Stereochemistry of optically active nickel(ii) and cobalt(ii) coordination compounds derived from N-acetyl aminoalcohols
Vargas-Díaz, Gabriela; López-Sandoval, Horacio; Vázquez-Palma, Adriana B.; Flores-Alamo, Marcos; Peña-Hueso, Adrián; Sánchez-Ruíz, Sonia A.; Flores-Parra, Angelina; Contreras, Rosalinda; Barba-Behrens, Norah; Dalton Transactions  (2007) 4185–; doi:10.1039/b705195f

data_7005761
_publ_section_title
;
 Stereochemistry of optically active nickel(ii) and cobalt(ii)
 coordination compounds derived from N-acetyl aminoalcohols
;
_journal_issue                   37
_journal_name_full               'Dalton Transactions'
_journal_page_first              4185
_journal_paper_doi               10.1039/b705195f
_journal_year                    2007
_chemical_absolute_configuration ad
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C24 H32 N2 Ni O6, 2(H2 O)'
_chemical_formula_sum            'C24 H36 N2 Ni O8'
_chemical_formula_weight         539.27
_chemical_name_common            (Ni(N-acetyl-(+)-ephedrine)!2$).2H!2$O
_chemical_name_systematic
;
[Ni(N-acetyl-(+)-ephedrine)~2~].2H~2~O
;
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      1
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2007-06-08T12:56:17-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                70.3550(15)
_cell_angle_beta                 81.6001(14)
_cell_angle_gamma                81.6535(14)
_cell_formula_units_Z            1
_cell_length_a                   7.2510(2)
_cell_length_b                   8.9808(3)
_cell_length_c                   10.9121(4)
_cell_measurement_reflns_used    8832
_cell_measurement_temperature    293
_cell_measurement_theta_max      27
_cell_measurement_theta_min      3
_cell_measurement_wavelength     0.71073
_cell_volume                     658.53(4)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997-2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_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    'SHELXS 97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      -0.13818
_diffrn_orient_matrix_UB_12      0.277033E-1
_diffrn_orient_matrix_UB_13      -0.36496E-2
_diffrn_orient_matrix_UB_21      -0.181849E-1
_diffrn_orient_matrix_UB_22      -0.241032E-1
_diffrn_orient_matrix_UB_23      0.970918E-1
_diffrn_orient_matrix_UB_31      0.147928E-1
_diffrn_orient_matrix_UB_32      0.113049
_diffrn_orient_matrix_UB_33      -0.01151
_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  0.049
_diffrn_reflns_av_unetI/netI     0.0576
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8611
_diffrn_reflns_theta_full        26.124
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         3.503
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.785
_exptl_absorpt_correction_T_max  0.889
_exptl_absorpt_correction_T_min  0.8547
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'light blue'
_exptl_crystal_density_diffrn    1.36
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             286
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.82
_refine_diff_density_min         -0.51
_refine_diff_density_rms         0.059
_refine_ls_abs_structure_details 'Flack (1983), 1982 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.052(14)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0838
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         4374
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_gt           0.0462
_refine_ls_shift/su_max          0.000129
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef F
_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:
2.14 -0.454 1.93 -0.396 0.404
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0672
_refine_ls_wR_factor_gt          0.0562
_refine_ls_wR_factor_ref         0.0562
_reflns_number_gt                4374
_reflns_number_total             4953
_reflns_threshold_expression     I>3.0\s(I)
_cod_data_source_file            b705195f.txt
_cod_data_source_block           5
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_formula_sum        'C24 H36 N2 Ni1 O8'
_cod_database_code               7005761