Controllable preparation and structures of two zinc phosphonocarboxylate frameworks with MER and RHO zeolitic topologies
Deng, Mingli; Liu, Xiaofeng; Zheng, Qingshu; Chen, Zhenxia; Fang, Changye; Yue, Bin; He, Heyong; CrystEngComm 15 (2013) 7056–; doi:10.1039/c3ce40673c

data_7210297
_publ_section_title
;
 Controllable preparation and structures of two zinc phosphonocarboxylate
 frameworks with MER and RHO zeolitic topologies
;
_journal_issue                   35
_journal_name_full               CrystEngComm
_journal_page_first              7056
_journal_paper_doi               10.1039/c3ce40673c
_journal_volume                  15
_journal_year                    2013
_chemical_formula_moiety         'C14 H10 O11 P2 Zn2.50'
_chemical_formula_sum            'C14 H10 O11 P2 Zn2.5'
_chemical_formula_weight         579.59
_chemical_name_systematic
;
?
;
_space_group_IT_number           222
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  '-P 4a 2bc 3'
_symmetry_space_group_name_H-M   'P n -3 n :2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            48
_cell_length_a                   32.652(5)
_cell_length_b                   32.652(5)
_cell_length_c                   32.652(5)
_cell_measurement_reflns_used    966
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.381
_cell_measurement_theta_min      2.334
_cell_volume                     34812(9)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.1027
_diffrn_reflns_av_sigmaI/netI    0.0449
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            122161
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         0.88
_exptl_absorpt_coefficient_mu    2.205
_exptl_absorpt_correction_T_max  0.8096
_exptl_absorpt_correction_T_min  0.7332
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.327
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cubic
_exptl_crystal_F_000             13776
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
The disordered solvents within the void were not crystallographically
well defined.

The SQUEEZE routine of the program PLATON was used
in order to eliminate the contribution of disordered solvents molecules,
thereby a final model based only on the ordered part of the crystal structure
was obtained.

The SQUEEZE routine suggested that
a total potential solvent area volume of 15497.6 Ang^3^,
and a void electron population of 3014 per cell.
The solvent we used in the synthesis is DMF and water. And there might be some dimethylamine
decomposed by DMF. So the amount of the disordered solvent was about 62 per cell suggested by electron count.
The overall formula should be Zn2.5(3-pbc)2(H2O).(H2N(CH3)2).2(H2O), considering the contribution of solvent.

Refinement after the SQUEEZE routine gave significantly improved R values.
[R values before SQUEEZE]
R1 = 0.1336, wR2 = 0.3245, GooF = S = 1.167 for all data
;
_refine_diff_density_max         1.242
_refine_diff_density_min         -0.783
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         5138
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0896
_refine_ls_R_factor_gt           0.0559
_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^)+(0.0781P)^2^+51.8819P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1345
_refine_ls_wR_factor_ref         0.1473
_reflns_number_gt                3780
_reflns_number_total             5138
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce40673c.txt
_cod_data_source_block           f70117as
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Cubic' changed to 'cubic' according
to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary
named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        34811(9)
_cod_original_sg_symbol_H-M      Pn-3n
_cod_original_formula_sum        'C14 H10 O11 P2 Zn2.50'
_cod_database_code               7210297