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_4328419
_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         'C16 H23 N O2'
_chemical_formula_sum            'C16 H23 N O2'
_chemical_formula_weight         261.35
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 111.900(9)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   9.9461(8)
_cell_length_b                   40.599(2)
_cell_length_c                   12.2510(10)
_cell_measurement_reflns_used    14100
_cell_measurement_temperature    100
_cell_measurement_theta_max      66.7347
_cell_measurement_theta_min      3.2630
_cell_volume                     4590.0(6)
_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      100
_diffrn_detector_area_resol_mean 10.4685
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'Enhance Ultra (Cu) X-ray Source'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.059
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -48
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            46384
_diffrn_reflns_theta_full        66.910
_diffrn_reflns_theta_max         66.910
_diffrn_reflns_theta_min         4.039
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.584
_exptl_absorpt_correction_T_max  0.849
_exptl_absorpt_correction_T_min  0.764
_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            colorless
_exptl_crystal_density_diffrn    1.135
_exptl_crystal_description       block
_exptl_crystal_F_000             1704
_exptl_crystal_size_max          0.698
_exptl_crystal_size_mid          0.456
_exptl_crystal_size_min          0.377
_refine_diff_density_max         0.31
_refine_diff_density_min         -0.29
_refine_ls_extinction_coef       49(3)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   0.9558
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     515
_refine_ls_number_reflns         8065
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0511
_refine_ls_R_factor_gt           0.0468
_refine_ls_shift/su_max          0.0009479
_refine_ls_shift/su_mean         0.0000786
_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: 
 0.217E+04 0.367E+04 0.229E+04 995. 236. 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1381
_refine_ls_wR_factor_gt          0.1351
_refine_ls_wR_factor_ref         0.1381
_reflns_limit_h_max              10
_reflns_limit_h_min              -11
_reflns_limit_k_max              48
_reflns_limit_k_min              0
_reflns_limit_l_max              14
_reflns_limit_l_min              0
_reflns_number_gt                7271
_reflns_number_total             8066
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.72
_oxford_diffrn_Wilson_scale      0.13
_oxford_refine_ls_r_factor_ref   0.0511
_oxford_refine_ls_scale          2.95(3)
_oxford_reflns_number_all        8065
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_cod_data_source_file            ic202493z_si_002_1.cif
_cod_data_source_block           OI343_H1L1
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_database_code               4328419
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
CONT EXTPARAM 
RIDE C   (   1,X'S) H   ( 311,X'S) H   ( 312,X'S) H   ( 313,X'S) 
RIDE C   (   2,X'S) H   ( 301,X'S) H   ( 302,X'S) H   ( 303,X'S) 
RIDE C   (   4,X'S) H   ( 323,X'S) H   ( 321,X'S) H   ( 322,X'S) 
RIDE C   (   6,X'S) H   ( 331,X'S) 
RIDE C   (   9,X'S) H   ( 381,X'S) H   ( 382,X'S) H   ( 383,X'S) 
RIDE C   (  10,X'S) H   ( 371,X'S) H   ( 372,X'S) H   ( 373,X'S) 
RIDE C   (  11,X'S) H   ( 391,X'S) H   ( 392,X'S) H   ( 393,X'S) 
RIDE C   (  12,X'S) H   ( 411,X'S) 
RIDE C   (  16,X'S) H   ( 241,X'S) H   ( 242,X'S) 
RIDE C   (  17,X'S) H   (  42,X'S) H   (  41,X'S) 
RIDE C   (  22,X'S) H   ( 112,X'S) H   ( 113,X'S) H   ( 111,X'S) 
RIDE C   (  23,X'S) H   ( 122,X'S) H   ( 121,X'S) H   ( 123,X'S) 
RIDE C   (  24,X'S) H   ( 102,X'S) H   ( 101,X'S) H   ( 103,X'S) 
RIDE C   (  25,X'S) H   ( 131,X'S) 
RIDE C   (  28,X'S) H   ( 201,X'S) H   ( 203,X'S) H   ( 202,X'S) 
RIDE C   (  29,X'S) H   ( 193,X'S) H   ( 192,X'S) H   ( 191,X'S) 
RIDE C   (  30,X'S) H   ( 212,X'S) H   ( 211,X'S) H   ( 213,X'S) 
RIDE C   (  31,X'S) H   ( 151,X'S) 
RIDE C   (  33,X'S) H   (  21,X'S) H   (  22,X'S) 
RIDE C   (  38,X'S) H   ( 473,X'S) H   ( 471,X'S) H   ( 472,X'S) 
RIDE C   (  39,X'S) H   ( 481,X'S) H   ( 482,X'S) H   ( 483,X'S) 
RIDE C   (  40,X'S) H   ( 461,X'S) H   ( 462,X'S) H   ( 463,X'S) 
RIDE C   (  41,X'S) H   ( 491,X'S) 
RIDE C   (  44,X'S) H   ( 541,X'S) H   ( 542,X'S) H   ( 543,X'S) 
RIDE C   (  45,X'S) H   ( 571,X'S) H   ( 572,X'S) H   ( 573,X'S) 
RIDE C   (  46,X'S) H   ( 551,X'S) H   ( 552,X'S) H   ( 553,X'S) 
RIDE C   (  47,X'S) H   ( 511,X'S) 
RIDE O   (   2,X'S) H   ( 231,X'S) 
RIDE O   (   3,X'S) H   (  31,X'S) 
RIDE O   (   5,X'S) H   (  11,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                                                                             
;