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_1512819
_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         'C48 H40 Cu2 N4 O16, 2(C4 H8 O2), 2(C H2 Cl2)'
_chemical_formula_sum            'C58 H60 Cl4 Cu2 N4 O20'
_chemical_formula_weight         1401.98
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 98.39(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.893(7)
_cell_length_b                   15.673(6)
_cell_length_c                   17.237(6)
_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                     6386(4)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf Nonius TurboCAD4'
_diffrn_measurement_method       'non-profiled \w scans'
_diffrn_orient_matrix_type
;
  x-axis points to radiation source
  the matrix is specified in reciprocal space
;
_diffrn_orient_matrix_UB_11      -0.024281
_diffrn_orient_matrix_UB_12      -0.044273
_diffrn_orient_matrix_UB_13      -0.030072
_diffrn_orient_matrix_UB_21      0.025938
_diffrn_orient_matrix_UB_22      -0.000809
_diffrn_orient_matrix_UB_23      -0.040576
_diffrn_orient_matrix_UB_31      0.022967
_diffrn_orient_matrix_UB_32      -0.045936
_diffrn_orient_matrix_UB_33      0.0298
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0213
_diffrn_reflns_av_unetI/netI     0.0473
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            5759
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         1.56
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_decay_%        2
_diffrn_standards_interval_time  166
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.909
_exptl_absorpt_correction_T_max  0.9982
_exptl_absorpt_correction_T_min  0.9522
_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            blue
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2888
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.326
_refine_diff_density_min         -0.319
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.06
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     434
_refine_ls_number_reflns         5613
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.06
_refine_ls_R_factor_all          0.0846
_refine_ls_R_factor_gt           0.042
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0319P)^2^+12.2234P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0877
_refine_ls_wR_factor_ref         0.1024
_reflns_number_gt                3930
_reflns_number_total             5613
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ICA-2013-394-729-740-1.cif
_cod_data_source_block           lfg1py
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               1512819