Reductive deoxygenation of CO2 by a bimetallic titanium bis(pentalene) complex
Alexander F. R. Kilpatrick; F. Geoffrey N. Cloke; Chem.Commun. 50 (2014) 2769–; doi:10.1039/c3cc48379g

data_7112044
_publ_section_title
;
 Reductive deoxygenation of CO2 by a bimetallic titanium bis(pentalene)
 complex
;
_journal_name_full               Chem.Commun.
_journal_page_first              2769
_journal_paper_doi               10.1039/c3cc48379g
_journal_volume                  50
_journal_year                    2014
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C54 H92 O2 Si4 Ti2'
_chemical_formula_sum            'C54 H92 O2 Si4 Ti2'
_chemical_formula_weight         981.43
_chemical_name_common            'Complex 3'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_creation_date             2013-10-28T17:37:10-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 92.18(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.894(3)
_cell_length_b                   22.342(5)
_cell_length_c                   19.113(4)
_cell_measurement_reflns_used    48981
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.2
_cell_measurement_wavelength     0.71073
_cell_volume                     5502(2)
_computing_cell_refinement
;
        CrystalClear-SM Expert 3.1 b18 (Rigaku, 20112)
;
_computing_data_collection
;
        CrystalClear-SM Expert 3.1 b18 (Rigaku, 20112)
;
_computing_data_reduction
;
        CrystalClear-SM Expert 3.1 b18 (Rigaku, 20112)
;
_computing_molecular_graphics    'Ortep-3 (Farrugia, 1997)'
_computing_publication_material
;
WINGX publication routines (Farrugia, 2013)
;
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0621
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            72543
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_min         3.159
_diffrn_source
;
        fine-focus sealed tube
;
_exptl_absorpt_coefficient_mu    0.415
_exptl_absorpt_correction_T_max  0.9877
_exptl_absorpt_correction_T_min  0.9519
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        [c.f. R.H. Blessing, Acta Cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    1.185
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             2128
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.997
_refine_diff_density_min         -0.793
_refine_diff_density_rms         0.11
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     557
_refine_ls_number_reflns         12581
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.1018
_refine_ls_R_factor_gt           0.0766
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1226P)^2^+10.5184P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2107
_refine_ls_wR_factor_ref         0.2279
_reflns_number_gt                9225
_reflns_number_total             12581
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3cc48379g.txt
_cod_data_source_block           shelx
_cod_original_cell_volume        5502.1(19)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7112044