Use of 2,2-Bipyrimidine for the Preparation of UO22±3d Diphosphonates
Adelani, Pius O.; Cook, Nathaniel D.; Burns, Peter C.; Crystal Growth & Design 14 (2014) 5692–; doi:10.1021/cg500972w

data_4512199
_publ_section_title
;
 Use of 2,2-Bipyrimidine for the Preparation of UO22+-3d Diphosphonates
;
_journal_issue                   11
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              5692
_journal_paper_doi               10.1021/cg500972w
_journal_volume                  14
_journal_year                    2014
_chemical_formula_moiety         'C34 H24 N8 Ni2 O26 P6 U3, 6(O)'
_chemical_formula_sum            'C34 H24 N8 Ni2 O32 P6 U3'
_chemical_formula_weight         2073.94
_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                107.204(4)
_cell_angle_beta                 90.137(4)
_cell_angle_gamma                115.826(4)
_cell_formula_units_Z            1
_cell_length_a                   9.961(3)
_cell_length_b                   11.128(3)
_cell_length_c                   14.199(4)
_cell_measurement_reflns_used    1243
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.45
_cell_measurement_theta_min      2.15
_cell_volume                     1337.5(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0718
_diffrn_reflns_av_sigmaI/netI    0.1178
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10752
_diffrn_reflns_theta_full        27.06
_diffrn_reflns_theta_max         27.06
_diffrn_reflns_theta_min         2.15
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.027
_exptl_absorpt_correction_T_max  0.8171
_exptl_absorpt_correction_T_min  0.3468
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SHELXPREP
_exptl_crystal_colour            yellow-green
_exptl_crystal_density_diffrn    2.575
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tablet
_exptl_crystal_F_000             962
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.876
_refine_diff_density_min         -1.995
_refine_diff_density_rms         0.328
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.986
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     385
_refine_ls_number_reflns         5919
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      0.982
_refine_ls_R_factor_all          0.0849
_refine_ls_R_factor_gt           0.0504
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0282P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0922
_refine_ls_wR_factor_ref         0.1053
_reflns_number_gt                4056
_reflns_number_total             5919
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg500972w_si_001.cif
_cod_data_source_block           p-1
_cod_depositor_comments
'Adding full bibliography for 4512198--4512200.cif.'
_cod_original_cell_volume        1337.4(7)
_cod_database_code               4512199