Change in electronic structure in a six-coordinate copper(II) complex accompanied by an anion order/disorder transition
Kilner, Colin A.; Halcrow, Malcolm A.; Acta Crystallographica Section B 66 (2010) 206–212; doi:10.1107/S0108768110003678

data_2104703
_publ_section_title
;
 Change in electronic structure in a six-coordinate copper(II) complex
 accompanied by an anion order/disorder transition
;
_journal_coeditor_code           ZB5011
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              206
_journal_page_last               212
_journal_paper_doi               10.1107/S0108768110003678
_journal_volume                  66
_journal_year                    2010
_chemical_formula_moiety         'C14 H14 Cu N6 O4, 2[Cl O4], 2[C3 H6 O]'
_chemical_formula_sum            'C20 H26 Cl2 Cu N6 O14'
_chemical_formula_weight         708.91
_chemical_name_systematic
;
Bis[2,6-bis{oximomethyl}pyridine]copper(II) diperchlorate bis-acetone
solvate
;
_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-97
_cell_angle_alpha                107.936(3)
_cell_angle_beta                 95.762(2)
_cell_angle_gamma                103.4315(15)
_cell_formula_units_Z            2
_cell_length_a                   7.0855(3)
_cell_length_b                   13.1506(5)
_cell_length_c                   17.2510(8)
_cell_measurement_reflns_used    24551
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.45
_cell_measurement_theta_min      3.01
_cell_volume                     1461.58(11)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'XSeed (Barbour, 2001)'
_computing_publication_material  'local program'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Nonius KappaCCD diffractometer'
_diffrn_measurement_method       '/w and /f scans'
_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  0.0958
_diffrn_reflns_av_sigmaI/netI    0.0729
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            24551
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         3.01
_exptl_absorpt_coefficient_mu    1.006
_exptl_absorpt_correction_T_max  0.856
_exptl_absorpt_correction_T_min  0.780
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 Using multiple and symmetry-related data measurements via the
 program SORTAV. See R.H. Blessing, Acta Cryst (1995), A51, 33-38
;
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.611
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'Rectangular prism'
_exptl_crystal_F_000             726
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.806
_refine_diff_density_min         -0.624
_refine_ls_extinction_coef       0.008(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
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_refine_ls_matrix_type           full
_refine_ls_number_parameters     413
_refine_ls_number_reflns         6483
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0822
_refine_ls_R_factor_gt           0.0568
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0967P)^2^+0.4298P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1513
_refine_ls_wR_factor_ref         0.1701
_reflns_number_gt                4699
_reflns_number_total             6483
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            zb5011.cif
_cod_data_source_block           mh68200
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        1461.57(11)
_cod_database_code               2104703
_cod_database_fobs_code          2104703