Dihydrogen Phosphate Clusters: Trapping H2PO4–Tetramers and Hexamers in Urea-Functionalized Molecular Crystals
Rajbanshi, Arbin; Wan, Shun; Custelcean, Radu; Crystal Growth & Design 13 (2013) 2233–; doi:10.1021/cg400336q

data_4507765
_publ_section_title
;
 Dihydrogen Phosphate Clusters: Trapping H2PO4--Tetramers and Hexamers in
 Urea-Functionalized Molecular Crystals
;
_journal_issue                   5
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              2233
_journal_paper_doi               10.1021/cg400336q
_journal_volume                  13
_journal_year                    2013
_chemical_formula_sum            'C45 H91 N6 O10 P2'
_chemical_formula_weight         938.18
_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_method           SHELXL-97
_cell_angle_alpha                83.775(2)
_cell_angle_beta                 79.502(2)
_cell_angle_gamma                68.296(2)
_cell_formula_units_Z            2
_cell_length_a                   12.5433(14)
_cell_length_b                   15.2724(16)
_cell_length_c                   16.7800(18)
_cell_measurement_temperature    173(2)
_cell_volume                     2933.6(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0376
_diffrn_reflns_av_sigmaI/netI    0.0645
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            18486
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.77
_exptl_absorpt_coefficient_mu    0.125
_exptl_absorpt_correction_T_max  0.9766
_exptl_absorpt_correction_T_min  0.9658
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_density_diffrn    1.062
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1026
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.19
_refine_diff_density_max         1.315
_refine_diff_density_min         -0.595
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     578
_refine_ls_number_reflns         10297
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.1317
_refine_ls_R_factor_gt           0.0934
_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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2727
_refine_ls_wR_factor_ref         0.3062
_reflns_number_gt                6210
_reflns_number_total             10297
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg400336q_si_002.cif
_cod_data_source_block           3
_cod_original_cell_volume        2933.6(5)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4507765