Versatile Chemical Transformations of Benzoxazole Based Ligands on Complexation with 3d-Metal Ions
Olga Iasco; Ghenadie Novitchi; Erwann Jeanneau; Jean Bernard Tommasino; Nans Roques; Dominique Luneau; Inorganic Chemistry 51 (2012) 2588–2596; doi:10.1021/ic202493z

data_4328421
_publ_contact_author_address
; 
Univ. Claude Bernard Lyon 1
Cristallography and Molecular Engineering
LMI (UMR 5615)
Domaine Scientifique de la Doua
69622 Villeurbanne cedex
;
_publ_contact_author_email       luneau@univ-lyon1.fr
_publ_contact_author_fax         '+33 472 440 618'
_publ_contact_author_name        'Dominique Luneau'
_publ_contact_author_phone       '+33 472 431 418'
_publ_section_title
;
 Versatile Chemical Transformations of Benzoxazole Based Ligands on
 Complexation with 3d-Metal Ions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2588
_journal_page_last               2596
_journal_paper_doi               10.1021/ic202493z
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C62 H82 N4 Ni1 O6'
_chemical_formula_sum            'C62 H82 N4 Ni O6'
_chemical_formula_weight         1038.07
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 104.710(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.2714(9)
_cell_length_b                   14.8637(6)
_cell_length_c                   17.3337(9)
_cell_measurement_reflns_used    3187
_cell_measurement_temperature    293
_cell_measurement_theta_max      29.2767
_cell_measurement_theta_min      2.6121
_cell_volume                     3307.2(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_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    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      293
_diffrn_detector_area_resol_mean 15.9897
_diffrn_measured_fraction_theta_full 0.939
_diffrn_measured_fraction_theta_max 0.838
_diffrn_measurement_device_type  'Xcalibur, Eos, Nova'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'Mova (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.000
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            16779
_diffrn_reflns_theta_full        25.232
_diffrn_reflns_theta_max         29.340
_diffrn_reflns_theta_min         2.617
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.339
_exptl_absorpt_correction_T_max  0.985
_exptl_absorpt_correction_T_min  0.937
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.042
_exptl_crystal_description       needle
_exptl_crystal_F_000             1116
_exptl_crystal_size_max          0.271
_exptl_crystal_size_mid          0.056
_exptl_crystal_size_min          0.054
_refine_diff_density_max         1.01
_refine_diff_density_min         -1.16
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.9654
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     330
_refine_ls_number_reflns         7620
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1788
_refine_ls_R_factor_gt           0.0885
_refine_ls_shift/su_max          0.0001366
_refine_ls_shift/su_mean         0.0000184
_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: 
 0.123E+06 0.190E+06 0.103E+06 0.496E+05 0.691E+04 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1833
_refine_ls_wR_factor_gt          0.1352
_refine_ls_wR_factor_ref         0.1833
_reflns_limit_h_max              16
_reflns_limit_h_min              -17
_reflns_limit_k_max              20
_reflns_limit_k_min              0
_reflns_limit_l_max              23
_reflns_limit_l_min              0
_reflns_number_gt                3639
_reflns_number_total             7620
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.76
_oxford_diffrn_Wilson_scale      0.01
_oxford_refine_ls_r_factor_ref   0.1788
_oxford_refine_ls_scale          38(5)
_oxford_reflns_number_all        7620
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_cod_data_source_file            ic202493z_si_002_3.cif
_cod_data_source_block           OI72_NiL3
_cod_original_sg_symbol_H-M      'P 2/n '
_cod_original_formula_sum        'C62 H82 N4 Ni1 O6'
_cod_database_code               4328421
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
RIDE C   (   1,X'S) H   ( 291,X'S) H   ( 292,X'S) H   ( 293,X'S) 
RIDE C   (   3,X'S) H   ( 281,X'S) H   ( 282,X'S) H   ( 283,X'S) 
RIDE C   (   4,X'S) H   ( 271,X'S) H   ( 272,X'S) H   ( 273,X'S) 
RIDE C   (   6,X'S) H   ( 231,X'S) 
RIDE C   (   9,X'S) H   ( 331,X'S) H   ( 332,X'S) H   ( 333,X'S) 
RIDE C   (  10,X'S) H   ( 321,X'S) H   ( 322,X'S) H   ( 323,X'S) 
RIDE C   (  11,X'S) H   ( 311,X'S) H   ( 312,X'S) H   ( 313,X'S) 
RIDE C   (  14,X'S) H   ( 251,X'S) 
RIDE C   (  17,X'S) H   ( 141,X'S) 
RIDE C   (  19,X'S) H   ( 111,X'S) 
RIDE C   (  22,X'S) H   (  81,X'S) H   (  82,X'S) H   (  83,X'S) 
RIDE C   (  23,X'S) H   (  91,X'S) H   (  92,X'S) H   (  93,X'S) 
RIDE C   (  24,X'S) H   ( 101,X'S) H   ( 102,X'S) H   ( 103,X'S) 
RIDE C   (  25,X'S) H   (  51,X'S) 
RIDE C   (  28,X'S) H   ( 371,X'S) H   ( 372,X'S) H   ( 373,X'S) 
RIDE C   (  29,X'S) H   ( 361,X'S) H   ( 362,X'S) H   ( 363,X'S) 
RIDE C   (  30,X'S) H   ( 351,X'S) H   ( 352,X'S) H   ( 353,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                                                                             
;