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_4336209
_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         'K4 Zr C24 Cl8 O16, 7(H2O)'
_chemical_formula_sum            'C24 H4 Cl8 K4 O23 Zr'
_chemical_formula_weight         1191.49
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_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                 124.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.884
_cell_length_b                   15.726
_cell_length_c                   14.071
_cell_measurement_reflns_used    8346
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      0.997
_cell_volume                     1996.669
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'KappaCCD Server Software (Nonius, 1997)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997) and Mercury (CCDC)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'Shelxs-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_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  0.0392
_diffrn_reflns_av_sigmaI/netI    0.0392
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4050
_diffrn_reflns_theta_full        26.31
_diffrn_reflns_theta_max         26.31
_diffrn_reflns_theta_min         2.17
_exptl_absorpt_coefficient_mu    1.314
_exptl_absorpt_correction_T_max  0.988
_exptl_absorpt_correction_T_min  0.910
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   scalepack
_exptl_crystal_colour            Violet
_exptl_crystal_density_diffrn    1.982
_exptl_crystal_description       Needle
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.637
_refine_diff_density_min         -1.654
_refine_diff_density_rms         0.128
_refine_ls_extinction_coef       0.0072(9)
_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   1.093
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         4050
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0638
_refine_ls_R_factor_gt           0.0455
_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^)+(0.0738P)^2^+5.8683P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1346
_refine_ls_wR_factor_ref         0.1452
_reflns_number_gt                3315
_reflns_number_total             4050
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic401474f_si_004.cif
_cod_data_source_block           compd_2
_cod_original_cell_volume        1996.5
_cod_original_sg_symbol_H-M      'P 2/c'
_cod_database_code               4336209