1,4-Phenylenebis(methylidyne)tetrakis(phosphonic acid): A New Building Block in Metal Organic Framework Synthesis
Monika Plabst; Thomas Bein; Inorganic Chemistry 48 (2009) 4331–4341; doi:10.1021/ic802294e

data_4302114
_publ_contact_author             'Bein, Thomas'
_publ_contact_author_email       tbein@cup.uni-muenchen.de
_publ_section_title
;
1,4-Phenylenebis(methylidyne)tetrakis(phosphonic acid): A New Building
Block in Metal Organic Framework Synthesis
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4331
_journal_page_last               4341
_journal_paper_doi               10.1021/ic802294e
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         LaNa[(PO3H)2CH-C6H4-CH(PO3H)2].4H2O
_chemical_formula_sum            'C8 H18 La Na O16 P4'
_chemical_formula_weight         656.01
_chemical_name_common            NaLa(H4L)
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2008-10-03T23:29:30-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 105.56
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.975
_cell_length_b                   21.691
_cell_length_c                   10.186
_cell_measurement_reflns_used    24954
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      3.134
_cell_volume                     1910.301
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_orient_matrix_type       'by Bruker AXS Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      -0.0723465
_diffrn_orient_matrix_UB_12      -0.0335251
_diffrn_orient_matrix_UB_13      0.010661
_diffrn_orient_matrix_UB_21      0.074283
_diffrn_orient_matrix_UB_22      -0.0316113
_diffrn_orient_matrix_UB_23      -0.0160783
_diffrn_orient_matrix_UB_31      0.0512441
_diffrn_orient_matrix_UB_32      -0.0015074
_diffrn_orient_matrix_UB_33      0.1000661
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0173
_diffrn_reflns_av_unetI/netI     0.027
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8563
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.28
_exptl_absorpt_coefficient_mu    2.675
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.267
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       square-bipyramidal
_exptl_crystal_F_000             1272
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.925
_refine_diff_density_min         -0.699
_refine_diff_density_rms         0.098
_refine_ls_extinction_coef       0.00090(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.08
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     340
_refine_ls_number_reflns         4370
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.08
_refine_ls_R_factor_all          0.026
_refine_ls_R_factor_gt           0.0202
_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^)+(0.0143P)^2^+2.3337P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.044
_refine_ls_wR_factor_ref         0.0463
_reflns_number_gt                3877
_reflns_number_total             4370
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic802294e_si_003.cif
_cod_data_source_block           ln245
_cod_original_cell_volume        1910.2
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4302114