Hydrothermal Synthesis and Characterization of 2D M(II)-Quinate (M = Co,Zn) Metal-Organic Lattice Assemblies: Solid-State Solution Structure Correlation in M(II)-Hydroxycarboxylate Systems
M. Menelaou; A. Konstantopai; N. Lalioti; C. P. Raptopoulou; V. Psycharis; A. Terzis; C. Mateescu; K. Tsarhopoulos; P. Rigas; A. Salifoglou; Inorganic Chemistry 49 (2010) 11449–11462; doi:10.1021/ic1013945

data_4317296
_publ_section_title
;
 Hydrothermal Synthesis and Characterization of 2D M(II)-Quinate (M =
 Co,Zn) Metal-Organic Lattice Assemblies: Solid-State Solution Structure
 Correlation in M(II)-Hydroxycarboxylate Systems
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11449
_journal_page_last               11462
_journal_paper_doi               10.1021/ic1013945
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C42 H68 O37 Zn3'
_chemical_formula_weight         1361.07
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 93.0360(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   5.70950(10)
_cell_length_b                   32.3254(6)
_cell_length_c                   13.2471(2)
_cell_measurement_temperature    293(2)
_cell_volume                     2441.48(7)
_computing_cell_refinement       'CrystalClear, Rigaku MSC, 2005'
_computing_data_collection       'CrystalClear, Rigaku MSC, 2005'
_computing_data_reduction        'CrystalClear, Rigaku MSC, 2005'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDER IPDS'
_diffrn_measurement_method       '\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.1610
_diffrn_reflns_av_sigmaI/netI    0.1254
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            32836
_diffrn_reflns_theta_full        65.00
_diffrn_reflns_theta_max         65.00
_diffrn_reflns_theta_min         6.69
_exptl_absorpt_coefficient_mu    2.780
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.566
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'CrystalClear, Rigaku MSC, 2005'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.851
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parall
_exptl_crystal_F_000             1412
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.372
_refine_diff_density_min         -0.918
_refine_diff_density_rms         0.144
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     750
_refine_ls_number_reflns         7911
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0679
_refine_ls_R_factor_gt           0.0655
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0725P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1554
_refine_ls_wR_factor_ref         0.1577
_reflns_number_gt                7286
_reflns_number_total             7911
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1013945_si_003.cif
_cod_data_source_block           salzn153
_cod_database_code               4317296