Ionothermal and Hydrothermal Flux Syntheses of Five New Uranyl Phosphonates
Parker, T. Gannon; Cross, Justin N.; Polinski, Matthew J.; Lin, Jian; Albrecht-Schmitt, Thomas E.; Crystal Growth & Design 14 (2014) 228–; doi:10.1021/cg401435w

data_4510003
_publ_section_title
;
 Ionothermal and Hydrothermal Flux Syntheses of Five New Uranyl
 Phosphonates
;
_journal_issue                   1
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              228
_journal_paper_doi               10.1021/cg401435w
_journal_volume                  14
_journal_year                    2014
_chemical_formula_moiety         'C12 H28 O34 P8 U5, 2(C8 H15 N2)'
_chemical_formula_sum            'C28 H58 N4 O34 P8 U5'
_chemical_formula_weight         2432.69
_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_method           SHELXL-97
_cell_angle_alpha                67.360(3)
_cell_angle_beta                 70.649(4)
_cell_angle_gamma                88.418(4)
_cell_formula_units_Z            1
_cell_length_a                   9.4611(18)
_cell_length_b                   13.424(3)
_cell_length_c                   13.453(3)
_cell_measurement_reflns_used    6827
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.55
_cell_measurement_theta_min      2.30
_cell_volume                     1478.0(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(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  0.0297
_diffrn_reflns_av_sigmaI/netI    0.0289
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            23140
_diffrn_reflns_theta_full        27.55
_diffrn_reflns_theta_max         27.55
_diffrn_reflns_theta_min         2.30
_exptl_absorpt_coefficient_mu    13.959
_exptl_absorpt_correction_T_max  0.248
_exptl_absorpt_correction_T_min  0.049
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sheltxprep
_exptl_crystal_colour            Yellow-Green
_exptl_crystal_density_diffrn    2.733
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1106
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_platon_squeeze_details
' 3======================================================================End'
_refine_diff_density_max         2.222
_refine_diff_density_min         -1.030
_refine_diff_density_rms         0.173
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     371
_refine_ls_number_reflns         6827
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0243
_refine_ls_R_factor_gt           0.0198
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0204P)^2^+0.8932P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0452
_refine_ls_wR_factor_ref         0.0465
_reflns_number_gt                6162
_reflns_number_total             6827
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg401435w_si_002.cif
_cod_data_source_block           g2
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4510003