Hydrothermal synthesis of zinc(II)-phosphonate coordination polymers with different dimensionality (0D, 2D, 3D) and dimensionality change in the solid phase (0D→3D) induced by temperature
Fernández-Zapico, Eva; Montejo-Bernardo, Jose; Fernández-González, Alfonso; García, José R.; García-Granda, Santiago; Journal of Solid State Chemistry 225 (2015) 285–296; doi:10.1016/j.jssc.2015.01.001

data_1562036
_publ_section_title
;
 Hydrothermal synthesis of zinc(II)-phosphonate coordination polymers with
 different dimensionality (0D, 2D, 3D) and dimensionality change in the
 solid phase (0D\\rightarrow 3D) induced by temperature
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              285
_journal_page_last               296
_journal_paper_doi               10.1016/j.jssc.2015.01.001
_journal_volume                  225
_journal_year                    2015
_chemical_formula_moiety         'C18 H16 N2 O10 P2 Zn3, 2.4(H2 O), O'
_chemical_formula_sum            'C18 H20.8 N2 O13.4 P2 Zn3'
_chemical_formula_weight         737.68
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                73.081(5)
_cell_angle_beta                 77.360(5)
_cell_angle_gamma                71.278(5)
_cell_formula_units_Z            2
_cell_length_a                   8.2580(5)
_cell_length_b                   10.3480(6)
_cell_length_c                   16.5720(9)
_cell_measurement_reflns_used    2891
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      31.0338
_cell_measurement_theta_min      3.2470
_cell_volume                     1270.81(14)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2009)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2009)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2009)'
_computing_molecular_graphics
;
ORTEP-3 (L.J. Farrugia, 1997) and Mercury CSD 2.0 (Macrae et al., 2008)
;
_computing_publication_material
;  
WinGX publication routines (Farrugia, 1999),
PARST (Nardelli, M., 1995) and PLATON (Spek, A. L., 2003)
;
_computing_structure_refinement  'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_solution    'SIR 2004 (Burla <i>et al.</i>, 2005)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 10.2673
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.883
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini'
_diffrn_measurement_method       '\w scans'
_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  0.0568
_diffrn_reflns_av_sigmaI/netI    0.1215
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            12756
_diffrn_reflns_theta_full        29.00
_diffrn_reflns_theta_max         31.10
_diffrn_reflns_theta_min         3.25
_exptl_absorpt_coefficient_mu    3.005
_exptl_absorpt_correction_T_max  0.943
_exptl_absorpt_correction_T_min  0.798
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.928
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             740.0
_exptl_crystal_size_max          0.1746
_exptl_crystal_size_mid          0.0627
_exptl_crystal_size_min          0.0197
_refine_diff_density_max         0.756
_refine_diff_density_min         -0.689
_refine_diff_density_rms         0.168
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     422
_refine_ls_number_reflns         7191
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.1072
_refine_ls_R_factor_gt           0.0633
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0128P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0803
_refine_ls_wR_factor_ref         0.0923
_reflns_number_gt                4927
_reflns_number_total             8138
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            JSSC-2015-225-285.cif
_cod_data_source_block           ZnPF2_LT
_cod_original_formula_sum        'C18 H20.80 N2 O13.40 P2 Zn3'
_cod_database_code               1562036