Biomimetic Self-Assembly of Co<sup>II</sup>-Seamed Hexameric Metal-Organic Nanocapsules.
Hu, Xiangquan; Chai, Jie; Zhang, Chen; Lang, Jinxin; Kelley, Steven P.; Feng, Sisi; Liu, Bin; Atwood, David A.; Atwood, Jerry L.; Journal of the American Chemical Society 141 (2019) 9151–9154; doi:10.1021/jacs.9b02857

data_4127269
_publ_section_title
;
 Biomimetic Self-Assembly of Co<sup>II</sup>-Seamed Hexameric
 Metal-Organic Nanocapsules.
;
_journal_issue                   23
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9151
_journal_page_last               9154
_journal_paper_doi               10.1021/jacs.9b02857
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         '0.5(C576 H132 Co36 N16 O196), 5(O)'
_chemical_formula_sum            'C288 H378 Co18 N8 O103'
_chemical_formula_weight         6660.70
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-03-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 116.955(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   27.458(3)
_cell_length_b                   36.623(4)
_cell_length_c                   21.558(3)
_cell_measurement_reflns_used    9192
_cell_measurement_temperature    100
_cell_measurement_theta_max      24.80
_cell_measurement_theta_min      2.29
_cell_volume                     19324(4)
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX II area detector'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1064
_diffrn_reflns_av_unetI/netI     0.0431
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            96177
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        18.914
_diffrn_reflns_theta_max         18.914
_diffrn_reflns_theta_min         2.224
_diffrn_source                   'Sealed Source Mo with TRIUMPH optics'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.820
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6155
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker AXScale'
_exptl_crystal_colour            'clear reddish violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.145
_exptl_crystal_description       needle
_exptl_crystal_F_000             6944
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.395
_refine_diff_density_min         -0.610
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.627
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     807
_refine_ls_number_reflns         7820
_refine_ls_number_restraints     737
_refine_ls_restrained_S_all      1.567
_refine_ls_R_factor_all          0.1530
_refine_ls_R_factor_gt           0.1176
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3582
_refine_ls_wR_factor_ref         0.3891
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5505
_reflns_number_total             7820
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b02857_si_002.cif
_cod_data_source_block           s1_a_sq
_cod_depositor_comments          'Adding full bibliography for 4127269.cif.'
_cod_database_code               4127269
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.937
_shelx_estimated_absorpt_t_min   0.866
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 N2S-C5S
 1.4 with sigma of 0.02
 C4S-N2S
 1.4 with sigma of 0.02
 C4S-O2S
 1.2 with sigma of 0.02
 C1AA-C7AA = C7AA-C5AA = C5AA-C3AA = C54-C53 = C53-C52 = C52-C51 = C3AA-C60 =
 C30-C29 = C31-C30 = C32-C31 = C32-C33 = C41-C40 = C42-C41 = C43-C42 = C44-C43 =
  C8-C7 = C9-C8 = C10-C9 = C11-C10 = C19-C18 = C20-C19 = C21-C20 = C22-C21
 1.54 with sigma of 0.02
 C16-C17 \\sim C16-C15 \\sim C15-C14 \\sim C17-C12 \\sim C13-C12 \\sim C14-C13
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: Co4A(0.8) Co1B(0.2) Co2'(0.25) Co1'(0.125) O5(0.91) O8(0.92)
 O2(0.92) Co1A(0.175) Co2(0.75) Co4B(0.2) O12(0.25) C55(0.5) C55'(0.5)
5.a Ternary CH refined with riding coordinates:
 C7(H7), C29(H29), C40(H40)
5.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C19(H19A,H19B), C30(H30A,H30B), C3AA(H3AA,H3AB)
5.c Aromatic/amide H refined with riding coordinates:
 C49(H49), C28(H28), C5(H5), C39(H39), C64(H64), C17(H17)
;
_shelx_res_checksum              99492
_shelx_hkl_checksum              42957
_shelx_fab_checksum              85324
_olex2_submission_special_instructions 'No special instructions were received'