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_4510002
_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         'C9 H9 O11 P3 U, C6 H11 N2, H2O'
_chemical_formula_sum            'C15 H20 N2 O12 P3 U'
_chemical_formula_weight         751.27
_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                118.0820(10)
_cell_angle_beta                 90.8820(10)
_cell_angle_gamma                91.9230(10)
_cell_formula_units_Z            2
_cell_length_a                   8.8825(5)
_cell_length_b                   11.7704(7)
_cell_length_c                   12.1185(7)
_cell_measurement_reflns_used    6824
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.57
_cell_measurement_theta_min      2.30
_cell_volume                     1116.51(11)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 1999)'
_computing_molecular_graphics
'SHELXP-97 (Sheldrick, 1997), CrystalMaker (Kohn, 1995)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       '0.5\% wide \w exposures'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'I\ms microfocused'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0221
_diffrn_reflns_av_sigmaI/netI    0.0233
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            20959
_diffrn_reflns_theta_full        30.57
_diffrn_reflns_theta_max         30.57
_diffrn_reflns_theta_min         2.30
_exptl_absorpt_coefficient_mu    7.549
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6263
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sheltxprep
_exptl_crystal_colour            Yellow-green
_exptl_crystal_density_diffrn    2.235
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             714
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.288
_refine_diff_density_min         -0.985
_refine_diff_density_rms         0.281
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.232
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     359
_refine_ls_number_reflns         6824
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.232
_refine_ls_R_factor_all          0.0213
_refine_ls_R_factor_gt           0.0185
_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^)+(0.0306P)^2^+0.0636P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0462
_refine_ls_wR_factor_ref         0.0549
_reflns_number_gt                6491
_reflns_number_total             6824
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg401435w_si_002.cif
_cod_data_source_block           '[Emim][UPhDPO]'
_cod_database_code               4510002