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_7112043
_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         'C62 H102 N2 O2 Si4 Ti2, C5 H5 N'
_chemical_formula_sum            'C67 H107 N3 O2 Si4 Ti2'
_chemical_formula_weight         1194.71
_chemical_name_common            'Complex 2_py_2'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_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             2013-10-29T12:46:06-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                85.689(3)
_cell_angle_beta                 86.517(3)
_cell_angle_gamma                66.630(4)
_cell_formula_units_Z            2
_cell_length_a                   13.7134(6)
_cell_length_b                   16.0497(6)
_cell_length_c                   18.5403(6)
_cell_measurement_reflns_used    12809
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      71.348
_cell_measurement_theta_min      3.757
_cell_measurement_wavelength     1.54184
_cell_volume                     3733.1(3)
_computing_cell_refinement
;
        crysalispro, agilent technologies,
        version 1.171.36.32 (release 02-08-2013 crysalis171 .net)
        (compiled aug  2 2013,16:46:58)
;
_computing_data_collection
;
        crysalispro, agilent technologies,
        version 1.171.36.32 (release 02-08-2013 crysalis171 .net)
        (compiled aug  2 2013,16:46:58)
;
_computing_data_reduction
;
        crysalispro, agilent technologies,
        version 1.171.36.32 (release 02-08-2013 crysalis171 .net)
        (compiled aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'ortep-3 (farrugia, 1997)'
_computing_publication_material
;
shelxl-2013 (sheldrick, 2013), platon (spek, 2003), and wingx (farrugia, 2013)
;
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution
;
        DIRDIF-08 (Beurskens et al., 2008)
;
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 16.1033
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device_type  'xcalibur, eos, gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0406
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            22701
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.48
_diffrn_reflns_theta_min         3.004
_diffrn_source
;
        Enhance Ultra (Cu) X-ray source
;
_exptl_absorpt_coefficient_mu    2.727
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.67895
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        crysalispro, agilent technologies,
        version 1.171.36.32 (release 02-08-2013 crysalis171 .net)
        (compiled aug  2 2013,16:46:58)
        empirical absorption correction using spherical harmonics,
 implemented in scale3 abspack scaling algorithm.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.063
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1292
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_platon_squeeze_details
;
;
_refine_diff_density_max         0.611
_refine_diff_density_min         -0.436
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     769
_refine_ls_number_reflns         13931
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.0652
_refine_ls_R_factor_gt           0.056
_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^)+(0.0822P)^2^+3.1648P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1561
_refine_ls_wR_factor_ref         0.1622
_reflns_number_gt                12023
_reflns_number_total             13931
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3cc48379g.txt
_cod_data_source_block           shelx
_cod_database_code               7112043
_shelx_estimated_absorpt_t_min   0.408
_shelx_estimated_absorpt_t_max   0.612