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_1518589
_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         'C68 H104 Co2 I2 N4 O2 P4 Ti2'
_chemical_formula_sum            'C68 H104 Co2 I2 N4 O2 P4 Ti2'
_chemical_formula_weight         1600.96
_chemical_properties_physical
'Air-sensitive, Moisture-sensitive, Hygroscopic, Oxygen-sensitive'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_creation_date             2014-09-09
_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                110.6819(17)
_cell_angle_beta                 94.623(2)
_cell_angle_gamma                117.1503(16)
_cell_formula_units_Z            1
_cell_length_a                   12.5912(5)
_cell_length_b                   13.4571(5)
_cell_length_c                   13.5956(5)
_cell_measurement_reflns_used    9901
_cell_measurement_temperature    120
_cell_measurement_theta_max      30
_cell_measurement_theta_min      3
_cell_volume                     1835.07(13)
_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    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.034
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            41967
_diffrn_reflns_theta_full        30.030
_diffrn_reflns_theta_max         30.030
_diffrn_reflns_theta_min         2.305
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.626
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.72
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             820
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: benzene'
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.180
_refine_diff_density_max         1.28
_refine_diff_density_min         -1.21
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9919
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         10702
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0420
_refine_ls_R_factor_gt           0.0327
_refine_ls_shift/su_max          0.0098159
_refine_ls_shift/su_mean         0.0005645
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.04P)^2^ + 3.21P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0890
_refine_ls_wR_factor_gt          0.0833
_refine_ls_wR_factor_ref         0.0890
_reflns_limit_h_max              17
_reflns_limit_h_min              -17
_reflns_limit_k_max              17
_reflns_limit_k_min              -18
_reflns_limit_l_max              19
_reflns_limit_l_min              0
_reflns_number_gt                8716
_reflns_number_total             10702
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0420
_oxford_refine_ls_scale          0.12167(3)
_oxford_reflns_number_all        10702
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'bw_374_0m in P-1'
_cod_data_source_file            c4sc03772c2.cif
_cod_data_source_block           4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Other' changed to 'other'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/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 2935 2014-11-11 08:27:57Z andrius 

 Adding full bibliography for 1518587--1518589.cif.
;
_cod_original_cell_volume        1835.07(7)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               1518589