Multifunctional Vesicles from a Self-assembled Cluster-Containing Diblock Copolymer.
Voevodin, Anastasia; Campos, Luis M.; Roy, Xavier; Journal of the American Chemical Society 140 (2018) 5607–5611; doi:10.1021/jacs.8b02041

data_4132170
_publ_section_title
;
 Multifunctional Vesicles from a Self-assembled Cluster-Containing Diblock
 Copolymer.
;
_journal_issue                   16
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5607
_journal_page_last               5611
_journal_paper_doi               10.1021/jacs.8b02041
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C54 H99 Co6 N O2 P6 Se8, F6 P, 2(C H2 Cl2)'
_chemical_formula_sum            'C56 H103 Cl4 Co6 F6 N O2 P7 Se8'
_chemical_formula_weight         2280.24
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-01-26
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3461 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 90.584(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.6351(3)
_cell_length_b                   23.0852(7)
_cell_length_c                   25.6213(5)
_cell_measurement_reflns_used    10650
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      72.1890
_cell_measurement_theta_min      3.8290
_cell_volume                     8064.4(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0549
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w   -104.00 -20.00   1.00    3.00    --  -36.45 -57.00 120.00   84
  2  \w    -63.00  31.00   1.00    3.00    --  -36.45  77.00  90.00   94
  3  \w     55.00 109.00   1.00    3.00    --   36.45-178.00 -90.00   54
  4  \w      1.00  75.00   1.00    3.00    --   36.45 -99.00  60.00   74
  5  \w     57.00 109.00   1.00    3.00    --   36.45 178.00  60.00   52
  6  \w     73.00 178.00   1.00   30.00    --  111.00  15.00 -30.00  105
  7  \w     93.00 178.00   1.00   30.00    --  111.00  61.00 150.00   85
  8  \w     43.00 128.00   1.00   30.00    --  111.00 -45.00 -30.00   85
  9  \w     42.00 109.00   1.00   30.00    --  111.00 -94.00 -30.00   67
 10  \w     93.00 178.00   1.00   30.00    --  111.00  61.00-150.00   85
 11  \w     43.00 128.00   1.00   30.00    --  111.00 -45.00  60.00   85
 12  \w     43.00 113.00   1.00   30.00    --  111.00 -81.00  19.79   70
 13  \w     48.00  96.00   1.00   30.00    --  111.00 -94.00-150.00   48
 14  \w     44.00  73.00   1.00   30.00    --  111.00-111.00 -60.00   29
 15  \w     60.00  87.00   1.00   30.00    --  111.00 -43.00 -73.00   27
 16  \w     53.00  81.00   1.00   30.00    --  111.00 -67.00  70.85   28
 17  \w     85.00 131.00   1.00   30.00    --  111.00 -67.00  70.85   46
 18  \w     90.00 133.00   1.00   30.00    --  111.00  77.00-180.00   43
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0616738000
_diffrn_orient_matrix_UB_12      -0.0077926000
_diffrn_orient_matrix_UB_13      -0.0502833000
_diffrn_orient_matrix_UB_21      -0.0022153000
_diffrn_orient_matrix_UB_22      0.0662221000
_diffrn_orient_matrix_UB_23      -0.0075476000
_diffrn_orient_matrix_UB_31      0.0945433000
_diffrn_orient_matrix_UB_32      -0.0034040000
_diffrn_orient_matrix_UB_33      -0.0321318000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0817
_diffrn_reflns_av_unetI/netI     0.1000
_diffrn_reflns_Laue_measured_fraction_full 0.968
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            44055
_diffrn_reflns_point_group_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.987
_diffrn_reflns_theta_min         3.450
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    16.536
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.130
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.878
_exptl_crystal_description       irregular
_exptl_crystal_F_000             4492
_exptl_crystal_size_max          0.285
_exptl_crystal_size_mid          0.139
_exptl_crystal_size_min          0.046
_refine_diff_density_max         1.086
_refine_diff_density_min         -0.860
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1043
_refine_ls_number_reflns         15331
_refine_ls_number_restraints     541
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0782
_refine_ls_R_factor_gt           0.0566
_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^)+(0.0578P)^2^+7.5582P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1388
_refine_ls_wR_factor_ref         0.1525
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11404
_reflns_number_total             15331
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b02041_si_002.cif
_cod_data_source_block           dan3corr2
_cod_database_code               4132170
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'Co6 Se8 P7 F6 C55 N O2 H55'
_reflns_odcompleteness_completeness 93.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     73.59
_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
 P5-C53 = P5-C55 = P5-C53B = P5-C55B
 1.82 with sigma of 0.02
 C53-C54 = C55-C56 = C53B-C54B = C55B-C56B
 1.54 with sigma of 0.02
 P71-F72 = P71-F73 = P71-F74 = P71-F75 = P71-F76 = P71-F77
 1.58804 with sigma of 0.02
 P71B-F72B = P71B-F73B = P71B-F74B = P71B-F75B = P71B-F76B = P71B-F77B
 1.58804 with sigma of 0.02
 F72-F73 = F72-F74 = F72-F76 = F72-F77 = F73-F74 = F73-F75 = F73-F77 = F74-F75
 = F74-F76 = F75-F76 = F75-F77 = F76-F77
 2.245489 with sigma of 0.02
 F72B-F73B = F72B-F74B = F72B-F76B = F72B-F77B = F73B-F74B = F73B-F75B = F73B-
 F77B = F74B-F75B = F74B-F76B = F75B-F76B = F75B-F77B = F76B-F77B
 2.245489 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.1A with sigma of 0.01 and sigma
for terminal atoms of 0.01
4. Rigid body (RIGU) restrains
 P5, C53, C54, C53B, C54B, C55, C56, C55B, C56B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 P6, C61, C62, C63, C64, C65, C66, P6B, C61B, C62B, C63B, C64B, C65B, C66B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 P71, F72, F73, F74, F75, F76, F77, P71B, F72B, F73B, F74B, F75B, F76B, F77B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Same fragment restrains
{Co5, P5, C51, C52, C53B, C54B, C55, C56, C55B, C56B} sigma for 1-2: 0.02, 1-3:
0.04
as
{Co5, P5, C51, C52, C53, C54, C53B, C54B, C55, C56}
{Co2, P2, C21, C22, C23, C24, C25, C26} sigma for 1-2: 0.02, 1-3: 0.04
{Co6, P6B, C61B, C62B, C63B, C64B, C65B, C66B} sigma for 1-2: 0.02, 1-3: 0.04
as
{Co6, P6, C61, C62, C63, C64, C65, C66}
{C1_2, Cl2_2, Cl3_2}
{C1_3, Cl2_3, Cl3_3}
{C1_4, Cl2_4, Cl3_4}
{C1_5, Cl2_5, Cl3_5}
{C1_6, Cl2_6, Cl3_6}
as
{C1_1, Cl2_1, Cl3_1} sigma for 1-2: 0.02 1-3: 0.04
6. Others
 1*[Sof(C1)+Sof(H1A)+Sof(H1B)+Sof(Cl2)+Sof(Cl3)]+1*[Sof(C1)+Sof(H1A)+Sof(H1B)+
 Sof(Cl2)+Sof(Cl3)]+1*[Sof(C1)+Sof(H1A)+Sof(H1B)+Sof(Cl2)+Sof(Cl3)]+1*[Sof(C1)+
 Sof(H1A)+Sof(H1B)+Sof(Cl2)+Sof(Cl3)+Sof(Q1)+Sof(Q2)+Sof(Q3)+Sof(Q4)+Sof(Q5)+
 Sof(Q6)+Sof(Q7)+Sof(Q8)+Sof(Q9)+Sof(Q10)+Sof(Q11)+Sof(Q12)+Sof(Q13)+Sof(Q14)+
 Sof(Q15)+Sof(Q16)+Sof(Q17)+Sof(Q18)+Sof(Q19)+Sof(Q20)+Sof(Q21)+Sof(Q22)+
 Sof(Q23)+Sof(Q24)+Sof(Q25)+Sof(Q26)+Sof(Q27)+Sof(Q28)+Sof(Q29)+Sof(Q30)+
 Sof(Q31)+Sof(Q32)+Sof(Q33)+Sof(Q34)+Sof(Q35)+Sof(Q36)+Sof(Q37)+Sof(Q38)+
 Sof(Q39)+Sof(Q40)+Sof(Q41)+Sof(Q42)+Sof(Q43)+Sof(Q44)+Sof(Q45)+Sof(Q46)+
 Sof(Q47)+Sof(Q48)+Sof(Q49)+Sof(Q50)]=1 with esd of 0.001
 Sof(C53B)=Sof(H53C)=Sof(H53D)=Sof(C54B)=Sof(H54D)=Sof(H54E)=Sof(H54F)=1-FVAR(1)
 Sof(C53)=Sof(H53A)=Sof(H53B)=Sof(C54)=Sof(H54A)=Sof(H54B)=Sof(H54C)=FVAR(1)
 Sof(C55B)=Sof(H55C)=Sof(H55D)=Sof(C56B)=Sof(H56D)=Sof(H56E)=Sof(H56F)=1-FVAR(2)
 Sof(C55)=Sof(H55A)=Sof(H55B)=Sof(C56)=Sof(H56A)=Sof(H56B)=Sof(H56C)=FVAR(2)
 Sof(P6B)=Sof(C61B)=Sof(H61C)=Sof(H61D)=Sof(C62B)=Sof(H62D)=Sof(H62E)=
 Sof(H62F)=Sof(C63B)=Sof(H63C)=Sof(H63D)=Sof(C64B)=Sof(H64D)=Sof(H64E)=
 Sof(H64F)=Sof(C65B)=Sof(H65C)=Sof(H65D)=Sof(C66B)=Sof(H66D)=Sof(H66E)=
 Sof(H66F)=1-FVAR(3)
 Sof(P6)=Sof(C61)=Sof(H61A)=Sof(H61B)=Sof(C62)=Sof(H62A)=Sof(H62B)=Sof(H62C)=
 Sof(C63)=Sof(H63A)=Sof(H63B)=Sof(C64)=Sof(H64A)=Sof(H64B)=Sof(H64C)=Sof(C65)=
 Sof(H65A)=Sof(H65B)=Sof(C66)=Sof(H66A)=Sof(H66B)=Sof(H66C)=FVAR(3)
 Sof(P71B)=Sof(F72B)=Sof(F73B)=Sof(F74B)=Sof(F75B)=Sof(F76B)=Sof(F77B)=Sof(C1)=
 Sof(H1A)=Sof(H1B)=Sof(Cl2)=Sof(Cl3)=1-FVAR(4)
 Sof(P71)=Sof(F72)=Sof(F73)=Sof(F74)=Sof(F75)=Sof(F76)=Sof(F77)=Sof(C1)=
 Sof(H1A)=Sof(H1B)=Sof(Cl2)=Sof(Cl3)=FVAR(4)
 1(DFIX)=1(DFIX)=FVAR(5)
 1(DFIX)=1(DFIX)=1.414*FVAR(6)
 Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(Cl2)=Sof(Cl3)=FVAR(6)
 Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(Cl2)=Sof(Cl3)=FVAR(7)
 Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(Cl2)=Sof(Cl3)=FVAR(8)
 Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(Cl2)=Sof(Cl3)=Sof(Q1)=Sof(Q2)=Sof(Q3)=Sof(Q4)=
 Sof(Q5)=Sof(Q6)=Sof(Q7)=Sof(Q8)=Sof(Q9)=Sof(Q10)=Sof(Q11)=Sof(Q12)=Sof(Q13)=
 Sof(Q14)=Sof(Q15)=Sof(Q16)=Sof(Q17)=Sof(Q18)=Sof(Q19)=Sof(Q20)=Sof(Q21)=
 Sof(Q22)=Sof(Q23)=Sof(Q24)=Sof(Q25)=Sof(Q26)=Sof(Q27)=Sof(Q28)=Sof(Q29)=
 Sof(Q30)=Sof(Q31)=Sof(Q32)=Sof(Q33)=Sof(Q34)=Sof(Q35)=Sof(Q36)=Sof(Q37)=
 Sof(Q38)=Sof(Q39)=Sof(Q40)=Sof(Q41)=Sof(Q42)=Sof(Q43)=Sof(Q44)=Sof(Q45)=
 Sof(Q46)=Sof(Q47)=Sof(Q48)=Sof(Q49)=Sof(Q50)=FVAR(9)
7.a Ternary CH refined with riding coordinates:
 C119(H119), C120(H120), C123(H123), C125(H125)
7.b Secondary CH2 refined with riding coordinates:
 C113(H11A,H11B), C114(H11C,H11D), C115(H11E,H11F), C124(H12A,H12B), C21(H21A,
 H21B), C23(H23A,H23B), C25(H25A,H25B), C31(H31A,H31B), C33(H33A,H33B),
 C35(H35A,H35B), C41(H41A,H41B), C43(H43A,H43B), C45(H45A,H45B), C51(H51A,H51B),
  C53(H53A,H53B), C53B(H53C,H53D), C55(H55A,H55B), C55B(H55C,H55D), C61(H61A,
 H61B), C63(H63A,H63B), C65(H65A,H65B), C61B(H61C,H61D), C63B(H63C,H63D),
 C65B(H65C,H65D), C1(H1A,H1B), C1(H1A,H1B), C1(H1A,H1B), C1(H1A,H1B), C1(H1A,
 H1B), C1(H1A,H1B)
7.c Me refined with riding coordinates:
 C54B(H54D,H54E,H54F), C56B(H56D,H56E,H56F), C62(H62A,H62B,H62C), C64(H64A,
 H64B,H64C), C66(H66A,H66B,H66C), C62B(H62D,H62E,H62F), C64B(H64D,H64E,H64F),
 C66B(H66D,H66E,H66F)
7.d Aromatic/amide H refined with riding coordinates:
 C102(H102), C103(H103), C104(H104), C105(H105), C106(H106), C108(H108),
 C109(H109), C110(H110), C111(H111), C112(H112), C121(H121), C122(H122)
7.e Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C32(H32A,H32B,
 H32C), C34(H34A,H34B,H34C), C36(H36A,H36B,H36C), C42(H42A,H42B,H42C), C44(H44A,
 H44B,H44C), C46(H46A,H46B,H46C), C52(H52A,H52B,H52C), C54(H54A,H54B,H54C),
 C56(H56A,H56B,H56C)
;
_shelx_res_checksum              95522
_shelx_hkl_checksum              16237
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.998
_oxdiff_exptl_absorpt_empirical_full_min 0.642