Synthesis and Characterization of Prussian Blue Analogues Incorporating the Edge-Bridged Octahedral [Zr6BCl12]2+Cluster Core
Beauvais, Laurance G.; Long, Jeffrey R.; Inorganic Chemistry 45 (2006) 236–243; doi:10.1021/ic051087y

data_4331567
_publ_section_title
;
 Synthesis and Characterization of Prussian Blue Analogues Incorporating
 the Edge-Bridged Octahedral [Zr6BCl12]2+Cluster Core
;
_journal_issue                   1
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              236
_journal_page_last               243
_journal_paper_doi               10.1021/ic051087y
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety         (Et4N)5[Zr6BCl12(CN)6]1.5MeCN
_chemical_formula_sum            'C49 H104.5 B Cl12 N12.5 O0 S0 Zr6'
_chemical_formula_weight         1852.48
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           81
_symmetry_space_group_name_Hall  'P -4'
_symmetry_space_group_name_H-M   'P -4'
_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                   23.7023(11)
_cell_length_b                   23.7023(11)
_cell_length_c                   13.7979(9)
_cell_measurement_temperature    443(2)
_cell_volume                     7751.6(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      443(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.1014
_diffrn_reflns_av_sigmaI/netI    0.1149
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            22700
_diffrn_reflns_theta_full        19.77
_diffrn_reflns_theta_max         19.77
_diffrn_reflns_theta_min         1.71
_exptl_absorpt_coefficient_mu    1.230
_exptl_crystal_density_diffrn    1.587
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3740
_refine_diff_density_max         0.543
_refine_diff_density_min         -0.447
_refine_diff_density_rms         0.112
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.39(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     435
_refine_ls_number_reflns         7007
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.1074
_refine_ls_R_factor_gt           0.0556
_refine_ls_shift/su_max          2.370
_refine_ls_shift/su_mean         0.114
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0370P)^2^+25.8943P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1000
_refine_ls_wR_factor_ref         0.1184
_reflns_number_gt                4777
_reflns_number_total             7007
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic051087ysup1.cif
_cod_data_source_block           lgb19m
_cod_original_formula_sum        'C49 H104.50 B Cl12 N12.50 O0 S0 Zr6'
_cod_database_code               4331567