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_4513249
_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 H19 Na O17 S4, C6 H7 N2, 2(C H7 N4), 3(H2O)'
_chemical_formula_sum            'C36 H40 N10 Na O20 S4'
_chemical_formula_weight         1084.05
_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   difmap
_atom_sites_solution_primary     iterative
_cell_angle_alpha                90
_cell_angle_beta                 95.903(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.7300(5)
_cell_length_b                   30.0399(11)
_cell_length_c                   14.0781(7)
_cell_measurement_reflns_used    7653
_cell_measurement_temperature    175
_cell_measurement_theta_max      28.7730
_cell_measurement_theta_min      1.8740
_cell_volume                     4934.4(4)
_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 0.959
_diffrn_measured_fraction_theta_max 0.872
_diffrn_measurement_details
;
  1 omega   -8.00   60.00   1.0000  110.5300
omega____ theta____ kappa____ phi______ frames
    -       17.9231   38.0000   90.0000 68

  2 omega  -17.00   24.00   1.0000  110.5300
omega____ theta____ kappa____ phi______ frames
    -      -18.7043 -100.0000   60.0000 41

  3 omega  -74.00  -22.00   1.0000  110.5300
omega____ theta____ kappa____ phi______ frames
    -      -18.7043    0.0000  -60.0000 52

  4 omega    4.00   50.00   1.0000  110.5300
omega____ theta____ kappa____ phi______ frames
    -      -18.7043    0.0000  -60.0000 46

  5 omega  -16.00   23.00   1.0000  110.5300
omega____ theta____ kappa____ phi______ frames
    -      -18.7043 -100.0000 -150.0000 39

;
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0153481000
_diffrn_orient_matrix_UB_12      0.0216284000
_diffrn_orient_matrix_UB_13      -0.0170664000
_diffrn_orient_matrix_UB_21      -0.0587448000
_diffrn_orient_matrix_UB_22      -0.0051741000
_diffrn_orient_matrix_UB_23      0.0017949000
_diffrn_orient_matrix_UB_31      0.0033687000
_diffrn_orient_matrix_UB_32      0.0079040000
_diffrn_orient_matrix_UB_33      0.0476637000
_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  0.030
_diffrn_reflns_av_sigmaI/netI    0.0471
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            24304
_diffrn_reflns_theta_full        25.249
_diffrn_reflns_theta_max         29.022
_diffrn_reflns_theta_min         1.604
_exptl_absorpt_coefficient_mu    0.286
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92751
_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            red
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2244
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.600
_exptl_crystal_size_min          0.300
_refine_diff_density_max         2.26
_refine_diff_density_min         -1.22
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0500
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     667
_refine_ls_number_reflns         9148
_refine_ls_number_restraints     189
_refine_ls_R_factor_all          0.1489
_refine_ls_R_factor_gt           0.1304
_refine_ls_shift/su_max          0.0002578
_refine_ls_shift/su_mean         0.0000205
_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: 
 25.5 20.8 20.7 9.01 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1455
_refine_ls_wR_factor_gt          0.1347
_refine_ls_wR_factor_ref         0.1347
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              40
_reflns_limit_k_min              0
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_gt                9148
_reflns_number_total             11452
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.39
_oxford_diffrn_Wilson_scale      0.33
_oxford_refine_ls_r_factor_ref   0.1304
_oxford_refine_ls_scale          2.076(7)
_oxford_reflns_number_all        11452
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_cod_data_source_file            cg5b00596_si_001.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 4513247--4513249.cif.'
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_database_code               4513249
_cell_oxdiff_length_a            11.7265(5)
_cell_oxdiff_length_b            30.0532(13)
_cell_oxdiff_length_c            14.0763(4)
_cell_oxdiff_angle_alpha         89.925(3)
_cell_oxdiff_angle_beta          95.907(3)
_cell_oxdiff_angle_gamma         89.953(4)
_cell_oxdiff_volume              4934.4(3)
_montpellier_reflns_maxres       0.73
_montpellier_reflns_completeness_maxres 87.23
_montpellier_reflns_redundancy_maxres 2.11
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
RIDE C   (   8,X'S) H   (  81,X'S) H   (  82,X'S) 
RIDE O   (  11,X'S) H   ( 111,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) 
RIDE C   (  20,X'S) H   ( 202,X'S) H   ( 201,X'S) 
RIDE O   (  23,X'S) H   ( 231,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) H   ( 252,X'S) 
RIDE O   (  28,X'S) H   ( 281,X'S) 
RIDE C   (  30,X'S) H   ( 301,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) 
RIDE C   (  33,X'S) H   ( 332,X'S) H   ( 331,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) 
RIDE C   (  37,X'S) H   ( 371,X'S) 
RIDE C   (  42,X'S) H   ( 421,X'S) 
RIDE C   (  44,X'S) H   ( 441,X'S) 
RIDE N   (  57,X'S) H   ( 571,X'S) H   ( 572,X'S) 
RIDE N   (  59,X'S) H   ( 591,X'S) 
RIDE N   (  60,X'S) H   ( 601,X'S) H   ( 602,X'S) 
RIDE N   (  61,X'S) H   ( 612,X'S) H   ( 611,X'S) 
RIDE N   (  62,X'S) H   ( 621,X'S) H   ( 622,X'S) 
RIDE N   (  64,X'S) H   ( 641,X'S) 
RIDE N   (  65,X'S) H   ( 651,X'S) H   ( 652,X'S) 
RIDE N   (  66,X'S) H   ( 661,X'S) H   ( 662,X'S) 
RIDE C   (  68,X'S) H   ( 681,X'S) 
RIDE C   (  69,X'S) H   ( 691,X'S) 
RIDE C   (  70,X'S) H   ( 701,X'S) 
RIDE C   (  71,X'S) H   ( 711,X'S) 
RIDE N   (  74,X'S) H   ( 741,X'S) H   ( 743,X'S) H   ( 742,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
REM   DELU   START (DO NOT REMOVE THIS LINE) 
VIBR .0, 0.00200 = S(1) TO C(31,2,1,0,0,-1) 
VIBR .0, 0.00200 = S(1) TO O(2) 
VIBR .0, 0.00200 = S(1) TO O(3) 
VIBR .0, 0.00200 = S(1) TO O(50) 
VIBR .0, 0.00500 = O(2) TO C(31,2,1,0,0,-1) 
VIBR .0, 0.00500 = O(3) TO C(31,2,1,0,0,-1) 
VIBR .0, 0.00500 = O(3) TO O(2) 
VIBR .0, 0.00500 = O(50) TO C(31,2,1,0,0,-1) 
VIBR .0, 0.00500 = O(50) TO O(2) 
VIBR .0, 0.00500 = O(50) TO O(3) 
VIBR .0, 0.00200 = O(3) TO NA(4) 
VIBR .0, 0.00500 = NA(4) TO S(1) 
VIBR .0, 0.00200 = NA(4) TO O(46,2,1,-1,0,-1) 
VIBR .0, 0.00200 = NA(4) TO O(5) 
VIBR .0, 0.00200 = NA(4) TO O(11) 
VIBR .0, 0.00200 = NA(4) TO O(49) 
VIBR .0, 0.00500 = O(3) TO O(46,2,1,-1,0,-1) 
VIBR .0, 0.00500 = O(5) TO O(46,2,1,-1,0,-1) 
VIBR .0, 0.00500 = O(5) TO O(3) 
VIBR .0, 0.00500 = O(11) TO O(46,2,1,-1,0,-1) 
VIBR .0, 0.00500 = O(11) TO O(3) 
VIBR .0, 0.00500 = O(11) TO O(5) 
VIBR .0, 0.00500 = O(49) TO O(46,2,1,-1,0,-1) 
VIBR .0, 0.00500 = O(49) TO O(3) 
VIBR .0, 0.00500 = O(49) TO O(5) 
VIBR .0, 0.00500 = O(49) TO O(11) 
VIBR .0, 0.00200 = O(5) TO C(6) 
VIBR .0, 0.00500 = C(6) TO NA(4) 
VIBR .0, 0.00200 = C(6) TO C(7) 
VIBR .0, 0.00200 = C(6) TO C(34) 
VIBR .0, 0.00500 = C(7) TO O(5) 
VIBR .0, 0.00500 = C(34) TO O(5) 
VIBR .0, 0.00500 = C(34) TO C(7) 
VIBR .0, 0.00200 = C(7) TO C(8) 
VIBR .0, 0.00200 = C(7) TO C(37) 
VIBR .0, 0.00500 = C(8) TO C(6) 
VIBR .0, 0.00500 = C(37) TO C(6) 
VIBR .0, 0.00500 = C(37) TO C(8) 
VIBR .0, 0.00200 = C(8) TO C(9) 
VIBR .0, 0.00500 = C(9) TO C(7) 
VIBR .0, 0.00200 = C(9) TO C(10) 
VIBR .0, 0.00200 = C(9) TO C(15) 
VIBR .0, 0.00500 = C(10) TO C(8) 
VIBR .0, 0.00500 = C(15) TO C(8) 
VIBR .0, 0.00500 = C(15) TO C(10) 
VIBR .0, 0.00200 = C(10) TO O(11) 
VIBR .0, 0.00200 = C(10) TO C(12) 
VIBR .0, 0.00500 = O(11) TO C(9) 
VIBR .0, 0.00500 = C(12) TO C(9) 
VIBR .0, 0.00500 = C(12) TO O(11) 
VIBR .0, 0.00500 = NA(4) TO C(10) 
VIBR .0, 0.00200 = C(12) TO C(13) 
VIBR .0, 0.00200 = C(12) TO C(20) 
VIBR .0, 0.00500 = C(13) TO C(10) 
VIBR .0, 0.00500 = C(20) TO C(10) 
VIBR .0, 0.00500 = C(20) TO C(13) 
VIBR .0, 0.00200 = C(13) TO C(14) 
VIBR .0, 0.00500 = C(14) TO C(12) 
VIBR .0, 0.00200 = C(14) TO C(15) 
VIBR .0, 0.00200 = C(14) TO S(16) 
VIBR .0, 0.00500 = C(15) TO C(13) 
VIBR .0, 0.00500 = S(16) TO C(13) 
VIBR .0, 0.00500 = S(16) TO C(15) 
VIBR .0, 0.00500 = C(9) TO C(14) 
VIBR .0, 0.00200 = S(16) TO O(17) 
VIBR .0, 0.00200 = S(16) TO O(18) 
VIBR .0, 0.00200 = S(16) TO O(19) 
VIBR .0, 0.00500 = O(17) TO C(14) 
VIBR .0, 0.00500 = O(18) TO C(14) 
VIBR .0, 0.00500 = O(18) TO O(17) 
VIBR .0, 0.00500 = O(19) TO C(14) 
VIBR .0, 0.00500 = O(19) TO O(17) 
VIBR .0, 0.00500 = O(19) TO O(18) 
VIBR .0, 0.00200 = C(20) TO C(21) 
VIBR .0, 0.00500 = C(21) TO C(12) 
VIBR .0, 0.00200 = C(21) TO C(22) 
VIBR .0, 0.00200 = C(21) TO C(44) 
VIBR .0, 0.00500 = C(22) TO C(20) 
VIBR .0, 0.00500 = C(44) TO C(20) 
VIBR .0, 0.00500 = C(44) TO C(22) 
VIBR .0, 0.00200 = C(22) TO O(23) 
VIBR .0, 0.00200 = C(22) TO C(24) 
VIBR .0, 0.00500 = O(23) TO C(21) 
VIBR .0, 0.00500 = C(24) TO C(21) 
VIBR .0, 0.00500 = C(24) TO O(23) 
VIBR .0, 0.00200 = C(24) TO C(25) 
VIBR .0, 0.00200 = C(24) TO C(42) 
VIBR .0, 0.00500 = C(25) TO C(22) 
VIBR .0, 0.00500 = C(42) TO C(22) 
VIBR .0, 0.00500 = C(42) TO C(25) 
VIBR .0, 0.00200 = C(25) TO C(26) 
VIBR .0, 0.00500 = C(26) TO C(24) 
VIBR .0, 0.00200 = C(26) TO C(27) 
VIBR .0, 0.00200 = C(26) TO C(32) 
VIBR .0, 0.00500 = C(27) TO C(25) 
VIBR .0, 0.00500 = C(32) TO C(25) 
VIBR .0, 0.00500 = C(32) TO C(27) 
VIBR .0, 0.00200 = C(27) TO O(28) 
VIBR .0, 0.00200 = C(27) TO C(29) 
VIBR .0, 0.00500 = O(28) TO C(26) 
VIBR .0, 0.00500 = C(29) TO C(26) 
VIBR .0, 0.00500 = C(29) TO O(28) 
VIBR .0, 0.00200 = C(29) TO C(30) 
VIBR .0, 0.00200 = C(29) TO C(33) 
VIBR .0, 0.00500 = C(30) TO C(27) 
VIBR .0, 0.00500 = C(33) TO C(27) 
VIBR .0, 0.00500 = C(33) TO C(30) 
VIBR .0, 0.00200 = C(30) TO C(31) 
VIBR .0, 0.00500 = C(31) TO C(29) 
VIBR .0, 0.00200 = C(31) TO C(32) 
VIBR .0, 0.00500 = C(30) TO S(1,2,1,-1) 
VIBR .0, 0.00500 = C(32) TO S(1,2,1,-1) 
VIBR .0, 0.00500 = C(32) TO C(30) 
VIBR .0, 0.00500 = C(26) TO C(31) 
VIBR .0, 0.00200 = C(33) TO C(34) 
VIBR .0, 0.00500 = C(34) TO C(29) 
VIBR .0, 0.00200 = C(34) TO C(35) 
VIBR .0, 0.00500 = C(6) TO C(33) 
VIBR .0, 0.00500 = C(35) TO C(33) 
VIBR .0, 0.00500 = C(35) TO C(6) 
VIBR .0, 0.00200 = C(35) TO C(36) 
VIBR .0, 0.00500 = C(36) TO C(34) 
VIBR .0, 0.00200 = C(36) TO C(37) 
VIBR .0, 0.00200 = C(36) TO S(38) 
VIBR .0, 0.00500 = C(37) TO C(35) 
VIBR .0, 0.00500 = S(38) TO C(35) 
VIBR .0, 0.00500 = S(38) TO C(37) 
VIBR .0, 0.00500 = C(36) TO C(7) 
VIBR .0, 0.00200 = S(38) TO O(39) 
VIBR .0, 0.00200 = S(38) TO O(40) 
VIBR .0, 0.00200 = S(38) TO O(41) 
VIBR .0, 0.00500 = O(39) TO C(36) 
VIBR .0, 0.00500 = O(40) TO C(36) 
VIBR .0, 0.00500 = O(40) TO O(39) 
VIBR .0, 0.00500 = O(41) TO C(36) 
VIBR .0, 0.00500 = O(41) TO O(39) 
VIBR .0, 0.00500 = O(41) TO O(40) 
VIBR .0, 0.00200 = C(42) TO C(43) 
VIBR .0, 0.00500 = C(43) TO C(24) 
VIBR .0, 0.00200 = C(43) TO C(44) 
VIBR .0, 0.00200 = C(43) TO S(45) 
VIBR .0, 0.00500 = C(44) TO C(42) 
VIBR .0, 0.00500 = S(45) TO C(42) 
VIBR .0, 0.00500 = S(45) TO C(44) 
VIBR .0, 0.00500 = C(43) TO C(21) 
VIBR .0, 0.00200 = S(45) TO O(46) 
VIBR .0, 0.00200 = S(45) TO O(47) 
VIBR .0, 0.00200 = S(45) TO O(48) 
VIBR .0, 0.00500 = O(46) TO C(43) 
VIBR .0, 0.00500 = O(47) TO C(43) 
VIBR .0, 0.00500 = O(47) TO O(46) 
VIBR .0, 0.00500 = O(48) TO C(43) 
VIBR .0, 0.00500 = O(48) TO O(46) 
VIBR .0, 0.00500 = O(48) TO O(47) 
VIBR .0, 0.00500 = S(45) TO NA(4,2) 
VIBR .0, 0.00200 = O(52) TO O(53) 
VIBR .0, 0.00200 = N(57) TO C(58) 
VIBR .0, 0.00200 = C(58) TO N(59) 
VIBR .0, 0.00200 = C(58) TO N(61) 
VIBR .0, 0.00500 = N(59) TO N(57) 
VIBR .0, 0.00500 = N(61) TO N(57) 
VIBR .0, 0.00500 = N(61) TO N(59) 
VIBR .0, 0.00200 = N(59) TO N(60) 
VIBR .0, 0.00500 = N(60) TO C(58) 
VIBR .0, 0.00200 = N(62) TO C(63) 
VIBR .0, 0.00200 = C(63) TO N(64) 
VIBR .0, 0.00200 = C(63) TO N(66) 
VIBR .0, 0.00500 = N(64) TO N(62) 
VIBR .0, 0.00500 = N(66) TO N(62) 
VIBR .0, 0.00500 = N(66) TO N(64) 
VIBR .0, 0.00200 = N(64) TO N(65) 
VIBR .0, 0.00500 = N(65) TO C(63) 
VIBR .0, 0.00200 = N(67) TO C(68) 
VIBR .0, 0.00200 = N(67) TO C(72) 
VIBR .0, 0.00500 = C(72) TO C(68) 
VIBR .0, 0.00200 = C(68) TO C(69) 
VIBR .0, 0.00500 = C(69) TO N(67) 
VIBR .0, 0.00200 = C(69) TO C(70) 
VIBR .0, 0.00500 = C(70) TO C(68) 
VIBR .0, 0.00200 = C(70) TO C(71) 
VIBR .0, 0.00500 = C(71) TO C(69) 
VIBR .0, 0.00200 = C(71) TO C(72) 
VIBR .0, 0.00500 = C(72) TO C(70) 
VIBR .0, 0.00200 = C(72) TO C(73) 
VIBR .0, 0.00500 = C(71) TO N(67) 
VIBR .0, 0.00500 = C(73) TO N(67) 
VIBR .0, 0.00500 = C(73) TO C(71) 
VIBR .0, 0.00200 = C(73) TO N(74) 
VIBR .0, 0.00500 = N(74) TO C(72) 
REM   DELU   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;