Metal-Directed Self-Assembly of Cavitand Frameworks
Menozzi, Edoardo; Busi, Marco; Massera, Chiara; Ugozzoli, Franco; Zuccaccia, Daniele; Macchioni, Alceo; Dalcanale, Enrico; Journal of Organic Chemistry 71 (2006) 2617–2624; doi:10.1021/jo052460m

data_4021599
_publ_contact_author
;
 Prof. Enrico Dalcanale
 Dipartimento di Chimica Organica ed Industriale and Unit\`a INSTM 
 Universit\`a di Parma, Parco Area delle Scienze 17/A, 43100 Parma (Italy)
;
_publ_contact_author_email       enrico.dalcanale@unipr.it
_publ_section_title
;
 Metal-Directed Self-Assembly of Cavitand Frameworks
;
_journal_coden_ASTM              JOCEAH
_journal_issue                   7
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              2617
_journal_page_last               2624
_journal_paper_doi               10.1021/jo052460m
_journal_volume                  71
_journal_year                    2006
_chemical_formula_sum            'C65 H62 Cl2 N2 O9'
_chemical_formula_weight         1086.07
_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                90.000(5)
_cell_angle_beta                 106.457(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            4
_cell_length_a                   22.432(5)
_cell_length_b                   17.535(5)
_cell_length_c                   14.577(5)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    173(2)
_cell_volume                     5499(3)
_computing_data_collection       'Belletti & al. 1988'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR 92'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Enraf Nonius CAD 4'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0655
_diffrn_reflns_av_sigmaI/netI    0.0405
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9521
_diffrn_reflns_theta_full        65.03
_diffrn_reflns_theta_max         65.03
_diffrn_reflns_theta_min         3.25
_diffrn_standards_decay_%        1
_diffrn_standards_interval_count 100
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    1.560
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.312
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2288
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.961
_refine_diff_density_min         -0.893
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     714
_refine_ls_number_reflns         9158
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.1007
_refine_ls_R_factor_gt           0.0738
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1537P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2124
_refine_ls_wR_factor_ref         0.2323
_reflns_number_gt                6247
_reflns_number_total             9158
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo052460msi20051129_060556.cif
_cod_depositor_comments
;
 Updated bibliographic information.

 Antanas Vaitkus,
 2019-10-10
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4021599