Extending the Pore Size of Crystalline Metal Phosphonates toward the Mesoporous Regime by Isoreticular Synthesis
Michael T. Wharmby; John P. S. Mowat; Stephen P. Thompson; Paul A. Wright; Journal of the American Chemical Society 133 (2011) 1266–1269; doi:10.1021/ja1097995

data_4105602
_publ_contact_author_address
;
School of Chemistry,
University of St Andrews,
Purdie Building,
North Haugh,
St Andrews,
KY16 9ST,
UK
;
_publ_contact_author_email       paw2@st-andrews.ac.uk
_publ_contact_author_fax         '+44 (0)1334 463808'
_publ_contact_author_name        'Prof. Paul A. Wright'
_publ_contact_author_phone       '+44 (0)1334 463791'
_publ_section_title
;
 Extending the Pore Size of Crystalline Metal Phosphonates toward the
 Mesoporous Regime by Isoreticular Synthesis
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1266
_journal_page_last               1269
_journal_paper_doi               10.1021/ja1097995
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         'C12 H26 N2 O6 P2, 4(O)'
_chemical_formula_sum            'C12 H26 N2 O10 P2'
_chemical_formula_weight         420.2923
_chemical_name_common
;
 N,N'-4,4'-bipiperidinebis(methylenephosphonic acid) 
;
_chemical_name_systematic
; 
 4,4'-bipiperidine-1,1'-diylbis(methylene)diphosphonic acid 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.0000(0)
_cell_angle_beta                 95.866(4)
_cell_angle_gamma                90.0000(0)
_cell_formula_units_Z            2
_cell_length_a                   10.240(3)
_cell_length_b                   6.0262(16)
_cell_length_c                   15.832(5)
_cell_measurement_reflns_used    2420
_cell_measurement_temperature    93.1500
_cell_measurement_theta_max      28.1667
_cell_measurement_theta_min      3.1037
_cell_volume                     971.8(5)
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      93.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 99.4000
_diffrn_measured_fraction_theta_max 28.1667
_diffrn_measurement_details
;
scan:
    Number of images: 360
               Slice: -75.0000 - 105.0000
         Image width: 0.5000
            Exp time: 40.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 0.0000
                 Phi: 0.0000
                 XTD: 49.9273
              2theta: 14.6410
scan:
    Number of images: 360
               Slice: -75.0000 - 105.0000
         Image width: 0.5000
            Exp time: 40.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 0.0000
                 XTD: 49.9273
              2theta: 14.6410
scan:
    Number of images: 360
               Slice: -75.0000 - 105.0000
         Image width: 0.5000
            Exp time: 40.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 120.0000
                 XTD: 49.9273
              2theta: 14.6410
scan:
    Number of images: 1
               Slice: -75.0000 - -74.5000
         Image width: 0.5000
            Exp time: 40.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 0.0000
                 Phi: 0.0000
                 XTD: 49.9273
              2theta: 14.6410

;
_diffrn_measurement_device
;
Saturn70 (4x4 bin mode)
;
_diffrn_measurement_device_details
;
AFC8: Eulerian 3 circle
;
_diffrn_measurement_method       dtprofit.ref
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.0175
_diffrn_orient_matrix_UB_12      0.0952
_diffrn_orient_matrix_UB_13      -0.0164
_diffrn_orient_matrix_UB_21      -0.1632
_diffrn_orient_matrix_UB_22      0.0300
_diffrn_orient_matrix_UB_23      0.0000
_diffrn_orient_matrix_UB_31      0.0031
_diffrn_orient_matrix_UB_32      0.0167
_diffrn_orient_matrix_UB_33      0.0612
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0330
_diffrn_reflns_av_sigmaI/netI    0.0581
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            1952
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        28.1667
_diffrn_reflns_theta_max         28.1667
_diffrn_reflns_theta_min         3.1037
_diffrn_source_current           16.0000
_diffrn_source_power             0.8000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    0.275
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9174
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;  Shape and scale corrections using equivalent reflections.
   Shape function based on spherical harmonics.
   Highest even and odd order for spherical harmonics:  4  and  1
   Laue group:  2/m (b)
   Friedel opposites are equivalent.
;
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.436
_exptl_crystal_description       Platelet
_exptl_crystal_F_000             444
_exptl_crystal_size_max          0.1000
_exptl_crystal_size_mid          0.0300
_exptl_crystal_size_min          0.0100
_refine_diff_density_max         0.602
_refine_diff_density_min         -0.438
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     123
_refine_ls_number_reflns         1766
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.139
_refine_ls_R_factor_all          0.0553
_refine_ls_R_factor_gt           0.0511
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0748P)^2^+1.6931P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1527
_refine_ls_wR_factor_ref         0.1560
_reflns_number_gt                1605
_reflns_number_total             1766
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja1097995_si_002.cif
_cod_data_source_block           shelxl
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4105602