Copper-(II) and -(I) co-ordination by hexa-amine ligands of different rigidities. A thermodynamic, structural and electrochemical investigation †
Bazzicalupi, Carla; Bencini, Andrea; Ciattini, Samuele; Giorgi, Claudia; Masotti, Andrea; Paoletti, Piero; Valtancoli, Barbara; Navon, Nadav; Meyerstein, Dan; Journal of the Chemical Society, Dalton Transactions  (2000) 2383–; doi:10.1039/b002102o

data_7009575
_publ_section_title
;
 Copper-(II) and -(I) co-ordination by hexa-amine ligands of different
 rigidities. A thermodynamic, structural and electrochemical
 investigation&#x200A;&#x2020;
;
_journal_issue                   14
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2383
_journal_paper_doi               10.1039/b002102o
_journal_year                    2000
_chemical_formula_moiety
;
(Cu 2+)2, (C20 H29 N6 +1), (O H -1), (Cl O4 -1)3, Br -1, (H2 O)0.5
;
_chemical_formula_structural
;
[(Cu)2 (C20 H29 N6) (O H) (BR) (Cl O4)2] (Cl O4) (H2 O)0.5
;
_chemical_formula_sum            'C20 H31 Br Cl3 Cu2 N6 O13.5'
_chemical_formula_weight         884.85
_chemical_name_systematic
;
 ?
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 101.12(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.450(8)
_cell_length_b                   22.613(4)
_cell_length_c                   16.394(9)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298
_cell_measurement_theta_max      13
_cell_measurement_theta_min      7
_cell_volume                     3074(3)
_computing_cell_refinement       'P4 Siemens'
_computing_data_collection       'P4 Siemens'
_computing_data_reduction        'P4 Siemens'
_computing_molecular_graphics    'ORTEP-3 (Ver. 1.01\b)(Farrugia,1997)'
_computing_publication_material
;
SHELXL-93 (Sheldrick, 1993), PARST93 (Nardelli,1993)
;
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SIR92 (Altomare, 1993)'
_diffrn_ambient_temperature      298
_diffrn_measurement_device       'P4 Siemens'
_diffrn_measurement_method       \q/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1052
_diffrn_reflns_av_sigmaI/netI    0.0631
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            3341
_diffrn_reflns_theta_max         50.00
_diffrn_reflns_theta_min         3.37
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    6.301
_exptl_absorpt_correction_T_max  0.53
_exptl_absorpt_correction_T_min  0.44
_exptl_absorpt_correction_type   'refdelf (Walker and Stuart, 1983)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.912
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1780
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.773
_refine_diff_density_min         -0.732
_refine_diff_density_rms         0.170
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.061
_refine_ls_goodness_of_fit_obs   1.030
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     400
_refine_ls_number_reflns         3102
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.068
_refine_ls_restrained_S_obs      1.030
_refine_ls_R_factor_all          0.1227
_refine_ls_R_factor_obs          0.0920
_refine_ls_shift/esd_max         0.052
_refine_ls_shift/esd_mean        0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1819P)^2^+28.4912P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2971
_refine_ls_wR_factor_obs         0.2405
_reflns_number_observed          2268
_reflns_number_total             3104
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b002102o.txt
_cod_data_source_block           '[Cu2(HL3)(\m-OH)(ClO4)2Br]'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1819P)^2^+28.4912P] 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^)+(0.1819P)^2^+28.4912P] 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        3073.8(34)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C20 H31 Br Cl3 Cu2 N6 O13.50'
_cod_database_code               7009575