Polymorphs of a pyrazole nitronyl nitroxide and its complexes with metal(ii) hexafluoroacetylacetonates
Catala, Laure; Wurst, Klaus; Amabilino, David B.; Veciana, Jaume; Journal of Materials Chemistry 16 (2006) 2736–; doi:10.1039/b604598g

data_7203410
_publ_section_title
;
 Polymorphs of a pyrazole nitronyl nitroxide and its complexes with
 metal(ii) hexafluoroacetylacetonates
;
_journal_issue                   26
_journal_name_full               'Journal of Materials Chemistry'
_journal_page_first              2736
_journal_paper_doi               10.1039/b604598g
_journal_volume                  16
_journal_year                    2006
_chemical_formula_sum            'C40 H34 Co2 F24 N8 O12'
_chemical_formula_weight         1392.61
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 118.260(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   32.361(1)
_cell_length_b                   8.8752(4)
_cell_length_c                   21.1416(5)
_cell_measurement_reflns_used    13350
_cell_measurement_temperature    218(2)
_cell_measurement_theta_max      23.0
_cell_measurement_theta_min      1.0
_cell_volume                     5348.3(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      218(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'phi- and omega-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  0.0332
_diffrn_reflns_av_sigmaI/netI    0.0340
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            11193
_diffrn_reflns_theta_full        22.94
_diffrn_reflns_theta_max         22.94
_diffrn_reflns_theta_min         1.97
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.769
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.729
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2784
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.437
_refine_diff_density_min         -0.346
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    'constr, refined at N4'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     450
_refine_ls_number_reflns         3665
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0368
_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^)+(0.0433P)^2^+8.5373P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0874
_refine_ls_wR_factor_ref         0.0928
_reflns_number_gt                3020
_reflns_number_total             3665
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b604598g.txt
_cod_data_source_block           co
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7203410