Heterobimetallic Ti/Co Complexes That Promote Catalytic N-N Bond Cleavage.
Wu, Bing; Gramigna, Kathryn M.; Bezpalko, Mark W.; Foxman, Bruce M.; Thomas, Christine M.; Inorganic chemistry 54 (2015) 10909–10917; doi:10.1021/acs.inorgchem.5b01962

data_4344397
_publ_section_title
;
 Heterobimetallic Ti/Co Complexes That Promote Catalytic N-N Bond
 Cleavage.
;
_journal_issue                   22
_journal_name_full               'Inorganic chemistry'
_journal_page_first              10909
_journal_page_last               10917
_journal_paper_doi               10.1021/acs.inorgchem.5b01962
_journal_volume                  54
_journal_year                    2015
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C42 H69 Co1 I1 N3 P3 Ti1'
_chemical_formula_sum            'C42 H69 Co I N3 P3 Ti'
_chemical_formula_weight         942.69
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2014-02-26
_audit_creation_method           CRYSTALS_ver_14.52
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.3305(4)
_cell_length_b                   15.8386(5)
_cell_length_c                   40.4713(12)
_cell_measurement_reflns_used    9052
_cell_measurement_temperature    120
_cell_measurement_theta_max      29
_cell_measurement_theta_min      2
_cell_volume                     9186.0(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 0.997
_diffrn_measured_fraction_theta_max 0.995
_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  0.057
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       55
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            76887
_diffrn_reflns_theta_full        28.482
_diffrn_reflns_theta_max         29.063
_diffrn_reflns_theta_min         1.381
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.342
_exptl_absorpt_correction_T_max  0.81
_exptl_absorpt_correction_T_min  0.73
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.363
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3912
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.160
_refine_diff_density_max         1.33
_refine_diff_density_min         -0.77
_refine_ls_abs_structure_details 'Flack (1983), 10533 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.059(11)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9695
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     919
_refine_ls_number_reflns         23799
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0582
_refine_ls_R_factor_gt           0.0415
_refine_ls_shift/su_max          0.0059954
_refine_ls_shift/su_mean         0.0001792
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.03P)^2^ + 7.30P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0910
_refine_ls_wR_factor_gt          0.0862
_refine_ls_wR_factor_ref         0.0910
_reflns_limit_h_max              19
_reflns_limit_h_min              -19
_reflns_limit_k_max              21
_reflns_limit_k_min              0
_reflns_limit_l_max              55
_reflns_limit_l_min              0
_reflns_number_gt                18810
_reflns_number_total             23799
_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   0.0582
_oxford_refine_ls_scale          0.046739(3)
_oxford_reflns_number_all        23799
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'bw_326_1_0m in P2(1)2(1)2(1)'
_cod_data_source_file            ic5b01962_si_002.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 4344395--4344402.cif.'
_cod_original_cell_volume        9186.0(3)
_cod_original_sg_symbol_Hall     'P 2ac 2ab '
_cod_original_sg_symbol_H-M      'P 21 21 21 '
_cod_original_formula_sum        'C42 H69 Co1 I1 N3 P3 Ti1'
_cod_database_code               4344397