A short intramolecular hydrogen bond is a key factor in the self-assembly of a dimeric complex with a 22-membered metallamacrocyclic cavity
Fritsky, Igor O.; Kozłowski, Henryk; Prisyazhnaya, Elena V.; Karaczyn, Aldona; Kalibabchuk, Valentina A.; Głowiak, Tadeusz; Journal of the Chemical Society, Dalton Transactions  (1998) 1535–; doi:10.1039/a801781f

data_7028091
_publ_contact_author             'Igor O.Fritsky'
_publ_section_title
;
 A short intramolecular hydrogen bond is a key factor in the self-assembly
 of a dimeric complex with a 22-membered metallamacrocyclic cavity
;
_journal_issue                   10
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1535
_journal_paper_doi               10.1039/a801781f
_journal_year                    1998
_chemical_formula_sum            'C10 H21 Cl Cu N4 O10'
_chemical_formula_weight         456.30
_chemical_name_systematic
; 
bis{[N,N'-bis(2-hydroxyiminopropionyl)-1,4-diaminobutane (1-)] 
[aqua] copper(II)} diperchlorate  dihydrate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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_creation_method           SHELXL
_cell_angle_alpha                103.20(3)
_cell_angle_beta                 90.87(3)
_cell_angle_gamma                107.56(3)
_cell_formula_units_Z            2
_cell_length_a                   8.734(2)
_cell_length_b                   9.497(2)
_cell_length_c                   11.988(2)
_cell_measurement_reflns_used    50
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      42.0
_cell_measurement_theta_min      22.0
_cell_volume                     919.2(4)
_computing_cell_refinement       'Kuma KM4 software 1996'
_computing_data_collection       'Kuma KM4 software 1996'
_computing_data_reduction        'Kuma KM4 software 1996'
_computing_publication_material  'ORTEP, 1964'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Kuma KM4 automatic diffractometer'
_diffrn_measurement_method       'profile data from omega/2theta scans'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0315
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4200
_diffrn_reflns_theta_max         30.05
_diffrn_reflns_theta_min         2.32
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.390
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.649
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             470
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.726
_refine_diff_density_min         -0.634
_refine_diff_density_rms         0.097
_refine_ls_extinction_coef       0.0138(25)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.068
_refine_ls_goodness_of_fit_obs   1.152
_refine_ls_hydrogen_treatment    'see experimental'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     238
_refine_ls_number_reflns         4200
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_restrained_S_obs      1.152
_refine_ls_R_factor_all          0.0586
_refine_ls_R_factor_obs          0.0436
_refine_ls_shift/esd_max         0.175
_refine_ls_shift/esd_mean        0.012
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0938P)^2^+0.1834P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1393
_refine_ls_wR_factor_obs         0.1294
_reflns_number_observed          3162
_reflns_number_total             4200
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            f801781sup1.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0938P)^2^+0.1834P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0938P)^2^+0.1834P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        919.2(3)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7028091