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_4513248
_publ_section_title
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 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 O16.5 S4, 2(C6 H9 N2), 2(C H7 N4)'
_chemical_formula_sum            'C42 H51 N12 Na O16.5 S4'
_chemical_formula_weight         1139.22
_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                 102.545(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.6234(9)
_cell_length_b                   14.1631(8)
_cell_length_c                   20.9416(11)
_cell_measurement_reflns_used    8106
_cell_measurement_temperature    175
_cell_measurement_theta_max      28.6280
_cell_measurement_theta_min      1.9140
_cell_volume                     4812.8(5)
_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 0.994
_diffrn_measured_fraction_theta_max 0.854
_diffrn_measurement_details
;
  1 omega   35.00   78.00   1.0000  388.2300
omega____ theta____ kappa____ phi______ frames
    -       17.9231  179.0000 -180.0000 43

  2 omega  -46.00   60.00   1.0000  388.2300
omega____ theta____ kappa____ phi______ frames
    -       17.9231  -19.0000  120.0000 106

  3 omega   -2.00   77.00   1.0000  388.2300
omega____ theta____ kappa____ phi______ frames
    -       17.9231   38.0000  -30.0000 79

  4 omega  -26.00   -1.00   1.0000  388.2300
omega____ theta____ kappa____ phi______ frames
    -       17.9231   19.0000 -180.0000 25

;
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0045699000
_diffrn_orient_matrix_UB_12      -0.0194199000
_diffrn_orient_matrix_UB_13      0.0302280000
_diffrn_orient_matrix_UB_21      -0.0365214000
_diffrn_orient_matrix_UB_22      0.0267627000
_diffrn_orient_matrix_UB_23      -0.0018733000
_diffrn_orient_matrix_UB_31      -0.0235700000
_diffrn_orient_matrix_UB_32      -0.0376444000
_diffrn_orient_matrix_UB_33      -0.0169047000
_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  0.100
_diffrn_reflns_av_sigmaI/netI    0.0886
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            24273
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.109
_diffrn_reflns_theta_min         1.749
_exptl_absorpt_coefficient_mu    0.293
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86647
_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            yellow
_exptl_crystal_density_diffrn    1.572
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2376
_exptl_crystal_size_max          0.550
_exptl_crystal_size_mid          0.500
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.96
_refine_diff_density_min         -1.37
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0444
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     685
_refine_ls_number_reflns         7545
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1225
_refine_ls_R_factor_gt           0.0820
_refine_ls_shift/su_max          0.0008942
_refine_ls_shift/su_mean         0.0000343
_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: 
 8.44 5.92 6.28 1.57 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1217
_refine_ls_wR_factor_gt          0.0955
_refine_ls_wR_factor_ref         0.0955
_reflns_limit_h_max              20
_reflns_limit_h_min              -21
_reflns_limit_k_max              19
_reflns_limit_k_min              0
_reflns_limit_l_max              26
_reflns_limit_l_min              0
_reflns_number_gt                7545
_reflns_number_total             11049
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.99
_oxford_diffrn_Wilson_scale      1.16
_oxford_refine_ls_r_factor_ref   0.0820
_oxford_refine_ls_scale          1.020(3)
_oxford_reflns_number_all        11049
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_cod_data_source_file            cg5b00596_si_002.cif
_cod_data_source_block           1
_cod_depositor_comments
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Adding full bibliography for 4513247--4513249.cif.

2024-02-12
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
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_cod_original_formula_sum            'C84 H102 N24 Na2 O33 S8'
_cod_original_formula_weight         2278.44
_cod_original_formula_moiety    'C56 H38 Na2 O33 S8, 4(C6 H9 N2), 4(C H7 N4)'
_cod_original_formula_units_Z            2
_cod_original_cell_volume        4812.7(5)
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_database_code               4513248
_cell_oxdiff_length_a            16.6243(8)
_cell_oxdiff_length_b            14.1564(8)
_cell_oxdiff_length_c            20.9485(10)
_cell_oxdiff_angle_alpha         89.981(4)
_cell_oxdiff_angle_beta          102.524(4)
_cell_oxdiff_angle_gamma         89.969(4)
_cell_oxdiff_volume              4812.7(4)
_montpellier_reflns_maxres       0.73
_montpellier_reflns_completeness_maxres 85.52
_montpellier_reflns_redundancy_maxres 2.17
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
RIDE C   (   6,X'S) H   (  61,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) H   ( 122,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   (  28,X'S) H   ( 281,X'S) 
RIDE O   (  31,X'S) H   ( 311,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) H   ( 352,X'S) 
RIDE O   (  38,X'S) H   ( 381,X'S) 
RIDE C   (  40,X'S) H   ( 401,X'S) H   ( 402,X'S) 
RIDE C   (  41,X'S) H   ( 411,X'S) 
RIDE C   (  43,X'S) H   ( 431,X'S) 
RIDE O   (  50,X'S) H   ( 501,X'S) H   ( 502,X'S) 
RIDE N   (  51,X'S) H   ( 511,X'S) H   ( 513,X'S) H   ( 512,X'S) 
RIDE C   (  52,X'S) H   ( 521,X'S) H   ( 522,X'S) 
RIDE C   (  55,X'S) H   ( 551,X'S) 
RIDE C   (  56,X'S) H   ( 561,X'S) 
RIDE C   (  57,X'S) H   ( 571,X'S) 
RIDE C   (  58,X'S) H   ( 581,X'S) 
RIDE N   (  59,X'S) H   ( 593,X'S) H   ( 592,X'S) H   ( 591,X'S) 
RIDE C   (  60,X'S) H   ( 602,X'S) H   ( 601,X'S) 
RIDE C   (  63,X'S) H   ( 631,X'S) 
RIDE C   (  64,X'S) H   ( 641,X'S) 
RIDE C   (  65,X'S) H   ( 651,X'S) 
RIDE C   (  66,X'S) H   ( 661,X'S) 
RIDE N   (  67,X'S) H   ( 672,X'S) H   ( 671,X'S) 
RIDE N   (  69,X'S) H   ( 691,X'S) 
RIDE N   (  70,X'S) H   ( 701,X'S) H   ( 702,X'S) 
RIDE N   (  71,X'S) H   ( 711,X'S) H   ( 712,X'S) 
RIDE N   (  72,X'S) H   ( 721,X'S) H   ( 722,X'S) 
RIDE N   (  74,X'S) H   ( 742,X'S) H   ( 741,X'S) 
RIDE N   (  75,X'S) H   ( 751,X'S) 
RIDE N   (  76,X'S) H   ( 762,X'S) H   ( 761,X'S) 
END                                                                             
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_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
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