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_4302115
_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         La[(PO3H)2CH-C6H4-CH(PO3H)(PO3H2)].4H2O
_chemical_formula_sum            'C8 H19 Nd O16 P4'
_chemical_formula_weight         639.35
_chemical_name_common            'Nd(H5L) a'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2008-10-03T23:14:42-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                73.03
_cell_angle_beta                 85.47
_cell_angle_gamma                76.74
_cell_formula_units_Z            2
_cell_length_a                   5.673
_cell_length_b                   12.193
_cell_length_c                   14.474
_cell_measurement_reflns_used    22191
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      3.134
_cell_volume                     931.978
_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      200(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD; rotation images; thick slices'
_diffrn_orient_matrix_type       'by Bruker AXS Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      -0.0420788
_diffrn_orient_matrix_UB_12      0.0687149
_diffrn_orient_matrix_UB_13      -0.0583951
_diffrn_orient_matrix_UB_21      0.1749807
_diffrn_orient_matrix_UB_22      -0.0094321
_diffrn_orient_matrix_UB_23      -0.01943
_diffrn_orient_matrix_UB_31      -0.0204269
_diffrn_orient_matrix_UB_32      -0.0538812
_diffrn_orient_matrix_UB_33      -0.0378382
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0306
_diffrn_reflns_av_unetI/netI     0.0519
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8022
_diffrn_reflns_theta_full        27.5
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         3.46
_exptl_absorpt_coefficient_mu    3.211
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.279
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             630
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.087
_refine_diff_density_min         -0.878
_refine_diff_density_rms         0.132
_refine_ls_extinction_coef       0.0028(3)
_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   1.075
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         4256
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0278
_refine_ls_shift/su_max          5.41
_refine_ls_shift/su_mean         0.02
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0185P)^2^+0.0975P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0519
_refine_ls_wR_factor_ref         0.0545
_reflns_number_gt                3668
_reflns_number_total             4256
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic802294e_si_004.cif
_cod_data_source_block           ln472
_cod_original_cell_volume        931.9
_cod_database_code               4302115