Noninnocent Behavior of Bidentate Amidophosphido [NP]2-Ligands upon Coordination to Copper
Mark W. Bezpalko; Bruce M. Foxman; Christine M. Thomas; Inorganic Chemistry 52 (2013) 12329–12331; doi:10.1021/ic402257z

data_4336664
_publ_section_title
;
 Noninnocent Behavior of Bidentate Amidophosphido [NP]2-Ligands upon
 Coordination to Copper
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12329
_journal_page_last               12331
_journal_paper_doi               10.1021/ic402257z
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C48 H64 Cu2 N2 P6'
_chemical_formula_sum            'C48 H64 Cu2 N2 P6'
_chemical_formula_weight         981.98
_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             2012-12-03
_audit_creation_method           CRYSTALS_ver_14.43
_cell_angle_alpha                82.895(3)
_cell_angle_beta                 82.387(3)
_cell_angle_gamma                79.554(4)
_cell_formula_units_Z            1
_cell_length_a                   9.3693(7)
_cell_length_b                   10.5850(8)
_cell_length_c                   14.8420(10)
_cell_measurement_reflns_used    7828
_cell_measurement_temperature    120
_cell_measurement_theta_max      30
_cell_measurement_theta_min      2
_cell_volume                     1427.27(18)
_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 1.000
_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  0.047
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8313
_diffrn_reflns_theta_full        29.452
_diffrn_reflns_theta_max         30.053
_diffrn_reflns_theta_min         1.967
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.942
_exptl_absorpt_correction_T_max  0.89
_exptl_absorpt_correction_T_min  0.88
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.142
_exptl_crystal_description       prism
_exptl_crystal_F_000             514.000
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.120
_platon_squeeze_details
;During the structure solution, electron density 
difference maps revealed that there were considerable 
disordered solvent molecules which could not be successfully 
modeled.  From history, the remaining solvate was likely 
benzene in a volume of 245.9 \%A3 per unit cell (17.2%).  
It appeared that the cavity area contained ca. two benzene 
molecules, located near the center of symmetry at (0, 1/2 , 0). 
Modeling with or without restraints was unsuccessful, 
as was step by step acquisition of peaks using successive 
electron density difference maps.  Thus, the structure 
factors were modified using the PLATON SQUEEZE technique, 
in order to produce a "solvate-free" structure factor set.  
PLATON reported a total electron density of 75 e- per unit 
cell, likely representing two benzene, consistent with 
our earlier observations.  Use of the SQUEEZE technique 
resulted in a decrease of ca. 6.0 % in R.   
;
_refine_diff_density_max         0.67
_refine_diff_density_min         -0.62
_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     262
_refine_ls_number_reflns         8313
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0403
_refine_ls_shift/su_max          0.0015875
_refine_ls_shift/su_mean         0.0000401
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.04P)^2^ + 1.03P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0942
_refine_ls_wR_factor_gt          0.0895
_refine_ls_wR_factor_ref         0.0942
_reflns_limit_h_max              13
_reflns_limit_h_min              -12
_reflns_limit_k_max              14
_reflns_limit_k_min              -14
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                6301
_reflns_number_total             8313
_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   0.0571
_oxford_refine_ls_scale          0.22175(10)
_oxford_reflns_number_all        8313
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'mwb2_163_0m in P-1'
_iucr_refine_instructions_details_constraints
;
BLOCK 
CONT SCALE 
CONT CU   (    1 ,X'S,U'S)  UNTIL C    (   24 ) 
CONT C    (  220 ,X'S,U[ISO])  UNTIL C    (  221 ) 
SUMFIX PART(1001,OCC) AND PART(1002,OCC) 
RIDE C   (   2,X'S) H   (  21,X'S) 
RIDE C   (   3,X'S) H   (  31,X'S) 
RIDE C   (   4,X'S) H   (  41,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) 
RIDE C   (   8,X'S) H   (  81,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) 
RIDE C   (  18,X'S) H   ( 181,X'S) 
RIDE C   (  19,X'S) H   ( 193,X'S) H   ( 192,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   (  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   ( 220,X'S) H   (2201,X'S) H   (2202,X'S) H   (2203,X'S) 
RIDE C   ( 221,X'S) H   (2211,X'S) H   (2212,X'S) H   (2213,X'S) 
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            ic402257z_si_002_1.cif
_cod_data_source_block           5a
_cod_original_sg_symbol_Hall     '-P 1 '
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4336664