Polymorphs or solvates? Coordination of 3,5-dihydroxybenzoate to copper and zinc metal centers
Linsheng Feng; Zhichao Chen; Matthias Zeller; Rudy L. Luck; Inorganica Chimica Acta 394 (2013) 729–740; doi:10.1016/j.ica.2012.09.036

data_1512822
_publ_section_title
;
 Polymorphs or solvates? Coordination of 3,5-dihydroxybenzoate to copper
 and zinc metal centers
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              729
_journal_page_last               740
_journal_paper_doi               10.1016/j.ica.2012.09.036
_journal_volume                  394
_journal_year                    2013
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety
'C24 H20 N2 O8 Zn, 0.75(C H4 O), 1.25(C H2 Cl2)'
_chemical_formula_sum            'C26 H25.5 Cl2.5 N2 O8.75 Zn'
_chemical_formula_weight         660.00
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                110.64(3)
_cell_angle_beta                 98.48(2)
_cell_angle_gamma                110.50(3)
_cell_formula_units_Z            2
_cell_length_a                   11.236(4)
_cell_length_b                   11.941(5)
_cell_length_c                   12.956(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      10
_cell_measurement_wavelength     0.71073
_cell_volume                     1449.1(11)
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Giacovazzo et al, 1997)'
_diffrn_ambient_temperature      294(2)
_diffrn_detector                 'scintillation LiI'
_diffrn_detector_dtime           1.195
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf Nonius TurboCAD4'
_diffrn_measurement_method       'non-profiled \w/2\t scans'
_diffrn_orient_matrix_type
;
  x-axis points to radiation source
  the matrix is specified in reciprocal space
;
_diffrn_orient_matrix_UB_11      -0.044587
_diffrn_orient_matrix_UB_12      -0.099359
_diffrn_orient_matrix_UB_13      -0.035173
_diffrn_orient_matrix_UB_21      -0.022423
_diffrn_orient_matrix_UB_22      -0.003318
_diffrn_orient_matrix_UB_23      -0.078698
_diffrn_orient_matrix_UB_31      0.0866
_diffrn_orient_matrix_UB_32      -0.002075
_diffrn_orient_matrix_UB_33      -0.007622
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.105
_diffrn_reflns_av_unetI/netI     0.0519
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3993
_diffrn_reflns_theta_full        22.49
_diffrn_reflns_theta_max         22.49
_diffrn_reflns_theta_min         1.77
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_decay_%        3
_diffrn_standards_interval_time  166
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.13
_exptl_absorpt_correction_T_max  0.9998
_exptl_absorpt_correction_T_min  0.9397
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351
        Number of psi-scan sets used was   9
        Theta correction was applied.
        Averaged transmission function was used.
        No Fourier smoothing was applied.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             677.6
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.423
_refine_diff_density_min         -0.682
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     392
_refine_ls_number_reflns         3763
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0921
_refine_ls_R_factor_gt           0.0575
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0840P)^2^+3.1702P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1457
_refine_ls_wR_factor_ref         0.1666
_reflns_number_gt                2872
_reflns_number_total             3763
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ICA-2013-394-729-740-4.cif
_cod_data_source_block           lfzng1
_cod_original_cell_volume        1449.1(9)
_cod_original_formula_sum        'C26 H25.50 Cl2.50 N2 O8.75 Zn'
_cod_database_code               1512822