Crystallization-Driven Multicomponent Encapsulation of Coulombically Repulsive Guests
Barboiu, Mihail; Dumitrescu, Dan; Petit, Eddy; Legrand, Yves-Marie; van der Lee, Arie; Crystal Growth & Design 15 (2015) 3525–; doi:10.1021/acs.cgd.5b00596

data_4513247
_publ_section_title
;
 Crystallization-Driven Multicomponent Encapsulation of Coulombically
 Repulsive Guests
;
_journal_issue                   7
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              3525
_journal_paper_doi               10.1021/acs.cgd.5b00596
_journal_volume                  15
_journal_year                    2015
_chemical_formula_moiety
'C28 H20 O16 S4, C6 H10 N2, 2(C H7 N4), 6(H2 O)'
_chemical_formula_sum            'C36 H56 N10 O22 S4'
_chemical_formula_weight         1109.19
_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   difmap
_atom_sites_solution_primary     iterative
_cell_angle_alpha                65.072(4)
_cell_angle_beta                 80.169(3)
_cell_angle_gamma                83.094(3)
_cell_formula_units_Z            2
_cell_length_a                   12.5102(5)
_cell_length_b                   13.4656(5)
_cell_length_c                   15.4021(6)
_cell_measurement_reflns_used    8892
_cell_measurement_temperature    175
_cell_measurement_theta_max      28.8410
_cell_measurement_theta_min      1.5540
_cell_volume                     2314.94(17)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      175
_diffrn_detector_area_resol_mean 8.0072
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.848
_diffrn_measurement_details
;
  1 omega    0.00   87.00   1.0000    8.0200
omega____ theta____ kappa____ phi______ frames
    -       18.0793   57.0000   30.0000 87

  2 omega  -52.00   35.00   1.0000    8.0200
omega____ theta____ kappa____ phi______ frames
    -       18.0793  -38.0000  120.0000 87

  3 omega   -3.00   46.00   1.0000    8.0200
omega____ theta____ kappa____ phi______ frames
    -       18.0793   57.0000  150.0000 49

  4 omega  -50.00   39.00   1.0000    8.0200
omega____ theta____ kappa____ phi______ frames
    -       18.0793  -57.0000 -120.0000 89

  5 omega  -25.00    1.00   1.0000    8.0200
omega____ theta____ kappa____ phi______ frames
    -       18.0793  101.0000   -3.6471 26

  6 omega  -14.00   11.00   1.0000    8.0200
omega____ theta____ kappa____ phi______ frames
    -      -18.7824  -77.0000    0.0000 25

  7 omega   -4.00   23.00   1.0000    8.0200
omega____ theta____ kappa____ phi______ frames
    -      -18.7824 -100.0000  150.0000 27

;
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0563924000
_diffrn_orient_matrix_UB_12      -0.0143363000
_diffrn_orient_matrix_UB_13      -0.0057284000
_diffrn_orient_matrix_UB_21      -0.0074616000
_diffrn_orient_matrix_UB_22      -0.0484567000
_diffrn_orient_matrix_UB_23      0.0430653000
_diffrn_orient_matrix_UB_31      -0.0092229000
_diffrn_orient_matrix_UB_32      -0.0288150000
_diffrn_orient_matrix_UB_33      -0.0271695000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.029
_diffrn_reflns_av_sigmaI/netI    0.0498
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            18628
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.106
_diffrn_reflns_theta_min         1.654
_exptl_absorpt_coefficient_mu    0.301
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.99113
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.591
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1164
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.500
_exptl_crystal_size_min          0.400
_refine_diff_density_max         0.76
_refine_diff_density_min         -0.93
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1075
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     685
_refine_ls_number_reflns         9143
_refine_ls_number_restraints     21
_refine_ls_R_factor_all          0.0642
_refine_ls_R_factor_gt           0.0544
_refine_ls_shift/su_max          0.0006867
_refine_ls_shift/su_mean         0.0000287
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 16.9 3.91 12.6 5.55 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0579
_refine_ls_wR_factor_gt          0.0554
_refine_ls_wR_factor_ref         0.0554
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              17
_reflns_limit_k_min              -16
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                9143
_reflns_number_total             10560
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.44
_oxford_diffrn_Wilson_scale      0.03
_oxford_refine_ls_r_factor_ref   0.0544
_oxford_refine_ls_scale          4.050(6)
_oxford_reflns_number_all        10560
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_cod_data_source_file            cg5b00596_si_003.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 4513247--4513249.cif.'
_cod_original_cell_volume        2314.96(17)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C36 H56 N10 O22 S4 '
_cod_database_code               4513247
_cell_oxdiff_length_a            12.5102(5)
_cell_oxdiff_length_b            13.4656(5)
_cell_oxdiff_length_c            15.4021(6)
_cell_oxdiff_angle_alpha         65.072(4)
_cell_oxdiff_angle_beta          80.169(3)
_cell_oxdiff_angle_gamma         83.094(3)
_cell_oxdiff_volume              2314.96(15)
_montpellier_reflns_maxres       0.73
_montpellier_reflns_completeness_maxres 84.84
_montpellier_reflns_redundancy_maxres 1.76
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S , H(541,X'S) , H(542,X'S) 
CONT H(531,X'S) , H(532,X'S), H(491,X'S) , H(492,X'S) 
CONT H(501,X'S) , H(502,X'S) , H(511,X'S), H(512,X'S) 
CONT H(521,X'S) , H(522,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) 
RIDE O   (   9,X'S) H   (  91,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) 
RIDE C   (  12,X'S) H   ( 122,X'S) H   ( 121,X'S) 
RIDE O   (  15,X'S) H   ( 151,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) 
RIDE C   (  19,X'S) H   ( 191,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) H   ( 242,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) 
RIDE O   (  35,X'S) H   ( 351,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) H   ( 362,X'S) 
RIDE C   (  38,X'S) H   ( 381,X'S) 
RIDE C   (  44,X'S) H   ( 441,X'S) 
RIDE O   (  47,X'S) H   ( 471,X'S) 
RIDE C   (  48,X'S) H   ( 482,X'S) H   ( 481,X'S) 
RIDE N   (  55,X'S) H   ( 553,X'S) H   ( 552,X'S) H   ( 551,X'S) 
RIDE C   (  56,X'S) H   ( 562,X'S) H   ( 561,X'S) 
RIDE N   (  58,X'S) H   ( 581,X'S) 
RIDE C   (  59,X'S) H   ( 591,X'S) 
RIDE C   (  60,X'S) H   ( 601,X'S) 
RIDE C   (  61,X'S) H   ( 611,X'S) 
RIDE C   (  62,X'S) H   ( 621,X'S) 
RIDE N   (  63,X'S) H   ( 631,X'S) 
RIDE N   (  64,X'S) H   ( 642,X'S) H   ( 641,X'S) 
RIDE N   (  66,X'S) H   ( 661,X'S) H   ( 662,X'S) 
RIDE N   (  67,X'S) H   ( 672,X'S) H   ( 671,X'S) 
RIDE N   (  68,X'S) H   ( 681,X'S) 
RIDE N   (  69,X'S) H   ( 692,X'S) H   ( 691,X'S) 
RIDE N   (  71,X'S) H   ( 712,X'S) H   ( 711,X'S) 
RIDE N   (  72,X'S) H   ( 721,X'S) H   ( 722,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
DIST 1.0, 0.01 = 
CONT O ( 54) TO H(541) 
DIST 0.82, 0.02 = 
CONT O ( 54) TO H(542) 
CONT O ( 53) TO H(531) 
CONT O ( 53) TO H(532) 
CONT O ( 49) TO H(491) 
CONT O ( 49) TO H(492) 
CONT O ( 50) TO H(501) 
CONT O ( 50) TO H(502) 
CONT O ( 51) TO H(511) 
CONT O ( 51) TO H(512) 
CONT O ( 52) TO H(521) 
CONT O ( 52) TO H(522) 
ANGLE 108,0.03  = H(541) TO O(54) TO H(542) 
ANGLE 108,0.03  = H(531) TO O(53) TO H(532) 
ANGLE 108,0.03  = H(491) TO O(49) TO H(492) 
ANGLE 108,0.03  = H(501) TO O(50) TO H(502) 
ANGLE 108,0.03  = H(511) TO O(51) TO H(512) 
ANGLE 108,0.03  = H(521) TO O(52) TO H(522) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
REM   SHIFTLIMIT   START (DO NOT REMOVE THIS LINE) 
LIMIT      0.01000000 H(541,X) 
LIMIT      0.01000000 H(541,Y) 
LIMIT      0.01000000 H(541,Z) 
REM   SHIFTLIMIT   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;