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_7203411
_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            'C30.5 H32.5 Cl1.5 F12 N8 Ni O8'
_chemical_formula_weight         979.03
_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                95.901(8)
_cell_angle_beta                 110.85(1)
_cell_angle_gamma                103.85(1)
_cell_formula_units_Z            2
_cell_length_a                   13.111(3)
_cell_length_b                   13.153(4)
_cell_length_c                   13.664(4)
_cell_measurement_reflns_used    4413
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      19.0
_cell_measurement_theta_min      1.0
_cell_volume                     2091.6(10)
_computing_data_collection       COLLECT
_computing_data_reduction        'DENZO and SCALEPACK'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'phi-and omega scan'
_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  0.1717
_diffrn_reflns_av_sigmaI/netI    0.2349
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5862
_diffrn_reflns_theta_full        19.00
_diffrn_reflns_theta_max         19.00
_diffrn_reflns_theta_min         1.63
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.669
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             994
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.015
_refine_diff_density_max         0.356
_refine_diff_density_min         -0.421
_refine_diff_density_rms         0.072
_refine_ls_extinction_coef       0.0031(10)
_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   0.976
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     545
_refine_ls_number_reflns         3347
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.976
_refine_ls_R_factor_all          0.2209
_refine_ls_R_factor_gt           0.0922
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0762P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1718
_refine_ls_wR_factor_ref         0.2124
_reflns_number_gt                1500
_reflns_number_total             3347
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b604598g.txt
_cod_data_source_block           ni
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C30.50 H32.50 Cl1.50 F12 N8 Ni O8'
_cod_database_code               7203411