A heterobimetallic complex featuring a Ti‒Co multiple bond and its application to the reductive coupling of ketones to alkenes
Wu, Bing; Bezpalko, Mark W.; Foxman, Bruce M.; Thomas, Christine M.; Chem. Sci. 6 (2015) 2044–; doi:10.1039/C4SC03772C

data_1518588
_publ_section_title
;
 A heterobimetallic complex featuring a Ti--Co multiple bond and its
 application to the reductive coupling of ketones to alkenes
;
_journal_issue                   3
_journal_name_full               'Chem. Sci.'
_journal_page_first              2044
_journal_paper_doi               10.1039/C4SC03772C
_journal_volume                  6
_journal_year                    2015
_chemical_formula_moiety         'C31 H55 Cl1 Co1 N2 P3 Ti1'
_chemical_formula_sum            'C31 H55 Cl Co N2 P3 Ti'
_chemical_formula_weight         691.00
_chemical_properties_physical
'Air-sensitive, Moisture-sensitive, Hygroscopic, Oxygen-sensitive'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2014-09-12
_audit_creation_method           CRYSTALS_ver_14.61
_audit_update_record
;
2014-12-04 deposited with the CCDC.
2015-01-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.540(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.0138(7)
_cell_length_b                   18.8395(13)
_cell_length_c                   21.5085(16)
_cell_measurement_reflns_used    9940
_cell_measurement_temperature    120
_cell_measurement_theta_max      30
_cell_measurement_theta_min      2
_cell_volume                     3652.3(5)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.044
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            10380
_diffrn_reflns_theta_full        25.289
_diffrn_reflns_theta_max         30.106
_diffrn_reflns_theta_min         2.162
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.899
_exptl_absorpt_correction_T_max  0.84
_exptl_absorpt_correction_T_min  0.82
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.257
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1464
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: diethyl ether'
_exptl_crystal_size_max          0.310
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.190
_refine_diff_density_max         0.76
_refine_diff_density_min         -1.40
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     351
_refine_ls_number_reflns         10380
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0835
_refine_ls_R_factor_gt           0.0584
_refine_ls_shift/su_max          0.0020163
_refine_ls_shift/su_mean         0.0001160
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.08P)^2^ +22.68P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1820
_refine_ls_wR_factor_gt          0.1454
_refine_ls_wR_factor_ref         0.1820
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              26
_reflns_limit_k_min              0
_reflns_limit_l_max              30
_reflns_limit_l_min              0
_reflns_number_gt                7540
_reflns_number_total             10380
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.40
_oxford_diffrn_Wilson_scale      196.27
_oxford_refine_ls_r_factor_ref   0.0835
_oxford_refine_ls_scale          0.08674(3)
_oxford_reflns_number_all        10380
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'bw_334_0m in P2(1)/n'
_cod_data_source_file            c4sc03772c2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 1518587--1518589.cif.'
_cod_original_cell_volume        3652.3(3)
_cod_original_sg_symbol_Hall     '-P 2yn '
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        'C31 H55 Cl1 Co1 N2 P3 Ti1'
_cod_database_code               1518588