Influence of Hydrogen Bonding in Competition with Lattice Interactions on Carbonyl Coordination at Phosphorus. Implications for Phosphoryl Transfer Activated States1
A. Chandrasekaran; Natalya V. Timosheva; Roberta O. Day; Robert R. Holmes; Inorganic Chemistry 42 (2003) 3285–3292; doi:10.1021/ic020666p

data_4313602
_publ_section_title
;
 Influence of Hydrogen Bonding in Competition with Lattice Interactions on
 Carbonyl Coordination at Phosphorus. Implications for Phosphoryl Transfer
 Activated States1
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3285
_journal_page_last               3292
_journal_paper_doi               10.1021/ic020666p
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C46 H48 N O5 P'
_chemical_formula_weight         725.82
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.0000(6)
_cell_angle_beta                 75.2424(5)
_cell_angle_gamma                90.0000(6)
_cell_formula_units_Z            2
_cell_length_a                   11.11280(10)
_cell_length_b                   14.2208(2)
_cell_length_c                   13.1669(2)
_cell_measurement_temperature    293(2)
_cell_volume                     2012.16(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.832
_diffrn_measured_fraction_theta_max 0.832
_diffrn_measurement_device_type  'Nonius Kappa-CCD area detector'
_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  0.0209
_diffrn_reflns_av_sigmaI/netI    0.0340
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14737
_diffrn_reflns_theta_full        28.94
_diffrn_reflns_theta_max         28.94
_diffrn_reflns_theta_min         4.12
_exptl_absorpt_coefficient_mu    0.114
_exptl_absorpt_correction_T_max  0.9665
_exptl_absorpt_correction_T_min  0.9242
_exptl_crystal_density_diffrn    1.198
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             772
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.196
_refine_diff_density_min         -0.193
_refine_diff_density_rms         0.039
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.04(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         8190
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0411
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0529P)^2^+0.2323P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1016
_refine_ls_wR_factor_ref         0.1091
_reflns_number_gt                7082
_reflns_number_total             8190
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020666p_5.cif
_cod_data_source_block           acp43
_cod_database_code               4313602