X-Ray diffraction and molecular mechanics studies of 12-, 13-, and 14-membered tetraaza macrocycles containing pyridine: effect of the macrocyclic cavity size on the selectivity of the metal ion
Félix, Vitor; Costa, Judite; Delgado, Rita; Drew, Michael G. B.; Duarte, Maria Teresa; Resende, Catarina; Journal of the Chemical Society, Dalton Transactions  (2001) 1462–; doi:10.1039/b009773j

data_7702528
_publ_section_title
;
 X-Ray diffraction and molecular mechanics studies of 12-, 13-, and
 14-membered tetraaza macrocycles containing pyridine: effect of the
 macrocyclic cavity size on the selectivity of the metal ion
;
_journal_issue                   9
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1462
_journal_paper_doi               10.1039/b009773j
_journal_year                    2001
_chemical_formula_sum            'C12 H20 Cl2 N4 Ni O8'
_chemical_formula_weight         477.93
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                91.36(3)
_cell_angle_beta                 104.48(2)
_cell_angle_gamma                113.52(2)
_cell_formula_units_Z            2
_cell_length_a                   8.162(2)
_cell_length_b                   8.874(2)
_cell_length_c                   13.989(2)
_cell_measurement_temperature    293(2)
_cell_volume                     890.8(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  CAD4
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0108
_diffrn_reflns_av_sigmaI/netI    0.0151
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            3742
_diffrn_reflns_theta_full        26.03
_diffrn_reflns_theta_max         26.03
_diffrn_reflns_theta_min         1.52
_exptl_absorpt_coefficient_mu    1.440
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.782
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             492
_refine_diff_density_max         1.491
_refine_diff_density_min         -0.952
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         3500
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0772
_refine_ls_R_factor_gt           0.0690
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w==1/[\s^2^(Fo^2^)+(0.1215P)^2^+1.9627P] where P==(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1826
_refine_ls_wR_factor_ref         0.1943
_reflns_number_gt                3072
_reflns_number_total             3500
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b009773j.txt
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Triclinic' was changed to
'triclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

data item '_refine_ls_weighting_scheme' value 'calc
w==1/[\s^2^(Fo^2^)+(0.1215P)^2^+1.9627P] where P==(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. A new data item '_refine_ls_weighting_details'
was created with the value set to
'w==1/[\s^2^(Fo^2^)+(0.1215P)^2^+1.9627P] where P==(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7702528