Cation-Dependent Nuclearity of the Copper-Azido Moiety: Synthesis, Structure, and Magnetic Study
Sandip Saha; Subratanath Koner; Jean-Pierre Tuchagues; Athanassios K. Boudalis; Ken-Ichi Okamoto; Surajit Banerjee; Dasarath Mal; Inorganic Chemistry 44 (2005) 6379–6385; doi:10.1021/ic050117u

data_4309474
_publ_section_title
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Cation-Dependent Nuclearity of the Copper-Azido Moiety: Synthesis,
Structure, and Magnetic Study
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6379
_journal_page_last               6385
_journal_paper_doi               10.1021/ic050117u
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C16 H40 Cu N14'
_chemical_formula_weight         492.16
_space_group_IT_number           87
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4'
_symmetry_space_group_name_H-M   'I 4/m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.4869(10)
_cell_length_b                   10.4869(10)
_cell_length_c                   12.084(2)
_cell_measurement_reflns_used    34
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.47
_cell_measurement_theta_min      3.39
_cell_volume                     1328.9(3)
_computing_cell_refinement       'Bruker XSCANS (Bruker, 2001)'
_computing_data_collection       'Bruker XSCANS (Bruker, 2001)'
_computing_data_reduction        'Bruker SHELXTL (Bruker, 1997)'
_computing_molecular_graphics    'ZORTEP (Zsolnai, 1995)'
_computing_publication_material
'SHELXL-97 (Sheldrick, 1997), PARST 95 (Nardelli, 1995)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\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  0.0090
_diffrn_reflns_av_sigmaI/netI    0.0135
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            1470
_diffrn_reflns_theta_max         27.70
_diffrn_reflns_theta_min         2.57
_diffrn_standards_decay_%        <3
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.852
_exptl_absorpt_correction_T_max  0.782
_exptl_absorpt_correction_T_min  0.675
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.230
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             526
_exptl_crystal_size_max          40
_exptl_crystal_size_mid          30
_exptl_crystal_size_min          20
_refine_diff_density_max         0.371
_refine_diff_density_min         -0.214
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.207
_refine_ls_goodness_of_fit_obs   1.220
_refine_ls_matrix_type           full
_refine_ls_number_parameters     41
_refine_ls_number_reflns         796
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.207
_refine_ls_restrained_S_obs      1.220
_refine_ls_R_factor_all          0.0355
_refine_ls_R_factor_obs          0.0343
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0753P)^2^+0.0896P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1102
_refine_ls_wR_factor_obs         0.1092
_reflns_number_observed          767
_reflns_number_total             796
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic050117usi20050125_040712_1.cif
_cod_data_source_block           s1a
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
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:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0753P)^2^+0.0896P] 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^)+(0.0753P)^2^+0.0896P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               4309474