Self-assembly of dynamic orthoester cryptates
Rene-Chris Brachvogel; Frank Hampel; Max von Delius; Nature Communications 6 (2015) 7129–; doi:10.1038/ncomms8129

data_1548274
_publ_section_title
;
 Self-assembly of dynamic orthoester cryptates
;
_journal_name_full               'Nature Communications'
_journal_page_first              7129
_journal_paper_doi               10.1038/ncomms8129
_journal_volume                  6
_journal_year                    2015
_chemical_formula_moiety         'C16 H30 Na O9, C32 H12 B F24'
_chemical_formula_sum            'C48 H42 B Cl0.25 F24 Na O9'
_chemical_formula_weight         1261.48
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_cell_angle_alpha                90
_cell_angle_beta                 107.372(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.3769(4)
_cell_length_b                   16.7983(4)
_cell_length_c                   18.7409(5)
_cell_measurement_reflns_used    3192
_cell_measurement_temperature    107(4)
_cell_measurement_theta_max      61.0340
_cell_measurement_theta_min      3.9440
_cell_volume                     5521.4(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2013)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      107(4)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6144
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.822
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_details
;
  1 omega   56.00  155.00   1.0000    1.2350
omega____ theta____ kappa____ phi______ frames
    -       82.2806   45.0000  120.0000 99

  2 omega   51.00  156.00   1.0000    1.2350
omega____ theta____ kappa____ phi______ frames
    -       82.2806   77.0000   30.0000 105

  3 omega    2.00  104.00   1.0000    1.2350
omega____ theta____ kappa____ phi______ frames
    -       82.2806  -94.0000  -60.0000 102

  4 omega  -89.00  -35.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000 -178.0000   60.0000 54

  5 omega  -85.00  -37.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  178.0000  -90.0000 48
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0024978000
_diffrn_orient_matrix_UB_12      -0.0442277000
_diffrn_orient_matrix_UB_13      -0.0727392000
_diffrn_orient_matrix_UB_21      -0.0540358000
_diffrn_orient_matrix_UB_22      0.0641228000
_diffrn_orient_matrix_UB_23      -0.0458246000
_diffrn_orient_matrix_UB_31      0.0691662000
_diffrn_orient_matrix_UB_32      0.0484128000
_diffrn_orient_matrix_UB_33      -0.0057526000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0346
_diffrn_reflns_av_unetI/netI     0.0510
_diffrn_reflns_Laue_measured_fraction_full 0.822
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6750
_diffrn_reflns_point_group_measured_fraction_full 0.822
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         61.408
_diffrn_reflns_theta_min         3.643
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.577
_exptl_absorpt_correction_T_max  0.903
_exptl_absorpt_correction_T_min  0.815
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_description
;
;
_exptl_crystal_F_000             2553
_exptl_crystal_recrystallization_method 'crystallized from DCM/Cyclopentane'
_exptl_crystal_size_max          0.2637
_exptl_crystal_size_mid          0.1303
_exptl_crystal_size_min          0.0996
_refine_diff_density_max         0.477
_refine_diff_density_min         -0.407
_refine_diff_density_rms         0.069
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     432
_refine_ls_number_reflns         4259
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0881
_refine_ls_R_factor_gt           0.0667
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1044P)^2^+6.5070P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1748
_refine_ls_wR_factor_ref         0.1934
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3156
_reflns_number_total             4259
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ncomms8129-s2.cif
_cod_data_source_block           rb01_4
_cod_database_code               1548274
_chemical_oxdiff_formula         'C16 H30 Na B4 F24 C28'
_reflns_odcompleteness_completeness 94.37
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     61.93
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O2-C5 \\sim O2A-C5 \\sim O2-C4 \\sim O2A-C4
 with sigma of 0.02
 C5-C6 \\sim C5-C6A
 with sigma of 0.02
 O3A-C6A \\sim O3-C6 \\sim O3-C7 \\sim O3A-C7
 with sigma of 0.02
 O1-C2 \\sim O1A-C2
 with sigma of 0.02
 C4-C3 \\sim C4-C3A
 with sigma of 0.02
 O1-C3 \\sim O1A-C3A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O1) = Uanis(O1A)
Uanis(O2) = Uanis(O2A)
Uanis(C6) = Uanis(C6A)
Uanis(O3A) = Uanis(O3)
Uanis(C3A) = Uanis(C3)
4. Others
 Fixed Sof: H1A(0.5) H1B(0.5) H1C(0.5) C3(0.5) H3A(0.5) H3B(0.5) C3A(0.5)
 H3AA(0.5) H3AB(0.5) C6(0.5) H6A(0.5) H6B(0.5) C6A(0.5) H6AA(0.5) H6AB(0.5)
 H8A(0.5) H8B(0.5) H8C(0.5) C9(0.5) H9A(0.5) H10A(0.5) H10B(0.5) H11A(0.5)
 H11B(0.5) C12(0.5) H12A(0.5) H12B(0.5) O1(0.5) O1A(0.5) O2(0.5) O2A(0.5)
 O3(0.5) O3A(0.5) O4(0.5) O5(0.5) O6(0.5)
5.a Riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B)
5.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C3A(H3AA,H3AB), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C6A(H6AA,
 H6AB)
5.c Aromatic/amide H refined with riding coordinates:
 C22(H22), C24(H24), C32(H32), C34(H34), C36(H36), C42(H42), C44(H44)
5.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C8(H8A,H8B,H8C)
;
_shelx_res_checksum              5673
_shelx_hkl_checksum              75847
_olex2_submission_special_instructions 'No special instructions were received'