C-Branched chiral (racemic) macrocyclic amino acids: structure of their Ni(ii), Zn(ii) and Cu(ii) complexes.
Pellico, Daniel; Gómez-Gallego, Mar; Escudero, Rosa; Ramírez-López, Pedro; Oliván, Montserrat; Sierra, Miguel A.; Dalton transactions (Cambridge, England : 2003) 40 (2011) 9145–9153; doi:10.1039/c1dt10539f

data_7016459
_publ_section_title
;
 C-Branched chiral (racemic) macrocyclic amino acids: structure of
 their Ni(ii), Zn(ii) and Cu(ii) complexes.
;
_journal_issue                   36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9145
_journal_page_last               9153
_journal_paper_doi               10.1039/c1dt10539f
_journal_volume                  40
_journal_year                    2011
_chemical_formula_moiety         'C21 H22 N2 Ni O6, 7(H2 O)'
_chemical_formula_sum            'C21 H36 N2 Ni O13'
_chemical_formula_weight         583.23
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 108.0310(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.5486(10)
_cell_length_b                   16.1100(15)
_cell_length_c                   15.8867(15)
_cell_measurement_reflns_used    3302
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      21
_cell_measurement_theta_min      2
_cell_volume                     2567.2(4)
_computing_cell_refinement       'APEX2 v2008.4-0, Bruker AXS'
_computing_data_collection       'APEX2 v2008.4-0, Bruker AXS'
_computing_data_reduction
;
SAINT-Bruker integration program embedded in APEX2 v2008.4-0, Bruker AXS
;
_computing_molecular_graphics    'XP, SHELXTL v. 6.1 (Bruker, 2000)'
_computing_publication_material  'XCIF, SHELXTL v. 6.1 (Bruker, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Bruker SMART APEX CCD system'
_diffrn_measurement_method       '\w rotations with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0640
_diffrn_reflns_av_sigmaI/netI    0.0896
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            27115
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         1.85
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    0.825
_exptl_absorpt_correction_T_max  0.940
_exptl_absorpt_correction_T_min  0.766
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Absorption correction performed with SADABS program. This is based on the
method of Blessing: Blessing, R. H., Acta Crystallogr., Sect. A 1995, 51, 33.

SADABS: Area-Detector Absorption Correction. Bruker-AXS
within SAINT+ package, v. 6.1 (2000).
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.509
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.494
_refine_diff_density_min         -0.412
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.892
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     376
_refine_ls_number_reflns         6253
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      0.892
_refine_ls_R_factor_all          0.0933
_refine_ls_R_factor_gt           0.0429
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0320P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0832
_refine_ls_wR_factor_ref         0.0958
_reflns_number_gt                3550
_reflns_number_total             6253
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1dt10539f.txt
_cod_data_source_block           montse2as
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7016459