A combined experimental and theoretical charge density study of the chemical bonding and magnetism in 3-amino-propanolato Cu(II) complexes containing weakly coordinated anions.
Farrugia, Louis J.; Middlemiss, Derek S.; Sillanpää, Reijo; Seppälä, Petri; The journal of physical chemistry. A 112 (2008) 9050–9067; doi:10.1021/jp804865j

data_1504409
_publ_section_title
;
 A combined experimental and theoretical charge density study of the
 chemical bonding and magnetism in 3-amino-propanolato Cu(II) complexes
 containing weakly coordinated anions.
;
_journal_issue                   38
_journal_name_full               'The journal of physical chemistry. A'
_journal_page_first              9050
_journal_page_last               9067
_journal_paper_doi               10.1021/jp804865j
_journal_volume                  112
_journal_year                    2008
_chemical_compound_source        'synthesis as described'
_chemical_formula_sum            'C6 H16 Cu2 N4 O8'
_chemical_formula_weight         399.31
_space_group_IT_number           14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             '31-May-05 T16:40:11-00:00'
_audit_creation_method           'XD routine XDCIF'
_cell_angle_alpha                90
_cell_angle_beta                 104.8180(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.8024(3)
_cell_length_b                   8.0562(2)
_cell_length_c                   9.2531(3)
_cell_measurement_reflns_used    9589
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      57.9177
_cell_measurement_theta_min      2.3934
_cell_measurement_wavelength     0.71073
_cell_volume                     634.35(3)
_computing_cell_refinement       'SAINT V7.34A integration software'
_computing_data_collection       'Bruker APEX software'
_computing_data_reduction        'SORTAV (Blessing, 1995)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'APEX-II CCD'
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker-Nonius APEX-II'
_diffrn_measurement_method       '\f or \w oscillation scans'
_diffrn_orient_matrix_type       'x-axis to radiation source'
_diffrn_orient_matrix_UB_11      -0.840419E-1
_diffrn_orient_matrix_UB_12      -0.162843E-1
_diffrn_orient_matrix_UB_13      -0.946408E-1
_diffrn_orient_matrix_UB_21      0.786857E-1
_diffrn_orient_matrix_UB_22      -0.509325E-1
_diffrn_orient_matrix_UB_23      -0.477643E-1
_diffrn_orient_matrix_UB_31      -0.235593E-1
_diffrn_orient_matrix_UB_32      -0.112019
_diffrn_orient_matrix_UB_33      0.354753E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            112898
_diffrn_reflns_reduction_process
;
 Scaled and merged with Sortav
 R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;
_diffrn_reflns_theta_full        60.04
_diffrn_reflns_theta_max         60.04
_diffrn_reflns_theta_min         2.39
_diffrn_source                   'sealed x-ray tube'
_exptl_absorpt_coefficient_mu    3.398
_exptl_absorpt_correction_T_max  0.607
_exptl_absorpt_correction_T_min  0.433
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
   P. Coppens, L. Leiserowitz, D Rabinovich, Acta Cryst.
   (1965), 18, 1035-1038
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.091
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             404
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.687
_refine_diff_density_min         -0.34
_refine_diff_density_rms         0.068
_refine_ls_extinction_coef       0.008(4)
_refine_ls_extinction_expression
;
        Becker, P.J. & Coppens, P. (1974) Acta Cryst., A30, 129-153.
;
_refine_ls_extinction_method     'Becker-Coppens type 1 Lorentzian isotropic'
_refine_ls_goodness_of_fit_ref   0.977
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         7905
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.032
_refine_ls_R_factor_gt           0.017
_refine_ls_shift/su_max          0
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
        calc w1 = 1/[s^2^(Fo)]
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.018
_reflns_number_gt                7908
_reflns_number_total             9485
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            jp804865j_si_004.cif
_cod_data_source_block           nitrate
_cod_database_code               1504409