Crystal Structures and Magnetic Properties of Metal Complexes Bearing Four Nitronyl Nitroxide Moieties in the Same Coordination Sphere
Giancarlo Francese; Francisco M. Romero; Antonia Neels; Helen Stoeckli-Evans; Silvio Decurtins; Inorganic Chemistry 39 (2000) 2087–2095; doi:10.1021/ic991236a

data_4320936
_publ_section_title
;
 Crystal Structures and Magnetic Properties of Metal Complexes Bearing
 Four Nitronyl Nitroxide Moieties in the Same Coordination Sphere
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2087
_journal_page_last               2095
_journal_paper_doi               10.1021/ic991236a
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C40 H57 Cl2 Cu N11 O16'
_chemical_formula_weight         1082.41
_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                84.191(8)
_cell_angle_beta                 73.392(8)
_cell_angle_gamma                66.072(8)
_cell_formula_units_Z            2
_cell_length_a                   12.1604(9)
_cell_length_b                   12.6961(9)
_cell_length_c                   18.1028(12)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      26.05
_cell_measurement_theta_min      1.65
_cell_volume                     2447.8(4)
_computing_cell_refinement       'CELL, Stoe & Cie Company, Germany'
_computing_data_collection       'EXPOSE, Stoe & Cie Company, Germany'
_computing_data_reduction        'INTEGRATE, Stoe & Cie Company, Germany'
_computing_molecular_graphics    'PLATON97 (Spek, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.929
_diffrn_measured_fraction_theta_max 0.929
_diffrn_measurement_device_type  'IPDS, Stoe & Cie Company, Germany'
_diffrn_measurement_method       'Phi oscillation 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  0.0909
_diffrn_reflns_av_sigmaI/netI    0.2373
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            19400
_diffrn_reflns_theta_full        25.97
_diffrn_reflns_theta_max         25.97
_diffrn_reflns_theta_min         2.08
_exptl_absorpt_coefficient_mu    0.635
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.469
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1130
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.281
_refine_diff_density_min         -0.521
_refine_diff_density_rms         0.055
_refine_ls_extinction_coef       0.00246(16)
_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   0.599
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     668
_refine_ls_number_reflns         8892
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.599
_refine_ls_R_factor_all          0.1333
_refine_ls_R_factor_gt           0.0396
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0571
_refine_ls_wR_factor_ref         0.0755
_reflns_number_gt                3483
_reflns_number_total             8892
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic991236a_5.cif
_cod_data_source_block           compound5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        2447.8(3)
_cod_database_code               4320936