Discovery of a cyclic 6 + 6 hexamer of d-biotin and formaldehyde
Lisbjerg, Micke; Jessen, Bo M.; Rasmussen, Brian; Nielsen, Bjarne E.; Madsen, Anders Ø.; Pittelkow, Michael; Chemical Science 5 (2014) 2647–; doi:10.1039/c4sc00990h

data_1515378
_publ_section_title
;
 Discovery of a cyclic 6 + 6 hexamer of d-biotin and formaldehyde
;
_journal_issue                   7
_journal_name_full               'Chemical Science'
_journal_page_first              2647
_journal_paper_doi               10.1039/c4sc00990h
_journal_volume                  5
_journal_year                    2014
_chemical_absolute_configuration ad
_chemical_formula_sum            'C70 H114 I N12 Na O23 S6'
_chemical_formula_weight         1833.98
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 103.28(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.468(12)
_cell_length_b                   16.713(16)
_cell_length_c                   21.06(2)
_cell_measurement_reflns_used    20983
_cell_measurement_temperature    151(2)
_cell_measurement_theta_max      28.278
_cell_measurement_theta_min      2.288
_cell_volume                     4271(7)
_computing_cell_refinement       'SAINT V8.27B (Bruker AXS Inc., 2012)'
_computing_data_collection       'Bruker Instrument Service v3.0.26'
_computing_data_reduction        'SAINT V8.27B (Bruker AXS Inc., 2012)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      151(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART X2S benchtop diffractometer'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0912
_diffrn_reflns_av_unetI/netI     0.0944
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            72578
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.278
_diffrn_reflns_theta_min         2.288
_diffrn_source                   'microfocus sealed tube'
_exptl_absorpt_coefficient_mu    0.604
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9276
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.426
_exptl_crystal_description       prism
_exptl_crystal_F_000             1924
_exptl_crystal_size_max          0.184
_exptl_crystal_size_mid          0.123
_exptl_crystal_size_min          0.085
_refine_diff_density_max         2.343
_refine_diff_density_min         -1.004
_refine_diff_density_rms         0.097
_refine_ls_abs_structure_details
;
 Flack x determined using 5414 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.010(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1063
_refine_ls_number_reflns         20983
_refine_ls_number_restraints     780
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.1125
_refine_ls_R_factor_gt           0.0641
_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^)+(0.0772P)^2^+2.5121P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1375
_refine_ls_wR_factor_ref         0.1590
_reflns_Friedel_coverage         0.917
_reflns_Friedel_fraction_full    0.992
_reflns_Friedel_fraction_max     0.980
_reflns_number_gt                14442
_reflns_number_total             20983
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4sc00990h2.cif
_cod_data_source_block           mo_D8V297_0m
_cod_depositor_comments
'Adding full bibliography for 1515377--1515378.cif.'
_cod_original_cell_volume        4272(7)
_cod_database_code               1515378
_shelx_estimated_absorpt_t_min   0.897
_shelx_estimated_absorpt_t_max   0.950
_shelxl_version_number           2013-4
_shelx_res_checksum              64767