3d Early Transition Metal Complexes Supported by a New Sterically Demanding Aryloxide Ligand
Keith Searles; Ba L. Tran; Maren Pink; Chun-Hsing Chen; Daniel J. Mindiola; Inorganic Chemistry 52 (2013) 11126–11135; doi:10.1021/ic401363p

data_4336189
_publ_section_title
;
 3d Early Transition Metal Complexes Supported by a New Sterically
 Demanding Aryloxide Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11126
_journal_page_last               11135
_journal_paper_doi               10.1021/ic401363p
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C80 H82 Na2 O4'
_chemical_formula_sum            'C80 H82 Na2 O4'
_chemical_formula_weight         1153.51
_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             13-08-05
_audit_creation_method           CRYSTALS_ver_14.40
_cell_angle_alpha                80.374(3)
_cell_angle_beta                 76.077(3)
_cell_angle_gamma                80.536(4)
_cell_formula_units_Z            1
_cell_length_a                   10.3211(17)
_cell_length_b                   12.777(2)
_cell_length_c                   13.069(2)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    150
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     1635.3(4)
_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      150
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.987
_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  0.030
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            31025
_diffrn_reflns_theta_full        25.267
_diffrn_reflns_theta_max         30.079
_diffrn_reflns_theta_min         1.630
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.082
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.96
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.171
_exptl_crystal_description       plate
_exptl_crystal_F_000             616
_exptl_crystal_size_max          0.414
_exptl_crystal_size_mid          0.198
_exptl_crystal_size_min          0.098
_refine_diff_density_max         0.44
_refine_diff_density_min         -0.49
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.0355
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     425
_refine_ls_number_reflns         9471
_refine_ls_number_restraints     77
_refine_ls_R_factor_all          0.0724
_refine_ls_R_factor_gt           0.0542
_refine_ls_shift/su_max          0.0265866
_refine_ls_shift/su_mean         0.0009360
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.08P)^2^ + 0.70P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1651
_refine_ls_wR_factor_gt          0.1386
_refine_ls_wR_factor_ref         0.1648
_reflns_limit_h_max              14
_reflns_limit_h_min              -13
_reflns_limit_k_max              17
_reflns_limit_k_min              -17
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_gt                7247
_reflns_number_total             9499
_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   0.0723
_oxford_refine_ls_scale          0.20914(16)
_oxford_reflns_number_all        9476
_oxford_reflns_threshold_expression_ref I>0.0\s(I)
_oxford_structure_analysis_title 'mo_12015_0m in P-1'
_cod_data_source_file            ic401363p_si_005.cif
_cod_data_source_block           12015
_cod_original_cell_volume        1635.4(5)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4336189
_iucr_refine_instruction_details_constraints
;
BLOCK 
CONT SCALE 
CONT NA    (    1 ,X'S,U'S)  UNTIL C    (   36 ) 
CONT C    (   37 ,X'S,U'S)  UNTIL C    (  401 ) 
SUMFIX PART(1001,OCC) AND PART(1002,OCC) 
RIDE C   (   3,X'S) H   (  31,X'S) 
RIDE C   (   5,X'S) H   (  51,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) H   ( 102,X'S) H   ( 103,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) 
RIDE C   (  13,X'S) H   ( 131,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   (  19,X'S) H   ( 191,X'S) 
RIDE C   (  20,X'S) H   ( 201,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) 
RIDE C   (  27,X'S) H   ( 271,X'S) 
RIDE C   (  28,X'S) H   ( 281,X'S) 
RIDE C   (  29,X'S) H   ( 291,X'S) 
RIDE C   (  30,X'S) H   ( 301,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) 
RIDE C   (  36,X'S) H   ( 361,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) 
RIDE C   (  40,X'S) H   ( 401,X'S) H   ( 402,X'S) 
RIDE C   ( 371,X'S) H   (3711,X'S) H   (3712,X'S) 
RIDE C   ( 381,X'S) H   (3811,X'S) H   (3812,X'S) 
RIDE C   ( 391,X'S) H   (3911,X'S) H   (3912,X'S) 
RIDE C   ( 401,X'S) H   (4011,X'S) H   (4012,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) 
SAME 0.01, 0.1 
CONT O(2) C(37) C(38) C(39) C(40) AND 
CONT O(2) C(40) C(39) C(38) C(37) AND 
CONT O(2) C(371) C(381) C(391) C(401) AND 
CONT O(2) C(401) C(391) C(381) C(371) 
DISTANCE 1.450000 , 0.001000 = C(371) TO C(381) 
U(IJ)'S  0.0, 0.005000 = C(38) TO C(381) 
U(IJ)'S  0.0, 0.005000 = C(39) TO C(391) 
U(IJ)'S  0.0, 0.005000 = C(40) TO C(401) 
U(IJ)'S  0.0, 0.005000 = C(37) TO C(40) 
U(IJ)'S  0.0, 0.005000 = C(37) TO C(38) 
U(IJ)'S  0.0, 0.005000 = C(371) TO C(381) 
U(IJ)'S  0.0, 0.005000 = C(371) TO C(371) 
END                                                                             
;