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_4313603
_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            'C48.5 H50 Cl5 N O6 P'
_chemical_formula_weight         951.11
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.2998(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.3662(2)
_cell_length_b                   13.22590(10)
_cell_length_c                   25.7310(4)
_cell_measurement_temperature    293(2)
_cell_volume                     5145.09(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.937
_diffrn_measured_fraction_theta_max 0.937
_diffrn_measurement_device_type  'Nonius KappaCCD 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  0.0302
_diffrn_reflns_av_sigmaI/netI    0.0429
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            16099
_diffrn_reflns_theta_full        25.06
_diffrn_reflns_theta_max         25.06
_diffrn_reflns_theta_min         4.09
_exptl_absorpt_coefficient_mu    0.358
_exptl_absorpt_correction_T_max  0.9159
_exptl_absorpt_correction_T_min  0.6158
_exptl_crystal_density_diffrn    1.228
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1984
_exptl_crystal_size_max          1.50
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.674
_refine_diff_density_min         -0.567
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     563
_refine_ls_number_reflns         8550
_refine_ls_number_restraints     141
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.1360
_refine_ls_R_factor_gt           0.0976
_refine_ls_shift/su_max          0.025
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1835P)^2^+6.4331P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2794
_refine_ls_wR_factor_ref         0.3177
_reflns_number_gt                5642
_reflns_number_total             8550
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020666p_6.cif
_cod_data_source_block           acp42
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_formula_sum        'C48.50 H50 Cl5 N O6 P'
_cod_database_code               4313603