -87.00  22.00   1.00   70.00    --  -17.00 -72.00  30.00  109
  4  \w    -66.00  68.00   1.00   70.00    --  -17.00   0.00-180.00  134
  5  \w     58.00  73.00   1.00   70.00    --  -17.00  36.00 -60.00   15
  6  \w   -107.00 -37.00   1.00   70.00    --  -17.00   0.00-150.00   70
;
_diffrn_measurement_device_type
'Rigaku FRE+ equipped with VHF Varimax confocal mirrors and an AFC10 goniometer and HG Saturn 724+ detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_collimation    0.2
_diffrn_radiation_monochromator  'Confocal mirrors, VHF Varimax'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1678
_diffrn_reflns_av_unetI/netI     0.1115
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            65678
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.028
_diffrn_reflns_theta_max         25.028
_diffrn_reflns_theta_min         2.177
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    0.383
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.46621
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    1.162
_exptl_crystal_description       Block
_exptl_crystal_F_000             2288
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene'
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.354
_refine_diff_density_min         -0.311
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     785
_refine_ls_number_reflns         10592
_refine_ls_number_restraints     100
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.1258
_refine_ls_R_factor_gt           0.0610
_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^)+(0.0625P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1218
_refine_ls_wR_factor_ref         0.1448
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6290
_reflns_number_total             10592
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc07726b2.cif
_cod_data_source_block           3
_cod_database_code               7120817
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.977
_shelx_estimated_absorpt_t_max   0.985
_shelx_res_checksum              82345
_olex2_date_sample_data_collection 2016-06-01
_olex2_date_sample_submission    2016-04-15
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a mylar loop in oil'
_olex2_submission_original_sample_id 2016NTL8p33
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.329
_oxdiff_exptl_absorpt_empirical_full_min 0.197