Multifunctional single-layered vesicles derived from Cu(ii)-metal-organic-polyhedra.
Sarkar, Koushik; Paul, Mithun; Dastidar, Parthasarathi; Chemical communications (Cambridge, England) 52 (2016) 13124–13127; doi:10.1039/c6cc07804d

data_7125243
_publ_section_title
;
 Multifunctional single-layered vesicles derived from
 Cu(ii)-metal-organic-polyhedra.
;
_journal_issue                   89
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              13124
_journal_page_last               13127
_journal_paper_doi               10.1039/c6cc07804d
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety         'C264 H288 Cl6 Cu6 N48 O24, 6(N O3), 6(H2O)'
_chemical_formula_sum            'C264 H300 Cl6 Cu6 N54 O48'
_chemical_formula_weight         5591.59
_chemical_name_systematic        MOP1
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-05-02
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-07-25 deposited with the CCDC.
2016-10-13 downloaded from the CCDC.
;
_cell_angle_alpha                118.745(2)
_cell_angle_beta                 91.861(2)
_cell_angle_gamma                118.748(2)
_cell_formula_units_Z            1
_cell_length_a                   24.331(3)
_cell_length_b                   24.388(3)
_cell_length_c                   24.415(3)
_cell_measurement_reflns_used    9939
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      23.51
_cell_measurement_theta_min      2.31
_cell_volume                     10460(2)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      120.0
_diffrn_measured_fraction_theta_full 0.455
_diffrn_measured_fraction_theta_max 0.553
_diffrn_measurement_device_type  'Bruker CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0600
_diffrn_reflns_av_unetI/netI     0.1594
_diffrn_reflns_Laue_measured_fraction_full 0.455
_diffrn_reflns_Laue_measured_fraction_max 0.553
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            33387
_diffrn_reflns_point_group_measured_fraction_full 0.455
_diffrn_reflns_point_group_measured_fraction_max 0.553
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         23.542
_diffrn_reflns_theta_min         1.669
_exptl_absorpt_coefficient_mu    0.392
_exptl_absorpt_correction_T_max  0.7449
_exptl_absorpt_correction_T_min  0.4777
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.1712 before and 0.0853 after correction.
The Ratio of minimum to maximum transmission is 0.6413.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    0.886
_exptl_crystal_description       block
_exptl_crystal_F_000             2910
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.300
_refine_diff_density_min         -0.343
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.977
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1714
_refine_ls_number_reflns         17221
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.979
_refine_ls_R_factor_all          0.1350
_refine_ls_R_factor_gt           0.0823
_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^)+(0.1367P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2204
_refine_ls_wR_factor_ref         0.2475
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9236
_reflns_number_total             17221
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc07804d3.cif
_cod_data_source_block           MOP-TO-1
_cod_original_cell_volume        10461(2)
_cod_database_code               7125243
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   /
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 H45B-H40A
 2 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C102(H10A,H10B), C43(H43A,H43B), C121(H12A,H12B), C123(H12C,H12D), C67(H67A,
 H67B), C69(H69A,H69B), C41(H41A,H41B), C68(H68A,H68B), C72(H72A,H72B),
 C40(H40A,H40B), C14(H14A,H14B), C125(H12H,H12I), C9(H9A,H9B), C42(H42A,H42B),
 C101(H10C,H10D), C70(H70A,H70B), C8(H8A,H8B), C100(H10E,H10F), C74(H74A,H74B),
 C7(H7A,H7B), C47(H47A,H47B), C45(H45A,H45B), C10(H10G,H10H), C12(H12P,H12Q)
3.b Aromatic/amide H refined with riding coordinates:
 N3(H3), N20(H20), N14(H14), N18(H18), N2(H2), N22(H22), N16(H16), N12(H12),
 N23(H23), N10(H10), N5(H5), C30(H30), N8(H8), C60(H60), C79(H79), C51(H51),
 C117(H117), C53(H53), C21(H21), C118(H118), C120(H120), C20(H20A), C54(H54),
 C52(H52), C87(H87), C119(H119), C58(H58), C18(H18A), C78(H78), C59(H59),
 C80(H80), C81(H81), C31(H31), C84(H84), C129(H129), C114(H114), C111(H111),
 C131(H131), C108(H108), C24(H24), C27(H27), C57(H57), C33(H33), C106(H106),
 C32(H32), C105(H105), C85(H85), C132(H132), C93(H93), C26(H26), C92(H92),
 C130(H130), C107(H107), C113(H113), C25(H25), C90(H90), C112(H112), C86(H86),
 C19(H19), C91(H91)
3.c Idealised Me refined as rotating group:
 C75(H75A,H75B,H75C), C122(H12E,H12F,H12G), C15(H15A,H15B,H15C), C46(H46A,H46B,
 H46C), C124(H12J,H12K,H12L), C73(H73A,H73B,H73C), C71(H71A,H71B,H71C),
 C44(H44A,H44B,H44C), C48(H48A,H48B,H48C), C126(H12M,H12N,H12O), C13(H13A,H13B,
 H13C), C11(H11A,H11B,H11C)
;
_shelx_res_checksum              95131
_shelx_fab_checksum              72959
_olex2_submission_special_instructions 'No special instructions were received'