Metal-Metal Bonding in Low-Coordinate Dicobalt Complexes Supported by Phosphinoamide Ligands
Ramyaa Mathialagan; Subramaniam Kuppuswamy; Alexandra T. De Denko; Mark W. Bezpalko; Bruce M. Foxman; Christine M. Thomas; Inorganic Chemistry 52 (2013) 701–706; doi:10.1021/ic3018375

data_4333550
_publ_contact_author_address
;Brandeis University
Dept. of Chemistry    
415 South St MS 015    
Waltham, MA 02454    
;
_publ_contact_author_email       thomasc@brandeis.edu
_publ_contact_author_name        'Christine M. Thomas'
_publ_section_title
;
 Metal-Metal Bonding in Low-Coordinate Dicobalt Complexes Supported by
 Phosphinoamide Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              701
_journal_page_last               706
_journal_paper_doi               10.1021/ic3018375
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C36 H68 Co2 N2 P4'
_chemical_formula_sum            'C36 H68 Co2 N2 P4'
_chemical_formula_weight         770.71
_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     direct
_audit_creation_date             2012-06-16
_audit_creation_method           CRYSTALS_ver_14.43
_cell_angle_alpha                106.184(2)
_cell_angle_beta                 105.840(2)
_cell_angle_gamma                110.519(2)
_cell_formula_units_Z            1
_cell_length_a                   8.7710(5)
_cell_length_b                   11.5687(6)
_cell_length_c                   12.0272(6)
_cell_measurement_reflns_used    9347
_cell_measurement_temperature    120
_cell_measurement_theta_max      30
_cell_measurement_theta_min      3
_cell_volume                     1000.13(10)
_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 0.999
_diffrn_measured_fraction_theta_max 0.994
_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  0.025
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            31883
_diffrn_reflns_theta_full        29.459
_diffrn_reflns_theta_max         30.060
_diffrn_reflns_theta_min         1.935
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.015
_exptl_absorpt_correction_T_max  0.89
_exptl_absorpt_correction_T_min  0.81
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_description       prism
_exptl_crystal_F_000             412
_exptl_crystal_size_max          0.580
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.41
_refine_diff_density_min         -0.29
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.0088
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         5836
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0221
_refine_ls_R_factor_gt           0.0203
_refine_ls_shift/su_max          0.0002353
_refine_ls_shift/su_mean         0.0000167
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.02P)^2^ + 0.39P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0524
_refine_ls_wR_factor_gt          0.0506
_refine_ls_wR_factor_ref         0.0524
_reflns_limit_h_max              11
_reflns_limit_h_min              -12
_reflns_limit_k_max              15
_reflns_limit_k_min              -16
_reflns_limit_l_max              16
_reflns_limit_l_min              0
_reflns_number_gt                5439
_reflns_number_total             5836
_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   0.0221
_oxford_refine_ls_scale          0.24379(9)
_oxford_reflns_number_all        5836
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'RM_106_0m in P-1'
_iucr_refine_instructions_details_constraints
;
BLOCK 
CONT SCALE 
CONT CO   (    1 ,X'S,U'S)  UNTIL C    (   18 ) 
CONT H    (   11 ,X'S,U[ISO])  UNTIL H    (  183 ) 
END                                                                             
;
_iucr_refine_instructions_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;
_cod_data_source_file            ic3018375_si_002_3.cif
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4333550