The Activation of Tertiary Carboxamides in Metal Complexes: An Experimental and Theoretical Study on the Methanolysis of Acylated Bispicolylamine Copper(II) Complexes
Nicole Niklas; Frank W. Heinemann; Frank Hampel; Tim Clark; Ralf Alsfasser; Inorganic Chemistry 43 (2004) 4663–4673; doi:10.1021/ic0496774

data_4311348
_publ_contact_author
;
        Dr. R. ALSFASSER
        Institut f\"ur Anorganische Chemie
        Universit\"at Erlangen-N\"urnberg
        Egerlandstr. 1
        D-91058 Erlangen
        Bundesrepublik Deutschland
;
_publ_contact_author_email       ALSFASSR@ANORGANIK.CHEMIE.UNI-ERLANGEN.DE
_publ_contact_author_fax         '049 9131 852-7387'
_publ_contact_author_phone       '049 9131 852-7357'
_publ_section_title
;
 The Activation of Tertiary Carboxamides in Metal Complexes: An
 Experimental and Theoretical Study on the Methanolysis of Acylated
 Bispicolylamine Copper(II) Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4663
_journal_page_last               4673
_journal_paper_doi               10.1021/ic0496774
_journal_volume                  43
_journal_year                    2004
_chemical_formula_moiety         'C19 H26 Cu N4 O4, 2(C F3 S O3), C H2 Cl2'
_chemical_formula_sum            'C22 H28 Cl2 Cu F6 N4 O10 S2'
_chemical_formula_weight         821.04
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   'difmap except solvate H atoms geom'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 104.83(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.296(1)
_cell_length_b                   15.165(3)
_cell_length_c                   18.470(3)
_cell_measurement_reflns_used    66
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      12.40
_cell_measurement_theta_min      2.80
_cell_volume                     3329.4(9)
_computing_cell_refinement       'XSCAnS 2.31 (Bruker AXS, 1999)'
_computing_data_collection       'XSCAnS 2.31 (Bruker AXS, 1999)'
_computing_data_reduction        'XSCAnS 2.31 (Bruker AXS, 1999)'
_computing_molecular_graphics    'SHELXTL 5.1 (Bruker AXS, 1998)'
_computing_publication_material  'SHELXTL 5.1 (Bruker AXS, 1998)'
_computing_structure_refinement  'SHELXTL 5.1 (Bruker AXS, 1998)'
_computing_structure_solution    'SHELXTL 5.1 (Bruker AXS, 1998)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       'profile data from \w-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  0.0452
_diffrn_reflns_av_sigmaI/netI    0.0537
_diffrn_reflns_limit_h_max       1
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            8915
_diffrn_reflns_theta_full        27.01
_diffrn_reflns_theta_max         27.01
_diffrn_reflns_theta_min         1.76
_diffrn_standards_decay_%        1.78
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.031
_exptl_absorpt_correction_T_max  0.357
_exptl_absorpt_correction_T_min  0.326
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
 North A C T, Phillips D C, Mathews F S, Acta Cryst. A24 (1968), 351-359.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.638
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1668
_exptl_crystal_size_max          0.96
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.486
_refine_diff_density_min         -0.533
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    'noref except solvate H atoms riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     434
_refine_ls_number_reflns         7260
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0844
_refine_ls_R_factor_gt           0.0519
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0670P)^2^+2.4884P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1214
_refine_ls_wR_factor_ref         0.1381
_reflns_number_gt                5082
_reflns_number_total             7260
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0496774si20040312_050529_2.cif
_cod_data_source_block           nn0102
_cod_depositor_comments
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The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'Psi-scan' changed to 'psi-scan'
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 

The following automatic conversions were performed:
data name '_publ_contact_autor' replaced with '_publ_contact_author'
as specified in the replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 4998 2017-03-02 13:24:31Z antanas 
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_cod_database_code               4311348