Flexibility of CuCl4-tetrahedra in Bis[Cinchoninium Tetrachlorocuprate(II)]trihydrate Single Crystals. X-ray Diffraction and EPR Studies
A. Wesełucha-Birczyńska; B. J. Oleksyn; S. K. Hoffmann; J. Śliwiński; B. Borzęcka-Prokop; J. Goslar; W. Hilczer; Inorganic Chemistry 40 (2001) 4526–4533; doi:10.1021/ic001402a

data_4320159
_publ_section_title
;
 Flexibility of CuCl4-tetrahedra in Bis[Cinchoninium
 Tetrachlorocuprate(II)]trihydrate Single Crystals. X-ray Diffraction and
 EPR Studies
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4526
_journal_page_last               4533
_journal_paper_doi               10.1021/ic001402a
_journal_volume                  40
_journal_year                    2001
_chemical_formula_moiety         '[(C19H24N2O)CuCl4]2.3H2O'
_chemical_formula_sum            'C19 H27 Cl4 Cu N2 O2.5'
_chemical_formula_weight         528.76
_chemical_name_common
'bis[cinchoninium tetrachlorocuprate(II)]trihydrate'
_chemical_name_systematic
;
bis[cinchoninium tetrachlorocuprate(II)]trihydrate
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.3948(16)
_cell_length_b                   36.695(7)
_cell_length_c                   7.9806(7)
_cell_measurement_reflns_used    64
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      50.2
_cell_measurement_theta_min      4.9
_cell_volume                     4508.3(11)
_computing_cell_refinement       'local KUMA Diffraction programme'
_computing_data_collection       'local KUMA Diffraction programme'
_computing_data_reduction        'local KUMA Diffraction programme'
_computing_molecular_graphics    'ORTEP 32 (Johnson, Burnett, 1997)'
_computing_publication_material
'PLATON(Spek, 1990); PARST97 (Nardelli, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean no
_diffrn_measured_fraction_theta_full 0.000
_diffrn_measured_fraction_theta_max 0.939
_diffrn_measurement_device_type  'single crystal diffractometer KM-4'
_diffrn_measurement_method       '\w--2\q scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.0821
_diffrn_reflns_av_sigmaI/netI    0.0346
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            9808
_diffrn_reflns_theta_full        0.50
_diffrn_reflns_theta_max         80.33
_diffrn_reflns_theta_min         2.41
_diffrn_standards_decay_%        5.7
_diffrn_standards_interval_count 50
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    5.902
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellowish-green
_exptl_crystal_density_diffrn    1.558
_exptl_crystal_density_meas      1.57(1)
_exptl_crystal_density_method    'flotation in bromoform/xylene mixture'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2176
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.051
_refine_diff_density_min         -1.137
_refine_diff_density_rms         0.126
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.04(2)
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     646
_refine_ls_number_reflns         8765
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0713
_refine_ls_R_factor_gt           0.0696
_refine_ls_shift/su_max          0.080
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1185P)^2^+7.0096P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1892
_refine_ls_wR_factor_ref         0.1918
_reflns_number_gt                8486
_reflns_number_total             8765
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic001402a_2.cif
_cod_data_source_block           cucy9rti
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1185P)^2^+7.0096P] 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^)+(0.1185P)^2^+7.0096P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 

The following automatic conversions were performed:

'_atom_sites_solution_hydrogens' value 'difmap and geom' was changed
to 'mixed'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_cell_volume        4508.4(10)
_cod_database_code               4320159