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_4342487
_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         'C90 H78 Co2 N18 O6, 4(B F4)'
_chemical_formula_sum            'C90 H78 B4 Co2 F16 N18 O6'
_chemical_formula_weight         1972.80
_chemical_name_common            M2L3OH
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_Hall           '-R 3 2"c'
_space_group_name_H-M_alt        'R -3 c'
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :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            12
_cell_length_a                   18.885(3)
_cell_length_b                   18.885(3)
_cell_length_c                   101.44(2)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.9
_cell_measurement_theta_min      2.4
_cell_volume                     31331(9)
_computing_cell_refinement
'CrystalClear-SM Expert 3.1 b27 (Rigaku, 20112)'
_computing_data_collection
'CrystalClear-SM Expert 3.1 b27 (Rigaku, 20112)'
_computing_data_reduction
'CrystalClear-SM Expert 3.1 b27 (Rigaku, 20112)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL 2013'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.717
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  Mirrors
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.156
_diffrn_reflns_av_unetI/netI     0.0700
_diffrn_reflns_Laue_measured_fraction_full 0.717
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       131
_diffrn_reflns_limit_l_min       -55
_diffrn_reflns_number            4534
_diffrn_reflns_point_group_measured_fraction_full 0.717
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        27.9
_diffrn_reflns_theta_max         27.9
_diffrn_reflns_theta_min         2.4
_diffrn_source                   'Sealed Tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.402
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.508
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.255
_exptl_crystal_density_method    "'not measured'"
_exptl_crystal_description       Plate
_exptl_crystal_F_000             12120
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.818
_refine_diff_density_min         -0.878
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.692
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         4534
_refine_ls_number_restraints     463
_refine_ls_restrained_S_all      1.680
_refine_ls_R_factor_all          0.2427
_refine_ls_R_factor_gt           0.1876
_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          0.4864
_refine_ls_wR_factor_ref         0.5191
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2120
_reflns_number_total             4534
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic502780b_si_003.cif
_cod_data_source_block           2013ncs0568
_cod_depositor_comments
'Adding full bibliography for 4342486--4342489.cif.'
_cod_original_cell_volume        31333(11)
_cod_database_code               4342487
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H47C of O47A, All C(H,H) groups
 At 1.5 times of:
  H47F of O47B, H12F of O12B, H12C of O12A
2. Shared sites
{C12A, C12B}
{C47A, C47B}
3. Restrained distances
 C44A-C47A
 1.55 with sigma of 0.01
 C47A-C45A
 2.54 with sigma of 0.02
 C47A-C43A
 2.54 with sigma of 0.02
 C12A-O12A
 1.33 with sigma of 0.01
 C18A-O12A
 2.73 with sigma of 0.02
 C12A-C13A
 1.55 with sigma of 0.01
 C12A-C14A
 2.54 with sigma of 0.02
 C12A-C18A
 2.54 with sigma of 0.02
 O12A-C14A
 3.69 with sigma of 0.02
 Co2-N36A
 3.32 with sigma of 0.01
 Co2-C37A
 4.4 with sigma of 0.01
 Co2-C38A
 4.23 with sigma of 0.01
 Co2-C39A
 2.95 with sigma of 0.01
 Co2-N40A
 2.1 with sigma of 0.01
 B1-F1 \\sim B1-F2A \\sim B1-F2B
 with sigma of 0.02
 C12A-O12A \\sim C12B-O12B \\sim C47A-O47A \\sim C47B-O47B
 with sigma of 0.02
4. Restrained planarity
 C14A, C13A, C18A, C12A, O12A
 with sigma of 0.01
5. Rigid bond restraints
 C12A, C12B, C13A, C14A, C15A, C17A, C18A, C20A, C21A, C22A, C24A, C51, C52,
 C53, C54, C55, C56, C64, C63, C62, C61, C35A, C37A, C38A, C39A, C42A, C43A,
 C44A, C45A, C46A, C47A, C47B, N16A, N19A, N23A, N36A, N40A, N41A, O12A, O12B,
 O47A, O47B, B1, F1, F2A, F2B
 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 C12B \\sim C13A \\sim C14A \\sim C15A \\sim C17A \\sim C18A \\sim
C20A \\sim C21A \\sim C22A \\sim C24A \\sim C51 \\sim C52 \\sim C53 \\sim C54
\\sim C55 \\sim C56 \\sim C64 \\sim C63 \\sim C62 \\sim C61 \\sim C35A \\sim
C37A \\sim C38A \\sim C39A \\sim C42A \\sim C43A \\sim C44A \\sim C45A \\sim
C46A \\sim C47A \\sim C47B \\sim N16A \\sim N19A \\sim N23A \\sim N36A \\sim
N40A \\sim N41A \\sim O12A \\sim O12B \\sim O47A \\sim O47B \\sim B1 \\sim F1
\\sim F2A \\sim F2B: within 1.7A with sigma of 0.003 and sigma for terminal
atoms of 0.006
Uanis(C12A) = Uanis(C12B)
Uanis(C47A) = Uanis(C47B)
7. Others
 Sof(C12B)=Sof(H12D)=Sof(H12E)=Sof(O12B)=Sof(H12F)=Sof(C47B)=Sof(H47D)=
 Sof(H47E)=Sof(O47B)=Sof(H47F)=1-FVAR(1)
 Sof(C12A)=Sof(H12A)=Sof(H12B)=Sof(O12A)=Sof(H12C)=Sof(C47A)=Sof(H47A)=
 Sof(H47B)=Sof(O47A)=Sof(H47C)=FVAR(1)
 Sof(F2B)=1-FVAR(2)
 Sof(F2A)=FVAR(2)
8.a Secondary CH2 refined with riding coordinates:
 C12A(H12A,H12B), C12B(H12D,H12E), C24A(H24A,H24B), C35A(H35A,H35B), C47A(H47A,
 H47B), C47B(H47D,H47E)
8.b Aromatic/amide H refined with riding coordinates:
 C14A(H14A), C15A(H15A), C18A(H18A), C21A(H21A), C22A(H22A), C52(H52),
 C53(H53), C54(H54), C63(H63), C62(H62), C61(H61), C37A(H37A), C38A(H38A),
 C42A(H42A), C43A(H43A), C45A(H45A)
8.c Fitted pentagon refined as free rotating group:
 N19A(C20A,C21A,C22A,N23A), N36A(C37A,C38A,C39A,N40A)
8.d Fitted hexagon refined as free rotating group:
 C13A(C14A,C15A,N16A,C17A,C18A), N41A(C42A,C43A,C44A,C45A,C46A)
8.e Tetrahedral OH refined with riding coordinates:
 O12A(H12C), O12B(H12F), O47A(H47C), O47B(H47F)
8.f Naphthalene refined as free rotating group:
 C51(C52,C53,C54,C55,C56,C64,C63,C62,C61)
;
_shelx_res_checksum              21422
_shelx_hkl_checksum              33300
_olex2_submission_special_instructions 'No special instructions were received'