The Reductive Activation of CO2 Across a Ti=Ti Double Bond: Synthetic, Structural, and Mechanistic Studies.
Kilpatrick, Alexander F. R.; Green, Jennifer C.; Cloke, F Geoffrey N; Organometallics 34 (2015) 4816–4829; doi:10.1021/acs.organomet.5b00315

data_4086022
_publ_section_title
;
 The Reductive Activation of CO2 Across a Ti=Ti Double Bond: Synthetic,
 Structural, and Mechanistic Studies.
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              4816
_journal_page_last               4829
_journal_paper_doi               10.1021/acs.organomet.5b00315
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C52 H92 S2 Si4 Ti2'
_chemical_formula_sum            'C52 H92 S2 Si4 Ti2'
_chemical_formula_weight         989.53
_chemical_name_common            Compound_13
_space_group_crystal_system      tetragonal
_space_group_IT_number           133
_space_group_name_Hall           '-P 4ac 2b'
_space_group_name_H-M_alt        'P 42/n b c'
_symmetry_space_group_name_Hall  '-P 4ac 2b'
_symmetry_space_group_name_H-M   'P 42/n b c :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-01-26
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.714(2)
_cell_length_b                   15.714(2)
_cell_length_c                   24.660(5)
_cell_measurement_reflns_used    39525
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.5
_cell_volume                     6089.3(17)
_computing_cell_refinement
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 20112)
;
_computing_data_collection
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 20112)
;
_computing_data_reduction
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 20112)
;
_computing_molecular_graphics    'Ortep-3 (Farrugia, 1997)'
_computing_publication_material
;
OLEX2 (Dolomanov et al, 2009), SHELXL-2013 (Sheldrick, 2013), 
PLATON (Spek, 2003), WinGX (Farrugia, 2013)
;
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type
;
Rigaku Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0887
_diffrn_reflns_av_unetI/netI     0.0326
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            46997
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.460
_diffrn_reflns_theta_min         3.014
_diffrn_source                   'Sealed Tube'
_exptl_absorpt_coefficient_mu    0.439
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.630
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Multi-scan (Blessing, 1995)
;
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.079
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Rod
_exptl_crystal_F_000             2144
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_platon_squeeze_details
;
;
_refine_diff_density_max         0.397
_refine_diff_density_min         -0.472
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.280
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     161
_refine_ls_number_reflns         3468
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.280
_refine_ls_R_factor_all          0.1026
_refine_ls_R_factor_gt           0.0864
_refine_ls_shift/su_max          0.002
_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^+10.6605P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1710
_refine_ls_wR_factor_ref         0.1786
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2966
_reflns_number_total             3468
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00315_si_003.cif
_cod_data_source_block           Compound12
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 4086017--4086022.cif.

 Adding full bibliography for 4086017--4086022.cif.
;
_cod_original_cell_volume        6089(2)
_cod_database_code               4086022
_shelxl_version_number           2013-3
_shelx_estimated_absorpt_t_max   0.987
_shelx_estimated_absorpt_t_min   0.894
_olex2_refinement_description
;
1. Others
 Fixed Sof: S1(0.5)
 Fixed U13: Ti1(0)
 Fixed U23: Ti1(0)
 Fixed Uiso: H2(0.045) H4(0.046) H5(0.075) H6A1(0.079) H6A2(0.079) H6A3(0.079)
 H6B1(0.087) H6B2(0.087) H6B3(0.087) H7A(0.102) H7B(0.102) H7C(0.102) H8(0.055)
 H9A(0.101) H9B(0.101) H9C(0.101) H10A(0.11) H10B(0.11) H10C(0.11) H11(0.084)
 H12A(0.054) H12B(0.054) H12C(0.054) H12D(0.07) H12E(0.07) H12F(0.07)
 H13A(0.132) H13B(0.132) H13C(0.132)
 Fixed X: H2(0.9351) H4(0.8262) H5(0.7849) H6A1(0.9094) H6A2(0.9363)
 H6A3(0.8515) H6B1(0.8765) H6B2(0.8889) H6B3(0.7966) H7A(0.7747) H7B(0.7462)
 H7C(0.8375) H8(0.937) H9A(0.9693) H9B(1.0414) H9C(1.0567) H10A(1.0181)
 H10B(1.0874) H10C(1.0715) H11(1.0042) H12A(0.8912) H12B(0.9157) H12C(0.9814)
 H12D(0.8588) H12E(0.8636) H12F(0.9218) H13A(1.0758) H13B(1.0828) H13C(1.0175)
 Ti1(0.75)
 Fixed Y: H2(0.2848) H4(0.3965) H5(0.0167) H6A1(-0.0426) H6A2(-0.0935) H6A3(-
 0.1192) H6B1(-0.0764) H6B2(-0.1217) H6B3(-0.118) H7A(0.0074) H7B(-0.0767) H7C(-
 0.0725) H8(0.0422) H9A(0.1874) H9B(0.1285) H9C(0.1714) H10A(-0.0479)
 H10B(0.026) H10C(-0.0165) H11(0.048) H12A(0.0931) H12B(0.1894) H12C(0.1306)
 H12D(0.0611) H12E(0.1627) H12F(0.1121) H13A(0.1634) H13B(0.1666) H13C(0.2279)
 Ti1(0.25)
 Fixed Z: H2(0.1082) H4(0.1251) H5(0.1653) H6A1(0.2121) H6A2(0.1586)
 H6A3(0.1906) H6B1(0.2058) H6B2(0.1483) H6B3(0.1755) H7A(0.0671) H7B(0.0988)
 H7C(0.0702) H8(0.043) H9A(0.0355) H9B(0.0092) H9C(0.0673) H10A(0.1004)
 H10B(0.107) H10C(0.0489) H11(0.2035) H12A(0.2575) H12B(0.2432) H12C(0.2757)
 H12D(0.2405) H12E(0.2374) H12F(0.2798) H13A(0.1581) H13B(0.2228) H13C(0.1919)
;
_olex2_submission_special_instructions 'No special instructions were received'