Tetradihydrobenzoquinonate and Tetrachloranilate Zr(IV) Complexes: Single-Crystal-to-Single-Crystal Phase Transition and Open-Framework Behavior for K4Zr(DBQ)4
Inhar Imaz; Georges Mouchaham; Nans Roques; Stéphane Brandès; Inorganic Chemistry 52 (2013) 11237–11243; doi:10.1021/ic401474f

data_4336208
_publ_contact_author_address
;LCC-CNRS
205 route de Narbonne
31077 Toulouse (France)
;
_publ_contact_author_email       sutter@lcc-toulouse.fr
_publ_contact_author_name        'Jean-Pascal Sutter'
_publ_section_title
;
 Tetradihydrobenzoquinonate and Tetrachloranilate Zr(IV) Complexes:
 Single-Crystal-to-Single-Crystal Phase Transition and Open-Framework
 Behavior for K4Zr(DBQ)4
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11237
_journal_page_last               11243
_journal_paper_doi               10.1021/ic401474f
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C24 H8 K4 O16 Zr'
_chemical_formula_sum            'C24 H8 K4 O16 Zr'
_chemical_formula_weight         799.92
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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            8
_cell_length_a                   17.340(2)
_cell_length_b                   20.333(2)
_cell_length_c                   16.515(2)
_cell_measurement_temperature    373(2)
_cell_volume                     5822.8(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      373(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0363
_diffrn_reflns_av_sigmaI/netI    0.0231
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            22989
_diffrn_reflns_theta_full        21.95
_diffrn_reflns_theta_max         21.95
_diffrn_reflns_theta_min         2.35
_exptl_absorpt_coefficient_mu    1.026
_exptl_absorpt_correction_T_max  0.786
_exptl_absorpt_correction_T_min  0.407
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   scalepack
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.825
_exptl_crystal_description       cubic
_exptl_crystal_F_000             3168
_exptl_crystal_size_max          1.00
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.226
_refine_diff_density_min         -1.282
_refine_diff_density_rms         0.258
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.242
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     401
_refine_ls_number_reflns         3529
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.242
_refine_ls_R_factor_all          0.0828
_refine_ls_R_factor_gt           0.0527
_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^)+(0.1267P)^2^+5.2501P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1418
_refine_ls_wR_factor_ref         0.2016
_reflns_number_gt                2738
_reflns_number_total             3529
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401474f_si_003.cif
_cod_data_source_block           cmpd_1b
_cod_original_cell_volume        5823.1(11)
_cod_database_code               4336208