1:1 Molecular Complex Between Water and a Macrocyclic Crown Phosphonamide
Declercq, Jean-Paul; Delangle, Pascale; Dutasta, Jean-Pierre; Van Oostenryck, Luc; Tinant, Bernard; Acta Crystallographica Section C 53 (1997) 1484–1486; doi:10.1107/S0108270197006604

data_2006591
_publ_contact_author
;
Dr Bernard Tinant
Universite Catholique de Louvain
Laboratoire de Chimie Physique et de Cristallographie
Unite CPMC
1 Place Louis Pasteur
B 1348 Louvain-la-Neuve
Belgium
;
_publ_section_title
;
 1:1 Molecular Complex Between Water and a Macrocyclic Crown
 Phosphonamide
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1484
_journal_page_last               1486
_journal_paper_doi               10.1107/S0108270197006604
_journal_volume                  53
_journal_year                    1997
_chemical_formula_moiety         'C21 H29 N2 O4 P S, H2 O'
_chemical_formula_sum            'C21 H31 N2 O5 P S'
_chemical_formula_weight         454.52
_chemical_name_systematic
;
3-methyl-11,14,17,20-tetraoxa-
2,4,3-diazaphospha-tricyclo[20,3,1,1^5,9^]-heptacosa-
1(26),5,7,9(27),22,24-hexaene-3-sulfide
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_method           SHELXL
_cell_angle_alpha                71.88(2)
_cell_angle_beta                 63.47(2)
_cell_angle_gamma                73.18(2)
_cell_formula_units_Z            2
_cell_length_a                   10.766(2)
_cell_length_b                   10.825(2)
_cell_length_c                   11.857(3)
_cell_measurement_reflns_used    17
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      5
_cell_volume                     1156.5(5)
_computing_cell_refinement       'local program'
_computing_data_collection       'local program'
_computing_data_reduction        'local program'
_computing_molecular_graphics    'PLATON (Spek, 1995)'
_computing_publication_material  SHELXL93
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device_type  'Huber four-circle diffractometer'
_diffrn_measurement_method       '\w scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0455
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5307
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.96
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 50
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    0.243
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.305
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             484
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.387
_refine_diff_density_min         -0.240
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.022
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         5307
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0687
_refine_ls_R_factor_gt           0.0502
_refine_ls_shift/esd_mean        0.001
_refine_ls_shift/su_max          -0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0893P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.1400
_refine_ls_wR_factor_ref         0.1322
_reflns_number_gt                3952
_reflns_number_total             5307
_reflns_threshold_expression     F>4\s(F)
_cod_data_source_file            jz1208.cif
_cod_data_source_block           z1
_cod_original_cell_volume        1156.5(4)
_cod_database_code               2006591