Superexpanded Prussian-Blue Analogue with [Fe(CN)6]4-, [Nb6Cl12(CN)6]4-, and [Mn(salen)]+ as Building Units
Jianjun Zhang; Abdessadek Lachgar; Journal of the American Chemical Society 129 (2007) 250–251; doi:10.1021/ja066104c

data_4108966
_publ_section_title
;
 Superexpanded Prussian-Blue Analogue with [Fe(CN)6]4-, [Nb6Cl12(CN)6]4-,
 and [Mn(salen)]+ as Building Units
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              250
_journal_page_last               251
_journal_paper_doi               10.1021/ja066104c
_journal_volume                  129
_journal_year                    2007
_chemical_formula_sum            'C108 H95 Cl12 Fe Mn6 N24 Nb6 O17'
_chemical_formula_weight         3369.43
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           148
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                120.00
_cell_formula_units_Z            3
_cell_length_a                   16.3466(18)
_cell_length_b                   16.3466(18)
_cell_length_c                   42.227(9)
_cell_measurement_reflns_used    4258
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      23.288
_cell_measurement_theta_min      3.822
_cell_volume                     9772(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_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  0.0597
_diffrn_reflns_av_sigmaI/netI    0.0430
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       54
_diffrn_reflns_limit_l_min       -54
_diffrn_reflns_number            29017
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.82
_exptl_absorpt_coefficient_mu    1.487
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.715811
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.718
_exptl_crystal_density_meas      0
_exptl_crystal_description       block
_exptl_crystal_F_000             5019
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.910
_refine_diff_density_min         -0.972
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     269
_refine_ls_number_reflns         4988
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0672
_refine_ls_R_factor_gt           0.0528
_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^)+(0.0578P)^2^+53.5969P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1225
_refine_ls_wR_factor_ref         0.1282
_reflns_number_gt                4103
_reflns_number_total             4988
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja066104csi20060831_094121.cif
_cod_data_source_block           q1
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4108966