A Macrobicyclic Thiophosphonamide Polyether Ligand
Van Oostenryck, Luc; Tinant, Bernard; Declercq, Jean-Paul; Dutasta, Jean-Pierre; Acta Crystallographica, Section C: Crystal Structure Communications 51 (1995) 80–84; doi:10.1107/S0108270194003914

data_2003169
_publ_section_title
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 A Macrobicyclic Thiophosphonamide Polyether Ligand
;
_journal_coden_ASTM              ACSCEE
_journal_coeditor_code           HU1098
_journal_issue                   1
_journal_name_full
'Acta Crystallographica, Section C: Crystal Structure Communications'
_journal_page_first              80
_journal_page_last               84
_journal_paper_doi               10.1107/S0108270194003914
_journal_volume                  51
_journal_year                    1995
_chemical_formula_moiety         'C29 H35 N2 O5 P S'
_chemical_formula_sum            'C29 H35 N2 O5 P S'
_chemical_formula_weight         554.62
_chemical_name_systematic
; 31-phenyl-13,16,19,22,25-pentoxa-2,6,31-diazaphosphatetracyclo
[24,4,0,1^2,6^,0^7,12^]hentriaconta-1(26),7,9,11,27,29-hexene-31-sulfide
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 96.11(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.674(3)
_cell_length_b                   20.023(4)
_cell_length_c                   11.494(3)
_cell_measurement_reflns_used    15
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      2.5
_cell_volume                     2900.3(12)
_computing_cell_refinement       'local program'
_computing_data_collection       'local program'
_computing_data_reduction        'local program'
_computing_molecular_graphics
'PLUTO (Motherwell & Clegg, 1978); ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL93
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Syntex P2~1~ four-circle diffractometer'
_diffrn_measurement_method       '\w scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         xray-tube
_diffrn_radiation_type           'Molybdenum K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0
_diffrn_reflns_av_sigmaI/netI    0.0342
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5699
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.91
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 50
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    0.207
_exptl_crystal_density_diffrn    1.270
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.618
_refine_diff_density_min         -0.211
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.061
_refine_ls_goodness_of_fit_obs   1.176
_refine_ls_hydrogen_treatment    'refall with U common for all H atoms'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         5699
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_restrained_S_obs      1.176
_refine_ls_R_factor_all          0.0671
_refine_ls_R_factor_obs          0.0487
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(F~o~^2^)+(0.0747P)^2^+0.5425P] where P = (F~o~^2^+2F~c~^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1386
_refine_ls_wR_factor_obs         0.1306
_reflns_number_observed          4197
_reflns_number_total             5699
_reflns_observed_criterion       >2sigma(I)
_cod_depositor_comments
;
 Added additional information after consulting the original publication
 and the supplementary material.

 Antanas Vaitkus,
 2021-09-27
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_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2003169