Structural and kinetic study of self-assembling macrocyclic dimer natural product aminoglycoside 66-40C and unnatural variants
Hanessian, Stephen; Maianti, Juan Pablo; Ly, Vu Linh; Deschênes-Simard, Benoît; Chemical Science 3 (2012) 249–; doi:10.1039/c1sc00538c

data_1515276
_publ_section_title
;
 Structural and kinetic study of self-assembling macrocyclic dimer natural
 product aminoglycoside 66-40C and unnatural variants
;
_journal_issue                   1
_journal_name_full               'Chemical Science'
_journal_page_first              249
_journal_paper_doi               10.1039/c1sc00538c
_journal_volume                  3
_journal_year                    2012
_chemical_absolute_configuration rmad
_chemical_compound_source        'Synthesized by the authors. See text'
_chemical_formula_moiety         'C24 H42 N6 O8, 2(O4 S), 14(H2 O)'
_chemical_formula_sum            'C24 H70 N6 O30 S2'
_chemical_formula_weight         986.98
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.975(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.8516(4)
_cell_length_b                   26.1435(15)
_cell_length_c                   12.6653(7)
_cell_measurement_reflns_used    18335
_cell_measurement_temperature    200
_cell_measurement_theta_max      53.23
_cell_measurement_theta_min      3.38
_cell_volume                     2210.7(2)
_computing_cell_refinement       'SAINT V7.60A(Bruker AXS, 2008)'
_computing_data_collection       'APEX2 (Bruker AXS, 2008)'
_computing_data_reduction        'SAINT V7.60A(Bruker AXS, 2008)'
_computing_molecular_graphics    'SHELXTL v6.12 (Bruker AXS, 2001)'
_computing_publication_material  'UdMX (Maris, 2004)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200
_diffrn_detector_area_resol_mean 5.5
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker Smart 6000'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'Helios optics'
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.000
_diffrn_reflns_av_sigmaI/netI    0.0400
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            28784
_diffrn_reflns_theta_full        53.69
_diffrn_reflns_theta_max         53.69
_diffrn_reflns_theta_min         3.38
_exptl_absorpt_coefficient_mu    2.018
_exptl_absorpt_correction_T_max  0.9413
_exptl_absorpt_correction_T_min  0.6632
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs (Sheldrick, 1996)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.483
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.225
_refine_diff_density_min         -0.231
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details 'Flack H D (1983), 2714 Friedel Pairs'
_refine_ls_abs_structure_Flack   0.07(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_matrix_type           full
_refine_ls_number_parameters     689
_refine_ls_number_reflns         5428
_refine_ls_number_restraints     572
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0437
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0487P)^2^+1.2198P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1022
_refine_ls_wR_factor_ref         0.1060
_reflns_number_gt                4867
_reflns_number_total             5428
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c1sc00538c.txt
_cod_data_source_block           bent66
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      P21
_cod_database_code               1515276