An Interconverting Family of Coordination Cages and a meso-Helicate; Effects of Temperature, Concentration, and Solvent on the Product Distribution of a Self-Assembly Process.
Cullen, William; Hunter, Christopher A.; Ward, Michael D.; Inorganic chemistry 54 (2015) 2626–2637; doi:10.1021/ic502780b

data_4342488
_publ_section_title
;
 An Interconverting Family of Coordination Cages and a meso-Helicate;
 Effects of Temperature, Concentration, and Solvent on the Product
 Distribution of a Self-Assembly Process.
;
_journal_issue                   6
_journal_name_full               'Inorganic chemistry'
_journal_page_first              2626
_journal_page_last               2637
_journal_paper_doi               10.1021/ic502780b
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety
'C540 H468 Co12 N108 O36, 24(B1 F4), 1.5(H2O)'
_chemical_formula_sum            'C540 H471 B24 Co12 F96 N108 O37.5'
_chemical_formula_weight         11863.82
_chemical_name_common            M12L18OH
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2014-10-06
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   44.705(9)
_cell_length_b                   44.705(9)
_cell_length_c                   68.621(14)
_cell_measurement_reflns_used    62572
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.1
_cell_measurement_theta_min      2.3
_cell_volume                     118768(4)
_computing_data_collection
'CrystalClear-SM Expert 3.1 b27 (Rigaku, 2012)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.492
_diffrn_measured_fraction_theta_max 0.506
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_unetI/netI     0.0544
_diffrn_reflns_Laue_measured_fraction_full 0.492
_diffrn_reflns_Laue_measured_fraction_max 0.506
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_h_min       -52
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -53
_diffrn_reflns_limit_l_max       63
_diffrn_reflns_limit_l_min       -81
_diffrn_reflns_point_group_measured_fraction_full 0.492
_diffrn_reflns_point_group_measured_fraction_max 0.506
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.008
_diffrn_reflns_theta_min         2.312
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    0.319
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.599
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    0.995
_exptl_crystal_description       block
_exptl_crystal_F_000             36450
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.284
_refine_diff_density_min         -0.694
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.839
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1767
_refine_ls_number_reflns         23528
_refine_ls_number_restraints     2282
_refine_ls_restrained_S_all      1.806
_refine_ls_R_factor_all          0.2453
_refine_ls_R_factor_gt           0.1991
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4972
_refine_ls_wR_factor_ref         0.5222
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14043
_reflns_number_total             23528
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic502780b_si_004.cif
_cod_data_source_block           2013ncs0814
_cod_depositor_comments
'Adding full bibliography for 4342486--4342489.cif.'
_cod_original_cell_volume        118768(54)
_cod_original_formula_sum        'C540 H471 B24 Co12 F96 N108 O37.50'
_cod_database_code               4342488
_shelxl_version_number           2013-4
_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 O(H) groups
2. Shared sites
{C17B, C18B}
3. Restrained distances
 C17A-C13A \\sim C17A-C15A
 with sigma of 0.02
 C37A-C33A \\sim C37A-C35A
 with sigma of 0.02
 C17B-C13B \\sim C17B-C15B
 with sigma of 0.02
 C37B-C33B \\sim C37B-C35B
 with sigma of 0.02
 C17C-C13C \\sim C17C-C15C
 with sigma of 0.02
 C37C-C33C \\sim C37C-C35C
 with sigma of 0.02
 C17D-C13D \\sim C17D-C15D
 with sigma of 0.02
 C37D-C33D \\sim C37D-C35D
 with sigma of 0.02
 C17E-C13E \\sim C17E-C15E
 with sigma of 0.02
 C17F-C13F \\sim C17F-C15F
 with sigma of 0.02
 C17G-C13G \\sim C17G-C15G
 with sigma of 0.02
 C14A-C17A \\sim C14B-C17B \\sim C14C-C17C \\sim C14D-C17D
 with sigma of 0.02
 C14E-C17E \\sim C14F-C17F \\sim C14G-C17G
 with sigma of 0.02
 C34A-C37A \\sim C34B-C37B \\sim C34C-C37C \\sim C34D-C37D
 with sigma of 0.02
 B1-F1 \\sim B1-F2
 with sigma of 0.02
 B2-F5 \\sim B2-F6 \\sim B2-F7 \\sim B2-F8
 with sigma of 0.02
 F5-F6 \\sim F5-F7 \\sim F5-F8 \\sim F6-F7 \\sim F6-F8 \\sim F7-F8
 with sigma of 0.02
4. Restrained planarity
 C17A, C13A, C14A, C15A
 with sigma of 0.1
 C37A, C33A, C34A, C35A
 with sigma of 0.1
 C17B, C13B, C14B, C15B
 with sigma of 0.1
 C37B, C33B, C34B, C35B
 with sigma of 0.1
 C17C, C13C, C14C, C15C
 with sigma of 0.1
 C37C, C33C, C34C, C35C
 with sigma of 0.1
 C17D, C13D, C14D, C15D
 with sigma of 0.1
 C37D, C33D, C34D, C35D
 with sigma of 0.1
 C17E, C13E, C17E, C15E
 with sigma of 0.1
 C17F, C13F, C14F, C15F
 with sigma of 0.1
 C17G, C13G, C14G, C15G
 with sigma of 0.1
5. Rigid bond restraints
 C12A, C13A, C14A, C15A, C16A, C17A, C23A, C24A, C25A, C26A, C32A, C33A, C34A,
 C35A, C36A, C37A, C43A, C44A, C45A, C46A, C51A, C52A, C53A, C54A, C55A, C56A,
 C57A, C58A, C59A, C60A, C12B, C13B, C14B, C15B, C16B, C17B, C18B, C23B, C24B,
 C25B, C26B, C32B, C33B, C34B, C35B, C36B, C37B, C43B, C44B, C45B, C46B, C51B,
 C52B, C53B, C54B, C55B, C56B, C57B, C58B, C59B, C60B, C12C, C13C, C14C, C15C,
 C16C, C17C, C23C, C24C, C25C, C26C, C32C, C33C, C34C, C35C, C36C, C37C, C43C,
 C44C, C45C, C46C, C51C, C52C, C53C, C54C, C55C, C56C, C57C, C58C, C59C, C60C,
 C12D, C13D, C14D, C15D, C16D, C17D, C23D, C24D, C25D, C26D, C32D, C33D, C34D,
 C35D, C36D, C37D, C43D, C44D, C45D, C46D, C51D, C52D, C53D, C54D, C55D, C56D,
 C57D, C58D, C59D, C60D, C12E, C13E, C14E, C15E, C16E, C17E, C23E, C24E, C25E,
 C26E, C43E, C44E, C45E, C46E, C51E, C52E, C53E, C54E, C55E, C56E, C57E, C58E,
 C59E, C60E, C12F, C13F, C14F, C15F, C16F, C17F, C23F, C24F, C25F, C26F, C46F,
 C51F, C52F, C53F, C54F, C55F, C56F, C57F, C58F, C59F, C60F, C12G, C13G, C14G,
 C15G, C16G, C17G, C23G, C24G, C25G, C12H, C13H, C14H, C15H, C16H, C17H, N11A,
 N21A, N22A, N31A, N41A, N42A, N11B, N21B, N22B, N31B, N41B, N42B, N11C, N21C,
 N22C, N31C, N41C, N42C, N11D, N21D, N22D, N31D, N41D, N42D, N11E, N21E, N22E,
 N41E, N42E, N11F, N21F, N22F, N11G, N22G, N21G, N11H, B1, B2, F1, F2, F5, F6,
 F7, F8, O18A, O38A, O18B, O19B, O38B, O18C, O38C, O18D, O38D, O18E, O18F, O18G,
  O18H, O36
 with sigma for 1-2 distances of 0.003 and sigma for 1-3 distances of 0.006
6. Uiso/Uaniso restraints and constraints
C12A \\sim C13A \\sim C14A \\sim C15A \\sim C16A \\sim C17A \\sim C23A \\sim
C24A \\sim C25A \\sim C26A \\sim C32A \\sim C33A \\sim C34A \\sim C35A \\sim
C36A \\sim C37A \\sim C43A \\sim C44A \\sim C45A \\sim C46A \\sim C51A \\sim
C52A \\sim C53A \\sim C54A \\sim C55A \\sim C56A \\sim C57A \\sim C58A \\sim
C59A \\sim C60A \\sim C12B \\sim C13B \\sim C14B \\sim C15B \\sim C16B \\sim
C17B \\sim C18B \\sim C23B \\sim C24B \\sim C25B \\sim C26B \\sim C32B \\sim
C33B \\sim C34B \\sim C35B \\sim C36B \\sim C37B \\sim C43B \\sim C44B \\sim
C45B \\sim C46B \\sim C51B \\sim C52B \\sim C53B \\sim C54B \\sim C55B \\sim
C56B \\sim C57B \\sim C58B \\sim C59B \\sim C60B \\sim C12C \\sim C13C \\sim
C14C \\sim C15C \\sim C16C \\sim C17C \\sim C23C \\sim C24C \\sim C25C \\sim
C26C \\sim C32C \\sim C33C \\sim C34C \\sim C35C \\sim C36C \\sim C37C \\sim
C43C \\sim C44C \\sim C45C \\sim C46C \\sim C51C \\sim C52C \\sim C53C \\sim
C54C \\sim C55C \\sim C56C \\sim C57C \\sim C58C \\sim C59C \\sim C60C \\sim
C12D \\sim C13D \\sim C14D \\sim C15D \\sim C16D \\sim C17D \\sim C23D \\sim
C24D \\sim C25D \\sim C26D \\sim C32D \\sim C33D \\sim C34D \\sim C35D \\sim
C36D \\sim C37D \\sim C43D \\sim C44D \\sim C45D \\sim C46D \\sim C51D \\sim
C52D \\sim C53D \\sim C54D \\sim C55D \\sim C56D \\sim C57D \\sim C58D \\sim
C59D \\sim C60D \\sim C12E \\sim C13E \\sim C14E \\sim C15E \\sim C16E \\sim
C17E \\sim C23E \\sim C24E \\sim C25E \\sim C26E \\sim C43E \\sim C44E \\sim
C45E \\sim C46E \\sim C51E \\sim C52E \\sim C53E \\sim C54E \\sim C55E \\sim
C56E \\sim C57E \\sim C58E \\sim C59E \\sim C60E \\sim C12F \\sim C13F \\sim
C14F \\sim C15F \\sim C16F \\sim C17F \\sim C23F \\sim C24F \\sim C25F \\sim
C26F \\sim C46F \\sim C51F \\sim C52F \\sim C53F \\sim C54F \\sim C55F \\sim
C56F \\sim C57F \\sim C58F \\sim C59F \\sim C60F \\sim C12G \\sim C13G \\sim
C14G \\sim C15G \\sim C16G \\sim C17G \\sim C23G \\sim C24G \\sim C25G \\sim
C12H \\sim C13H \\sim C14H \\sim C15H \\sim C16H \\sim C17H \\sim N11A \\sim
N21A \\sim N22A \\sim N31A \\sim N41A \\sim N42A \\sim N11B \\sim N21B \\sim
N22B \\sim N31B \\sim N41B \\sim N42B \\sim N11C \\sim N21C \\sim N22C \\sim
N31C \\sim N41C \\sim N42C \\sim N11D \\sim N21D \\sim N22D \\sim N31D \\sim
N41D \\sim N42D \\sim N11E \\sim N21E \\sim N22E \\sim N41E \\sim N42E \\sim
N11F \\sim N21F \\sim N22F \\sim N11G \\sim N22G \\sim N21G \\sim N11H \\sim B1
\\sim B2 \\sim F1 \\sim F2 \\sim F5 \\sim F6 \\sim F7 \\sim F8 \\sim O18A \\sim
O38A \\sim O18B \\sim O19B \\sim O38B \\sim O18C \\sim O38C \\sim O18D \\sim
O38D \\sim O18E \\sim O18F \\sim O18G \\sim O18H \\sim O36: within 1.7A with
sigma of 0.003 and sigma for terminal atoms of 0.006
Uanis(C17B) = Uanis(C18B)
7. Others
 Sof(C18B)=Sof(H18C)=Sof(H18D)=Sof(O19B)=Sof(H19B)=1-FVAR(1)
 Sof(C17B)=Sof(H17C)=Sof(H17D)=Sof(O18B)=Sof(H18B)=FVAR(1)
 Fixed Sof: O36(0.5)
8.a Secondary CH2 refined with riding coordinates:
 C17A(H17A,H17B), C26A(H26A,H26B), C37A(H37A,H37B), C46A(H46A,H46B), C17B(H17C,
 H17D), C18B(H18C,H18D), C26B(H26C,H26D), C37B(H37C,H37D), C46B(H46C,H46D),
 C17C(H17E,H17F), C26C(H26E,H26F), C37C(H37E,H37F), C46C(H46E,H46F), C17D(H17G,
 H17H), C26D(H26G,H26H), C37D(H37G,H37H), C46D(H46G,H46H), C17E(H17I,H17J),
 C26E(H26I,H26J), C46E(H46I,H46J), C17F(H17K,H17L), C26F(H26K,H26L), C46F(H46K,
 H46L), C17G(H17M,H17N), C17H(H17O,H17P)
8.b Aromatic/amide H refined with riding coordinates:
 C12A(H12A), C13A(H13A), C15A(H15A), C24A(H24A), C25A(H25A), C32A(H32A),
 C33A(H33A), C35A(H35A), C44A(H44A), C45A(H45A), C52A(H52A), C53A(H53A),
 C54A(H54A), C58A(H58A), C59A(H59A), C60A(H60A), C12B(H12B), C13B(H13B),
 C15B(H15B), C24B(H24B), C25B(H25B), C32B(H32B), C33B(H33B), C35B(H35B),
 C44B(H44B), C45B(H45B), C52B(H52B), C53B(H53B), C58B(H58B), C59B(H59B),
 C60B(H60B), C12C(H12C), C13C(H13C), C15C(H15C), C24C(H24C), C25C(H25C),
 C32C(H32C), C33C(H33C), C35C(H35C), C44C(H44C), C45C(H45C), C52C(H52C),
 C54C(H54C), C58C(H58C), C59C(H59C), C60C(H60C), C12D(H12D), C13D(H13D),
 C15D(H15D), C24D(H24D), C25D(H25D), C32D(H32D), C33D(H33D), C35D(H35D),
 C44D(H44D), C45D(H45D), C52D(H52D), C53D(H53D), C54D(H54D), C58D(H58D),
 C59D(H59D), C60D(H60D), C12E(H12E), C13E(H13E), C15E(H15E), C24E(H24E),
 C25E(H25E), C44E(H44E), C45E(H45E), C52E(H52E), C53E(H53E), C54E(H54E),
 C58E(H58E), C59E(H59E), C60E(H60E), C12F(H12F), C13F(H13F), C15F(H15F),
 C24F(H24F), C25F(H25F), C52F(H52F), C53F(H53F), C54F(H54F), C58F(H58F),
 C59F(H59F), C60F(H60F), C12G(H12G), C13G(H13G), C15G(H15G), C24G(H24G),
 C25G(H25G), C12H(H12H), C13H(H13H), C15H(H15H)
8.c Fitted pentagon refined as free rotating group:
 N21A(N22A,C23A,C24A,C25A), N41A(N42A,C43A,C44A,C45A), N21B(N22B,C23B,C24B,
 C25B), N41B(N42B,C43B,C44B,C45B), N21C(N22C,C23C,C24C,C25C), N41C(N42C,C43C,
 C44C,C45C), N21D(N22D,C23D,C24D,C25D), N41D(N42D,C43D,C44D,C45D), N21E(N22E,
 C23E,C24E,C25E), N41E(N42E,C43E,C44E,C45E), N21F(N22F,C23F,C24F,C25F),
 N22G(N21G,C23G,C24G,C25G)
8.d Fitted hexagon refined as free rotating group:
 N11A(C12A,C13A,C14A,C15A,C16A), N31A(C32A,C33A,C34A,C35A,C36A), N11B(C12B,
 C13B,C14B,C15B,C16B), N31B(C32B,C33B,C34B,C35B,C36B), N11C(C12C,C13C,C14C,C15C,
 C16C), N31C(C32C,C33C,C34C,C35C,C36C), N11D(C12D,C13D,C14D,C15D,C16D),
 N31D(C32D,C33D,C34D,C35D,C36D), N11E(C12E,C13E,C14E,C15E,C16E), N11F(C12F,C13F,
 C14F,C15F,C16F), N11G(C12G,C13G,C14G,C15G,C16G), N11H(C12H,C13H,C14H,C15H,C16H)
8.e Tetrahedral OH refined with riding coordinates:
 O18A(H18A), O38A(H38A), O18B(H18B), O19B(H19B), O38B(H38B), O18C(H18E),
 O38C(H38C), O18D(H18F), O38D(H38D), O18E(H18G), O18F(H18H), O18G(H18I),
 O18H(H18J)
8.f Naphthalene refined as free rotating group:
 C51A(C52A,C53A,C54A,C55A,C56A,C57A,C58A,C59A,C60A), C51B(C52B,C53B,C54B,C55B,
 C56B,C57B,C58B,C59B,C60B), C51C(C52C,C53C,C54C,C55C,C56C,C57C,C58C,C59C,C60C),
 C51D(C52D,C53D,C54D,C55D,C56D,C57D,C58D,C59D,C60D), C51E(C52E,C53E,C54E,C55E,
 C56E,C57E,C58E,C59E,C60E), C51F(C52F,C53F,C54F,C55F,C56F,C57F,C58F,C59F,C60F)
;
_shelx_res_checksum              90141
_shelx_hkl_checksum              34299
_olex2_submission_special_instructions 'No special instructions were received'