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_1512820
_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 Cu N2 O8, C H4 O, 2(C H2 Cl2)'
_chemical_formula_sum            'C27 H28 Cl4 Cu N2 O9'
_chemical_formula_weight         729.8
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 105.488(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.532(2)
_cell_length_b                   15.229(3)
_cell_length_c                   15.657(3)
_cell_measurement_reflns_used    7407
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.214
_cell_measurement_theta_min      2.6749
_cell_measurement_wavelength     0.71073
_cell_volume                     3109.4(10)
_computing_cell_refinement       'SAINT V7.66A integration software'
_computing_data_collection       'Bruker APEX2 software'
_computing_data_reduction        'SORTAV (Blessing, 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    'SIR2004 (Giacovazzo et al, 2004)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'APEX-II CCD'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       '\f or \w oscillation scans'
_diffrn_orient_matrix_type       'x-axis to radiation source'
_diffrn_orient_matrix_UB_11      -0.25627E-1
_diffrn_orient_matrix_UB_12      0.618443E-1
_diffrn_orient_matrix_UB_13      -0.81892E-2
_diffrn_orient_matrix_UB_21      0.722561E-1
_diffrn_orient_matrix_UB_22      0.21861E-1
_diffrn_orient_matrix_UB_23      0.143173E-1
_diffrn_orient_matrix_UB_31      -0.175718E-2
_diffrn_orient_matrix_UB_32      -0.301392E-2
_diffrn_orient_matrix_UB_33      -0.641906E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0386
_diffrn_reflns_av_unetI/netI     0.0454
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            28820
_diffrn_reflns_theta_full        28
_diffrn_reflns_theta_max         30.42
_diffrn_reflns_theta_min         1.9
_diffrn_source                   'sealed x-ray tube'
_exptl_absorpt_coefficient_mu    1.1
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.642
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.559
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1492
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.66
_refine_diff_density_min         -0.684
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     409
_refine_ls_number_reflns         9091
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0606
_refine_ls_R_factor_gt           0.0408
_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^)+(0.0404P)^2^+2.0384P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0932
_refine_ls_wR_factor_ref         0.1022
_reflns_number_gt                7020
_reflns_number_total             9091
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ICA-2013-394-729-740-2.cif
_cod_data_source_block           11mz006_0m
_cod_depositor_comments
;

2019-06-04
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C54 H56 Cl8 Cu2 N4 O18'
_cod_original_formula_weight         1459.7
_cod_original_formula_moiety       'C48 H40 Cu2 N4 O16, 2(C H4 O), 4(C H2 Cl2)'
_cod_original_formula_units_Z            2
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1512820