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_4086018
_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         'C53 H93 O Si4 Ti2'
_chemical_formula_sum            'C53 H93 O Si4 Ti2'
_chemical_formula_weight         954.43
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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                 92.283(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.4629(16)
_cell_length_b                   11.6983(8)
_cell_length_c                   39.655(3)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.5
_cell_volume                     10875.7(13)
_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 for Windows (Farrugia, 2012)'
_computing_publication_material
;
Olex2 (Dolomanov et al., 2009) and WinGX (Farrugia, 2012) publication routines
;
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.991
_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     0.71075
_diffrn_reflns_av_R_equivalents  0.0541
_diffrn_reflns_av_unetI/netI     0.0328
_diffrn_reflns_laue_measured_fraction_full 0.990
_diffrn_reflns_laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            66646
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         2.461
_diffrn_source                   'Sealed Tube'
_exptl_absorpt_coefficient_mu    0.416
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.718
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Multi-Scan (Blessing, 1995)
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.166
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             4152
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.826
_refine_diff_density_min         -0.432
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     580
_refine_ls_number_reflns         12339
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0591
_refine_ls_R_factor_gt           0.0411
_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^)+(0.0540P)^2^+16.2491P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1003
_refine_ls_wR_factor_ref         0.1107
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9738
_reflns_number_total             12339
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00315_si_003.cif
_cod_data_source_block           Compound7
_cod_depositor_comments
;Adding full bibliography for 4086017--4086022.cif.

 Adding full bibliography for 4086017--4086022.cif.
;
_cod_database_code               4086018
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.996
_shelx_estimated_absorpt_t_min   0.967
_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. Shared sites
{C50A, C50B}
3. Restrained distances
 C53A-O1A \\sim C53B-O1B
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
C53A \\sim C53B: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
Uanis(C50A) = Uanis(C50B)
5. Others
 Sof(C50B)=Sof(H50C)=Sof(H50D)=Sof(C51B)=Sof(H51D)=Sof(H51E)=Sof(H51F)=
 Sof(C52B)=Sof(H52D)=Sof(H52E)=Sof(H52F)=1-FVAR(1)
 Sof(C50A)=Sof(H50A)=Sof(H50B)=Sof(C51A)=Sof(H51A)=Sof(H51B)=Sof(H51C)=
 Sof(C52A)=Sof(H52A)=Sof(H52B)=Sof(H52C)=FVAR(1)
 Sof(C53B)=1-FVAR(2)
 Sof(C53A)=FVAR(2)
 Sof(O1B)=1-FVAR(3)
 Sof(O1A)=FVAR(3)
6.a Ternary CH refined with riding coordinates:
 C17(H17), C20(H20), C23(H23), C26(H26), C29(H29), C32(H32), C35(H35),
 C38(H38), C41(H41), C44(H44), C47(H47)
6.b Me refined with riding coordinates:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C28(H28A,
 H28B,H28C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C33(H33A,H33B,H33C),
 C34(H34A,H34B,H34C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C39(H39A,H39B,
 H39C), C40(H40A,H40B,H40C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C45(H45A,
 H45B,H45C), C46(H46A,H46B,H46C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C),
 C51A(H51A,H51B,H51C), C52A(H52A,H52B,H52C), C51B(H51D,H51E,H51F), C52B(H52D,
 H52E,H52F)
6.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C6(H6), C7(H7), C10(H10), C11(H11), C14(H14), C15(H15)
;
_olex2_submission_special_instructions 'No special instructions were received'