Utilization of Phosphinoamide Ligands in Homobimetallic Fe and Mn Complexes: The Effect of Disparate Coordination Environments on Metal-Metal Interactions and Magnetic and Redox Properties
Subramaniam Kuppuswamy; Mark W. Bezpalko; Tamara M. Powers; Mark M. Turnbull; Bruce M. Foxman; Christine M. Thomas; Inorganic Chemistry 51 (2012) 8225–8240; doi:10.1021/ic300776y

data_4329852
_publ_section_title
;
 Utilization of Phosphinoamide Ligands in Homobimetallic Fe and Mn
 Complexes: The Effect of Disparate Coordination Environments on
 Metal-Metal Interactions and Magnetic and Redox Properties
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8225
_journal_page_last               8240
_journal_paper_doi               10.1021/ic300776y
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety
'C19.50 H44.29 Cl1 Li0.50 Mn1 N1.50 O1.50 P1.50'
_chemical_formula_sum            'C19.5 H44.29 Cl Li0.5 Mn N1.5 O1.5 P1.5'
_chemical_formula_weight         464.18
_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             11-10-05
_audit_creation_method           CRYSTALS_ver_14.30
_cell_angle_alpha                90.101(10)
_cell_angle_beta                 93.261(11)
_cell_angle_gamma                107.517(10)
_cell_formula_units_Z            4
_cell_length_a                   11.866(2)
_cell_length_b                   12.897(3)
_cell_length_c                   17.631(4)
_cell_measurement_reflns_used    8213
_cell_measurement_temperature    120
_cell_measurement_theta_max      28
_cell_measurement_theta_min      2
_cell_volume                     2568.4(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 0.998
_diffrn_measured_fraction_theta_max 0.982
_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  0.051
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            46212
_diffrn_reflns_theta_full        27.875
_diffrn_reflns_theta_max         28.738
_diffrn_reflns_theta_min         2.039
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.723
_exptl_absorpt_correction_T_max  0.92
_exptl_absorpt_correction_T_min  0.87
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.200
_exptl_crystal_description       prism
_exptl_crystal_F_000             999.173
_exptl_crystal_size_max          0.430
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.120
_refine_diff_density_max         1.93
_refine_diff_density_min         -1.21
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.0053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     526
_refine_ls_number_reflns         13083
_refine_ls_number_restraints     93
_refine_ls_R_factor_all          0.0822
_refine_ls_R_factor_gt           0.0550
_refine_ls_shift/su_max          0.0003724
_refine_ls_shift/su_mean         0.0000140
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.07P)^2^ + 4.09P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1444
_refine_ls_wR_factor_gt          0.1339
_refine_ls_wR_factor_ref         0.1444
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              17
_reflns_limit_k_min              -17
_reflns_limit_l_max              23
_reflns_limit_l_min              0
_reflns_number_gt                9279
_reflns_number_total             13083
_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   0.0822
_oxford_refine_ls_scale          0.16602(7)
_oxford_reflns_number_all        13083
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'sk_277_0m in P-1'
_cod_data_source_file            ic300776y_si_002_6.cif
_cod_data_source_block           8
_cod_original_cell_volume        2568.4(9)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum
'C19.50 H44.29 Cl1 Li0.50 Mn1 N1.50 O1.50 P1.50'
_cod_database_code               4329852
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S C(42,OCC) 
SUMFIX PART(1001,OCC) AND PART(1002,OCC) 
SUMFIX PART(1003,OCC) AND PART(1004,OCC) 
RIDE C   (   1,X'S) H   (  11,X'S) 
RIDE C   (   2,X'S) H   (  21,X'S) H   (  22,X'S) H   (  23,X'S) 
RIDE C   (   3,X'S) H   (  31,X'S) H   (  32,X'S) H   (  33,X'S) 
RIDE C   (   4,X'S) H   (  41,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) H   (  52,X'S) H   (  53,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) H   (  62,X'S) H   (  63,X'S) 
RIDE C   (   7,X'S) H   (  71,X'S) 
RIDE C   (   8,X'S) H   (  81,X'S) H   (  82,X'S) H   (  83,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) H   (  92,X'S) H   (  93,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) H   ( 112,X'S) H   ( 113,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) H   ( 122,X'S) H   ( 123,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) H   ( 142,X'S) H   ( 143,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) H   ( 152,X'S) H   ( 153,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) H   ( 172,X'S) H   ( 173,X'S) 
RIDE C   (  18,X'S) H   ( 181,X'S) H   ( 182,X'S) H   ( 183,X'S) 
RIDE C   (  19,X'S) H   ( 191,X'S) 
RIDE C   (  20,X'S) H   ( 201,X'S) H   ( 202,X'S) H   ( 203,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) H   ( 212,X'S) H   ( 213,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) H   ( 232,X'S) H   ( 233,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) H   ( 242,X'S) H   ( 243,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) H   ( 262,X'S) H   ( 263,X'S) 
RIDE C   (  27,X'S) H   ( 271,X'S) H   ( 272,X'S) H   ( 273,X'S) 
RIDE C   (  28,X'S) H   ( 281,X'S) H   ( 282,X'S) 
RIDE C   (  29,X'S) H   ( 291,X'S) H   ( 292,X'S) 
RIDE C   (  30,X'S) H   ( 301,X'S) H   ( 302,X'S) 
RIDE C   (  31,X'S) H   ( 311,X'S) H   ( 312,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) H   ( 334,X'S) 
CONT H   ( 332,X'S) H   ( 333,X'S) 
RIDE C   (  34,X'S) H   ( 342,X'S) H   ( 344,X'S) H   ( 345,X'S) 
CONT H   ( 341,X'S) H   ( 343,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) H   ( 352,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) H   ( 362,X'S) 
RIDE C   (  37,X'S) H   ( 371,X'S) H   ( 372,X'S) 
RIDE C   (  38,X'S) H   ( 381,X'S) H   ( 382,X'S) 
RIDE C   (  39,X'S) H   ( 391,X'S) H   ( 392,X'S) H   ( 395,X'S) 
CONT H   ( 393,X'S) H   ( 394,X'S) 
RIDE C   (  40,X'S) H   ( 402,X'S) H   ( 404,X'S) 
CONT     H   ( 401,X'S) H   ( 403,X'S) 
RIDE C   (  41,X'S) H   ( 411,X'S) H   ( 412,X'S) 
RIDE C   (  42,X'S) H   ( 421,X'S) H   ( 422,X'S) H   ( 425,X'S) 
CONT     H   ( 423,X'S) H   ( 424,X'S) H   ( 426,X'S) 
RIDE C   (  43,X'S) H   ( 431,X'S) H   ( 432,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
RESTRAIN 0.79346, 0.0003 = C(42,OCC) 
U(IJ)'S  0.0, 0.010000 = O(20) TO C(36) 
U(IJ)'S  0.0, 0.007000 = C(35) TO C(36) 
U(IJ)'S  0.0, 0.007000 = C(34) TO C(35) 
U(IJ)'S  0.0, 0.007000 = C(33) TO C(34) 
U(IJ)'S  0.0, 0.007000 = O(20) TO C(33) 
U(IJ)'S  0.0, 0.007000 = O(30) TO C(40) 
U(IJ)'S  0.0, 0.007000 = C(39) TO C(40) 
U(IJ)'S  0.0, 0.007000 = C(38) TO C(39) 
U(IJ)'S  0.0, 0.007000 = C(37) TO C(38) 
U(IJ)'S  0.0, 0.007000 = O(30) TO C(37) 
DISTANCE 1.470000 , 0.005000 = C(39) TO C(40) 
U(IJ)'S  0.0, 0.007000 = O(1) TO C(31) 
U(IJ)'S  0.0, 0.007000 = C(30) TO C(31) 
U(IJ)'S  0.0, 0.007000 = C(29) TO C(30) 
U(IJ)'S  0.0, 0.007000 = C(28) TO C(29) 
U(IJ)'S  0.0, 0.007000 = O(1) TO C(28) 
VIBRATION 0.0, 0.010000 = C(38) TO C(39) 
END                                                                             
;