Copper(II) Azide Complexes of Aliphatic and Aromatic Amine Based Tridentate Ligands: Novel Structure, Spectroscopy, and Magnetic Properties
P. Manikandan; R. Muthukumaran; K. R. Justin Thomas; B. Varghese; G. V. R. Chandramouli; P. T. Manoharan; Inorganic Chemistry 40 (2001) 2378–2389; doi:10.1021/ic0009223

data_4319591
_publ_section_title
;
 Copper(II) Azide Complexes of Aliphatic and Aromatic Amine Based
 Tridentate Ligands: Novel Structure, Spectroscopy, and Magnetic
 Properties
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2378
_journal_page_last               2389
_journal_paper_doi               10.1021/ic0009223
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C12 H34 Cl2 Cu2 N12 O8'
_chemical_formula_weight         672.49
_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
_cell_angle_alpha                77.136(9)
_cell_angle_beta                 87.503(10)
_cell_angle_gamma                80.344(8)
_cell_formula_units_Z            2
_cell_length_a                   9.442(2)
_cell_length_b                   11.472(3)
_cell_length_c                   12.722(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      14
_cell_measurement_theta_min      10
_cell_volume                     1324.4(5)
_computing_cell_refinement       'CAD4 PROGRAMS'
_computing_data_collection       'CAD4 PROGRAMS'
_computing_data_reduction        MolEn
_computing_molecular_graphics    ORTEP
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measurement_device       'CAD4 Diffractometer'
_diffrn_measurement_method       'Omega twotheta'
_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  0.0388
_diffrn_reflns_av_sigmaI/netI    0.0301
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4965
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.19
_diffrn_standards_decay_%        2
_diffrn_standards_interval_time  '1 Hour'
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.868
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.87
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            'Dark Green'
_exptl_crystal_density_diffrn    1.687
_exptl_crystal_description       Needle
_exptl_crystal_F_000             692
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.760
_refine_diff_density_min         -0.612
_refine_diff_density_rms         0.109
_refine_ls_extinction_coef       0.0000(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.133
_refine_ls_goodness_of_fit_obs   1.094
_refine_ls_hydrogen_treatment    'Riding model refinement'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         4642
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.612
_refine_ls_restrained_S_obs      1.094
_refine_ls_R_factor_all          0.0710
_refine_ls_R_factor_obs          0.0469
_refine_ls_shift/esd_max         -1.151
_refine_ls_shift/esd_mean        0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0644P)^2^+2.7200P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2047
_refine_ls_wR_factor_obs         0.1205
_reflns_number_observed          3515
_reflns_number_total             4656
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic0009223_4.cif
_cod_data_source_block           '[Cu(dpt)(N3)]2(ClO4)2'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'psi scan'
changed to 'psi-scan' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0644P)^2^+2.7200P] 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^)+(0.0644P)^2^+2.7200P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1324.3(5)
_cod_database_code               4319591