Structure of Two Azide Salts of a Copper(II) Macrocycle and Magnetic Properties of Cu(14ane)Cu(N3)4
Brooke Woodard; Roger D. Willett; Salim Haddad; Brendan Twamley; Carlos J. Gomez-Garcia; Eugenio Coronado; Inorganic Chemistry 43 (2004) 1822–1824; doi:10.1021/ic030272d

data_4310693
_publ_section_title
;
 Structure of Two Azide Salts of a Copper(II) Macrocycle and Magnetic
 Properties of Cu(14ane)Cu(N3)4
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1822
_journal_page_last               1824
_journal_paper_doi               10.1021/ic030272d
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C10 H24 B0 Cu2 F0 N16'
_chemical_formula_weight         495.53
_chemical_name_common            'copper(14ane) tetraazidocopper(II)'
_chemical_name_systematic
; 
 ? 
;
_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-97
_cell_angle_alpha                95.746(6)
_cell_angle_beta                 102.678(5)
_cell_angle_gamma                97.648(5)
_cell_formula_units_Z            1
_cell_length_a                   7.674(3)
_cell_length_b                   7.703(3)
_cell_length_c                   8.476(3)
_cell_measurement_temperature    293(2)
_cell_volume                     480.1(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD detector'
_diffrn_measurement_method       'phi and omega'
_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  0.0318
_diffrn_reflns_av_sigmaI/netI    0.0413
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            4192
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.49
_diffrn_standards_interval_count '50 frames, beginning and end'
_exptl_absorpt_coefficient_mu    2.250
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.714
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             254
_refine_diff_density_max         0.330
_refine_diff_density_min         -0.236
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       0.0000(15)
_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_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         1679
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0507
_refine_ls_R_factor_gt           0.0277
_refine_ls_shift/su_max          0.751
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0250P)^2^+0.0665P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0550
_refine_ls_wR_factor_ref         0.0602
_reflns_number_gt                1213
_reflns_number_total             1679
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic030272d_si1__1.cif
_cod_data_source_block           bt148a
_cod_database_code               4310693