Structural, Magnetic, and Electronic Properties of Phenolic Oxime Complexes of Cu and Ni
Alexander M. Whyte; Benjamin Roach; David K. Henderson; Peter A. Tasker; Michio M. Matsushita; Kunio Awaga; Fraser J. White; Patricia Richardson; Neil Robertson; Inorganic Chemistry 50 (2011) 12867–12876; doi:10.1021/ic2020644

data_4327192
_publ_contact_author_address
; 
 Alex Whyte
 The University of Edinburgh 
 Joseph Black Building 
 West Mains Road 
 Edinburgh 
 EH9 3JJ 
;
_publ_contact_author_email       A.Whyte-4@sms.ed.ac.uk
_publ_contact_author_name        'Alex Whyte'
_publ_contact_author_phone       '+44(0)131 6504806'
_publ_section_title
;
 Structural, Magnetic, and Electronic Properties of Phenolic Oxime
 Complexes of Cu and Ni
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12867
_journal_page_last               12876
_journal_paper_doi               10.1021/ic2020644
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C34 H54 Cu1 N2 O5 S1'
_chemical_formula_sum            'C34 H54 Cu N2 O5 S'
_chemical_formula_weight         666.42
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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             11-06-01
_audit_creation_method           CRYSTALS_ver_14.21
_cell_angle_alpha                99.417(4)
_cell_angle_beta                 97.842(3)
_cell_angle_gamma                104.953(3)
_cell_formula_units_Z            2
_cell_length_a                   8.0420(4)
_cell_length_b                   12.8510(8)
_cell_length_c                   17.6720(10)
_cell_measurement_reflns_used    7155
_cell_measurement_temperature    150
_cell_measurement_theta_max      26
_cell_measurement_theta_min      2
_cell_volume                     1709.88(17)
_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      150
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.076
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            28516
_diffrn_reflns_theta_full        25.679
_diffrn_reflns_theta_max         26.473
_diffrn_reflns_theta_min         1.677
_diffrn_source                   'sealed X-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.741
_exptl_absorpt_correction_T_max  0.84
_exptl_absorpt_correction_T_min  0.65
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.294
_exptl_crystal_description       block
_exptl_crystal_F_000             714
_exptl_crystal_size_max          0.390
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.240
_refine_diff_density_max         1.53
_refine_diff_density_min         -1.07
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.0029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         6975
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0849
_refine_ls_R_factor_gt           0.0539
_refine_ls_shift/su_max          0.0007328
_refine_ls_shift/su_mean         0.0000233
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 2.01 2.38 0.486 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1636
_refine_ls_wR_factor_gt          0.1325
_refine_ls_wR_factor_ref         0.1636
_reflns_limit_h_max              9
_reflns_limit_h_min              -10
_reflns_limit_k_max              15
_reflns_limit_k_min              -16
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                3721
_reflns_number_total             6977
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.59
_oxford_diffrn_Wilson_scale      137.28
_oxford_refine_ls_r_factor_ref   0.0849
_oxford_refine_ls_scale          0.09036(3)
_oxford_reflns_number_all        6975
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'NR9008 in P-1'
_cod_data_source_file            ic2020644_si_001_3.cif
_cod_data_source_block           NR9008
_cod_original_formula_sum        'C34 H54 Cu1 N2 O5 S1'
_cod_database_code               4327192
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
RIDE O   (   7,X'S) H   (   8,X'S) 
RIDE C   (   9,X'S) H   (  10,X'S) H   (  11,X'S) H   (  12,X'S) 
RIDE C   (  13,X'S) H   (  44,X'S) 
RIDE C   (  15,X'S) H   (  18,X'S) 
RIDE C   (  16,X'S) H   (  17,X'S) 
RIDE C   (  20,X'S) H   (  21,X'S) H   (  22,X'S) H   (  23,X'S) 
RIDE C   (  24,X'S) H   (  38,X'S) H   (  39,X'S) 
RIDE C   (  26,X'S) H   (  27,X'S) H   (  28,X'S) H   (  29,X'S) 
RIDE C   (  30,X'S) H   (  31,X'S) H   (  32,X'S) H   (  33,X'S) 
RIDE C   (  34,X'S) H   (  35,X'S) H   (  36,X'S) H   (  37,X'S) 
RIDE C   (  40,X'S) H   (  41,X'S) H   (  42,X'S) H   (  43,X'S) 
RIDE C   (  48,X'S) H   (  79,X'S) 
RIDE C   (  51,X'S) H   (  65,X'S) H   (  66,X'S) 
RIDE C   (  53,X'S) H   (  54,X'S) H   (  55,X'S) H   (  56,X'S) 
RIDE C   (  57,X'S) H   (  58,X'S) H   (  59,X'S) H   (  60,X'S) 
RIDE C   (  61,X'S) H   (  62,X'S) H   (  63,X'S) H   (  64,X'S) 
RIDE C   (  67,X'S) H   (  68,X'S) H   (  69,X'S) H   (  70,X'S) 
RIDE C   (  71,X'S) H   (  72,X'S) H   (  73,X'S) H   (  74,X'S) 
RIDE C   (  75,X'S) H   (  78,X'S) 
RIDE C   (  76,X'S) H   (  77,X'S) 
RIDE O   (  82,X'S) H   (  83,X'S) 
RIDE C   (  84,X'S) H   (  85,X'S) H   (  86,X'S) H   (  87,X'S) 
RIDE C   (  91,X'S) H   (  92,X'S) H   (  93,X'S) H   (  94,X'S) 
RIDE C   (  95,X'S) H   (  96,X'S) H   (  97,X'S) H   (  98,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) 
END                                                                             
;