Self-assembled meso-helicates of linear trinuclear nickel(II)-radical complexes with triple pyrazolate bridges.
Yamada, Susumu; Yasui, Masanori; Nogami, Takashi; Ishida, Takayuki; Dalton transactions (Cambridge, England : 2003)  (2006) 1622–1626; doi:10.1039/b513618k

data_7006752
_publ_section_title
;
 Self-assembled meso-helicates of linear trinuclear nickel(II)-radical
 complexes with triple pyrazolate bridges.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1622
_journal_page_last               1626
_journal_paper_doi               10.1039/b513618k
_journal_year                    2006
_chemical_formula_moiety         'C60 H84 N24 Ni3 O6 2(C2 H3 N1) 3(H2 O1)'
_chemical_formula_sum            'C64 H96 N26 Ni3 O9'
_chemical_formula_weight         1549.80
_space_group_IT_number           205
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  '-P 2ac 2ab 3'
_symmetry_space_group_name_H-M   'P a -3'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.827(2)
_cell_length_b                   20.827(2)
_cell_length_c                   20.827(2)
_cell_measurement_reflns_used    61025
_cell_measurement_temperature    98(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      3.09
_cell_volume                     9034.0(15)
_computing_cell_refinement       PROCESS-AUTO(1998)
_computing_data_collection       PROCESS-AUTO(1998)
_computing_data_reduction        PROCESS-AUTO(1998)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      98(2)
_diffrn_detector_area_resol_mean 0.1
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku R-AXIS Rapid'
_diffrn_measurement_method       '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  0.043
_diffrn_reflns_av_sigmaI/netI    0.0142
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       2
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            83036
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         3.24
_exptl_absorpt_coefficient_mu    0.678
_exptl_absorpt_correction_T_max  0.7909
_exptl_absorpt_correction_T_min  0.7404
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Shape (Higashi,1999)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.139
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3272
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.882
_refine_diff_density_min         -0.460
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         3457
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0810
_refine_ls_R_factor_gt           0.0742
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1892P)^2^+8.9900P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2531
_refine_ls_wR_factor_ref         0.2622
_reflns_number_gt                2957
_reflns_number_total             3457
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b513618k.txt
_cod_data_source_block           '[Ni3(pzIN)6]_x(solvent)'
_cod_original_cell_volume        9034.5(17)
_cod_original_sg_symbol_H-M      Pa-3
_cod_original_formula_sum        'C64 H96 N26 Ni3 O9 '
_cod_database_code               7006752