Ethyl <i>N</i>,<i>N</i>'-bis(3,4,5-trimethoxyphenyl)phosphorodiamidate
Li, Chen-Guang; Robinson, Paul D.; Dyer, Daniel J.; Acta Crystallographica Section E 62 (2006) o4233–o4235; doi:10.1107/S1600536806034374

data_2210537
_publ_section_title
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 Ethyl <i>N</i>,<i>N</i>'-bis(3,4,5-trimethoxyphenyl)phosphorodiamidate
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_journal_coeditor_code           CI2153
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o4233
_journal_page_last               o4235
_journal_paper_doi               10.1107/S1600536806034374
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          'C20 H29 N2 O8 P'
_chemical_formula_moiety         'C20 H29 N2 O8 P'
_chemical_formula_sum            'C20 H29 N2 O8 P'
_chemical_formula_weight         456.42
_chemical_melting_point          .434E-305
_chemical_name_systematic
;
Ethyl N,N'-bis(3,4,5-trimethoxyphenyl)phosphorodiamidate
;
_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
_cell_angle_alpha                93.596(3)
_cell_angle_beta                 98.968(3)
_cell_angle_gamma                117.066(2)
_cell_formula_units_Z            2
_cell_length_a                   10.0994(5)
_cell_length_b                   10.1542(5)
_cell_length_c                   11.9800(9)
_cell_measurement_reflns_used    6224
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.2
_cell_measurement_theta_min      2.4
_cell_volume                     1068.10(11)
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'SAINT and SADABS (Bruker, 2005)'
_computing_molecular_graphics
'PLATON (Spek, 2003) and SHELXTL (Bruker, 2005)'
_computing_publication_material  'SHELXL97 and PLATON'
_computing_structure_refinement
;
LS in TEXSAN (Molecular Structure Corporation, 1997) and
SHELXL97 (Sheldrick, 1997)
;
_computing_structure_solution    'SIR92 (Burla <i>et al.</i>,  1989)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.0
_diffrn_measured_fraction_theta_max 1.0
_diffrn_measurement_device_type  'Bruker Kappa APEXII CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.039
_diffrn_reflns_av_sigmaI/netI    0.031
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            31960
_diffrn_reflns_theta_full        26.4
_diffrn_reflns_theta_max         26.4
_diffrn_reflns_theta_min         1.7
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.179
_exptl_absorpt_correction_T_max  0.965
_exptl_absorpt_correction_T_min  0.862
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2005)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_description       'irregular fragment'
_exptl_crystal_F_000             484
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.38
_refine_diff_density_min         -0.44
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.03
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     295
_refine_ls_number_reflns         4358
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.03
_refine_ls_R_factor_all          0.049
_refine_ls_R_factor_gt           0.038
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0355P)^2^+0.7048P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.084
_refine_ls_wR_factor_ref         0.089
_reflns_number_gt                3628
_reflns_number_total             4358
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ci2153.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               2210537
_cod_database_fobs_code          2210537