Temperature Dependence of the Crystal Structure and g-Values of trans-Diaquabis(methoxyacetato)Copper(II): Evidence for a Thermal Equilibrium Between Complexes with tetragonally Elongated and Compressed Geometries
Charles J. Simmons; Horst Stratemeier; Michael A. Hitchman; Dirk Reinen; Vanessa M. Masters; Mark J. Riley; Inorganic Chemistry 50 (2011) 4900–4916; doi:10.1021/ic200554f

data_4325315
_publ_contact_author_address
;Dr. Charles J. Simmons
Chemistry Department
University of Hawaii at Hilo
200 W. Kawili Street
Hilo, Hawaii 96720
;
_publ_contact_author_email       ' simmonsc@hawaii.edu'
_publ_contact_author_fax         808-974-7693
_publ_contact_author_name        'Dr. Charles J. Simmons'
_publ_contact_author_phone       '808-974-7317 '
_publ_section_title
;
 Temperature Dependence of the Crystal Structure and g-Values of
 trans-Diaquabis(methoxyacetato)Copper(II): Evidence for a Thermal
 Equilibrium Between Complexes with tetragonally Elongated and Compressed
 Geometries
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4900
_journal_page_last               4916
_journal_paper_doi               10.1021/ic200554f
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C6 H14 Cu O8 '
_chemical_formula_sum            'C6 H14 Cu O8'
_chemical_formula_weight         277.72
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_cell_angle_alpha                90
_cell_angle_beta                 95.8447(12)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.91320(10)
_cell_length_b                   9.9450(2)
_cell_length_c                   7.20350(10)
_cell_measurement_reflns_used    4490
_cell_measurement_temperature    180
_cell_measurement_theta_max      35.6
_cell_measurement_theta_min      2.05
_cell_volume                     492.679(14)
_computing_cell_refinement       'HKL Scalepack'
_computing_data_collection       'KappaCCD Server Software'
_computing_data_reduction        'HKL Denzo and Scalepack'
_computing_publication_material  'teXsan for Windows v. 1.06 MSC'
_computing_structure_refinement  'teXsan for Windows v. 1.06 MSC'
_computing_structure_solution
;
SIR92 (Altomare, et. al. 1994)
;
_diffrn_ambient_temperature      180
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'Nonius CCD camera'
_diffrn_measurement_method       '\f scans \w scans with \k offsets'
_diffrn_radiation_detector       'Nonius Kappa CCD'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.01290
_diffrn_reflns_av_sigmaI/netI    0.035
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4490
_diffrn_reflns_theta_full        35.60
_diffrn_reflns_theta_max         35.60
_diffrn_reflns_theta_min         2.05
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.240
_exptl_absorpt_correction_T_max  0.891
_exptl_absorpt_correction_T_min  0.757
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(DENZO-SMN; Otwinowski & Minor, 1997)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.872
_exptl_crystal_description       sphere
_exptl_crystal_F_000             286.00
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_exptl_crystal_size_rad          0.30
_refine_diff_density_max         0.43
_refine_diff_density_min         -0.33
_refine_ls_extinction_coef       0.0000064(2)
_refine_ls_extinction_expression 'equ(3) Acta Cryst.(1968) A24, p213.'
_refine_ls_extinction_method     'Zachariasen (1967)'
_refine_ls_goodness_of_fit_all   1.992
_refine_ls_goodness_of_fit_ref   1.990
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     99
_refine_ls_number_reflns         1751
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0198
_refine_ls_R_factor_gt           0.0200
_refine_ls_shift/su_max          0.0100
_refine_ls_shift/su_mean         0.0020
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo)]'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.0220
_refine_ls_wR_factor_ref         0.0220
_reflns_number_gt                1751
_reflns_number_total             2370
_reflns_threshold_expression     I>4.00\s(I)
_cod_data_source_file            ic200554f_si_002_10.cif
_cod_data_source_block           '_Template_texray.inf5'
_cod_original_cell_volume        492.679(12)
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_original_formula_sum        'C6 H14 Cu O8 '
_cod_database_code               4325315