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_7005763
_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_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-(+)-pseudoephedrine)!2$).2H!2$O
_chemical_name_systematic
;
[Ni(N-acetyl-(+)-pseudoephedrine)~2~].2H~2~O
;
_space_group_IT_number           143
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 3'
_symmetry_space_group_name_H-M   'P 3'
_atom_sites_solution_hydrogens   difmap
_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             2007-06-22T17:05:46-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   17.611(12)
_cell_length_b                   17.611(12)
_cell_length_c                   7.158(6)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    293
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     1923(2)
_computing_cell_refinement       'USER DEFINED CELL REFINEMENT'
_computing_data_collection       'USER DEFINED DATA COLLECTION'
_computing_data_reduction        'USER DEFINED DATA REDUCTION'
_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_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  Unknown
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.074
_diffrn_reflns_av_unetI/netI     0.0773
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            23449
_diffrn_reflns_theta_full        26.294
_diffrn_reflns_theta_max         27.107
_diffrn_reflns_theta_min         3.534
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.806
_exptl_absorpt_correction_T_max  0.9605
_exptl_absorpt_correction_T_min  0.9375
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             858
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.25
_refine_diff_density_min         -0.39
_refine_diff_density_rms         0.065
_refine_ls_abs_structure_details 'Flack (1983), 2670 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.018(19)
_refine_ls_extinction_coef       0.0058(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0815
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         2896
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0738
_refine_ls_R_factor_gt           0.031
_refine_ls_shift/su_max          0.000439
_refine_ls_shift/su_mean         0
_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:
2.77 -2.51 3.01 -0.921 0.707
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0607
_refine_ls_wR_factor_gt          0.0346
_refine_ls_wR_factor_ref         0.0346
_reflns_number_gt                2896
_reflns_number_total             5490
_reflns_threshold_expression     I>3.0\s(I)
_cod_data_source_file            b705195f.txt
_cod_data_source_block           7
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal' 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               7005763