Functionalization of Intact Trimetaphosphate: A Triphosphorylating Reagent for C, N, and O Nucleophiles.
Shepard, Scott M.; Cummins, Christopher C.; Journal of the American Chemical Society 141 (2019) 1852–1856; doi:10.1021/jacs.8b12204

data_4127931
_publ_section_title
;
 Functionalization of Intact Trimetaphosphate: A Triphosphorylating
 Reagent for C, N, and O Nucleophiles.
;
_journal_issue                   5
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1852
_journal_page_last               1856
_journal_paper_doi               10.1021/jacs.8b12204
_journal_volume                  141
_journal_year                    2019
_chemical_formula_sum            'C48 H58 N4 O11 P6'
_chemical_formula_weight         1052.80
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                94.628(5)
_cell_angle_beta                 97.727(6)
_cell_angle_gamma                92.077(5)
_cell_formula_units_Z            2
_cell_length_a                   10.7896(12)
_cell_length_b                   14.973(2)
_cell_length_c                   15.5499(18)
_cell_measurement_reflns_used    9577
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      2.30
_cell_volume                     2478.4(5)
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 7.4
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker Photon2 CPAD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0679
_diffrn_reflns_av_unetI/netI     0.0294
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            169841
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.362
_diffrn_reflns_theta_min         2.398
_diffrn_source
'I\mS micro-focus sealed tube, multilayer optics'
_exptl_absorpt_coefficient_mu    0.281
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Herbst-Irmer et al., 2015)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.108
_exptl_crystal_size_mid          0.069
_exptl_crystal_size_min          0.053
_exptl_transmission_factor_max   0.7457
_exptl_transmission_factor_min   0.7038
_refine_diff_density_max         0.510
_refine_diff_density_min         -0.587
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     675
_refine_ls_number_reflns         12323
_refine_ls_number_restraints     747
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0394
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0406P)^2^+2.4533P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0930
_refine_ls_wR_factor_ref         0.1019
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10010
_reflns_number_total             12323
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b12204_si_002.cif
_cod_data_source_block           9
_cod_original_cell_volume        2478.3(5)
_cod_database_code               4127931
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.970
_shelx_estimated_absorpt_t_max   0.985
_shelx_res_checksum              46475
_shelx_hkl_checksum              32951