Water Encapsulation in a Polyoxapolyaza Macrobicyclic Compound
Pedro Mateus; Rita Delgado; Patrick Groves; Sara R. R. Campos; António M. Baptista; Paula Brandão; Vítor Félix; Journal of Organic Chemistry 77 (2012) 6816–6824; doi:10.1021/jo300799s

data_4027375
_publ_contact_author_address
;Instituto de Tecnologia Qu\'imica e Biol\'ogica,
UNL, Av. da Rep\'ublica ? EAN,
2780?157 Oeiras, Portugal. 
;
_publ_contact_author_email       delgado@itqb.unl.pt.
_publ_contact_author_fax         ' (+351) 21 441 12 77'
_publ_contact_author_name        'Rita Delgado'
_publ_section_title
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 Water Encapsulation in a Polyoxapolyaza Macrobicyclic Compound
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_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              6816
_journal_page_last               6824
_journal_paper_doi               10.1021/jo300799s
_journal_volume                  77
_journal_year                    2012
_chemical_formula_sum            'C36 H70 Cl3 N5 O11'
_chemical_formula_weight         855.32
_chemical_name_systematic
; 
 ? 
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                89.642(2)
_cell_angle_beta                 84.485(2)
_cell_angle_gamma                87.787(2)
_cell_formula_units_Z            2
_cell_length_a                   9.2838(4)
_cell_length_b                   15.2658(7)
_cell_length_c                   15.8794(7)
_cell_measurement_temperature    150(2)
_cell_volume                     2238.41(17)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'PLATON (Speck, 2008)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       'omega and phi scans'
_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  0.0331
_diffrn_reflns_av_sigmaI/netI    0.0316
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            50322
_diffrn_reflns_theta_full        27.95
_diffrn_reflns_theta_max         27.95
_diffrn_reflns_theta_min         1.29
_diffrn_standards_interval_count 0.5
_diffrn_standards_interval_time  60
_exptl_absorpt_coefficient_mu    0.263
_exptl_absorpt_correction_T_max  0.9691
_exptl_absorpt_correction_T_min  0.9252
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.269
_exptl_crystal_description       block
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.115
_refine_diff_density_min         -0.586
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     572
_refine_ls_number_reflns         10577
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0670
_refine_ls_R_factor_gt           0.0480
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0993P)^2^+0.9966P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1407
_refine_ls_wR_factor_ref         0.1720
_reflns_number_gt                8248
_reflns_number_total             10577
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo300799s_si_002.cif
_cod_data_source_block           t2pn5o3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0993P)^2^+0.9966P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0993P)^2^+0.9966P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               4027375